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N36677 Louviers Library Technical Library Network I. DU PONT DE NEMOURS & CO. WILMINGTON, DELAWARE DUP050296492 j ii'Oflun' DUP050296493 1992 tn ANNUAL BOOK wa /STM SMND/4RDS H MB Paints, Related Coatings, and Aromatics VLU**E Paint-Pigments, Resins, - 06.02 and Polymers; Cellulose . Includes standards of the following committee: D-1 on Paint and Related Coatings and Materials Publication Code Number PCN): 01-060292-14 ASTM 1916 Race Street, Philadelphia. PA 19103-1187 USA (215)299-5400 TWX: 710-670-1037 FAX: 215-977-9679 DUP050296494 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 0-8031-1708-6 (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 o f 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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DUP050296498 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 toE 354 Volume 03.06 Analytical Chemistry for Metals, Ores, and Related Materials (II): E356 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 Rtfck; Dimension Stone; Geosynthetics Volume 04.09 Wood Section 5--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 vi T-- . L DUP050296499 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 ffi: C 3 77-D1600 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)--D69-D2484 . 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 IS--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 DUP050296500 ANNUAL BOOK OF ASTM STANDARDS Listed by Subjects SUBJECT VOLUME SUBJECT VOLUME Acoustics, Environmental.................................. .......... . 04.06 Glass................,............................................................. 15.02 Activated Carbon..,................................................. 15.01 Shipping............................. 15.09 Adhesives.......................................................................... 15.06 Coolants, Engine............................................................. 15.05 Advanced Ceramics........................................................ 15.01 Copper and Copper Alloys........................................... 02.01 Aerosols ............................................................................. 15.09 Corrosion, Metal.................... ........... ______...... 03.02 Aerospace Industry Methods......................................... 15.03 Criteria for the Evaluation ofTesting and Inspection Aggregates....................................................................... 04.02 Agencies ...................... ..;................................... 14.02 Aluminum and Aluminum Alloys............................. 02.02 Detention and Correctional Facilities......................... 04.07 Amusement Rides and Devices.................................. 15.07 Die-Cast Metals...................................... &.................... 02.04 Analytical Atomic Spectroscopy....................... 03.05, 03.06 Dimension Stone............................................................. 04.08 Anesthetic and Respiratory Equipment.................... 13.01 Dosimetry ...................................... 12.02 Appearance of Materials............................................... 14.02 Ductile Iron................................................................ 01.02 Aromatic Hydrocarbons and Related Durability of Nonmetallic Materials.................... 14.02 Chemicals............................................................. 06.03 ` Electrical Conductors........................................ 02.03 Atmospheric Analysis.................. 11.03 Electrical Contacts and Connectors........................... 03.04 Biological Effects and Environmental Fate............................. 11.04Electrical Insulating Materials........................... 10.01,10.02, Biotechnology ................................................................. 11.04 10.03 Bituminous Materials.................................................... 04.03 Electrical Protective Equipment for Workers...... 10.03 Building Constructions......... .................................... 04.07 Electronics....... .................................................... 10.04,10.05 Building Seals and Sealants........................................... 04.07 Emergency Medical Services.................... 13.01 Business Imaging Products........................................... 15.09 Emission Spectroscopy........................................ 03.05,03.06 Carbon Black.................................................................... 09.01 Erosion and Wear........................................ *.......... .... 03.02 Carbon Products, Manufactured..................................... 15.01 Evaluating Testing and Inspection Agencies___ __ 14.02 Cast Iron .......................................................................... 01.02 Exposure Tests................................................................. 14.02 Catalysts................................................................. 05.03 Fasteners.......................................................................... 1,5.08 Cellulose........... ......................................,.............. .. 06.02 Fatigue--------- ... ................ .................................... 03.01 Cement............................................................................... 04.01 Fences....................................................... ..................... .. 01,06 Hydraulic.................... ................................................. 04.01 Ferroalloys................. ......................... 01.02 Rubber.......................................................................... 09.01 Ferrous Castings ............................................... 01.02 Ceramic Materials............................... ...................... 15.02 . Fiber-Cement Products .................... v. *........................ 04^)5. Advanced Ceramics....................................................... 15.01 Filtratiop .. ..............................................*........... ,14.02 Ceramic Whitewares.................................................. 15.02 Fire Standards ....... ........................... 04.07 Ceramics for Electronics .......................................... 10.04. Hexible Barrier Materials .................................., .15.09' Porcelain Enamel........................................................... 02.05 Food Service Equipment............................................... 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.................... .......................................... 03.01 Chromatography................................................................ 14.01 Gaseous Fuels................................................................. 05.05 Closures............................................................................ 15.09 Gaskets................. 09.02 Coal and Coke......................................................... 05G.0e5otextiles and Related Products................................ 04.08 Compatibility and Sensitivity of Materials in Oxy Geothermal Resources and Energy............................. 12.Q2 gen-Enriched Atmospheres............................. 14.02 Glass................................................................... 15.02 Computerization of Material Property Data........... 14.01 Graphite Products, Manufactured ............................ 15.01 Computerized Systems..................................................... 14.01 Graphite Products, Nuclear......................................... 12.02 Concrete and Concrete Aggregates................................ 04.02 Gypsum.......................................... 04.01 Concrete Pipe and Tile.................................................... 04.05 Halogenated Organic Solvents........... ........................ 15.05 Concrete Products, Precast.............................................. 04.05 Hazardous Substances and Oil Spill Response___ 11.04 Concrete Reinforcing Steel.............................................. 01.04 Hazard Potential of Chemicals.................................... 14.02 Consumer Products........................................................ 15.07 Health Care Services and Equipment......................... 13.01 Containers: High Modulus Fibers and Composites...................... 15.03 Aerosol........................................................................... 15.09 Imaging Products, Business.......................................... 15.09 VIII "ip DUP050296501 LISTED BY SUBJECTS SUBJECT VOLUME SUBJECT VOLUMB Index (for all volumes)............................:>;*... 00.01 Refractories...................................................................... 15.01 Industrial Chemicals........... t. 15.0$ Resilient Eloor Coverings......... ................................... 15.04 Iron Casting................................................................... 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 Malleable Iron.................................................... ...........01.02. Masonry Units......................................................... 04.05 Security Systems and Equipment............................... 15.07 Sensory Evaluation of Materials and Products____ 15.07 Meat and Poultry................................... 15.07 , Shipbuilding........................... >...................................... 01.07 Medical and Surgical Materials and Devices............ 13.01 Sintered P/M Structural Parts...................................... 02.05 Metallic and Inorganic Coatings.......................... 02:05 Skiing, Snow .................. ................................................ 15.07 Metallography......... ........................................................ 03.01 Soap............... ................. .......................................... 15.04 Metal Powders........... ..................................................... 02.05 Soil and Rock................................................................. 04.08 Metals, Chemical Analysis'v.s............ 03.05, 03.06 Solar Energy Conversion...................... :........ ............. 12.02 Metals, Effect of Tertipejature on Propeftids...... 03.01 Space Simulation................................... ........................ 15.03 Metals, Physical andMechamcal Testing......... 03.01 Spectroscopy., -- .'........................................... 03.06, 14.01 Metric Practice.. .............................................. .. 14.02 Sports Equipment and Facilities....... .......................... 15.07 Mortars for Unit Masonry ............ . . .................... .. 04.05 Statistical Methods ........................... >......................... 14.02 Naval Stores.....................;.............................................. 06.03 Steel: Nickel and Nickel Alloys ............................................. 02.04 Bars.............................................................................. 01.05 Nondestructive Testing..................................1L..... 03:03 Bearing .SteSl............................................................... 01.05 Nonferrous Metals, General................................. 02.04 Bolting................................................................. 01.01, 15.08 Nonmetals, General Test Methods..................... 14.02 Castings........................................................................ 01.02 Nuclear Materials...................... 12.01,12.02 Chain......... .......... 01.05 Oaupatidnal Health ajnd Safety................11.03 Concrete Reinforcing........................................ 01.04 Oil Spill Response, Hazardous Substances................ 11.04 Detention and Correctional Facilities.................... 04.07 Ores, Mtal Bearing, Sampling and Analysis . 03.05,03.06 Fasteners ........................... ......................................... 15.08-s. Orthotics, External Prosthetics, and Mobility Forgings.....,............. 01.04, 01.05 Aids .......................................................................... 13.01 Galvanized.............................................. 01.06 Packaging.............................................................................. 15.09 Piping, Tubing, and Fittings.................................... 01.01 Paint and Related Coatings and Materials: Plate; Sheet, and Strip ............................................... 01.03 Fatty Oils and Acids, Solvents, Miscellaneous... 06.03 Pressure Vessel Plate and Forgings........................ 01.04 Pigments, Resins, and Polymers................ ;........... 06.02 Rails, Wheels, and Tires ........................................... -01.04 Tests for Formulated Products and Applied Coat- . ,.< ings....................................................................... Springs............................... 01.05 06.01 Stainless Steel....... ...........'...................................... .... 01.61, Paper ..................................................................................... 15.09 .... 01.62, 01.03,,01.04, 61.05 Pavement Management Technologies....................... 04:03 Structural Steel ................................--................ ........-- 01.64 Particle Size Measurement................................... 14.02Wire....:_,,................. 01.03 Pesticides ...............::........................ ...'.............. .... 11.04 Surface Analysis........... ........ .......................................... 03.06 Petroleum Products and Lubricants........................... 05.01, Surgical Materials and Devices.................... 13J0l 05.02, 05.03,05.04 Temperature Measurement.......................... 14.03 Plastics..,........... ............................................ Te0x8ti.l0e1s, ..`................. .07.01, 07.02 08.62,08.03 Thermal Measurements. ^............................................. 14.02 Plastic Pipe and Building Products.............................. 08.04. Thermal Insulation .................................................. 04.06 Polishes ................................................................................ 15.04 Thermocouples ............... 14.03 Porcelain Enamel...................................................... 02.0T5hermostats, Electrical Heating and Resistance, Pressure Vessel Plate and Forgings................................ 01.04 Contacts, and Connectors............................... 03.04 Products Liability Litigation, Technical Aspects Tires......... .......-................................................... ............. 0902 of..................................................................................14.02 Traveled Surface Characteristics............................... , 04.03 Protective Clothing.................................................. 15.V07acuum Cleaners......... .............................................. 15.07 Protective Coating and Lining Work for Power Vitrified Clay Pipe........................................................... 04.05 Generation Facilities............................... 06.01,12.01 Waste Management...................................... ................. 11.04 Protective Equipment, Electrical, for Workers......... 10.03 Water................................. 11.01,11.02 Radioisotopes and Radiation Effects............................ 12.02 Wear and Erosion................. 03.02 Reactive and Refractory Metals..................................... 02.04 Wood................................................................................. 04.09 DUP050296502 Contents 1992 ANNUAL BOOK OF ASTM STANDARDS, Volumes 06.01, 06.02, and 06.03 St a n d a r d s Re l a t in g t o Pa in t --Te s t s f o r Fo r mu l a t e d Pr o d u c t s a n d Ap p l ie d Co a t in g s ; Pig me n t s , Re s in s a n d Po l y me r s ; Ce l l u l o s e ; Fa t t y Oil s a n d Ac id s , Mis c e l l a n e o u s ; Ar o ma t ic Hy d r o c a r b o n s A complete Subject Index begins on p. 561 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 numbers 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 of 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 thah 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 reapproval 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)el D 12-88 D 13 - 82 (1987) D 16-91 D 29 -- 81 (1987)ei D 34-91 D 49-83(1990)el D 50 - 90 D 56 - 87 D 79-86 D 81 -87 D 83-84(1989) D 85 -- 87 (1991)e* D 86 - 90 D 93 - 90 D 95 - 83 (1990) D 124 - 88 D 126 - 87(1991)el D 130-88 D 153 - 84 (1989)ei D 154- 85(1989)1 D 185 - 84(1989)ei D 207 - 55 (1987) D 209 - 81 (1989) D 210 - 81a (1991)e` D 211 -67 (1989)*1 D 212-87 D 215-91 D 233 - 65 (1981)CI D 234 - 82 (199 l)ei D 235 - 87s 1 VOLUME Method of Salt Spray (Fog) Testing................................ 06.01 Methodof Acetic Acid-Salt Spray (Fog) Testing (Discontinued 1988f--Replaced by Practice G 85) .<06.01 Specification for Raw Tung Oil........................................................... 06113 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 ofYellow, Orange, Red, and Brown Pigments Containing Iron arid 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 ........................ ............ .............. .. v06.03' Test Methods for Flash Point by Pensky-Martens Closed Tester...................................... 06.03 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation............06.01, 06.Q3 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...........................................................................................................................06411 Test Methods for Coarse Particles in Pigments, Pastes, and Paints.......................................... . .06.01,064)2 Specification for Dry Bleached Lac.................. 064)2 Specification for Lampblack Pigment........................................................................................................... 06.02 Specification for Bone Black Pigment.............. ,.............................................................. ........ .. 06102 Specification for Chrome Yellow and Chrome Orange Pigments................................................................06.02 Specification for Chrome Green Pigment......................................................................................................06.02 Methods of Chemical Analysis of White Linseed Oil Paints........................... 06.01 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) ....................96.03 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 information only. X ae DUP050296503 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 237-91 Specification for Orange Shellac and Other Lacs...................................................................................... 06.02 260-86(1990) Specification for Boiled Linseed Oil...........................................................................................................06.03 261-75 (1987)" Specification for Iron Blue Pigment.......................................................................................................... 06.02 262 - 81(1987)" Specification for Ultramarfine Blue Pigment...................................................................... --.......... 06.02 263-75 (1987) Specification for Chrome Oxide Green Pigment........ ..............................................................................06.02 267 - 82 (1987)" Specification for Gold Bronze Powder................. .............. ....................................................... .......... 06.02 268 - 90 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Materials .............................................................................................................06.03 269-(1987)" Test Method for Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark)........ 06.03 279-87 (1991)" Test Methods for Bleeding of Pigments ........ ............................................................................................ 06.02 280 - 81 (1987) Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments................................................................................................ '.................................................06.02 281-84(1989) Test Method for Oil Adsorption of Pigments by Spatula Rub-Out ...... ..................................................06.02 283 - 84(1990)" Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments...................................... 06.02 284-88 Test Methods for Chemical Analysis of Mercuric Oxide Pigment ...................................................... 06.02 301 -89 Test Methods for Soluble Cellulose Nitrate .......... : --..........................................................................06.02 302 - 85 Specification for Ethyl Acetate (85 to 88 % Grade) (Discontinued 1987T--Replaced by Specification D4614)............................................ -..................................... ........................,..................................... 06.03 D 303-85 Specification of n-Butyl Acetate (90 to 92 % Grade) (Discontinued 1987f--Repaced by Specification D 4615)...................................................................................................................................................... 06-03 D 304-90 D 305 - 84(1990)" D 319-90 Specification for w-Butyl Alcohol (Butanol)............ ............................ ..................................................06.03 Test Method for Solvent-Extractable Material in Black Pigments .......................................................... 06.02 Specification for Amyl Alcohol (Synthetic) ................................................................................................ 06.03 D 329 - 90 Specification for Acetone ............................................................................ D 330 - 89 Specification for 2-Butoxyethanol............................................. .....;......................................................... 06.03 D 331-90 D 332-87(1991)" D 333-87 D 344-89 D 358-83(1988) D 360-89 Specification for 2-Ethoxyethanol................................................................................................................ 06.03 Test Method for Relative Tinting Strength of White Pigments by Visual Observation.......................... 06.02 Test Methods for Clear and Pigmented Lacquers .................................................................................... 06.01 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............................................................... D 362-84 Specification for Industrial Grade Toluene (See Section on Aromatic Hydrocarbons) .......................... 06.03 D 363-90 D 365 - 84(1989)" D 387-86 D 411-83(1987) 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 06.03 D 444 - 88 D 464-91 Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow) ...................... 06.02 Test Methods for Saponification Number of Naval Store Products Including Tall Oil and Other Related Products .....................................................................................................................................................06.03 D 465 - 82 (1987)" Test Methods for Add Number of Rosin ................................................................................................ 06.03 D 475 - 67(1989) Specification for Pure Para Red Toner Pigments .................................................................................... 06.02 D 476 - 84(1989) D 477 - 78 Specification for Titanium Dioxide Pigments ............................................................................................ 06.02 Specification for Zinc Sulfide Pigmentrs (Discontinued 1988f) .................. ............................................06:02 D 478 - 86(1991)" D 480 - 88 D 509-70(1987) Specification for Zinc Yellow (Zinc Chromate) Pigments.................... ................................................... 06.02 Test Methods for Sampling and Testing of Flaked Aluminum Powders and Pastes ...................... . 06.03 Test Methods of Sampling and Grading Roan ......................................................................... 06.03 D 520 - 84(1989) D 521-90 Specification for Zinc Dust Pigment .............. . --......................................................... 06.02 Methods for Chemical Analysis of Zinc Dust (metallic Zinc Powder).................................... r............. 06.02 ' 522-88" Test Methods for Mandrel Bend Test of Attached Organic Coatings...................................................... 06.01 D 523 - 89 Test Method for Specular Gloss ................................ ............. ..................................................................06.01... D 555-84(1988)" Guide for Testing Drying Oils ...................... ............................................................................. :...... 0603 D 561-82(1989) D 562 - 81(1990)" D 563-88 Specification for Carbon Black Pigment for Paint.......................... ......................................................... 06.02 Test Method for Consistency of Paints Using the Stormer Viscometer .................................................. 06.01 Test Method for Phthalic Anhydride Content of Alkyd Resins and Resin Solutions ............................ 06.02 D 564-87(1991)" Test Method for Liquid Paint Driers ............................ ..........................:............................................... 06.03 D 600 - 90 D 601 - 87 (1991)" D 602 - 81 (1991)" Specification for Liquid Paint Driers .......... ..................... .......................................................................06.03 Specification for Oiticica Oil (Permanently liquid) ................. ...................... ......................... ........... 06.03 Specification for Barium Sulfate Pigments.................................................................................... ........... 06.02 D 603 - 66(1989) Specification for Aluminum Silicate Pigments (Hydrous)...................... ............................................... . 06.02 D 604-81 (1989) Specification for Diatomaceous Silica Pigment ........................................................................................ 06.02 D 605 - 82 (1989) D 607-82(1987)" D 608-90 D 609-90 Specification for Magnesium Silicate Pigment (Talc) ................................................................................ 06.02 Specification for Wet Ground Mica Pigments.................................. ........................................................06.02 Specification for Dibutyl Phthalate.............................................................................................................. 06,03 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer and Related Products .. 06.01 D 610-85(1989)" D 611-82 (I987)f2 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 ...................................................................................... D 656-87 Specification for Pure Toluidine Red Toner .................................. ..........................................................06.02 D 658-91 D 659-86" 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 D 4214) ...................................................................................................................... 06.01 D 660 - 87 Test Method for Evaluating Degree of Checking of Exterior Paints........................................................ 06.01 I xi -k,... DUP0502 96504 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 661-86" D 662 - 86" D 711-89 D 7(3-90 D 714-87 D 715 - 86(1991)** D 716 - 86(1991)" D 717 - 86 (1991)" D 718 - 86(1991)" D 719 - 91 D 740 - 89. D 763-81 (1988)" D 765 - 87(1991)tI 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 D 856 - 49 (1987) D 867 - 81 (1986)" D 868 - 85 (1989)" D 869 - 85 (1989)" D 870 - 87 D 871 - 91 D 889 - 58 (1987) D 890 - 58 (1987) D 911 - 87 D 912 - 81 (198$) D 913 -88 ; D 914 - 72 (1989)" D 960 - 79 (1988) D 961 - 86 D 962 - 81 (1986)" D 963 - 81 (1986)" D 964 - 65 (1989) D 968 - 81 (1991) D 969 - 85 (1989)" D 970 - 86 (1991)" D 1005 - 84 (1990)" D1006 - 73 (1986)" D 1007 - 90 D 1013 - 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 1.135 86 (1991)" D 1150 - 55 (1987)" D1152 - - 89 0 1153 - 90 D 1155 - 89 D1186 - 87 D1193 - 91 D 1198 - 88 D1I99- - 86 (1991)" D 1200 - 88 D 1208 - - 84(1989)" D 1209 - 84 (1988)" Test Method for Evaluating Degree of Cracking of Exterior Paints .................................................. ....06.61 Test Method for Evaluating Degree of Erosion of Exterior Paints........................ 06.01 Test Method for No-Pick-Up Time of Traffic Paint........................ 06.01 Practice for Conducting Road Service Tests on Fluid Traffic Marking Materials......................................06.01 Test Method wifivaldatiiig Degree Of Bllstifiiiidif Paints......................... ..06.01 Test Methods for Analysis of Barium Sulfate Pigment..................................................................... 06.02 Test Methods for Evaluating Mica Pigmbnt.................................................. 06.02 Test Methods for Analysis of Magnesium Silicate Pigment................................... 06.02 Test Methods for Analysis ofAluminum Silicate Pigment .................... .....06.02 Test Methods for Analysis of Diatomaceous Silica Pigment.............................................................. ..:. 66.02 Specification for Methyl Ethyl Ketone.......... ;..................... .................................................... ........... 06.03 Specification for Raw and Burnt Umber Pigments ..................................................................................... 06.02 Specification for Raw and Burnt Sienna Pigments................. 06.02 Specification for Yellow Iron Oxide Hydrated".............................................................................................06.02 Specification for Black Synthetic Iron Oxide ........................................................................................... 06.02 Specification for Isopropyl Alcohol.................. .................................................;......................... !___ 06.03 Test Method for Evaluating Degree ofFlaking (Scaling).of Exterior Paints......... .................................. 06.01 Specification for Orange Shellac mid Other Indian Lara for Electrical Insulation.............................. 06.02 Test Methods for- Sampling and Testing Dipentene............................... 06.03 Test Methods for Sampling and Testing Pine Oil......................................................................................... 06.03 Test Methods for Testing Tall Oil............................ 06.03 Definitions of Terms Relating to Naval Stores and Related Products..........................................................06.03 Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate...................................... 06.02 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light and Water Exposure Apparatus................ 1..............................................................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 ......................................................................................................... 0602 Test Method far Evaluating Degree of Bleeding of Traffic Paint............ .............................. Test Method for Evaluating Degree of Settling of Paint............................................................................ 06.01 Practice for Testing Water Resistance ofCoatings Using Water Immersion............................................ 06.01 Methods of Testing Cellulose Acetate..................................... .. i................................................................06.02 Test Method for Volatile Oil in Rosin ............................ i.v....................................................................06.03 Test Method for Water in Liquid Naval Stores ........................ ................;............................................ 06.03. Specification for Mercuric Oxide for Use in Antifouling Paints...................................... 06.02 ' Specification for Cuprous Oxide for Use in Antifouling Paints....................................... 06.02 Test Method for Evaluating Degree of Resistance to Wear of Traffic Paint.................. ;................ L... 06.01' Test Methods for Ethylcellulose................................................................... 06.02 Specification for Raw Castor Oil................... .;............................................................................... .. 06.03 Specification for Dehydrated Castor Oil.......,......................................................... Specification for Aluminum Powder and Paste Pigments for Paints..................................................... .^ 06.02 Specification for Copper Phthalocyanine Blue Pigment............ .................. :.............................. ....... 06.02 . Specification for Copper Powder for Use in Antifouling Paints. ............................... ............. '. ......... . 06.02 Test Methods for Abrasion Resistance of Oiganic Coatings by Falling Abrasive................ 06.01 Test Method for Laboratory Determination of Degree ofBleeding of Traffic Paint___ .. ....... 06.01 Test Methods for Para Red and Toluidine Red Pigments'............. ...... t...... .'.T............. .'..-.. 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- .................................... Specification for rec-Butyl Alcohol..................................................................... Test Method for Determining Total Nitrogen in Resins and Plastics ... r................................... 06.02- Test Method for Conducting Exterior Exposure Tests of Paints on Steel ..................... ............. 06.01 Test Method for Ash In Rosin.......................... ............................................................................'......... 06.03 ; Test Method for Iron in Rosin ..................... ..................;.................................................................... .. 0603 Test Methods for Unsaponifiable Matter in Rosin....... ................................................................... . 0603" Test Method for Distillation Range of Volatile-Organic Liquids................................................................. 0603 Methods of Testing Rosin Oils........ ........... ......................'.................................... ..................v : ._____ .06.03 Test Method for Kauri-Butanol Value of Hydrocarbon Solvents ........................................................... 06.03 Test Methods for Chemical Analysis of Blue Pigments........... ....................................................................06.02 Single- and Multi-Panel Forms for Recording Results of Exposure Tests of Paints................................ 06.01 Specification for Methanol (Methyl Alcohol)............................. ........................................................ 0603 Specification for Methyl Isobutyl Ketone...................................................... 06.03 Test Method for Roundness of Glass Spheres............................................................................... 06.02 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base ................................................................ ................................................... . 0601 Specification for Reagent Water .................................................................................................................. 0603 Test Method for Solvent Tolerance of Amine Resins............................................................... Specification for Calcium Carbonate Pigments............................................................................................. 06.02 Test Method for Viscosity by Ford Viscosity Cup........................................................ Test Methods for Common Properties of Certain Pigments ....................................................................... 06.02 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)................................................. 06.01, 06.03 06.0 06.0 060 xn DUP050296505 CONTENTS, VOLUMES 06.01,06.02, AND 06.03 D 1210 - 79(1988)** D1211 - 87 D 1212 - 91 D1214 - 89 D1240 - 82 D1257 - 90 D 1258 - 90 D 1259 - 85 (1990)*1 D 1296-84(1988)" D 1301-91 D 1306 - 88 D 1308 - 87 D 1309 - 88 D 1310 - 86 (1990)" D1312 - 56(1987)" D1316 - 87 D 1343 - 91 D 1347-72(1989)" D 1348 - 89 D 1353 - 90 D, 1358 - 86 D1360 - 90a D 1363-88 D 1364 - 90 D 1366 - 86 (1991)" D1392 - 87 D 1394 - 76(1991)" D 1395 - 58 (1974) D 1396 - 73 (1987)" D 1397 - 88 D 1398 - 84 D 1399 - 90 D 1400 - 87 D 1439 - 83a (1989)" D 1462 - 87 D 1466 - 86 D 1467 - 89 D 1468 - 84 (1988)" D1469 - 73 (1988)" D 1474 - 85 (1991)" D 1475 - 90 D 1476 - 88 D 1483 - 84 (1989)*1 D 1537 - 60 (1988)" D1538 - 60 (1988)" D 1539 - 60 (1988) D 1540 - 82 (1987)" D 1541 - 86 D 1542 - 60 (1988)" D 1543 - 86 D 1545 - 89 D 1546 - 62 (1987) D1585 - 82 D1612 - 90 D 1613-91 D1614-91 D 1615 - 60 (1987) D 1617 - 90 D 1638 - 74" D 1639-90 D 1640 - 83 (1989)" D 1641 - 59 (1987) D 1642 - 70 (1987) Test Method for Fineness of Dispersion of PignienbYehicle Systems.........................................................06.01 Test Method for Temperature-Change Resistance of Clear Nitrocellulose Lacquer Films Applied to Wood.......................................................... .............................................................................................. 06.01 Methods for Measurement of Wet Film Thickness of Organic Coatings...........................-...................... 06.01 Test Method for Sieve Analysis of Glass Spheres................................................. 06.02 Test Method for Rosin Acids in Fatty Adds ................................................................................................06.03 Specification for High-Gravity Glycerin....................................................................................................... 06.03 Test Methods for Testing High-Gravity Glycerin......................................................................................... 06.03 Test Methods for Nonvolatile Content of Resin Solutions ............................................................... 06.02 Test Method for Odor of Volatile Solvents and Diluents............................................................................. 06.03 Test Methods for Chemical Analysis of White Lead Pigments................................................................... 06.02 Test Method for Phthalic Anhydride Content of Alkyd Resinsand Esters Containing Other Dibasic Adds (Gravimetric)............................ ;......................'.............................................................................06.02 Test Method for Effect of Household Chemicals on- Clear and Pigmented OrganicFinishes..................... 06.01 Test Method for Settling Properties of Traffic Paints During Storage.......................................................... 06.01 Test Method for Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus....................... 06.03 Test Methods for Apparent Free Phenols in Synthetic Phenolic Resins or Solutions Used for Coating Purposes............ .....'.................................................... ..................... ........................................ ............ 06.02 Test Method for Fineness of Grind of Printing Inks by the NPIRI Grindometer......................................06.01 Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method............................................. 06.02 Test Methods for Methylcellulose.................................. 06.02 Test Methods for Moisture in Cellulose ................. 06.02 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Related Products..... ...................... ................................................ ................................. ............................ .. 06.03 Test Method for Spectrophotometric Diene Value of Dehydrated Castor Oil and Its Derivatives......... 06.03 Test Method for Fire Retardancy of Paints (Cabinet Method) .:......................................................... 06.01 Test Method for Permanganate Time of Acetone and Methanol ...............................................................06.03 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)......................................06.03 Practice for Reporting Particle Size Characteristics of Pigments............................ 06.02 Specification for Safflower Oil....................................................................................................................... 06.03 Test Methods for Chemical Analysis of White Titanium Pigments.............................................................06.02 Test Method for Abrasion Resistance ofClear Floor Coatings (Discontinued 1989-f)...............................06.01 Test Methods for Chemical Analysis of Poly(Vinyl Butyral).......................................................................06.02 Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions..........................................06.02 Test Method for Fatty Add Content of Alkyd Resins and Alkyd Resin Solutions ..................... 06.02 Test Method for Unsaponifiable Content of Tricresyl.Phosphate............ .............................................. 06.03 Test Method far Nondestructive Measurement of Dry Film Thickness ofNonconductive Coatings Applied to a Nonferrous Metal Base.................................................................................................. 06.01 Test Methods for Sodium Carboxymethylcellulose............ ..................................................."...................06.02 Specification for Refined Soybean Oil................................................................. 06.03 Test Method for Sampling Liquid Oils and Fatty Adds Commonly Used in Paints, Varnishes, and Related Materials............................................ ........... ........................................................................06.03 Guide for Testing Fatty Adds Used in Protective Coatings.......................... '....,............................. .. 06.03 Test Method for Volatile Matter.in Tricresy! Phosphate ;............................................................................06.03 Test Method for Total Rosin Acids Content of Coating Vehicles............. ..................................................06.02 Test Methods for Indentation Hardness of Organic Coatings-................................................... 06.01 Test Method for Density of Paint, Varnish, Lacquer, and Related Products................. 06.01 Test Method for Heptane Miscibility of Lacquer Solvents................................ .................... ...... :.. 06.03' Test Method for Oil Absorption of Pigments by Gardner-Coleman Method........................................ 06.02 Specification for Distilled Soybean Fatty Adds............ :i............................................ ............ 06.03, Spedfication for Distilled Linseed Fatty Adds.............................................................................................. 06.03 Specification for Dehydrated Castor Acids..............................................................;................................. 06.03 Practice for Effect of Chemical'Agents on Organic Finishes Used in the TransportationIndustry -- . 06.01 Test Method for Total Iodine Value of Drying Oils and Their Derivatives................................................06.03 Test Method for Qualitative Detection of Rosin in Varnishes................. ;......................................06.01,06.02 Test Method for Color Permanence of White Architectural Enamels (Discontinued1992f) .....................06.01 Test Method for Viscosity of Transparent Liquids by Bubble Time Method.................... 06.01; 06.02,06.03 Method for Performance Tests of Clear Floor Sealers........................................................................06.01 Test Methods for Fatty Adds Content of Tall Oil Rosin............................... 06.03 Test Method for Acetone in-Methanol (Methyl Alcohol)..................................................... ................... _. 06.03 Test Method for Aridity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products ................ ,.......................... ...............................................................06.03 Test Method for Alkalinity in Acetone...................................................... 06.03 Test Methods for Glycerol, Ethylene Glycol, and Pentaerythritolin Alkyd Resins.....................................06.02 Test Method for Ester Value of Solvents and Thinners................................................................................ 06.03 Methods of Testing Urethane Foam Isocyanate Raw Materials (Discontinued 199 If)............................. 06.03 Test Method for Add Value of Organic Coating Materials ........................................................................ 06.01 Test Methods for Drying, Curing or Film Formation of Organic Coatings atRoom Temperature------ 06.01 Test Method for Exterior Durability of Varnishes........................................................................................ 06.01 Test Methods for Elasticity or Toughness of Varnishes ........................ 06.01 DU P050296506 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 1643 - 60 (1988) D 1644 - 88 D 1647 - 89 D 1648 - 86 D 1649 - 82 (1987)61 D 1650 - 91 D 1652 - 90 D 1653 - 91a D 1654- 79a (1984)" D 1695 - 77 (1989)1 D1696 - 90 D 1716-62 (1987) D 1718 -- 86 D 1719 - 90 D 1720 - 88 D 1721 -84(1988)ei D 1722 - 90 D 1725 - 62 (1989)I D1726-90 D 1728-83 D1730 - 67 (1984)l D 1731 - 67 (1984)1 D 1732 - 67 (1984) D 1734 - 63 (1980)I D 1735 - 87 D 1736 - 89 D 1737 - 85 D 1787 - 89 D 1794 - 89 D 1795 - 90 D 1836 - 91 D 1841 - 63 (1988)l D 1842 - 63(1988) D 1843 - 63 (1988)ei D 1844 - 86 (I991)1 D 1845 - 86 (I991)cl D 1847 - 87 D 1848 - 88 D 1849 - 80 (1987)1 D 1915 - 63 (1989)1 D 1926 - 89 D 1950 - 86 D 1951 - 86 D 1952-86 D 1954 - 86 D 1955 - 85 (I989)1 D 1957 - 86 D 1958 - 86 (1990) D 1959- 85 (1989)l D 1960 - 86 (1990) D 1962 - 85 (1989)l D 1963-85 (1989)1 D 1964 - 85 (1989)I D 1965 - 87 (1991)*1 D 1966 - 69 (1991)1 D 1967 - 86 D 1969-91 D 1978-91 D 1979 - 91 D 1980 - 87 (1991 ) 1 D 1981 -- 86 (1990) D 1982 - 85 (1989)l D 1983 - 90 D 1984-69(1988) D 2064 - 91 D 2065 - 91 D 2066 - 91 D 2071 - 87 (1991)1 Test Methods for Gas Checking and Draft Test of Varnish Films ............................................................ 06.01 Test Methods for Nonvolatile Content of Varnishes...................................................................................06.01 Test Methods for Resistance of Dried Films of Varnishes to Water and Alkali ...................................... 06.01 Specification for Basic Lead Silicochromate Pigment .................................................................................06.02 Specification for Strontium Chromate Pigment................................................................ 06.02 Methods of Sampling and Testing Shellac Varnish .................................................................................. 06.02 Test Method for Epoxy Content of Epoxy Resins.......................................................................................06.02 Test Methods for Water Vapor Transmission of Organic Coating Films.................................................. 06.01 Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments .......... 06.01 Terminology of Cellulose and Cellulose Derivatives ...................................................................................06.02 Test Method for Solubility of Cellulose in Sodium Hydroxide...............................................................06.02 Test Method for Cellulose Chain Length Uniformity by Fractional Precipitation of Cellulose Nitrate . 06.02 Specification for Isobutyl Acetate (95 % Grade) ......................................................................................... 06.03 Specification for Isobutyl Alcohol ................................................................................................................. 06.03 Test Method for Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions................................ 06.03 Test Method for Permanganate Time of Tricresyl Phosphate ...................................................................06.03 Test Method for Water Miscibility of Water-Soluble Solvents ...................................................................06.03 Test Method for Viscosity of Resin Solutions (Intent to Withdraw)-) ...........: ..................................... 06.02 Test Method for Hydrolyzable Chlorine Content of Liquid Epoxy Resins ............................................ 06.02 Test Method for Phthalate Ester Color ofHigh-Gravity Glycerin (Discontinued 199If). 06.03 Practices for Preparation of Aluminum and Aluminum Surfaces for Painting .........................................06.01 Practices for Preparation of Hot-Dip Aluminum Surfaces for Painting.....................................................06.01 Practices for Preparation of Magnesium Alloy Surfaces for Painting.............................................. 06.01 Method of Making and Preparing Concrete and Masonry Panels for Testing Paint Finishes...................06.01 Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus .......................................06.01 Test Method for Efflorescence of Interior Wall Paints .............. 06.01 Test Method for' Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus (Discontinued 1988f--Replaced by Test Methods D 522) .................................................................. 06.01 Test Method for Pentosans in Cellulose.................................................................................................. 06.02 Test Method for Alcohol-Benzene Soluble Matter in Cellulose (Intent to Withdrawf).............................06.02 Test Method for Intrinsic Viscosity of Cellulose ........................................................................ 06.02 Specification for Commercial Hexanes ............................................ 06.03 Specification for Distilled Coconut Fatty Acids.................................... 06.03 Specification for Distilled Com Fatty Adds................................................................................................. 06.03 Specification for Fractionated and Distilled Cottonseed Fatty Adds ..................................... 06.03 Test Methods for Chemical Analysis of Basic Lead Silicochromate............................................................06.02 Test Methods for Chemical Analysis of Strontium Chromate Pigment...................................................... 06.02 Test Method for Total Chlorine Content of Epoxy Resins ......................... 06.02 Classification for Reporting Paint Film Failures Characteristic Of Exterior Latex Paints .........................06.01 Test Method for Package Stability of Paint .................... ......................................................................... 06.01 Method for Chromatographic Analysis of Chemically Refined Cellulose ................................................. 06.02 Test Methods for Carboxyl Content of Cellulose .........................:........... 064)2 Test Method for Acetone Tolerance of Heat-Boded Drying Oils ........... 06.03 Test Method for Ash in Drying Oils and Fatty Adds ...................................... ;............ ...................... 0643 Test Method for Quantitative Determination of Break in Drying Oils ................ ....06.03 Test Method for Foots in Raw Linseed Oil (Volumetric Method) ....................................... 06,03 Test Method for Gel Time of Drying Oils ....................... i6.03 ' Test Method for Hydroxyl Value of Fatty Oils and Acids' t Test Method for Chloroform Insoluble Matter in Oiticica Oil .............................. 06.03 Test Method for Iodine Value of Drying Oils and Fatty Acids .................................................. 06.03 Test Method for Loss on Heating of Drying Oils ........................................................................................06.03 Test-Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Adds _____06.03 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/ 25`C ............................................................................ ...........................................................................06.03 Test Method for Tung Oil Quality ................................ 06.03 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds,and Polymerized Fatty Adds ... 06.03 Test Method for Foots in Raw Linseed Oil (Gravimetric Method) ............................................. .'____ 06.03 Test Method for Measuring Color After Heating of Drying Oils ............................................................... 06.03 Specification for 2-Ethylhetanol (Synthetic)..................................................................................................06.03 Guide for Analysis of Electrocoat Bath Samples ......................................................................................... 06.01 Test Method for Free Formaldehyde Consent of Amino Resins ...................................................... ..." 06.02 Test Method for Add Value of Fatty Adds and Polymerized Fatty Adds ............................................... 06.03 Test Method for Measuring Color After Heating of Fatty Acids ....................... 06.03 Test Method for Titer of Fatty Adds ............................................................................................................064)3 Test Method for Fatty Acid Composition by Gas-Liquid Chromatograph of Methyl Esters ................... 06.03 Spedfication for Tall Oil Fatty Adds............................................................................................................06.03 Test Method for Print Resistance of Architectural Paints........................................................................... 06.01 Test Method for Determination of Edge Performance of Composite Wood Products Under Surfactant Accelerated Moisture Stress.................................................................................................................... 06.01 Test Methods for Relative Tinting Strength of Printing Ink Dispersions...................................................06.01 Test Methods for Fatty Nitrogen Products ................................................................................................. 06.03 xiv DUP050296507 D 2072 - 66(1987)1 D2073 -66(1987)`l D 2074 - 66 (1987)*1 D 2075 - 89 D 2076 - 64 (1987)f| D 2077 - 64 (1987) D 2078 - 86 (1990) D 2079 - 82 (1987) D 2080 - 64 (1987) D2081 -64(1987) D 2082 -82(1987) D2083-66(1987) D 2086 - 89 D 2087 - 89 D 2090 - 88 D209I - 88 D 2092 - 86 D2134 - 66 (1980)f| D 2190 - 89 D 2191 - 89 D2192 - 89 D 2193 - 89 D 2194 - 89 D 2195 - 89 D 2196 -- 86 (199l)l 02197 - 86 (199l)l D 2198 - 84 (1989)l D 2199 - 82 (1987) D 2200 - 91 D2201 - 65 (1987)l D 2205 - 85 (1990) 1 D2218-67(1989)1 D 2243 - 90 D2244 - 89 D2245 - 90 D 2246 - 87 D 2247 - 87 D 2248 - 89 D2336 - 87 (1991)1 D 2337 - 84(1989) D2338-84(1989)1 D 2348 - 91 D 2349 - 90 02350 - 90 D 2351 - 90 D 2352 - 85 (1990)1 D 2353 - 83 D 2354 - 91 D 2363 - 79 (1989)| D 2364 - 89 D2366-68(1980)1 D 2369 - 90 D 2370 - 82 (1987)2 D 2371 - 85 (1990)! D 2372 - 85 (1990)1 D 2373 - 85 (1990)1 D 2374 - 85 (1990)1 D 2375 - 85 (1990)I D2376 - 84 (1989) D 2378 - 84 (1987) D 2379 - 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 ofFatty 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) Steel Surfaces for Painting..................................... 06.01 Test Method for Softening of Organic Coatings by Plastic Compositions (Discontinued 1990f)............. 06JI1 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-Newtonian Materials by Rotational (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 Galvanized Steel 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.....................................7.................06.01 Test Method for Calculation of Color Differences from InstrumentallyMeasured 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 Cycle Cracking........... 06.01 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity........................................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.................................... v :r\..................................................................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 1992f).................................................................................................... 06-01 Test Method for Minimum Film 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............................................................................................. 06.0T 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 ofFace Glazing and Bedding Compounds on Metal Sash....................................06.01 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.................................................................................1...........................06.02 xv* nsyi'Hww `"i t wi------------------- DUP050296508 % D 2448 -83(1989) D 2454 - 91 D 2455 - 89 D 2456-91 D 2485 - 91 D 2486 - 89 D 2571 - 88 D 2572 - 91 D 2574 - 86 D 2575 - 70 (1991)" D 2613 - 85 (1990)" D 2620 - 87 D 2621 - 87 D 2627 - 91 D 2634 - 86 D 2635 - 91 D 2636 - 91 D 2641 - 89 D 2689 - 88 D 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)" D 2803 - 82 (1987) D 2804 - 88 D 2805-88 D 2830 - 91 D 2832 - 83 (1991)" D2833-89 D 2916 - 88 D 2917 - 91 D292I - 88 D 2929 - 89 D 2931 - 84 (1989)" D 2932 - 80 (1988)" D 2933 - 74 (1986)" D 2998 - 89 D 2999 - 85 D 3002 - 8! (1987) D 3003 -- 71 (1987) D 3008 - 90 D 3009 - 72 (1981)" D 3021 - 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 06.02 of the Pigment.......................................................................................................................................... Practice for Determining the Effect of Overbaking on Organic Coatings.................................................... 06.01 Test Method for Identification ofCarboxylic Acids in Alkyd Resins.........................................................06.02 Test Method for Identification ofPolyhydric Alcohols in Alkyd Resins ...................... 06.02 Test Methods for Evaluating Coatings for High Temperature Service ........................................................06.01 Test Method for Scrub Resistance of Interior Latex Flat Wall Paints ..................................................... 06.01 Guide for Testing Wood Furniture Lacquers................................................................................................06.01 Test Method for Isocyanate Groups in Urethane Materials or Prepolymers .............................................06.02 Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms...........06.01 Test Methods for Polymerized Fatty Adds ..................................................................................................06.03 Test Method for Calcium or Zinc in Paint Driers by EDTA Method .......................................................06.03 Test Method for Light Stability of Clear Coatings.......................................................................................06.01 Test Method for Infrared Identification of Vehicle Solids from Solvent-Redudble Paints .......................06.01 Specification for Diacetone Alcohol .............................................................................................................06.03 Specification for Methyl Amyl Acetate (95% Grade) .................................................................................. 06.03 Specification for Methyl Isobutyl Carbinol ............................................................................................. 06.03 Specification for Hexylene Glycol ............................................................. 06.03 Test Method for Chlorine in Cellulose......................................................................................................... 06.02 Practices for Testing Alkyd Resins ................................................................................................................ 06.02 Test Method for Isophthalic Acid in Alkyd and Polyester Resins ..............................................................06.02 Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products . 06.01 Spedfication for Ethylene Glycol .................... 06.03 Spedfication for Diethylene Glycol .................. 06.03 Specification for Propylene Glycol (Discontinued1992f).............................................................................06.03 Spedfication for Dipropylene Glycol (Discontinued 1992f)...................................................................... 06.03 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings..........................................06.01 Method for Determination of the Pigment Content of Solvent-Redudble Paints by High-Speed Centrifuging ................................................................................... 06.01 Methods for Chemical Analysis of Tribasic Lead Phosphosilicate (Discontinued 1990f)......................... 06.02 Practices for Uniformity of Traffic Paint Vehicle Solids by Spectroscopy and Gas Chromatography .. 06.01 Specification for Tribasic Lead Phosphosilicate (Discontinued 1988t) ..................................................... 06.02 Test Method for Relative Tinting Strength of White Pigments by Reflectance Measurements..................06.02 Test Method for Solvent and Fuel Resistance of Traffic Paint....................................................................06.01 Test Method for Block Resistance of Organic Coatings on Wood Substrates ........................... 06.01 Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)........... 06.01 Test Method for Preparation of Methyl Esters from Oils for Determination of Fatty Add Composition by Gas Chromatography .....................................................................................................7................. 06.03 Test Method for Leveling Characteristics of Paints by Draw-Down Method (Discontinued 1990f) ... 06.01 Test Method for Filiform Corrosion Resistance of Organic Coatings on Metal ....................................... 06.01 Test Method for Purity of Methyl Ethyl Ketone by Gas Chromatography ............................................... 06.03 Test Method for Hiding Power of Paints by Reflectometry ....................................................................... 06dW Test Method for Durability and Compatibility of Factory-Primed Wood Products with Representative Finish Coats ...................................................................................................................... 06.01 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 .............................................................................................. 7~.. 0(6.03 Specification for Methyl Isoamyl Ketone................................... 06.03 Test Method for Qualitative Tests for the Presence of Water Repellents and Preservatives in Wood Products ............................................................ 06.01 Test Method for Sulfur Content of Cdlulosic Materials by X-ray Fluorescence ............................... 06.02 Guide for Testing Latex Flat Wall Paints ........................................................................................... 06.01 Guide for Testing Exterior Solvent-Reducible House and Trim Coatings ............................................ 06.01 Test Method for Corrosion Resistance ofCoated Steel Specimens (Cyclic Method) (Discontinued 1992t) Test Method for Polyhydric Alcohols in Alkyd Resins .............................................................................06.02 Test Method for Monopentaerythritol in Commercial Pentaerythritol (Discontinued 1989f--Replaced by Test Method D 2195) ........................................................................................................................ 06.03 Practice for Evaluation of Coatings for Plastics.........................................................................................06.01 Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates . 06.01' Test Method for Resin Acids in Rosin by Gas Chromatography ............................................................. '06.03 Test Method for Composition of Turpentine by Gas Chromatography................................................... 06.03 Specification for Phthalocyanine Green Pigments.....................................................................................06.02 Test Method for Color and Strength of Color Pigments by Use of a Miniature Sandmill .....................06.02 Practice for Determination of Resistance of Factory-Applied Coatings on Wood Products to Stains and Reagents .................................................................................................................................................... 06.01 Test Method for Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid .............................................................................................................................................. 06.03 Specification for -ButyI Acetate (98% Grade) (Discontinued 1987f--Replaced by Specification D4615)............................................................................................................................ 06.03 xvi DUP050296509 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 3127-83 D 3128-89 D 3129 - 91 D 3130 - 86 D 3131 - 88 D 3132 - 84 (1990)61 D3133-72(1989)| D 3168 - 85 (1990)1 D 3169 - 89 D3170-87(1991)l D 3256 - 86 (1991)l D 3257 - 88 D3258 - 80 (1987)l D 3259 - 84 (1990)l D 3260 - 82 (1991) D 3271-87 D3272 - 76 (1988)6' D 3273 - 86 (I991)I D 3274 - 82 (1988)1 D 3276 - 86 D 3278 - 89 D 3280 - 85 (1990)1 D 3281 - 84 (1989) D 3322 - 82 (1991) D 3323 - 80 (1988)1 D 3329 - 89 D 3335 - 85a1 (1991 )e 1 D3358 - 88 D 3359 - 90 D 3360 - 80 (1989) D 3361-87 D 3362 - 84 (1987) D 3363 - 74 (1989)l D 3383 - 79a (1988)I D 3424 - 75 D3425 -80(1988)1 D 3432 - 89 D 3450 - 90 D3451 - 76(1987)l D 3456 - 86 (1991)1 D 3457 - 87 (1991)l 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 D 3618 - 85a (1991)1 D 3619 - 77 (1989) D 3620 - 90 D 3621 - 84 D 3622 - 90 D 3623 - 78a (1987) D 3624 - 85a (1991)El Specification for n-Ethyl Acetate (99% Grade) (Discontinued 1987f--Replaced by Specification D4614)................ :.................................................................................................................................. 06.03 Specification for 2-Methoxyethanol ............................................................................... ........................ 063)3 Guide for Testing Exterior Latex House Paints............................................................................................ 06.01 Specification for n-Propyl Acetate (96 % Grade) .......................................................................................... 06.03 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.................................................................................. ................................................06.01 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 Test Methods 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 ofApplied Coatings on Wood Products During the Curing Cycle........................................................................................................................................06.01 Test Method for Add and Mortar Resistance ofFactory-Applied Clear Coatings on Extruded Aluminum Products........................... ...................................................................................................................... 063)1 Practice for Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph for Solvent Analysis............................................................................................................................. Practice for Vacuum Distillation of Solvents from Solvent-Redurible Paints for Analysis...................... 063)1 Test Method for Resistance to Growth of Mold on the Surface of Interior 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 andDirt Accumulation.........................................................................................06.01 Guide for Painting Inspectors (Metal Substrates).......................................................................................... 063)1 Test Methods for Hash Point ofLiquids by Setaflash Closed-Cup Apparatus........................................... 06.03 Test Methods for Analysis of White Zinc Pigments..................................................................................... 06.02 Test Method for Formability of Attached Organic Coalings with Impact-Wedge Bend Apparatus......... 063)1 Practice for Testing Primers and Primer Surfacers Over Preformed Metal ............................................... 06.01 Guide for Testing Interior Solvent-Redudble Flat Wall Paints....... ........................................................... 06.01 Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography ........................................... 06.03 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy............................................................................................................................................. 063)1 Guide for Testing Water-Borne Hoor Paints.............................................. ...................... i";................ 063)1 Test Methods for Measuring Adhesion by Tape Test............................................................ Test Method for Particle Size Distribution By Hydrometer of the CommonWhite Extender Pig . ments ... 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.......................................................... 063)3 Test Method for Film Hardness by Pencil Test ......................................................................................... 06311 Guide for Testing Solvent-Redudble Hoor Paints....................................................... Method of Evaluating the Lightfastness of Printed Matter.......................... .... 063)1 Guide for Testing Solvent-Redudble Interior Semigloss Wall and Trim Enamels .............. ..... 063)1 Test Method for Unreacted Toluene Diisocyanates inUrethane Prepolymers and Coating Solutions by' " Gas Chromatography................................ *............ * ; .................. ................................................ 063)2 Test Method for Washability Properties of Interior Architectural Coatings............................................. 063)1 Practices for Testing Polymeric Powders and Powder Coatings................................................... 063ilr 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-Ery Cycling for Coatings on Wood and Wood Products.................................. 063)1 Test Method for Ashing Cellulose................................................................................................................. 06.02 Test Methods for Evaporation Rates ofVolatile Liquids by Shell Thin-Film Evaporometer .................. 06.01 Specification for Primary Amyl Acetate, Synthetic (98 % Grade)...............................................................06.03 Specification for 2-Ethylhexyl Acrylate.........................................................................................................06.03 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography ...................... 063)3 Test Method for Formic Acid in Glacial Acetic Acid..................................................... '. 06.03 Specification for n-Butyl Acrylate................................................................................................................. 06.03 Specification for Ethyl Acrylate.................................................................................................................... 063)3 Test Method for Detection of Lead in Paint and Dried Paint Films........................................................... 06.01 Specification for Aluminum Silicate Pigments (Anhydrous)...................................................................... 063)2 Specification for Giadal Acetic Acid............................................................................................................ 063)3 Practioe for Determination ofWater in Acetate Esters (Discontinued 1988f--Replaced by Test Method D 1364)...................................................................................................................................................... 063)3 Specification 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 ...........06.01 xvu mm, TT DUP050296510 06. 06.0 1 D 3630 - 89 D 3680 - 89 D 3717 - 85a(1991)l D3718 - 85a {1991 )e 1 D 3719-87 D 3720 - 90 0 3721 -83(1991)" 0 3722 - 82(1991)" D 3723 - 84 (1990)" D 3724 - 82 (1987)" D 3725-78 (1988)" D 3726-84 D 3727 - 84 D 3728 -88 0 3729 - 84 D 3730-78 (1988)" D 3732-82 (1989)" 0 3733 - 78(1984)" 0 3734 - 91 0 3735 - 87 D 3792 - 91 0 3793 - 89 D 3794 - 79" D 3804 - 86 (1991)" D 3806-90a D3842-86(1991) D 3843-89 D 3845-89 D 3872-86 (1991)" D 3876-79 (1989)" 0 3891-90 03893-90 03911-89 0 3912 - 80(1989) D 3924 - 80 (1991)" D 3925-91 D 3926-80 (1991)" D 3927-87 D 3928-89 D 3934-90 D 3941 -90 D 3960 - 91 D 3964-80 (1989) 0 3969 - 85(1990)" 0 3970 - 80(1990)" 0 3971-89 0 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) D 4138-88 04139 - 82(1991)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Guide for E>eterriiiaing Constituents Classified Hazardous Contained in Protective Coatings.......... 063)1 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___ 063)1 Test Method for Low Concentrations of Chromium in Paint by Atomic Absorption Spectroscopy___ 06.01 Test Method for Quantifying Dirt Collection on Coated Exterior Panels................................................ 063)1 Test Method for Ratio ofAnatase to Rutile in Titanium Dioxide Pigments by X-Ray Diffraction___ 06.02 Specification for Synthetic Red Iron Oxide Pigment.................. .......................................................... 06.02 Specification for Natural Red and Brown Iron Oxide Pigments.................................................. ......... .. 063)2 Test Method for Pigment Content of Water-Emulsion Paints by Low-Temperature Ashing.................. 06.01 Specification for Synthetic Brown Iron Oxide Pigment ..:...................................................................... 06.02 Test Method for Semiquantitative Determination ofFish Oil in Drying Oils and Drying Oil Fatty Adds by Gas-Liquid Chromatography........................................... 06.03 Specification for n-Butyl Acetate (99.5 % Grade) (Discontinued 1987t--Replaced by Specification D4615)...................................... 06.03 Spedfication for Ethyl Acetate (99.5% Grade) (Discontinued 1987f--Replaced by Specification D4614)............................................................................................................ 06.03 Spedfication for 2-Ethoxyethyi Acetate (99-% Grade) ........................... ...................................... ......... 063)3 Spedfication for Methyl Ethyl Ketone (99.5 % Grade) (Discontinued 1989t--Replaced by Spedfication D 740)................................................................................ 06.03 Guide for Testing High-Performance Interior Architectural Wall Coatings............................................ 063)1 Practice for Reporting Cure Times of Ultraviolet-Cured Coatings.................................... ......................06.01 Test Method for Silicon Content of Silicone Polymers and Silicone-Modified Alkyds by Atomic Absorption....................................................................................................... 06.02 Spedfication for High-Flash Aromatic Naphthas.................................... 06.03 Spedfication for VM&P Naphthas ............................................................................................................ 063)3 Test Method for Water Content of Water-Redudble- Paints by Direct Injection Into a Gas' Chromatograph............................... 06.01 Test Method for Low-Temperature Coalescence of Latex Paint Films.................................. .......... 06.01 Practice for Testing Coil Coatings................................................................................................................ 06.01 Test Method for Iron in Paint Driers'by EDTA Method.......................................................................... 06.03 Test Method for Small-Scale Evaluation of Fire-Retardant Paints (2-Foot Tunnel Method) ................ 06.01 Guide for Selection of Test Methods for Coatings for Use in Light-Water Nudear Power Plants........ 06.01 Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities................ ........ 06.01 Specification for Glacial Methacrylic Add...................................................... 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.......................... ....................................................... ...................................................06.02 Practice for Preparation of Glass Panels for Testing Paint, Varnish, Lacquer, and Related'Products... 06.01 Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by Gas Chromatography 06.03 Test Method for Evaluating Coatings Used in Ught-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) Conditions.................................................... :................................................ 06.01 Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants............ 06101 Spedfication for Standard Environment for Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials.......... .............................................................................................'.........................06.01 Practice for Sampling Liquid Paints and Related Pigmented Coatings.......... ....................... ........ ... . 06.01 Test Method for Percent Solids in Titanium Dioxide Slurries............................ ............ .................... ,06.02 Guide for State and Institutional Purchasing of Paint (Intent to Withdraw) .......................... ...... 06.01 Test Method for Evaluation of Gloss or Sheen Uniformity'.":.................................................................... 06.01 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 063)3' 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...... ................................................. 06.02 Practice for Interlaboratory Testing of Paint and Related Materials........................................................ 06.01 Test Method for Vanadium in Paint Driers by EDTA Method.................................................. 063)3 Test Method for Total Rare Earth Metals in Paint Driers by EDTA Method.......................................... 06.03 Test Method for Water in Paints and Paint Materials by Karl Fischer Method........................................ 06.01 Test Method for Reflection Haze of High-Gloss Surfaces.................................................... 06.01 Test Method for Viscosity of Printing Inks and Vehicles by the Falling-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.............................. 06.01 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 Spectrophotometry...................................... 06.02 Practice for Photographic Documentation of Coating and Lining Failures and Defects........................ 06.01 Test Method for Measurement of Dry Film Thickness of Protective Coating Systems by Destructive Means...................................................................................................................................................... 06.01 Guide for Determining Volatile and Nonvolatile Content of Pigments..................................................06.02 xviii DUP050296511 : p 4140-82 (1991) P4141 82 (1987)" D 4142 89 I P 4143 89 i D 4144 82(1987) t D4145 83 (1990)" P4146 83 (1989)" ' P4I47 82(1987) P 4206 89 D 4207 91 P 4209 82(1991)" D4212- 88 D 4213- 87 fiP4214- 89 m P4227- 83(1989) I D4228 - 83 (1989) D4236- 91 P 4256 89 P 4257-87 D4258-83(1988) D 4259-88 P 4260-88 D4261 - 83 (1988) D'4262-83 (1988) P 4263 - 83 (1988)" D 4277-83 (1988)" P 4285-83 (1988) D 4286 -90 D 4287-88 D4288 - 83 (1989)" D4301-84(1989)" D.4302 - 90 D4303-91 ft P 4358-84 (1990)" D 4359-90 tl P 4360-90 D4361 - 89 D4366-91 D 4367-89 D 4368 -89 0 4370 - 84(1990)" D4399-90 D 4400 - 89a 0 4414 - 84(1990)" D 4415-91 D 4416-89 D 4417-84 04449-90 D 4450 - 85 (1990)" D 4451 - 85 (1991)" D 4457 -85 (1991)" 0 4462 - 85(1989) P 4487-90 D 4518-91 P 4537-91 D 4538-90a D4540 - 91 D 4541 -85 (1989)" D 4563-86 (1991)" D4584- 86 (1991)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Guide for DeteriiiiHing Volatile and Nbttvolatile Content of Driers, Drying Oils, Naval Stores, and Solvents........................................................................................................................ 06.03 Practice for Conducting Accelerated Outdoor Exposure Tests of Coatings.............................................. 06.01 Guide for Testing Epoxy Resins.....................................................................................'.......................... 06.02 Guide for Testing Latex Vehicles...................................................................................................................06.02 Method for Estimating Package Stability of Coatings for Ultraviolet Curing.......................................... 06.01 Test Method for Coating Flexibility of Prepainted Sheet..........................................................................06.01 Test Method for Formability of Zino-Rich Primer/Chrpmate Complex Coatings on Steel.................... 06.01 Practice for Applying Coil Coatings Using the Wire-Wound Drawdown Bar.......................................... 06.01 Test Method for Sustained Burning of Liquid Mixtures by the Setaflash Apparatus (Open Cup) 06.01,06.03 Test Method for Sustained Burning of Low-Viscosity Liquid Mixtures by the Wick Test.............. .. 06.03 Practice for Determining Volatile and Nonvolatile Content of Cellulosics, Emulsions, Resin Solutions, Shellac, and Varnishes........ ......................... 06.02 Test Method for Viscosity by Dip-.Type Viscosity Cups...... .....................................................................06.01 Test Method for Wet Abrasion Resistance of Interior Paints............ .................................................... ... 06.01 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films............................................ .. 06.01 Practice for Qualification of Journeyman Painters for Application of Coatings to Concrete Surfaces of Safety-Related Areas in Nuclear Facilities............ ..................................................................................06.01 Practice for Qualification of Journeyman Painters for Application of Coatings to Steel Surfaces of Safety-Related Areas in Nuclear Facilities.............. ,,............................................................................06.01 Practice for Labeling Art Materials for Chronic Health Hazards.............................................................. 06.01 Test Method for Determination of the Decontaminability of Coatings Used in Light-Water Nuclear Power Plants...................................................................................................... 06.01 Practice for Design and Use of Safety Alert System for Hazardous Work Locations in the Coatings and Lining Industry (Discontinued 1990+)................ .................................................................................... 06.01 Practice for Surface Cleaning Concrete for Coating.................................................................................. 06.01 Practice for Abrading Concrete.................................................................................................................... 06.01 Practice for Add Etching Concrete...................... ......................................................................................06.01 Practice for Surface Cleaning Concrete Unit Masonry for Coating........................................................ .. 06.01 Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces.............................................. 06.01 Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method...................................... 06.01 Guide' for Testing Amino Resins.................... 06.02 Test Method for Indicating Oil or Water in Compressed Air .................................................................06.01 Practice for Determining Coating Contractor Qualifications for Nuclear Powered Electric Generation Facilities.......................... ....................................................................................................................... 06.01 Test Method for High-Shear Viscosity Using the 1CI Cone/Plate Viscometer.................... . ............... 06.01 Specification for Caltium Borosilicate Pigments.............................. .... .............................................. 06.02 Test Method for Total Chlorine in Epoxy Resins and Compounds ................ ....................................... 06.02 Specification for Artists' Oil, Resin-Oil, and Alkyd Paints........... .........................................................06.01 Test Methods for Lightfastness of Pigments Used in Artists' Paints........................................................06.01 Test Method for Lead and Chromium in Air Particulate Filter Samples ofLead Chromate Type Pigment Dusts by Atomic Absorption Spectroscopy................ ................................. ..................................... J26-02 Test Method for Determining Whether a Material is a Liquid or a Solid................................................ 06.01 Specification for Methyl n-A.myl Ketone..................................................... ............................................ 06.03 Test Method for Apparent Tack of Printing Inks by the Inkometer........................................................ 06:01 Test Methods for Hardness of Organic Coatings by Pendulum Damping Tests...................__________ 06.01 Test Method for Benzene in Hydrocarbon Solvents by.Gas Chromatography........ ; rrr...'06.03 Guide for Testing Poiy(Vinyl Chloride) Resins....................... ................................................T............... 06.02 Test Methods for Acid and Base Milliequivalent Content of Electrocoat Bath...... ................................. 06.01 Test Method for Measuring Electrical Conductivity of Electrocoat Baths................................................ 06.01 Test Method for Sag Resistance of Paints Using a Multinotch Applicator.............................. 7......... ... 06.01 - Practice for Measurement of Wet Film Thickness by Notch Gages.............................................. ......... 06.01 Test Method for Determination of Dimer in Acrylic Acid .................... ..................................................06.03 Specification for Acrylic Acid ................................................................ ................................................... 06.03 Test Methods for Reid Measurement of Surface Profile of Blast Cleaned Steel...................................... 06.01 Test Method for Visual Evaluation of Gloss Differences Between Surfaces of Similar Appearance .... 06.01 Test Method for Analysis of Zinc Hydroxy Phosphite Pigment.................................................... ......... 06.02 Test Method for Pigment Content of Paints by Low-Temperature Ashing.............................................. 06.01 Test Method for Determination of Dichloromethane and 1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a Gas Chromatograph...................................................................................... 06.01 Specification for Zinc Hydroxy Phosphite Pigment.................................. .............................................-. 06.02 Test Methods for Analysis of Calcium Borosilicate.................................................................................. 06.02 Test Methods for Measuring Static Friction of Coating Surfaces...............................................................06.01 Guide for Establishing Procedures to Qualify and Certify .Inspection Personnel for Coating Work in Nuclear Facilities........ ............-..................................................................................... ............................06.01 Terminology Relating to Protective Coating and Lining Work for Power Generation Facilities............ 96.01 Guide for Testing Interior Latex Semigloss and Gloss Paints............ .................................................. 06.01 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers.................................. 06.01 Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered from Whole Paint.............................. .................................................................06.01 Test Method for Measuring Apparent pH of Electrocoat Baths .............................................................. 06.01 DUP050296512 D4585 -87el D4587-91 D 4610-86 D4613 - 86 (1990)61 D 4614-86 D46l5-86> D4618-87 D46I9-91 D4639-86(1990)1 D4640-86(1990)1 D 4706 - 87 04707 - 87 04708-91 D 4709 - 87 D 4710-87 D 4712-87a (1991) D4713 - 871 D 4747 - 87 D4752-87 04758-87 0 4764-88 04773-89 D 4787-88 D 4794 - 88 D 4795 -88 D 4796-88 D 4797-88 D 4827 - 88 0 4828-91 0 4834 - 88 0 4835 - 89 0 4836 - 90 0 4837 - 89 0 4838 - 88 0 4938 - 89 04939-89 0 4940-89 04941-89 04942-89 D 4946 - 89el 04948-89 0 4958 - 91 0 4960-89 D 5007 - 89 0 5008-89 0 5009 - 89 0 5010-91 D 5031 - 89 D 5043-90 0 5062 - 90" 0 5063 - 90 0 5064 - 90 0 5065 - 90 D 5066 -91 0 5067 - 90I D 5068 - 90 D 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 ofand Removing Microbial (Fungal or Algai)'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 n-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 ofThermosetting 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................ .................................. 063)1 Specification for Methyl Acrylate .................................. 063)3 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 ofEthyl Silicate (Inorganic) Zinc-Rich Primers by Solvent Rub................................................................................................ .....................................................06-0 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 Monoraethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene Glycol Monomethyl 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 ofLatexes Using Capillary Column Gas -v Chromatography............................................ .......... ...;...................... ............................................ 06.02 Test Method for Practical Washability of Organic Coatings ............ .................... ............................... 06.0i Test Method for Detection of Lead in Paint by Direct Aspiration Atomic Absorption Spectroscopy... 06.0i Specification for Propylene Glycol Monomethjrl Ether Acetate...... .......... ......................... ... -.......... 06.03 Specification for Dipropylene Glycol Monomethyl Ether ................ .................... .................. 06.03 Specification for Propylene Glycol Monomethyl Ether.............. ..................................................... . - 06.03 Test Method for Determining the Relative Tinting Strength of Chromatic-Paints.......................... . 06.01 Test Method for Erosion Testing of Antifouling Paints Using High Velocity Water..................... 06.01 Test Method for Subjecting Marine Antifouling Coating to Biofouling and Fluid Shear Forces in Natural Seawater ...................... .................................................................... i............. .` 06.01 Test Method for Conductimetric Analysis of Water Soluble Ionic Contaminatibti'of Blasting Abrasives.. 06.01 Practice for Preparing Drawdowns of Artists' Paste Paints .......................... .................. ................. .... 06.01 Test Methods for Water Pickup of Lithographic Printing Inks and Vehicles in a Laboratory Mixer ... 06.01 Test Method for Blocking Resistance of Architectural Paints...................... ........................................ .-3)63)1 Test Method for Determination of the Upper Layer Separated from a Viscous Liquid !............ ......... 06.03 Test Method for Comparison ofthe Brush Drag of Latex Paints ...................................... ................... 06.0) Test Method for Evaluation of Color for Thermoplastic Traffic Marking Materials.............. ............... 06.01 Test Method for Wet-to-Dry Hiding Change.................... ........................... ........................................ .. 06.01 Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol by Gas -- Chromatography ................................ ................................................................................................. 06.fi) Test Method for Evaluating and Comparing Transfer Efficiency Under Laboratory Conditions.......... 06.01 Guide for Testing Printing Inks and Related Materials............................ ........................... .............. 06.01 Practice for Conducting Tests on Paints and Related Coatings and Materials Using Enclosed Carbon-Arc . Light and Water Exposure Apparatus ......... .....................................1........... ........ .............. 06.0: Test Methods for Field Identification of Coatings...................................................................... ?........... 06.01 Test Method for Resin Solution Dilutability.............................................................................................. 06.0: Guide for Use of Certification of Coating Conformance Form............ ................................................... 06.0 Practice for Conducting a Patch Test to Assess Coating Compatibility..................................................... 063) Guide for Assessing the Condition of Aged Coatings on Steel Surfaces ................................................... 063) Test Method for Determination of the Transfer Efficiency Under Production Conditions for Spray Application of Automotive Paints--Weight Basis............................ .............................................. 063) Specification for Artists' Watercolor Paints................................................ .............................................. 06.0 Practice for Preparation of Paint Brushes for Evaluation........................................................................... 063) Practice for Preparation of Paint Roller Covers for Evaluation.................................................................. 06.0 pppw xx __ > v M **'*'- ' DUP050296513 D 5087 - 91 D 5095-90 D 5097 - 90 D 5098-90 D 5107-90 D 5108-90 D 5125-91 D 5137-90 i D 5139-90 D 5144-91 D 5145-90 D 5146-90 D5150-91 D 5161-91 D 5162-91 D5I63-91 D5164-91 D 5166 - 91 D 5178 -91 D 5179-91 D5181-91 D 5200 - 91 D 5201 -91 E 28 - 67 (I982)ei E 97 - 82(1987) E 259-91 E 430-91 /t , { E 852 - 82 (1987)" G 6-88 G 8-90 G 9-87 l! G 10 - 83(1988) G 11-88 G 12-83(1988) G 13-89 G 14-88 IL- G G 17-88 18-88 | G 19-88 G' 20-88 G 23-90 *; G 26-90 . ?. G G 42-90 53 - 88 D 362 - 84 D 835-90 D 836-84 D 841 - 90 D 843-90 D. 846-84 D 847 - 91 b 848-81 (1989)" D 849-88, D 850-91 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 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 of Antifouling 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 of Coatings 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 Electrocdat Baths................................................ 06.01 Guide to Testing Solvent-Borne Architectural Coatings................................ r........................................ .. 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 (Metal Substrates)___ . 06.01 Practice for Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates.................... ........................................... ................................................................................f 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 Using a 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) ofSolvent 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 ReBectometty...... ..........................................................:............................................................06.01 Practice for Preparation of Reference White Reflectance Standards ...................................................... 06.01 Method for Measurement of Gloss Of High-Gloss Surfaces by Goniophotoraetry .................. .......... 06.01 Test Methods for C4-Cj3 Plasticizer Grade Alcohols .......................... ......................................................06.03 Test Method for Abrasion Resistance of Pipeline Coatings .................................................................... 06.01 Test Methods for Cathodic Disbonding of Pipeline Coatings................................................ t.............. 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 on Steel.......... 06;Ol Test Method for Impact Resistance of Pipeline Coatings (limestone Drop Test) .............................. 06.01 Test Method for Impact Resistance ofPipeline 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........ ............. ........ ........................Q6.01 Test Method for Disbonding Characteristics of Pipeline Coatings by Direct Soil Burial.. 7"........... 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.............. i 06.01 Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetalhe Materials........ ........ :....................................................................................06.01 AROMATIC HYDROCARBONS AND RELATED CHEMICALS (see gray-edged pages 539 to 817 of Volume 06.03) Specification for Industrial Grade Toluene (Discontinued 199!) .......................................................... .. 06.03 Specification for Refined Benzene-485 ...................................................................................................... 06.03 Specification for.Industrial Grade Benzene (Discontinued 1993) ............................................................ 06.03 Specification for Nitration Grade Toluene.................................................................................................06113 Specification for Nitration Grade Xylene ........................................................ ................. ..................... 06.03 Specification for Ten-Degree Xylene (Discontinued 1991) ...................................................................... 06.03 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons .........................................................................................................................06.03 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons.............................. ............... 00.03 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons ............................................ 06.03 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials .................. 06.03 xxx DUP050296514 D 852- 87 (1991) D 853- 91 D 1015- 84 D 1016- 84 D 1492 - 91 D1493 - 90 D 1555 - 91 D1631 - 85 (1989)41 D 1685- 86 (1990) D 1686 - 81 (1990) 84(1989)" 84(1989)" 87 87 90 . 81 (1986)" 81(1985) 84(1989)" 81 (1989)" 82(1987)" 90 82 (1987)" 91 91 81 88" 86 80(1989)" 91 81(1985) 90 91 91 86 90 CONTENTS, VOLUMES 06.01, 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................................................................................. 064)3 Test Method for freezing Point of High-Purity Hydrocarbons ................................................................ 064)3 Test Method for Purity of Hydrocarbons from Freezing Points.................. .................................. 06.03 Test Method for Bromine Index of Aromatic Hydrocarbons by Coulometric 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-terf-Butylcatechol, in Styrene Monomer .......... ............................ . 064)3 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 (1 Degree) ................................ ....................................................... .. 06413 Test Method for Carbon Disulfide in Benzene ........................................................................................ 064)3 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 .. 06413 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-Hydrogen Combustion Methods) (Discontinued 1987t) ...................................... ............................................. :' 064)3 Test Method for Pyridine Bases in Tar Acids (Discontinued 1987t--Replaced by Test Method D4471)............................................................................................. 06.03 Specification for Styrene Monomer 996 .......................................................................................... .. -- 06.03: Test Method for Gel Time of Tar Acids ........................................ ......................................................... 064)3 Test Method for Maleic Acid in Maleic Anhydride by Potentiometric Titration .................................. 064)3 Test Method for Apparent Density of Industrial Aromatic Hydrocarbons ............................................ 064)3 Test Method for Purity and Benzene Content of Cyclohexane by. Gas Chromatography...................... 064)3 Specification for Cyclohexane 995 ............................................................................................................ 06.03 Test Method for Phenol Content of Isopropylbenzene (Cumene) ........................................................... 064)3 Specification for Ethylbenzene ....................................................... 06.03 Specification for Industrial Grade Aniline .......................... 06.03 Test Method for Color pf 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.......... 06.03 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.............................................. 064)3 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 ..............................................................06.03 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 Add ...................... .................................. . 06.03 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry ........................................................................................................................... 064)3 Test Method for Analysis of Styrene by Gas Chromatography........................................................ >.... 06.03 Specification for o-Xylene 950 .................................................................................................................... 06.03 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 Add by Direct Titration......................................................06.03 Test Method for Analysis of Benzene by Gas Chromatography..............................................................06.03 Test Method for Solidification Point of 4,4'-IsopropyIidenediphenol (Bisphenol A)..............................06.03 Test Method for Benzene Content of Cyclic Products by Gas Chromatography.................................... 06.03 Guide for Analysis ofp-Xylene (Discontinued 1992f--Replaced by Spedfication D 5136).................. 06.03 Test Method for Nitrobenzene in Aniline.................................................................. ............................... 06.03 Test Method for Colorimetric Determination ofp-tof-Butylcatechol in Styrene Monomer by Addition of Alcoholic NaOH.................................................................................................................................. 06.03 Specification for Refined Benzene-545 ........................ ............................................................................. 06.03 Test Method for Determination ofTrace Thiopene in Refined Benzene by Gas Chromatography -- 06.03 Test Method for Solution Color of 4,4'-Isopropylidenediphenol (Bisphenol A)......................................06.03 DUP050296515 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 4790 - 89a D 4961 -89 D 5060 - 90 D 5135 - 90 D 5136 - 90 D 5194 - 91 t D 5211 - 91 ' E 299-90 " E 300 - 86 E 691-87 Terminology ofAromatic Hydrocarbons and Related Chemicals............................................................. 06.03 Test Methods for Gas Chromatographic Analysis of Major Organic Impurities in Phenol Produced by the Cumene Process........................................................ ...................................................................... . 06.03 Test Method for Determining Impurities in High-Purity Ethylbenzeneby Gas Chromatography ..... 06.03 Test Methods for Analysis ofStyrene 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 RELATED MATERIAL ft list by Subjects, Volume 06.01 ...................... >........... ............. s-.............................. List by Subjects, Volume 06.02 ...................... .......................:........... :................ 'dl List by Subjects, Volume 06.03 ............................................................................................. a Metric Practice (Excerpts) (E 380)....................................... ................................................ i D! Index................................................................................................................................. Id Index ................................................................................................i........... ....................... jj: ASTM Membership Application VOLUME, PAGE 06.01 xxiv, 06.02 519, 06.03 821 06.01 1095,06.02 xxiv, 06.03 829 06.01 1100, 06.02 527, 06.03 xxiv 06.01 1107, 06.02 534, 06.03 835 06.01 1120, 06.02 547, 06.03 848 06.01 1133,06.02 561, 06.03 861 I*1 PENDING STANDARDS ACTION 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. p ' ' ' 4 Revision ofStandards: D 1492-91 D 3359-91 D 4417-91 '|` New Standards: 1' D 5165 - 91 D 5180 - 91 Practice for the Laboratory Preparation of Gelled Vehicles Using a Resin Kettle.................................. 06.02 Test Method for Quantitative Test for Turbidity in Clear Liquids.......................................................... 06.02 DUP050296516 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.02 Pa in t --Pig me n t s , Re s in s , a n d Po l y me r s ; Ce l l u l o s e 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 06.03, see pp. 519 and 527 A complete Subject Index begins on p. 561 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)" 0 4288 - 83(1989)" D 476-84(1989) D 81-87 D 4462-85 (1989) D 79-86 D 210-81a(199!)" D 561-82(1989) D 769-87(1991)" D 209-81 (1989) D 962-81 (1986)" D 267-82(1987)" D 964-65(1989) D 912-81 (1986) D 911-87 D 520 - 84(1989) D 963-81 (1986)" D 261-75(1987)" D 262-81 (1987)" D 212-87 D 263-75(1987) 0 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. xxiv V G3 DUP050296517 |D 3722 - 82 (1991)ei j;D3724-82 (1987)"  2218 - 67 (1989)" ; D 85-87 (1991)l I 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)" 02350-90 D 715 - 86(1991)" D 1135-86(1991)" D 4487 - 90 D 126-87(1991)" D 185-84(1989)" D 1208 - 84 (1989)" D 283 - 84(1990)" D 3872 -86 (1991)" D 280 - 81 (1987) D 4358-84 (1990)" D 717-86(1991)" D 284-88 D 716-86(1991)" 0 3256 - 86(1991)" D 49-83(1990)" D 970-86(1991)" D 719-86 0 1844 - 86(199!)" D 1845- 86 (1991)" D2351-90 D 2352-85 (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 0 4450 - 85(1990)" D 444-88 Practice for: D 34-91 Guidefor: D 4139 -- 82 (1991)*1 Test Methods for: 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 Pigments Iron Oxides, Natural Red and Brown Iron Oxide, Synthetic Red Para, Pure lied Toner Red Lead Tohiidine, Pure Red Tpnef ' 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 V Mercuric Oxide Pigment, Chemical Analysis of Mica Pigment, Evaluating ' . ' . Phthalocyanine Blue and Green Pigments, Chemic'al' Analysis Of Red Lead, Chemical Analysis of - . ,r ^ 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 ofAnatasc to Rutile by X-Ray Diffraction Titanium Dioxide Slurries, Percent Solids in Tribasic Lead Phosphosilicate, Chemical Analysis df (Discontinued 1990t) -- Water-Soluble Saits in Pigments by Measuring the SpecifitResistance 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 ofj ;- Zinc Hydroxy Phosphite, Analysis of Zinc Yellow (2iinc Chromate), Chemical Analysis of White Pigments, Chemical Analysis of Volatile and Nonvolatile Content of Pigments, Determining General Physical Tests Glass Spheres, Roundness Glass Spheres, Sieve Analysis Oil Absorption of Pigments by Gardner-Coleman Method f Although this standard has been officially withdrawn from Society approval, a brief description is included for information only. XXV DUP050296518 Test Methodsfor: D 281-84(1989) 03360 - 80(1989) D 153-84(1989)" Practice for: D 1366-86 (1991)" Test Methodsfor: D 279-87(1991)" D 3022 - 84(1989)" D 387 - 86 D 2745-89 D 332-87(1991)" Specificationsfor: D 207-55(1987) D 784-83(1987) D 237-91 D 360-89 Guide for: D4277 - 83 (1988)" D4142-89 D4143-89 D 4368-89 Test Methodsfor: D1979 - 91 D 29-81(1987)" D 365-84(1989)" D 411 -83(1987) D 1650 - 91 D 1439 - 83a (1989)" D 509 - 70(1987) Practice for: D 2689 - 88 Test Methodsfor: D 1926-89 0 2455 - 89 D1726 - 90 01847 - 87 0 1652 - 90 0 1398 - 84 D 1615-60(1987) D2572-91 D 2690 - 89 D 1013-88 D4613-86(1990)" D 1312 - 56(1987)" D 4706-87 D 563-88 D 1306 -88 D 1396-73 (1987)" 0 3680 - 89 D 1469 - 73(1988)" 0 1542 - 60(1988)" D 3733-78 (1984)" D 1397-88 D 465 - 82 (1987f* D1063-51 (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 ofWhite Pigments, Relative, by Reflectance Measurements Tinting Strength ofWhite 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 PolyfVinyl 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) Aikyd Resins, Testing Resin Chemical Tests Carboxyl Content ofCellulose ' Carboxylic Adds in Aikyd 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 Pentaerythritoi in Alkyds Isocyanate Groups in Urethane Materials or Prepolymers Isophthalic Add in Aikyd 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 Aikyd 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(Vinyl Chloride) Resins, Compound$,and Copolymers by Solution Injection Technique Rosin Adds Content of Coating Vehicles, Total Rosin in Varnishes, Qualitative Detection Silicon Content ofSilicone Polymers and Silicone-Modified Alkyds by Atomic Absorption Unsapomfiable Matter in Alkyds, Vinyl Chloride Acid Number ofRosin (see Vol 06.03) Ash in Rosin (see Vol 06.03) Fatty Acids in Tall Oil Rosin (see Vol 06.03) xxyi DUP05Q296519 LIST BY SUBJECTS, VOLUME 06.02 Test Methodsfor: D 1064 - 58 (1981) D 464-91 D1065 - 82 Test Methodsfor: ' D 2090-88 D 1544-80(1989)" Iron in Rosin (see Vol 06.05) Saponification Number ofRosin (see Vol 06.03) Unsaponifiable Matter in Rosin (see Vol 06.03) Color Tests Clarity and Cleanness of Paint and Ink Liquids Color of Transparent Liquids (Gardner Color Scale) . Test Methodsfor: D 5097-90 ; D 4758 - 87 D 1259 -85 (1990)" D 4613 -86 D 4640 - 86 (1990)" D 4639-86 (1990)" D 2998-89 D 2456-91 0 3432 - 89 D 4827-88 D 4747-87 D 3008 - 90 28-67(1982)^ D 889 - 58(1987) Resin Physical Tests Filter-Retained Solids Content of Polymer Latexes Nonvolatile Content of Latexes Nonvolatile Content of Resin Solutions pH, Apparent, of Water-Insoluble Phenol-Formaldehyde Resins Phenol-Formaldehyde Resins, Determining Stroke Cure Time of Thermosetting Phenolic Resins Volatile Content Polyhydric Alcohols in Alkyd Resins, Determination of Polyhydric Alcohols in Alkyd Resins, Identification of Toluene Diisocyanates, Unreacted, in Thermosetting Urethane Prepolymers and Coating Solutions Using 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) Softening Point by Ring- and Ball-Apparatus (see Vol 06.03) Volatile Oil in Rosin (see Vol 06.03) Practice for: D4209 - 82 (1991)" Volatile and Nonvolatile Content of Cellulosics, Emulsions, Resin Solutions, Shellac, and Varnishes Test Methodsfori D3132~ 84(1990)" D 1198 - 88 D 269 - 52(1987f` Solubility and Miscibility Tests Solubility Range of Resins and Polymers Solvent Tolerance of Amine Resins Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark) (see Vol 06.03) Definitions Definitions cf Terms Relating to: D 804 - 79 (1987) Naval Stores and Related Products (see Vol 06.03) Test Methodsfor: 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)" D 3971 -89 D 4794 - 88 D 914 -72(1989)" D2364 -89 D 2363 -79(1989)" D 1795 -90 D4085 -81 (1987) D 3876 -79(1989)" D 1347 -72(1989)" 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 CELLULOSE AND CELLULOSE DERIVATIVES Alcohol-Benzene Soluble Matter in Cellulose (Intent to Withdraw) Ashing Cellulose ~ Carboxyl Content of Cellulose ----- Cellulose 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 in Cellulose Ethoxyl Substitution in Cellulose Ether Products by Gas Chromatography, Determination of Ethylceliulose 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 Cellulosic Materials by X-ray Fluorescence Viscosity of Cellulose Derivatives by Ball-Drop Method DUP050296520 LIST BY SUBJECTS, VOLUME 06.02 Terminology of: D 1695 - 77 (1989)fI Cellulose and Cellulose Derivatives POLYMERS Test Methodsfor: D 3536 -76(1988)" D 3593 -- 50 (1986fi1 Molecular Weight Averages and Molecular Weight Distribution by Liquid Exclusion Chromatography (Ge 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 (set Vol 08.03) Practices for: D 3750 - 79 (3985) D 2857 -87 D 4001 - 81 (I986)el Number-Average Molecular Weight of Polymers by Membrane Osmometry, Determination of (see Vo, 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 STANDARDS Specifications for: ' E 100 - 81(1986) E 1-90 E 133-86 E 11-87 ASTM Hydrometers (see Vol i4.03) ASTM Thermometers (see Vol 14.03) Distillation Equipment (see Vol 14.02) Wire-Cloih Sieves fir Testing Purposes (see Vols 04.01, 04.02,' 04.06, 05.05, and 14,02) Test Methodsfor: E 70-90 pH ofAqueous Solutions with the Glass Electrode (see Vol 15.05) Practicesfor: D5166-91 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 1S.QSK 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 ofSolids, Liquids, and Gases (see Vols 04.02 and 15.05) METRIC PRACTICE Practicefor: E 380 - 91 Use of the International System of Units (SI) (die Modernized Metric System) (Exoerpts) (see. Related Material section) DUP050296521 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 superscript epsilon (e) indicates an editorial change since ihe 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. 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 acid 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 of improving 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, commer cial, 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 nonspecific hydrophobic association similar to surfactants that elevate viscosity presumably by association between thickener particles 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. Dis c u s s io n --The deposition rale 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 uniformity 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 150F (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 of coatings 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 ofthe appearance of an object dependent upon the spectral composition of the incident light, the spectral reflectance or transmittance of the DUP050296522 # 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 ofpermanency. It may be applied to individual protective, decorative, or functional properties, for example, "the durability of gloss," but if used in a gepefal 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 windborne 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 gum. extended pigments--organic pigments diluted with an ex tender (for example, alumina trihydrate, bianc 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 (b) resist ignition when exposed to high temperatures, or (c) insulate a substrate to which it hqs 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 ofthe coating (see intumescent coating); (2) resist ignition of the substrate when exposed to .high tempera ture; or (i) insulate the substrate to which the coating is applied and thereby prolong the time required to reach its ignition, melting pc structural-weakening temperature. . flaking resistance (coatings)--rthe ability of a coating to resist the actual detachment Pf film fragments either from the previously applied coating or the substrate':'Flaking is generally preceded by cracking, checking,'of "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(65G). fossil resin--under resin, natural, see fossil resin: ' gallon, U. S---a volume equal to 231 in/Forpairit, varrtlsh, lacquer, and-related products this is measured at 77F (25*0. glaze--a very thin coating of a paint" product usually a semi-transparent coating tinted with Van Dyke birown, burnt sienna, ora similar pigment, applied on a previously painted surface to produce a decorative .effect, glazing 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 a gallon of paint, or pound of pigment, as used, can be uniformly spread to produce a specified contrast ratio (see 2 DUP050296523 D 16 contrast ratio). The term covering power has no specific relationship, to hiding power, and actually has no precise ! meaning. Awe--under color of an object, see hue. hydroxyl 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, Mg3Si4Oio (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 beipg 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 honasbestiform' 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 resihate-base liquid drier, lacquer-- & 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 resihs, 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, (A) the more modem' and far more exten sive type made by precipitating from solution various coal-tar colors by means of a 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. Dis c u s s io 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 (1 x 10~7 to 1 x 10-' m2 s"1) at 104F (40C) 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 IQ"3 to 25.00 St (1 x 10-7 to 25.00 x 10"4 m2 s"1) at 104*F (40C) or an equivalent viscosity at ah agreed upon temperature. Class B, high viscosity--a liquid having a viscosity of 25.01 to 1 x 103 St (25.01 X 10"4to 1 X 10"1 m2s~,)at 104F (40C) or an equivalent viscosity at an agreed upon temperature. mass color--the color, when viewed by reflected light, of a pigment-vehicfe mixture of such thickness as to obscure completely the background. Sometimes called over-tone or mass-tone. moss-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. mildewstat--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. liondrying 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 hot 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. DUP0S0296524 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 rt, 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. oil paint--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. Dis c u s s io n --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-like) state of drying, causing a tacky resistance to the brush or roller and resulting in an unsightly nonuniform appearance in the 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 oftwo 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 glazing compound. resin, natural--a solid organic substance, originating in the secretion of certain plants or insects, which is thermo plastic, flammable, nonconductive ofLelectricity; 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 front 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 acids 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 4 DUP050296525 ,, # D 16 p I exposure to humid atmosphere or chemical attack. See i white rust. liust resistance (coatings)--the ability of a coating to protect I the substrate of iron or its alloys from rusting, fcaturation--under color of an object, see saturation. Iscaling resistance {coatings)--See flaking resistance. Isealer--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, jshade--a term descriptive of alightness difference between j- surface colors, the other attributes of color being essenf tially constant. A lighter shade of a color is one that has i 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 dear 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 plaster 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 103 St (1 x 10~l m2s~')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 ofcoating 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 color of 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 polyisocyanate 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 HI, 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 5 DUP050296526 second package. This type has limited pot-life after the two 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 groups. Such coatings convert to solid films primarily by solvent evaporation. varnish--a liquid composition that is converted to a trans parent or translucent solid film after application as a thin layer. bituminous varnish--a dark-colored varnish containing bituminous ingredients. The varnish may be either of the oil or spirit type. oil varnish--a varnish that contains resin and drying oil as the basic film-forming ingredients and is converted to a solid film primarily by chemical reaction. spar varnish--a varnish for exterior surfaces. The name originated from its use on spars of ships. spirit varnish--a varnish that is converted to a solid film primarily by solvent evaporation, vehicle--the liquid portion of a paint or printing ink. Anything that is dissolved in the liquid portion of a paint or printing ink is a part of the vehicle. vemonla oil--a low-viscosity epoxidized drying oil from the 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. Dis c u s s io n --It flows easily even at temperatures below 0`C 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 ofa coating that remains as part of the dry film expressed as percent by volume. Dis c u s s io n --This contrasts'to another convention of expressing solids content by weight percent. Often a percent is given without specifying whether it is volume or weight. This is confusing and leads to errors in coating calculations. water paint--under paint, see water paint. wet adhesion--the ability of a coating film to adhere tightly to the substrate directly beneath it under wet conditions such as rain, dew, washing, etc. wet storage stain (coatings)--See white rust, white rust--white corrosion products (zinc hydroxide and zinc oxide) on zinc-coated articles. They form when the 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. See rust. zinc-rich primer--a primer for ferrous metals, incorporating zinc dust at a concentration sufficient to make the dried film electrically conductive thus providing cathodic pro tection to the ferrous substrate. ~ 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. Yourcomments 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 79103. DUP050296527 Designation: D 29 - 81 (Reapproved 1987)61 1 Standard Test Methods for Sampling and Testing Lac Resins1 This standard is issued under the fixed designation D 29; 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 approvedfor use by agencies of the Department 0/ Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year qfissue which has been adopted by the Department ofDefense. B' 61 Editorial changes were made throughout in October 1987. 1. Scope 1.1 These test methods cover procedures for sampling and testing orange shellac, button lac, garnet lac, and bleached lac. 1.2 The sampling procedures and test methods appear in the following order Sections Sampling; Orange Shellac, Button Lac, and Garnet Lac Bleached Lac Identification of Samples General Requirements for Test Methods; Reagents Source and Preparation of Portions ofSample for Tests Insoluble Matter Iodine Value Purity Volatile Matter (Moisture) Wax Matter Soluble in Water Ash Color Color of Orange Shellac Acid Value Orpiment Saponification Value 3 4 5 6 7 8 to 9.5 10 to 10.3 11 to 13.2 14 to 15.2 16 to 16.4 17 to 17.2 1* to 18.2 19 to 19.4.3 20 to 20.4.4 21 to 21.4 22 to 22.4 23 to 23.4 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. Specific hazard statements are given in Note 1. 2. Referenced Documents 2.1 ASTM Standards: D 304 Specification for -Butyl Alcohol (Butanol)2 D331 Specification for 2-Ethoxyethanol2 D1193 Specification for Reagent Water3 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method4 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 E 11 Specification for Wire-Cloth Sieves for Testing PurposesJ SAMPLING 3. Orange Shellac, Button Lac, and Garnet Lac 3.1 Lot Size--For the purpose of sampling, the quantity of a lot of any one of these types oflac resin shall not exceed 500 bags or packages. The net weight of fac resin in each bag or package shall not exceed 164 lb (75 kg). 3.2 Source and Number of Samples--Only original un opened bags or packages shall be sampled. Ten percent ofthe containers in every lot of lac resin shall be taken at random, but not less than 5 nor more than 25 cotitainers shall be taken. 3.3 Free-Flowing Lac Resins--In sampling free-flowing lac resins, samples shall be drawn from different places in each container in double handfuls or by means of a suitable sampler.6 A total of approximately 6 lb (2.7 kg) shall be taken. ~ 3.4 Blocked or Matted Lac Resin--Pieces of blocked or matted lac read shall be chipped with an axe, pipk, or other suitable instrument from each container taken for sampjing. Approximately the same amount shall be taken from each container and the total amount taken shall be about 6 lb (2.7 kg). The pieces of lac resin shall then be ground.to pass a No. 4 (4.75-mm) sieve. 3.5 Preparation ofSamples for Observation or Analysis-- Whether free-flowing or rough ground, as in the case of blocked lac resin, the entire sample representing any lot shall be thoroughly mixed and divided into halves. The use of a mechanical mixer7 is recommended for mixing the resin and a riffle sampler* for dividing it into quarters. When these devices are not available for use, the entire sample shall be 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 D 01.33 on Varnish and Resins, Including Shellac. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 29 - 14 T. Last previous edition D 29 - 73. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vols 06.01, 06.02 and 06.03. s Annual Book ofASTM Standards,, Vol 14.02. 6 A grain sampler (Catalog No. 14-208) by the Fisher Scientific Co., 635 Greenwich St, New York, NY 10014, has been found satisfactory for this purpose. 7 The MacLellan mixer available from the Anglo-American Mill Corp., 75-1000 Kennaday St., Owensboro, KY, has been found satisfactory for this purpose. 8 The Jones sampler (Catalog No. 4-941) available from the Fisher Scientific Co., 635 Greenwich St., New York, NY 10014, has been found satisfactory for this purpose. DUP050296528 # D29 mixed, heaped, and quartered along two diameters that intersect at right angles and the opposite quarters combined. One half the sample, thus obtained, shall then be mixed and divided into quarters as before. Each quarter shall be placed in an airtight container, sealed, labeled (Section 5), and sent' to the interested parties as the "original observation sample." When agreed upon between the seller and the purchaser, the "original observation sample" shall be used for the determi nation of volatile matter (moisture) (Sections 14 to 15, as applicable). The other half of the sample shall be ground to pass a No. 10 (2.00-mm) sieve,3 mixed thoroughly, and divided into two equal portions A and B. Portion A shall be labeled the "reserve sample." Portion B shall then be ground to pass a No. 25 (710-pm) sieve,5 mixed thoroughly, and quartered as described above. Each quartet shall be packaged in an airtight container, sealed, labeled "prepared sample," and sent to the testing laboratory for analysis. 4. Bleached Lac 4.1 Lot Size--For the puipose of sampling, the quantity of a lot shall not exceed 200 packages. 4.2 Source and Number of Samples--Only original un opened packages shall be sampled. Twenty percent of the containers in every lot shall be taken at random, but not less than two containers in any lot shall be taken, except in the case where the entire lot is packaged in a single container. 4.3 Dry Bleached Lac (Free-Flowing)--Samples shall be drawn with a scoop or suitable sampler4 from different parts of each container directly after the packages are opened or bored. Approximately 1 lb (450 g) shall be drawn from each container. The samples shall be combined; mixed thor oughly, and where larger than 3 lb (1.4 kg), shall be reduced by quartering as prescribed in 3.5 to a sample of this size. 4.4 Dry Bleached Lac .{Blocked or Matted)--Samples aggregating at least 1 lb (450 g) shall be chopped or chiseled from different parts ofeach container. The composite sample from all the containers shall be quickly crushed to lumps about 1 in. (25 mm) square or smaller. The crushed lac resin shall be well mixed and where the amount is larger than 3 lb (1.4 kg), it shall be reduced by quartering, as prescribed in 3.5, to a sample of approximately this size. 4.5 Hanks, Bars, or Crushed Free-Ground Bleached Lac--This material, which generally contains approximately 25 % moisture, shall be sampled by the procedures described in 4.3 or 4.4, as applicable. 4.6 Preparation of Samplerfor Analysis--The composite sample obtained as described in 4.3 or 4.4 shall be mixed thoroughly and divided into two equal portions A and B as prescribed in 3.5. Each portion shall be placed in a clean, dry glass jar provided with a rubber-sealed cap or an airtight friction-top tin can. Portion A shall be labeled "reserve sample." Portion B obtained in accordance with 4.3 or 4.4 shall be further ground to pass a No. 20 (850-p.m) sieve,5 thoroughly mixed and replaced in the jar, sealed and labeled "prepared sample." Portion B obtained in accordance with 4.5 shall be further ground to pass a No. 10 (2.00-mm) sieve,5 thoroughly mixed, replaced in the jar, sealed, labeled "prepared sample," and sent to the laboratory for analysis. 5. Identification of Samples 5.1 The following information shall be legibly placed on the label, which shall be securely attached to each sample container: date of the sampling, number of bags, barrels or packages sampled, total number of containers in the lot, condition of the containers and their contents, manufactur er's name, lot and code numbers of the containers, and the purpose identification, namely "original observation sample" or "sample for determination of volatile matter (moisture)", "reserve sample" or "prepared sample" as may apply. TEST METHODS 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 American Chemical Society, where such specifications are available.9 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. 7. Source and Preparation of Specimens for Tests 7.1 Each portion of sample for iise in a given test shall be taken from the sample of lac resin only after it has been mixed, either by rolling on paper or by rolling and tumbling in its airtight container, as the condition of the sample requires, a sufficient number oftimes to ensure uniformity of the specimen taken. The test specimens shall be taken from the "prepared sample" (3.5 or 4.6), as received, except in the following cases: 7.1.1 When it has been previously agreed upon between the seller and the purchaser that the "original observation sample" shall be used for the determination of volatile matter (moisture). In this case, the "original observation sample" shall be mixed, quartered, ground, and sieved, in accordance with the procedure described in 3.5.for.obtaining the "prepared sample." All operations, shall be done- as expeditiously as possible and the test specimen taken imme diately after thesieved sample has been thoroughly mixed, to avoid any possible loss by evaporation. ,, 7.1.2 When the "prepared sample" is known to have a high moisture content, as in the case of certain forms of bleached lac (4.5), it shall be dried to a moisture, content of 6 % before the test specimens are taken. The lac resin shall be dried, by placing it in a thin layer in a flat-bottom dish (loosely covered to prevent dust contamination) and ex posing it to the atmosphere at room temperature for 24 h and then desiccating it over anhydrous calcium chloride. The partially dried lac resin shall be kept in a clean, dry, airtight container, and shall be thoroughly mixed by rolling and tumbling in the container before the specimens are taken for analysis. 9 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." 8 DUP050296529 #0 29 Weighing Bottle -dOStmm. iSHmm. l Extraction Cartrufag 3BtO.Smm.inside diam. ; Stales3mm.dim. Siphon Tube _5iHmm. -SO i/mm. StoiSmm.'jrsididiom. JSi/mm. mb's diam. FIG. 1 k 7it 1.5mm. F ~outside diam. A_0 Extraction Apparatus for Insoluble Matter, Test Method A INSOLUBLE MATTER 8. Test Method A--For Orange Shellac, Button Lac, Garnet Lac, and Regular Bleached 8.1 Apparatus: 8.1.1 Condenser--A four-bulb Allihn condenser of the dimensions and design shown in Fig. 1. 8.1.2 Siphon Tube--A Knoefler siphon tube of the di mensions shown in Fig. 1. 8.1.3 Filter Tube--A carbon filter tube of the dimensions shown in Fig. 1. 8.1.4 Flask--A borosilicate glass Erienmeyer flask 176 3 mm in height and 48 1.5 mm in inside diameter at the top. 8.1.5 Flask Support--A suitable ring support with an iron damp and a Nichrome or iron wire gauze square without an asbestos center. 8.1.6 Extraction Thimble--Extraction thimble 26 1 mm in diameter and 60 I mm in height10 8.1.7 Water Bath--A metal container with cover of the size and design shown in Fig. 2. The container and cover shall be made of 26-oz copper sheet. The cover shall have a flanged hole 57 1 mm in diameter for a 200-mL beaker and also a hole 35 1 mm in diameter for the carbon filter tube. Directly below this hole in die bottom of the container shall be a flanged hole 25 1 mm in diameter. 8.1.8 Heating Device--An electric hot plate or bunsen burner equipped with a draft shield. 8.1.9 Weighing Bottle--A glass-stoppered weighing bottle of the dimensions shown in Fig. 1. 8.2 Solvent--Specially denatured 95 % (190 proof) ethyl alcohol conforming to Formula No. 1 or No. 3A of the 10 No, 603 extraction thimbles, or equivalent, available from Schleicher & Schuell, 10 Optical Ave., Keene, NH 03431, have been found satisfactory for this purpose. r l*'vtL 35lmm. |---- 1 insidedim. 1 i! it ,, , k,, 1 5' 1 *......... -- t t i *25tmm.inside diam. 9 i [J s Ato 6 rubber stopper 1 FIG. 2 Hot-Water Bath for Insoluble Matter, Test Method A Alcohol, Tobacco and Firearms Division of Internal Rev enue Service, U.S. Treasury Department. Precautions--The reagents and samples used in these methods may, under some conditions, be hazardous. Refer to the supplier's Material Safety Data Sheet for specific handling and safety precautions. Safe laboratory handling procedures and all applicable OSHA regulations are to be followed. 8.3 Preparation ofExtraction Thimble: 8.3.1 Pass the stem of the condenser through a hole cut in the center of a cork stopper of such size that it will tightly fit the flask. Adjust the cork on the stem so that the bottom of the cork is just above the holes in the stem. Place an extraction thimble (use new thimbles only) in the siphon tube. Suspend the siphon tube from tire stem of the condenser by passing a piece of copper wire through the holes in the stem and fastening the ends of the wire through the holes in the siphon tube. The wire shall be sufficiently long to leave about 6-mm space between the tip of the condenser and the top of the siphon tube. 8.3.2 Place 125 mL ofethyl alcohol in the flask and attach the flask to the condenser by means of the cork stopper. Place the flask on an electric hot plate or a flask support. Run a steady stream of cold water through the condenser. Adjust the flame ofthe burner or the hot plate setting so as to give a cycle of filling and emptying of the siphon tube every 2 min, and extract the thimble for 30 min. Remove the extraction thimble from the siphon tube and allow to drain and air-dry for several minutes. - -- , 8.3.3 Placedhe thimble in a weighing bottle and dry in an oven for 2 h at 105 2C. Remove and stopper the weighing bottle and cool in a desiccator. Weigh the bqttle and thimble lifting the stopper momentarily before weighing. Continue drying and weighing as before after each hour of drying until the loss in weight between successive weighings does not exceed 2 mg. 8.3.4 A number of thimbles may be extracted and kept in weighing bottles or a desiccator until needed. 8.4. Procedure: 8.4.1 Weigh to 1 mg 5 0.2 g of the mixed sample (Section 7) and place in a 200-mL taE-form beaker. Add 125 mL of ethyl alcohol to the beaker and place it in the hot-water bath (Fig. 2), which has been previously heated to not less than 90C. Maintain the bath at this temperature, or above, during the solution and filtration of the sample. Boil the solution for 30 min, keeping the volume of alcohol constant to ensure complete solution of the lac resin. 8.4.2 Place an extracted, weighed extraction thimble (8.3) in the carbon filter tube (Fig. 2). Wet the thimble with hot 9 DU P050296530 FIG. 3 Apparatus for Insoluble Matter, Test Method B alcohol and decant the boiling solution into the warm thimble until the beaker is nearly empty. Wash the re maining solution and insoluble matter into the thimble with a stream of hot alcohol from a wash bottle using a "po liceman" if necessary. Finally, wash the thimble from,the top down. The transfer of the insoluble matter from the beaker and the washing down of the thimble will require at least 75 mL of hot alcohol. 8.4.3 Transfer the thimble with the insoluble matter to the siphon tube of the extraction apparatus (Fig. 1). Place 125 mL of alcohol in the flask and attack the condenser. Adjust the heating device so that a complete filling and emptying of the siphon tube with hot alcohol requires 2 min or 30 cycles per hour (Note 2), and extract for exactly 1 h (Note 3). Remove the thimble, and allow it to drain in an upright position. No t e 2--Occasionally, lac resins are encountered that will not yield: the required 30 siphons per hour due to slow filtration. In these instances the extraction shall be continued until 30 cycles have occurred and the determination reported as abnormal or stow filtering. No t e 3--During the 1-h extraction, all the remaining soluble matter should be extracted by the hot aicohol, leaving only the insoluble matter in the thimble. 8.4.4 Place the thimble in the weighed weighing bottle and dry in an oven at 105 TC for 2 h. Remove the weighing bottle front the oven, insert its stopper, cool in a desiccator, and weigh, lifting the stopper momentarily to break the vacuum before weighing. Continue drying and weighing as before after each hour of heating until the loss in weight between successive weighings does not exceed 2 mg. 8.5 Calculation--Calculate the percent of matter insol uble in hot alcohol as follows: Insoluble matter, % -- [RIS{\ -- M)\ x 100 where: R = insoluble matter obtained, g, 5 = sample used, g, and M = volatile matter (moisture) content of the sample, ex pressed as a decimal fraction. 9.Test Method B--For All Grades of Lac Resins Including Refined Bleached Lac11 9.1 Apparatus (Fig. 3): 9.1.1 Crucible--A borosilicate glass Gooch crucible having a capacity of 30 mL with a fritted-glass filter disk having a medium porosity. 9.1.2 Filter Tube--A carbon filter tube made of borosili cate to fit the crucible. 9.1.3 Heating Coil--A heating coil made of 3-mm diam eter copper tubing of such size and shape that the filter crucible and the large part of the carbon tube will fit snugly within it. The outside shall be insulated with sheet asbestos paper. 9.2 Solvent--Either of the following materials may be used as the solvent for the lac resin: 9.2.1 2-Ethoxyethanol, conforming to the requirements of Specification D 331. 9.2.2 Normal Butyl Alcohol {n-Butanol), conforming to the requirements of Specification D 304. 9.3 Preparation of'FilteringJJnit 9.3.1 Cut a disk of rapid, ashless filter paper to fit inside the crucible and place it on top of the glass filter. Introduce upon the filter paper, in the customary manner, an asbestos mat approximately 3 mm in thickness. Dry the crucible at 105 2C; then cool in a desiccator to constant weight. Weigh the prepared crucible and place it within the carbon tube, using thin rubber tubing to form an airtight connec tion. Place the combined filtering unit within the heating unit, attach to a suction flask, and pass a current of steam through the coil. .^ 9.4 Procedure: 9.4.1 Weigh to 1 mg 5 0.2 ofthe mixed sample (Section 7 and Note 4) into' a 200-mL beaker. Add 75 mL of the solvent (9.2) and bring the solution to boiling on an electric hot plate. Keep the solution boiling slowly for 5 min to ensure complete solution. No t e 4--For refined bleached shellac and other shellacs having a very low insoluble matter content take a 10 to 2Qrg specimen using proportionally more solvent , ___. ,, v about 10 mL of the bofling solvent from a wash, bottle into the heated crucible. Gently apply suction and immediately pour the boiling solution Into the crucible so as to retain as much as possible of the insoluble residue in the beaker. Wash the insoluble residue successively with three 20-mL portions of the solvent, boiling the solution oh. the electric hot plate for about ! min before each filtration. 9.4.3 Transfer the residue from the beaker, to the crucible. with a stream of the boiling solvent from a wash bottle, using a policeman when necessary. Wash down the inner walls of the crucible with the boiling solvent. The total volume ofthe solvent used will be approximately 175 mL. It is advisable to keep the crucible covered with a small watch glass at all times, except when actually transferring the solution from the beaker to crucible, or when washing down the inside walls of the crucible to maintain a higher temperature within the crucible. Allow the crucible to remain inside the heating 11 Hartman, C. C., "Determination of Insoluble Matter in Shellac," Journal of Research, Nat. Bureau Standards, Vol 7, No. 6, 1931, p. 1105. 10 wm DUP050296531 Isoil with the suction on for a few minutes, so as to suck it as dry as possible. No t e 5--The insoluble matter can be easily removed together with the asbestos mat and filler paper. The crucible may be used several times without further cleaning. Additional cleaning when necessary is easily accomplished by.immersing the crucible in a hot mixture ofsulfuric and nitric adds for a few minutes. 9.4.4 Remove the crucible and wash the outside with boiling solvent. Dry in an oven at 105 2C for 2 h, cool in ifdesiccator, and weigh. ^ 9.5 Calculation--Calculate the percent of matter insolpjfe in the hot solvent as follows; . . Insoluble,' % = [R/S(l - M)\x. 100 where: r 1 R = insoluble matter obtained, g, S'= sample used, g, and M= volatile matter (moisture) content of the sample, ex pressed as a decimal fraction. 10.Iodine Value 10.1 Reagents: 10.1.1 Potassium Iodide Solution (100 g/L)--Dissolve 10 g of iodate-free potassium iodide (KI) in water and dilute to 100 mL. 10.1.2 Reference Standard Shellac--Pure shellac of known iodine value.12 10.1.3 Sodium; Thiosulfate, Standard Solution (0,1 N)-- Prepare and standardize in accordance with Section 5 of Method D 1959. IQ. 1.4 Starch Indicator Solution--Prepare in accordance . with Test Method D 1959. 10.1.5 Wijs Solution--Prepare in accordance with Test Method D 1959. The Wijs solution should be tested against an orange shellac the-iodine value of which is accurately known." The iodine value thus obtained should be within 0.5 of the known iodine value; > 10,2Procedure: 1Q.2.1 Weigh to 0.1 mg about 0.2 g of the mixed sample (Section 7 and Notes. 6 and 7) intp a 250.-mL dry, clear glass. bottle having a ground-glass stopper. Add 20 . mL of glacial acetic acid and heat at 65 to 70C on a hot-water bath, gently swirling the contents of the bottle occasionally, until solution is complete, except for the ^ax. This should not require more than 15 min. Add 10 mL of chloroform and cool at 21.5 to 22.5C for xh h in an insulated, thermostatically controlled water bath. No t e 6--In the case of grossly adulterated samples, a smaller quantity (0.15 or 0.1 g) should be used instead of0,2 g of the material in order that the excess of iodine monochloride may not be too greatly reduced, since the excess of halogen is one of the factors in determining the amount of absorption. In case less than 25 mL of the Na2S203 solution is required, another test should be made using a smaller quantity of the lac resin. No t e 7--In weighing lac resin some difficulty is at times experienced on account of its electrical resistance properties. In very dry weather it may be found that the necessary handling to prepare it for weighing has electrostatically charged it, and that it may be necessary to leave it in the balance pan at rest for a few minutes before determining the weight. No t e 8--If a number of samples are being run, allow at least 5 min between the additions of the Wijs solution. il0.2.2 Add 20 mL ofthe Wijs solution to the bottle, using a pipet. Replace the stopper and half immerse the bottle in the water bath held from 21.5 to 22.5C for exactly 1 h (Note 8). Gently swirl the contents ofthe bottle occasionally during the hour. Remove the bottle from the bath and add 10 mL of the KI solution washing into the bottle any Wijs solution on the stopper with tiie same. , ,, . 10.2.3 Immediately titrate with the standard Na2Sj03 solution, allowing the solution, to run rapidly and swirling the contents, of- the bottle .vigorously and continuously until the solution becomes a straw color. Add 5 mL of the starch indicator solution and continue the titration dropwise until the blue colorjust disappears. The end point is sharp and any blue color returning after 30 s should be disregarded. 10.2.4 Blank--Run a blank determination on the re agents at the same time and through the entire procedure. The blank is necessary because of the effect of temperature changes on volume and possible loss in strength of the Wijs solution. 10.2.5 Reference, Standard--Run a determination on a sample of pure shellac of known iodine value (10.1.2) with each set of test specimens. 10.3 Calculation--Calculate the iodine value as follows:, . Iodine value- [(5 -r)N* 12.69]/S where: ,, V = Na2S20j solution required for titration of the spec imen,.mL, '' B = Na2S2G3 solution required for titration of the blank, mL, , N = normality of the Na2S203 solution, and S = sample used, g. PURITY 11. Qualitative Test for Rosin 11.1 Reagents; " 11.1.1 AbeticAcid (Glacial). 11.1.2 Ethyl Alcohol {Absolute). 11.1.3 Halphen-Hicks Reagent13--Prepare^the following two solutions: 11.1.3.1 Solution A--One part by volume-of phenol dissolved in 2 parts by volume of carbon tetrachloride. 11.1.3.2 Solution B--One part by volume of bromine dissolved in 4 parts by volume of carbon tetrachloride. 11.2 Procedure: . 11.2.1 Weigh 2 0.1 g of the mixed sample (Section 7) into a 2-L Florence flask and dissolve in 20. mL of either absolute ethyl alcohol or glacial acetic acid, warming on'a steam bath if necessary. Cool, add 100 mL of petroleum ether, and mix thoroughly. 11.2.2 Add sufficient water to bring the petroleum ether layer into the neck of the flask when separated. Add the water portionwise, shaking the flask between additions to 13 Standard samples of pure orange shellac, rosin-free of accurately known iodine number'may be purchased from the Secretary ofthe U. S. Shellac Importers Assn., Inc., 425 Park Ave., New York, NY 10022. 13 For more detailed information, reference may be made to Hicks, E. F., "New Color Reactions for Some of the Resins with Halphen's Reagent for Colophony," Industrial and Engineering Chemistry, Vol 3. 1911, p. 86. 11 mmm DU P050296532 i D 29 prevent coagulation of the precipitated lac resin. Allow to stand until the petroleum ether separates into a distinct layer. 11.2.3 Siphon off at least 50 mL of the petroleum ether solution, filter if cloudy, and heat on an electric hot plate or steam bath until the petroleum ether is completely removed. 11.2.4 Dissolve the residue in several millilitres of Solu tion A, and transfer 1 to 2 mL of the mixture to one of the cavities of a white porcelain spot plate. Immediately fill an adjacent cavity with Solution B. Cover the plate with an inverted watch glass and note the color developed in the Solution A mixture by the bromine vapors from Solution B. The development of a fugitive violet color, best observed on the flat portion of the spot plate, indicates the presence of rosin. A control sample containing rosin should be run simultaneously, as a guide in judging the color developed with the test specimen. 12. Qualitative Test for Copal 12.4 Reagents: 12.1.1 Ethyl Alcohol, Denatured--{See 8.2). 12.1.2 Methyl Alcohol {99 %). 12.2 Procedure: 12.2.1* Weigh to 0.1 g about 15 g of the mixed sample (Section 7) into an Erlenmeyer flask. Add twice its weight of the denatured alcohol, stopper the flask and let stand with periodic shaking until the sample is in the solution. Filter the solution through a folded filter paper, discarding the first 5 mL of filtrate. 12.22 Transfer 10 mL of the filtrate to a large test tube (6 by 3A in.) (150 by 20 mm) and nearly fill the tube with methyl, alcohol. Stopper the tube and mix its contents thoroughly. Immediate formation of a cloudiness or precipi tate indicates the presence of copal. Lac resin free of copal should remain clear. 13. Estimation of Adulteration 13.1 Since the variation between the highest and lowest iodine values of a pure lac resin is not great, it is recom mended that the following assumptions (Note 9) be made: Type of Lac Resin Assumed Iodine Value Rosin-free and copal-free shellac, button lac, and garnet lac Rosin-free and copal-free bleached lac* Roan Copal 15 10 228 130 13.2 Calculate the percent of adulteration as follows: Percent of rosin in orange shellac, button lac, and garnet lac = [(x - 15)/(228 - 15)] x 100 Percent of rosin in bleached lac = [(x -- l0)/(228 - 10)] x 100 Percent of copal in orange shellac, button lac, and garnet lac = [(x - 15)/(130 - 15)] X 100 Percent of copal in bleached lac = [(x - 10)/(130 - 10)] x 100 where: x = iodine value of the sample under test, determined in accordance with Section 10.2. No t e 9--The results obtained by assuming the values of 15 and 10 as the iodine value of orange and bleached shellac, respectively, and 228 as the iodine value ofrosiu may give a slightly lower percent rosin, under some circumstances, than that which is actually present. VOLATILE MATTER (MOISTURE) 14. Test Method A--For Orange Shellac, Button Lac, Garnet Lac, and Dry Bleached Lac 14.1 Procedure: 14.1.1 Weigh to 0.1 mg approximately 2 g of the mixed sample from the air-tight container (7.1.1 or 7.1.2) into a weighed, clean, dry, flat-bottom glass dish about 4 in. (100 mm) in diameter and provided with a ground-glass cover. Place the dish, with the cover removed, in a well-ventilated oven maintained at 40 10C for 6 h. 14.1.2 Transfer the dish and cover to a vacuum desiccator containing concentrated sulfuric add (H2S04, sp gr 1.84). Immediately evacuate the desiccator and keep the spedmen uncovered in the vacuum for 18 h. Release the vacuum, replace the cover on the dish, and weigh immediately. 14.2 Calculation--Calculate the percent volatile matter (moisture) in the sample as follows: Volatile matter (moisture), % = [1 - (S^S,)] x 100 where: Sx = sample used, g, and S2 = dried specimen, g. 15. Test Method B--For Bleached Lac in Form of Hanks, Bars, and Crushed Fresh-Ground 15.1 Procedure: 15.1.1 Thoroughly mix the "original observation" sample in its original airtight container by rolling and tumbling. Transfer 25 to 50 g to a mortar and crush as rapidly as possible into fine granules. Keep the mortar-covered as wellas possible to avoid any loss of moisture. Immediately transfer approximately 10 g of the crushed lac to a wdghed, dean, dry, flat-bottom glass dish about 4 in. (100 mm) in diameter, provided with a ground-glass cover, and weigh to 0.1 mg. Record the weight of the lac taken for use as S,. 15.1.2 Place the dish and contents in a vacuum desiccator containing H2S04 (sp gr 1.84). Remove the cover from the dish and immediately evacuate the desiccator. Keep the dish in the vacuum at room temperature fox 18 to 24 h. Replace the cover on the dish, remove from the-desiccator, and weigh. Recorifthe weight of the partially dried lac for use as S . 15.1.3 Grind the partially dried lac resin until it entirely-, passes a No. 40 (425-pm) sieve.5 Thoroughly mix the sieved lac on a mixing sheet (7.1). Transfer approximately a 2-g spedmen of it from the mixing sheet to a weighed, covered dish of the type described in 15.1.1, and weigh to 0.1 mg. Record the weight of the spedmen taken for use as S3. 15.1.4 Heat the dish with cover removed in a wellventilated oven at 40 1C for 18 h. Replace the cover on the dish, cool in a desiccator, and weigh. Record the weight of dried lac obtained for use as fi*. 15.2 Calculation--Calculate the percent of volatile matter (moisture) in the original lac sample as follows: Volatile matter (moisture), % = [1 - (S4 x S2)/(S} x S',)] x 100 where: 5, = crushed wet lac taken for drying in vacuum, g, (15.1.1) 52 = partially dried lac, g, (15.1.2), 53 -- partially dried, sieved lac used as spedmen for final oven diying, g, (15.1.3), and 12 DUP050296533 D 29 S4 = completely dried lac specimen obtained in 15.1.4, g. 16. Wax 16.1 Apparatus: 16.1.1 Extraction Apparatus--An assembly suitable for continuous extraction with hot solvent, such as that used for the determination of insoluble matter (Section 8). 16.1.2 Filtering Medium--A Buchner funnel, having an inside diameter of 2`A to 3Vi in. (55 to 90 mm), and prepared just before use in the following manner. Fit a disk of filter paper snugly over the bottom of the funnel and then with the suction on pour over the filter paper in a layer of uniform thickness 1 g of filter aid (16.2.3) suspended in water. 16.1.3 Extraction Thimble--A thimble, such as pre` scribed in 8.1.6, that has been previously extracted with chloroform by the procedure given in 8.3. 16.2 Reagents: 16.2.1 Chloroform, redistilled, free of nonvolatile residue. 16.2.2 Ethyl Alcohol, Denatured, as prescribed in 8.2. 16.2.3 Filter Aid14--A suitable filter aid, extracted with chloroform and dried before using. 16.2.4 Sodium Carbonate (Na2C03). 16.3 Procedure: 16.3.1 Weigh to 1 mg approximately 10 g of the mixed sample (Section 7) into a 200-mL tail-form beaker. Dissolve 2.5 g of Na2C03 in 150 mL of hot water and add to the beaker. Immerse the beaker in a boiling water bath and stir until the lac resin is in solution. Cover the beaker with a watch glass and allow to remain in the bath for 2 to 3 h, without agitation. 16.3.2 Remove the beaker from the bath and place it in cold water. The wax will come to the top of the solution where it will solidify as a layer or float as small, hard particles. Add 0.5 g of the filter aid to the lac solution and filter through the Buchner funnel with the aid of suction. Transfer all of the wax from the beaker to. the filter with a stream of water from a wash bottle, using a policeman if necessary. Finally pour a few millilitres of the alcohol over the filter to facilitate drying. Place the funnel in an oven and dry its contents at 60 2"C for several hours. 16.3.3 Insert a thin spatula under the edge of the filter paper and transfer the contents of the funnel to a sheet of filter paper. Securely wrap the transferred material in the filter paper, and bind it firmfy with fine copper wire. Place the packet in the prepared extraction thimble. Wash out both the beaker in which the lac resin was originally dissolved and the Buchner funnel with portions of hot chloroform, filtering the chloroform solutions through the extraction thimble into the flask to be used in the extraction. Place the thimble in the extraction apparatus, and extract with hot chloroform for 2 h. 16.3.4 Transfer the chloroform extract to a weighed beaker and heat on a steam-bath until most of the chloro form has been evaporated. Finally heat the residue in the beaker in an oven at 105 + 2'C to constant weight (within 10 mg). Cool in a desiccator and weigh.14 14 A diatomaceous silica such as Filter-Cel, tradename of Marivilie Corp., Filtration and Minerals Div., 137 W. Central Ave., Lompoc, CA 93436, has been found satisfactory for this purpose. 16.4 Calculation--Calculate the percent of wax in the lac resin as follows: Wax, % = IR/S{I - M)\ x 100 where: R = wax obtained, g, S= sample used, g, and M = volatile matter (moisture) content of the sample, ex pressed as a decimal fraction. 17. Matter Soluble in Water 17.1 Procedure: 17.1.1 Weigh to 0.1 g 10 g of the mixed sample (Section 7) into a 400-mL beaker. Add 200 'mL of water and stir thoroughly. Cover the beaker with a watch glass and let stand with occasional stirring for 4 h at 25 2C. 17.1.2 Filter the water solution through a filter paper into a 400-mL beaker. Transfer all the lab resin from the beaker to the filter paper with a stream of water from a wash'bottle using a policeman if necessary. Finally wash the lac resin and filter paper with approximately 100 mL of water. 17.1.3 Evaporate the filtrate almost to dryness in a weighed evaporating dish on a steam bath. Dry the extracted residue for i-h periods in an oven maintained at 105 2C until the difference in successive weighings does not exceed 1 mg. Cool in a desiccator and weigh. 17.2 Calculation--Calculate the percent of matter soluble in Water as follows: Matter soluble in water, % = (R/S(l - M)] x 100 where: R = residue obtained, g, S = sample used, g, and M= volatile matter (moisture) content of the sample, ex pressed as a decimal fraction. 18. Ash 18.1 Procedure: 18.1.1 Weigh to 1 mg between 3 and 5 g of the mixed sample (Section 7) into a weighed porcelain crucible. Place the crucible in a hood and heat with a-low flame until-the contents ofthecrucible are a dry, charred mass. Transfer to a muffle furnace and ignite the residue at a dull red heat (not exceeding 600"C) until the ash is free of carbon. Cool in a desiccator and weigh. Repeat , the ignition, cooling and ' weighing until the difference between successive weighings does not exceed 1 mg. 18.1.2 If a carbon-free ash cannot be obtained in this manner, add water to the crucible, bring the water to a slow boil and digest the ash for 5 to 10 min. Filter through an ashless filter paper, washing out the crucible with a stream of hot water from a wash bottle using a policeman if necessary. Retain the filtrate. Transfer the filter paper with die insoluble residue to the crucible and ignite at a dull red heat in a muffle furnace until all the carbon is consumed. Then add the filtrate to the crucible and evaporate to dryness over a low flame or hot plate. Finally ignite the crucible and its contents at dull red heat to constant weight (within I mg) as prescribed in 18.1.1. 18.2 Calculation--Calculate the percent ash of the lac resin as follows: Ash, % = [R/S(l - AO] x 100 13 DUP050296534 D 29 where: R = ash obtained, g, 5 = sample used, g, and M = volatile of matter (moisture) content of the sample, expressed as a decimal fraction. 19. Color 19.1 Apparatus: 19.1.1 Glass Tubes--Clear glass tubes with closed, flat, even bottom, an external length of approximately 114 mm, and a uniform internal diameter of 10.65 0.025 mm throughout the length of the tube. Viscosity tubes described in Test Method D 1545 are satisfactory. 19.1.2 Glass Plate--White Carrara or Vitrolite glass plate approximately 6 by 8 in., (150 by 200 mm), one side of which has been polished to a smooth, high gloss surface. 19.1.3 Film Applicator--Film applicator to case a film 2 in. (50 mm) wide and 2 mils (50 pm) thick. A clearance of 4 mils should provide the required thickness. 19.2 Reagent--Ethyl Alcohol, Denatured, as prescribed in 8.2. 19.3 Color Comparison Material--The lac resin mutually agreed upon by the purchaser and the seller for the color comparison. 19.4 Procedure: 19.4.1 Weigh 10 . 0.1 g each of the mixed sample (Section 7) and the comparison lac resin, which shall have been similarly prepared, into separate Erlenmeyer flasks. Add to each flask an amount of alcohol equal to twice the weight of the resin and stopper the flasks. Keep the flasks at 21 to 32C and shake at frequent intervals until the resins are completely dissolved (cut). Allow the flasks to stand undis turbed for xh h. Compare the color of the lac solutions by one or both of the following procedures as agreed upon by the purchaser and the seller. 19.4.2 Comparison ofSolutions--Fill separate glass tubes to their bottom lines with each of the solutions, being careful not to disturb any settlement that may have occurred in either flask. Place the tubes side by side and make the color comparison by viewing the liquids while they are held against a background substantially equal in illumination to that of a fairly light overcast northern sky. 19.4.3 Comparison of Films--Without disturbing any settlement that may have occurred in the flask, decant a suitable portion ofthe solution ofthe sample and draw down on the white glass plate with a film, 2-in. (50-mm) wide and 2 mils (50 pm) thick, using the apparatus described in 19.1.3. In a similar manner, draw down a film of the comparison solution on the same plate keeping the films as close together as possible. Air-dry the films at 21 to 32C for 24 h. Compare the color of the dried films by viewing them by reflected light at an illumination substantially equal to that of a fairly overcast northern sky.20 20. Color of Orange Shellac 20.1 Apparatus: 20.1.1 Funnel--Porcelain No. 1 Buchner funnel 55 mm in inside diameter. 20.1.2 Colorimetric Tubes--Nessler color comparison 20.1.3 Standard Light Source--A light source consisting of a 100-W frosted daylight bulb mounted at the center of the back wall of a 10-in. (255-mm) cubic box so that the tip of the bulb faces the front. The front opening of the box shall be covered with a white opaque paper or a ground-glass plate. The lamp shall be inserted in a socket which just protrudes through the wall of the box so that the distance from the tip of the lamp to the paper or glass is approxi mately 4.5 in. (115 mm). The five inside walls of the box shall be painted white. Any other suitable apparatus or standard daylight lamp may be used, provided it produces light of the same characteristics as specified above. 20.2 Reagents: 20.2.1 Ethyl Alcohol--Specially denatured 95 % (190 proof) ethyl alcohol;, either formula No. 1 or formula No. 30 of the U.S. Internal Revenue Bureau. 20.2.2 Filter Aid--Any high-grade analytical filter aid for rapid flow. 20.2-.3 Ferric Sulfate (Fe2(S04)3 -xH20)--Any hydrated analytical reagent. 20.2.4 Sodium Hydroxide, Standard Solution (1 N)-- Dissolve 40 g ofpure NaOH in 500 mL ofdistilled water and dilute to 1 L in a volumetric flask. Standardize against pure oxalic acid dihydrate. 20.2.5 Sodium Thiosulfate, Standard Solution (0.2 AO-- Dissolve 49.66 g sodium thiosulfate (Na2S203-5H20) in distilled water that has been previously boiled to free it from carbon dioxide and dilute to 1 L of the solution. It is best to let this solution stand about 2 weeks before standardizing with pure resublimed iodine or potassium bi-iodate. Preserve - in a brown1 stock bottle with a guard tube filled with soda lime. 20.2.6 Starch Solution--Make a paste of 0.2 g of soluble starch (potato starch) in cold water and pour into 100 mL of boiling water, cool and bottle or use the solution prepared for the iodine number determination (10.1.5). 20.2.7 Potassium Iodide (K1)--Iodate-free crystal. 20.2.8 Nickel Sulfate--Reagent grade (NiSQ4\6H20). 20.3 Preparation ofColor Standards_ ' ,_ 20.3.1 Ferric Sulfate--Dissolve 400 g of Fe2(sb4)3-xH26 in about 600 mL ofwater by heating to boiling while stirring constantly. After complete solution, cool to room tempera ture and dilute to 1 L in a volumetric flask. Standardize this stock solution by titrating with iodine in the, following manner: Dissolve 20 g of KI in 30 mL of water and add 5 mL ofthe stock solution. Add to this approximately 2 weight % of H2S04 (sp gr 1.84). Allow to stand for 5 min and titrate with 0.2 N sodium thiosulfate solution in the usual manner, not adding the starch indicator until near the end of the titration. Run at the same time a blank determination on the KI solution and correct for any nonuniformity- of this reagent. Adjust the stock solution to approximately 0.725 M Fe2(S04)3 solution (Note 10); 5 mL of the stock solution should then be equivalent to 36.2 0.8 mL of 0.2 N sodium thiosulfate solution. No t e 10 --The amount of coordinated water in ferric sulfate may vary, and has to be taken into account in weighing out the required amount of ferric salt. It is usually about 6 mols per mol of ferric sulfate for the powdered analyzed reagent. DUP050296535 20.3.2 Nickel Sulfate--Dissolve 50 g of NiS04 6H20 in I about 300 mL of water. After complete solution, dilute to 500 mL in a volumetric flask. 20.3.3 Reference Standard for All Grades15--Transfer | exactly 20 mL of the stock ferric sulfate solution (20.3.1) to a || 100-mL volumetric flask. Add 11.5 mL of the 1.0 N NaOH ft: solution from a buret, and shake until all the precipitate ft formed has dissolved. Then, add 10 mL of the nickel sulfate i solution and dilute to 100 mL with distilled water. If any of -j the solutions show permanent precipitates, prepare fresh gt solution, if 20.4 Procedure: 20.4.1 Transfer exactly 5 g of the sample to a clean 4-oz 7, (120-mL) wide-mouth bottle and add exactly 50 mL of * alcohol. Shake until solution is complete and then cool to v ioc. 20.4.2 Place a 55-mm tough, hard, close texture filter paper or its equivalent in the Buchner funnel which has been mounted in the neck of a 2-L suction flask with a rubber ^ stopper. Pour evenly upon the filter paper a 1-g suspension of " filter aid in 50 mL of alcohol, and suck completely dry with H1 a partial vacuum, using a water suction pump; Remove the funnel and add about 400 mL of alcohol to the flask. (Note ll) Place an 8-in. (200-mm) test tube in the suction flask, fsupporting, if necessary, with filter paper, so that the tip of the Buchner funnel when inserted in the neck of the flask will come well within the open test tube. Reinsert the funnel in the flask. 21. Acid Value 21.1 Definition: 21.1.1 acid value--the number of milligrams of potas sium hydroxide required to neutralize 1 g of moisture-free lac resin. 21.2 Reagents: 21.2.1 Neutral Ethyl Alcohol--Alcohol, as described in Section 8, that has been neutralized with, standard KOH or NaOH solution, using the phenoiphthaiein indicator to a faint but persistent pink color just prior to use. 21.2.2 Phenoiphthaiein Indicator Solution--Dissolve 1 g of phenoiphthaiein in 100 mLof ethanol (8.2), methanol, or isopropanol. 21.2.3 Potassium Hydroxide or Sodium Hydroxide Solu tion, Standard Aqueous or Alcoholic (0.1 N): 21.2.3.1 Preparation of Aqueous Solution--Prepare a stock concentrated solution by dissolving potassium hy droxide (KOH) or sodium hydroxide (NaOH) in water in the proportion of 112 g of KOH, or 85 g of NaOH in 200 mL of water. Allow the solution to cool and settle in a stoppered bottle for several days. Decant the clear liquid from the carbonate precipitate into another clean bottle. Add clear barium hydroxide (Ba(OH)2) solution until no further pre cipitate forms. Again allow to settle until clear. Draw off 175 mL and dilute to 10 L with water. Preserve in a stock bottle provided with a guard tube filled with soda-lime. 21.2.3.2 Preparation ofAlcoholic Solution--Place 5 to 10 g of KOH in a 2-L flask and add 1 to 1.5 L of alcohol 20.4.3 Add 1 g of filter aid to the cold shellac solution and ^ prescribed in 8.2. Boil on a water bath under a reflux ^ stir thoroughly. Transfer completely to the Buchner funnel condenser for 30 to 60 min. Distill and collect the alcohol. '1 and filter at the rate of 2 drops per second by means of aDissolve 5.6 g of KOH or 4 g of NaOH in 1 L ofthe distilled"^ carefully regulated vacuum. This may be conveniently done alcohol, keeping the temperature below 15.5C while the by the use of a water pump to which has been attached a trap carrying a stopcock to admit air. Slowly increase the amount of vacuum toward the end of the filtration in order to alkali is being dissolved. This solution should remain clear. 21.2.3.3 Standardization ofSolution--Standardize either solution by titrating against pure potassium acid phthalate,16 maintain a constant filtration rate until the filtration is practically complete, and then suck dry, The final volume in the test tube should be 49 to 50 mL. If it is less than 48 mL, repeat the procedure. using phenoiphthaiein indicator. The solution will be ap proximately 0.1 N. Determine its exact normality to 0.001 n: 21.2.4 Thymol Blue Indicator Solution^Dissolve 0.04, g No t e 11--The method used in preparing the solution for compar ison is very important. A slight loss in alcohol will materially affect the of thymol blue (thymol sulfonphthalein) in 100 mL of the alcohol prescribed in 8.2. color when diluted for comparison. Alcohol is placed in the flask to avoid undue evaporation of the solution during filtration. The rate of filtration is an important factor. 21.3 Procedure: 21.3.1 Weigh to 1 mg approximately 2 .g of the mixed sample (Section 7) into a 250-mL Erlenmeyer flask and add 20.4.4 Transfer 10 mL of filtered solution to one of the 100 mL of the neutral alcohol. The sample should com colorimetric tubes, and compare with 10 mL of the standard pletely dissolve at room temperature within a few hours with color solution by viewing the tubes transversely in front of the aid of periodic gentle swirling. Titrate in accordance with the standard light source. Dilute the shellac solution with 21.3.2 or 21.3.3. alcohol until it matches the reference standard color. Report 21.3.2 In case of bleached lac, add 1 mL of the phenoi the volume in millilitres of the diluted solution; this is taken phthaiein indicator solution and titrate with 0.1 N KOH or as the color number of the sample. Determine the color of NaOH solution, with constant swirling of the contents of the the filtered solution the same day upon which the samples flask.. Take as the end point when a faint pink color remains are dissolved. after continuous swirling for 30 s. ! 12--Most filtered solutions made by dissolving shellac that has been ground for analysis will darken appreciably in color if allowed to stand for periods longer than 12 h. 21.3.3 In case of orange shellac, place several drops of the thymol blue indicator solution on a white porcelain spot plate. Titrate the solution with 0.1 N KOH or NaOH 13 This standard color solution was designed to match the No. 5 iodine color standard of the Angelo color method which has been used by various laboratories for obtaining numerical color values for lacs. It is closer in hue to most lacs than 16 National Institute of Standards and Technology standard reference material No. 84d is recommended for this purpose and should be handled as directed in the certificate of analysis accompanying the sample. DUP050296536 D29 solution, with constant swirling, and determine the end point by transferring 1 or 2 drops of the solution on a glass rod to the indicator. The end point is reached when the first blue color is developed in the indicator. 21.4 Calculation--Calculate the acid value as follows: Acid value = (VN x 56.1)/S(1 - M) where: V = KOH or NaOH solution required for the titration, mL N = normality of the KOH or NaOH solution, S = sample used, g, and Af= volatile matter (moisture) content of the sample ex pressed as a decimal fraction. 22. Orpiment 22.1 Reagents and Materials: 22.1.1 In addition to conforming to the requirements of Section 6, all reagents shall be free of arsenic. 22.1.2 Ammonium Hydroxide (NH4OH)--Concentrated ammonium hydroxide (sp gr 0.90). 22.1.3 Carbon Disulfide (CS2). 22.1.4 Carbon Tetrachloride (CC14). 22.1.5 Ethyl Alcohol, Denatured, as prescribed in 8.2. 22.1.6 Ferrous Sulfate or Ferrous Ammonium Sulfate (FeS04 or FeSQ4 (NH4)2S04). 22.1.7 Hydrochloric Acid (HQ)--Concentrated hydro chloric add (sp gr 1.19). 22.1.8 Hydrogen Peroxide (H202)--Concentrated hy drogen peroxide 30 %. 22.1.9 Hydrogen Sulfide (H2S)--A supply or source of gaseous hydrogen sulfide. 22.1.10 Nitric Acid (HN03)--Concentrated nitric add (sp gr 1.42). , 22.1.11 Sulfuric Acid (H2S04)--Concentrated sulfuric add (sp gr 1.84). 22.2 Apparatus: 22.2.1 Filter Paper--Ashless, medium-porosity filter paper. ' 22.2.2 Funnel--A jacketed-giass funnel or funnel about which has been wound a coil of copper or tin tubing through which steam may be passed to heat it 22.2.3 Gooch Crucible--A Gooch crumble that has been prepared with an asbestos mat in the usual manner, ignited, cooled, and stored in a desiccator. 22.2.4 Distillation Asseikbly-r-A 300-mL Kjeldahl flask, fitted with a 2-hole rubber stopper, and attached to a bulb-type glass condenser by"a U-tube having about Vi-in. (6.4-mm) bore and a distance of 8 in. (205 mm) between arms. Through the other hole in the stopper a double-bulb safety tube or a small separatory funnel with a long, slim stem is inserted. The tip ofthe safety tube or funnel is bent to form a short U, the orifice of which points upward. The tube or funnel is fitted into the flask so that the U tip nearly touches the bottom of the flask. A 250-mL beaker, which serves as a receiver, is held on a movable support, immedi ately under the condenser tip. 22.3 Procedure: 22.3.1 Weigh to 0.1 g approximately 50 g of the mixed sample (Section 7) into a 500-mL Kjeldahl flask. Add 450 mL of the alcohol to the flask and heat its contents in a hot water bath at a gentle boil until the lac resin is completely dissolved. 22.3.2 Remove the flask from the bath and wait just long enough to permit settlement of the bulk of the insoluble matter from the solution. Decant the solution from the flask to the filter paper held in the jacketed funnel which must be kept hot during the entire filtration by passing steam through the coil or jacket. Keep a watch glass over the funnel when not pouring the solution into it (Note 13). 22.3.3 Wash the sediment layer in die flask with four successive 50-mL portions of boiling alcohol, and decant the washings through the filter. Finally wash the filter paper with 50 mL ofthe boiling alcohol. Continue heating the fbnnel to drive off most of the alcohol. Pour slowly over the entire surface of the filter paper approximately 200 mL of boiling carbon tetrachloride to dissolve any of the lac wax that may have remained on the filter paper (Note 14). Now leave thewatch glass off and continue passing the steam through the funnel jacket to dry the solvent from the paper. No t e 13--Ifthe funnel and its contents are not kept hot the wax will congeal and clog the filter paper, thus slowing up the filtration. No t e H--All wax should be removed from the filter paper and inside of the flask, as otherwise the subsequent digestion procedure may be materially prolonged. 22.3.4 Carefully transfer the filter paper and its contents to the flask. Add 25 mL of HN03 (sp gr 1.42) to the flask, and apply gentle heat, digesting the contents of the flask for 20 min. Cool, add 25 mL of H2S04 and again heat gently until most of the nitrous fumes have been driven off. Increase the heat and continue boiling until the evolution of sulfur trioxide (S03) fumes occurs. 22.3.5 If organic matter or charring is evident at this point, allow the flask to cool to room temperature. Rinse down the inside of the flask with a small amount of water and carefully add 3 to 4 mL of H202. Afteriany initial violent gas evolution has subsided again heat to S03 fumes. If discoloration reappears, repeat the hydrogen peroxide treat ment and heating until a clear carbon-free solution is obtained. 22.3.6 Transfer the clear solution to the 300-mL Kjeldahl flask, rinsing the flask thoroughly with small portions-of water until the volume of the solution and washing is between 125 arid 150 mL. Heat the~solulion - rapidly to boiling and evaporate just short of filming to ensure com plete removal of both HN03 and H202. 22.3.7 Add 20 g of either ferrous sulfate or ferrous ammonium sulfate to the flask and connect the flask to the distillation assembly. Place 50 mL of water in the beaker, serving as receiver, and raise the beaker on its support until the end ofthe condenser is immersed in the water. Start H2S bubbling into the water in the beaker (Note 15) and cold water flowing through the condenser. Place 50 mL of HQ in the safety tube or separatory funnel and adjust the stopcock so that die acid runs in a slow stream into the flask. Apply gentle heat and bring the solution to a steady -boil. If orpiment is present a yellow precipitate will appear in the receiver when distillation starts. Discontinue the distillation when bumping begins. 22.3.8 Remove the flame, change the receiver, add an other 50-mL portion of the HC1 to the contents of the flask and repeat the distillation procedure (Note 16). When the second distillation is completed, lower the receiver, and wash down the inside of the condenser and the outside of the 16 DUP050296537 t D 29 gondenser tip with water. If any orpiment adheres to the 11s of the condenser, wash it ofF with a small amount of J4OH, allow it to drain into the receiver, and then rinse _ in with water. Check the contents of the beaker for lucidity, adding more acid if necessary, and allow the HjS to rbubble through the solution for a few minutes longer. No t e IS--The supply should be ofsufficient amount to afford a {(uniform and good rate of flow during the entire distillation. No t e 16--With a properly prepared specimen, practically all of the lirsenic comes over in the first distillation, the second one serving mainly ps a safeguard. 22.3.9 Filter the contents of both beakers through the (prepared and weighed Gooch crucible. Wash all of the Ipredpitate from each beaker into the crucible with a stream pf hot water from a wash bottle, using a policeman if jjfiecessary. Next, wash out the beaker with two 50-mL portions of alcohol followed by two 50-mL portions of ((boiling CS2 (Note 17). When filtering these washings, adjust j|he suction so that each portion will be retained in the jjprucible for approximately 5 min (Note 18). Dry the crucible land its contents at 105 2C for 2 h. Cool in a desiccator |and weigh. . No t e 17--Bring the CS2 to a boil on a steam bath, making sure there is no gas flame or electric ate in the immediate area in which the CS2 is being used. No t e 18--This treatment ensures complete removal of all traces of sulfur that may have precipitated with the orpiment and which, ifleft in, would materially affect the final result, especially with a sample quite low in arsenic. 22.3.10 If there is any reason for believing that the reagents used are' not arsenic-free, run blank determinations concurrently, using the same reagents in the same amounts and make the proper correction for the amount of orpiment thus found. 22.4Calculation--Calculate the percentage of orpiment (AS2S3) as follows: I; where: Orpiment, % = [(.R - B)/S(l - M)] X 100 % R = residue from specimen, g (22.3.9), B = residue from blank, g (if any) (22.3.10), S = sample used, g, and M = volatile matter (moisture) content of the sample, ex pressed as a decimal fraction. * 23.Saponification Value 23.1 Definition: 23.1.1 saponification value--the number of milligrams of potassium hydroxide that react with 1 g of the moisture-free sample. It is a measure of the alkali reactive groups in lac resins. 23.2 Reagents'. 23.2.1 Hydrochloric Acid, Standard (0.5 N)--Add 45 mL of concentrated hydrochloric add (HQ, sp gr 1.19) to about 900 mL of water, cool, and dilute to 1 L. Standardize against freshly standardized NaOH solution or by any other accurate method. 23.2.2 Neutral Alcohol, as prescribed in Section 21.2.1. 23.2.3 Pkenolphthalein Indicator Solution, as prescribed in 21.2.2. 23.2.4 Potassium Hydroxide, Alcoholic Solution (0.5 N)--Prepare the solution as prescribed in 21.2.3, Item 2, except use 33 g of KOH in 1 L of the alcohol. 23.2.5 Thymol Blue Indicator Solution, as prescribed in 21.2.4. 23.3 Procedure-. 23.3.1 Weigh to 1 mg approximately 1 g of the mixed sample (Section 7) into an alkali-resistant, standard-taper, ground-glass joint, 250-mL Erlenmeyer flask. Using a con stant volume pipet, add 25 mL of the alcoholic KOH solution to the flask containing the specimen and to a second flask for use as a blank. Add 25 mL ofthe neutral alcohol to each flask and attach a standard-taper, ground-glass joint condenser to each flask. Connect the condensers with soda-iime tubes and reflux on a steam bath for at least 1 h. Wash down the condensers and the sides ofthe flasks with 20 mL of the neutral alcohol and titrate in accordance with 23.3.2 or 23.3.3. 23.3.2 In the case ofbleached lac, add several drops of the phenolphthalein solution to each flask and titrate with 0.5 HC1, with constant swirling of the contents of the flask, until the pink color just disappears. 23.3.3 In the case of orange shellac place several drops of the thymol blue indicator sulution on a white porcelain spon plate. Titrate the solutions with 0.5 N HQ, with constant swirling, and determine the end point by transferring one or two drops of the solution on a glass rod to the indicator..The end point is when the color of the indicator changes to red. 23.4 Calculation--Calculate the saponificatidn value as follows: '- Saponification value = [(5 - V)N x 56.1]/S(1 -- M) where: .* V -- HC1 required for titration of the specimen, mL, B -- HQ required for titration of the blank, mL, N = normality of the HQ, S = sample used, g, and M -- volatile matter (moisture) content of the sample ex pressed as a decimal fraction. 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 thst determination of the validity of any such patent rights, snd the risk of infringement of such rights, am entirely their own responsibility. This standard is subject to revision at any tune 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 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. It you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 191B Race St., Philadelphia, PA 19103. DUP050296538 Designation: D 34 - 91 Standard Guide for Chemical Analysis of White Pigments1 This standard is issued under the fixed designation D 34; 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 reapprovol. A superscript epsilon (t) indicates an editorial change since the last revision or rcapprovaL These methods hove been approvedfor use by agencies ofthe Department ofDefense to replace Method 1091, 7253 offederal Test Method Standard No. HI A andfor listing in the DoD Index ofSpecifications and Standards. 1. Scope 1.1 This guide covers procedures for the chemical analysis of white pigments. 2. Referenced Documents 2:1 ASTM Standards: C 471 Test Methods for Chemical Analysis of Gypsum . and Qypsum Products*2 D 715 Tost Methods for Analysis ,pf Barium Sulfate Pignient3 18 6.717 Test Methods for Analysis of Magnesium Silicate Pigment3 . D718 Test Methods for Analysis of Aluminum Silicate Pigment3 . D 719 Test Methods for Analysis of Diatpmaeeous Silica Pigment3 D1199 Specification for Calcium Carbonate Pigments3 : D1301 jest Methods for Chemical Analysis of White Lead Pigments3 . .1 This guide is under the jurisdiction of ASTM Committee D-J on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee* D01.21 on Chemical Analysis' of Paints and Paint Mkterialsi Current edition approved Sept. 15,1991. Published November 199t.;Originally pubtishedas D 34-15.,Last previous edition D 34 - 87. . 2 Annual Book ofASTM Standards] Vol 04.01. 3 AHnial Bbok qfASTM'Standards, Vol Off.02. ` D1394 Test Methods for Chemical Analysis of White Titanium Pigments3 D3280 Test Methods for Analysis of White Zinc Pigments3 ` ; 3. Significance and Use 3.1 This compilation of available ASTM methods for the analysis of white pigment serves as a guide to chemists. 4. Test Methods 4.1 Tests shall be conducted in accordance with the fol- lowing ASTM methods. Test procedures not covered by ASTM methods shall be agreed upon by the purchaser and seller. 4.2 Lead Pigments--Test Method D 1301. 4.3 Zinc Pigments--Test Methods D 3280. u, 4.4 Titanium Dioxide Pigments-^Test Methods D 1394. 4.5 Calcium Carbonate Pigments: Whiting, Parts White, Spanish White, Chalk--Specification D 1199. 4.6 Calcium Sulfate Pigments: Gypsum, Terra Alba, Plaster ofParis--Methods C 471. . < ,4.7, Barium-Pigments: Baryte^ or Barite and Blanc Fixe-- Test Methods D 715. 4.8 Silica Pigments--Test Methods D 71,9. 4.9 China Clay--Test Method D 718. -- 4.10 Magnesium,Silicate--Test Methods D 717. 5. Keyword 5.1 chemical analysis; white pigment- . . The American Society for Testing end Materials takes no position respecting the validity of any patent rights assertedin connection vWtft 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 at such rights, are entirety their own responsibility. This standard le subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproverfor withdrawn. Your comments are Invited either for revision 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 mayattend, if you feet Mel your comments have not race/yeti a fair bearing you should make yoUr views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19t03, '; 18 DUP050296539 Designation: D 49 - 83 (Reapproved 1990)61 Standard Methods of. Chemical Analysis of Red Lead1 This standard is Issued under the fixed designation D 49; 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 (e) indicates an editorial Change since the last revision or reapproval. ei`NoTE--Sections were updated editorially in September 1990. ' 1. Scope 1.1 These methods cover procedures for the chemical analysis of red lead having the approximate formula Pb304 i (probably PbO2-2Pb0). 1. 2 It is the responsibility ofthe user of this standard to Establish appropriate safety practices arid to determine the applicability of-regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 50 Test Methods for Chemical Analysis of Yeilow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D 215 Methods of Chemical Analysis ofWhite Linseed Oil Paints3 4 . D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the . Test Conditions) in Pigments2 D1193 Specification for Reagent Water* D1208 Test Methods for Common . Properties of Certain Pigments2 D1301 Test Methods for Chemical Analysis of White Lead Pigments2 D1959 Test Method for Iodine Value of.Drying Oils and Fatty Acids5 3. Treatment of Sample I 3.1 If the pigment is lumpy or not finely ground, grind it to a fine powder and mix thoroughly. Large samples may be thoroughly mixed and a representative portion taken and powdered if lumpy or not finely ground: The sample in all cases shall be thoroughly mixed before taking portions for analysis. All samples shall be preserved in stoppered bottles or containers. 4. Purity of Reagents 4.1 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 1 These methods'are under thejurisdiction of ASTM Committee D-l on Paint and Related Coalings and Materials and are the direct responsibility of Subcoin* raittee D 01.2] on Chemical Analysis of Paint and Point-Materials. Current edition approved Dec. 20, 1983. Published January 1984. Originally published as D 49 - 17 T. Last previous edition D 49 - 82. 2 Annual Book ofASTM Standards* Vol 06.02. 3 Annual Book ofASTM Standards* Vol 06.01. 4 Annual Book ofASTM Standards* Vol 1J .01. 5 Annual Book ofASTM Standards* Vol 06.03. 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. 4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 5. Moisture , 5.1 Determine moisture content with a 2-g 'specimen in accordance with Method A of Method D 280. The specimen is dried for 2 h at I05C. The loss iii weight is considered as moisture. 6. Organic Color 6.1 Boil 2 g of the sample with 25 mL. Qf 95 % ethyl alcohol, let settle, decaiit the supernatant liquid; boil the residue with 25 mL of distilled water and, decant as before; boil the residue with 25 mL of diluted NH4OH (l+4) and again decant. Boil another 2-g portion of the sample with 25 mL of chloroform, let settle, and decant the supernatant liquid. If any one of the above solutions is colored, organic coloring matter is indicated. Ifthe solutions remain colorless, organic cdldrs are prdbably absent! ; No t e I--If it is desired to test for organic .colors resistant to-.the above reagents, the test procedures described in the followingbooks may ' be Used,'taking into-'afccount the nature of the pigment involved: Zerr and Mayer, Tests fdr Coal Tar Colors in Aniline 'Laker, Schultz and Julius, A Systematic Swvtjt ofthe Organic Coloring Matters-, Mulliken, Identification ofPure Organic Compounds; Commercial Dyestuffs, Vol III..,. ... 7. Total Lead and Insoluble Matter 7.1 Treat 1 g of the sample with 15 mL of HN03 (1+1) and sufficient H^02 to dissolve all Pb02 on warming; If any insoluble matter is present, add 25 mL of water, boil, filter, and wash with hot water. The insoluble-matter contains free Si02 and should be examined for BaS04 and silicates, if appreciable. 7.2 To the original' solution or filtrate from the insoluble matter add 20 mL of H2S04 (sp gr 1.84) and evaporate to S03 fumes. Cool, add 150 mL of water, and 150 mL of 95 % 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." ------ ?P DUP050296540 D 49 ethyl alcohol, let stand cold for 2 h, filter, on a Gooch crucible, wash with 95 % alcohol, dry at 105 to 110C, and weigh as PbS04. Calculate to PbO. 7.3 Red lead is rarely adulterated, but should the spec imen contain soluble barium compounds, the PbS04 ob tained in 8.2 will contain BaS04. In this case, precipitate the lead as sulfide from a slightly acid (HQ) solution, dissolve the PbS in hot diluted HN03, and determine the lead as sulfate or chromate. 7.4 If the specimen contains significant amounts of cal cium or magnesium, boil the HNOj -- H202 solution (7.1) until all the lead is converted into nitrate and then determine the lead as PbCr04. 7.5 If soluble barium, calcium, or magnesium are to be determined, precipitate the lead as sulfide from a slightly acid solution (HC1), dissolve the PbS in hot diluted HN03, and determine the lead as sulfate. Boil the filtrate from the PbS to expel H2S, add a little bromine water to oxidi2e iron (if present), boil to expel bromine, and precipitate the barium with a few millilitres of H2S04 (1+3). Filter and weigh as BaS04. Calculate to BaO or Ba003. To the filtrate from the BaS04 add NH40H in slight excess, filter off any precipitate of Fe(OH)3 + Al(OH)3, wash with hot water. Manganese, if present, can be precipitated by adding bro mine and NH40H and warming. Filter, wash with hot water, ignite, and weigh as Mn304. Unite ail the filtrates, make slightly acid with acetic acid, heat to boiling and pass H2S into the hot solution until saturated (20 to 30 min); add 5 g ofNH4C1 and let stand 5 h, filter offany ZnS, wash with H2S water, dissolve the ZnS in hot diluted HCI and determine the zinc by titration with K4Fe(CN)6. Or, boil off the H2S, filter out any separated sulfur and determine the zinc as Zn2P207. Calcium may be determined in the filtrate from the ZnS by expelling H2S and then adding NH40H and ammonium oxalate. Titrate the calcium oxide precipitate using the procedure described in 13.3 of Method D 50. In the filtrate from calcium determine magnesium by precipitating with sodium phosphate solution, finally weighing as Mg2P207. 8. Lead Peroxide (PbO^ and True Red Lead (Pb304). No t e 2--Method of Diehl7 modified by Topf8--not applicable when substances are present, other than oxides of lead, that liberate iodine under conditions given, or substances such as metallic lead which reduce Pb02 to PbO without the liberation of iodine. 8.1 Solutions Required: (a) Red Lead Solution--Dissolve in 1-L beaker 600 g ofcrystallized sodium acetate and 48 g of KI in about 500 mL of acetic add (1+3) (made by mixing 150 mL of gladal acetic add with'450 mL of water). Warm the beaker and contents on a steam bath, stirring occasion ally, until a clear solution is obtained. Cool this solution to room temperature, dilute to exactly 1000 mL with the acetic acid (1+3) and mix thoroughly. If preferred, the red lead solution may be prepared separately for each titration, as follows: Dissolve 30 g of the crystallized sodium acetate and 2.4 g of KI in 25 mL ofthe acetic add (1+3), Wanning gently and stirring until a dear solution is obtained. Cool this solution to room temperature, dilute to 50 mL with the acetic add solution (1+3), and mix thoroughly. 8.2 Sodium Thiosulfate Solution (0.1 AO--Dissolve 24.83 g of sodium thiosulfate (Na2S203 5H20), freshly pulverized and dried between filter paper, and dilute with water to 1 litre at the temperature at which the titrations are to be made. The solution is best made with well-boiled water free from C02, or let stand 8 to 14 days before standardizing, as described in Section 5 of Method D 1959. 8.3 Starch Solution--Stir 2 to 3 g of potato starch with 100 mL of salicylic add solution (1 %), and boil the mixture until the starch is practically dissolved, then dilute to 1 L (Note 3), or prepare as described in 7.8.2 ofMethod D 1959. "#$% 3: Lead Peroxide--If the pigment contains an appreciable amount of nitrite (nitrate has no effect on the method), leach out water-soluble matter as below, dry the residue and determine Pb02 as above, calculating to basis of original specimen. 9. Procedure 9.1 Weigh 1 g of the finely ground sample, transfer to a 200-mL Erlenmeyer flask, add 20 mL of water; then add as quickly as possible 40 mL ofthe "red lead solution" at room temperature. Ifthe sample is red lead that has been extracted from a paint or paste, in place of the water use 10 mL of a mixture of 7 parts by volume of chloroform and 3 parts by volume ofgladal acetic add, and then add without delay the red lead solution. Add 30 mL ofwater containing 5 or 6 g of sodium acetate and titrate at once with 0.1 N Na2S203 solution, adding the latter rather slowly and keeping the liquid constantly in motion by whirling die flask. When the solution has become fight yellow, rub-up any undissolved particles with the rod until free iodine no longer forms, wash off rod, add the Na2S203 solution until - pale yellow, add... starch solution, and titrate until colorless. Add the 0.1 N iodine solution until blue color is just restored and subtract the amount used for the volume of Na2S203 that had been added. 10. Calculation 10.1 Calculate the lead peroxide and true red lead-con tents as follows: Pb02 = I X 0.942 Pb304 = J?h02 X 2.866 = I x 2.7. where: I = iodine value of the Na2S203 solution. 0.942 = ^ = ^,and I, 253.81 ' Pb,Q4 685.57 2.86616' ' PbO, " 239.19 11. Zinc 11.1 If the volume is appreciable, evaporate off the alcohol from the filtrate from total lead, make alkaline with NH4OH, then acid with HQ (sp gr 1.19), add 3 mL more of HQ, dilute to about 250 mL with water, heat'nearly to boiling and titrate with standard K4Fe(CN)6 solution in accordance with 16.1.11 of Method D 215. Report as ZnO (includes cadmium). Iron, copper, or other interfering sub stances should first be removed as described in 25.2.3 of Method D 215. DUP050296541 # D 49 " present in accordance with the procedure in Section 5 of Methods D 1208 or determine in accordance with Test | Method D 1301. i13. Total Silica 13.1 Digest 5 g of the sample in a covered casserole with 5 mL ofHCI and 15 mL of HN03 (1+1). Evaporate to dryness to dehydrate. Cool, treat with hot water and HN03, boil, , filter, wash with hot acid ammonium acetate solution* then I dilute HCI and finally hot water. Ignite and weigh as Si02. The residue may be treated with H2S04 and HF in cases of ,, doubt as to purity. *. 14. Carbon Dioxide 14.1 Determine carbon dioxide by the evolution method, ; using diluted HQ and stannous chloride. 15. Soluble Sulfates 15.1 Sulfates Other Than Barium Sulfate--Treat 0.5 g of 1 the sample with 5 mL of water, 3 g of NH4CI, and 5 mL of Sfj HCI saturated with bromine. Digest (covered) on steam bath ' about 15 min. Add 25 mL of water, neutralize with dry Na2C03, and add about 2 g more. Boil 10 to 15 min, let settle, dilute with hot water, filter, and wash with hot water. Redissolve in HQ, repfecipitate as above, and wash thoroughly with hot water. Acidify the united filtrates with HCI, adding a slight excess; boil and add a slight excess of BaCl2 K solution (10%). Let stand on a steambath for' 1 h. Filter and * wash with hot water. Ignite and weigh as BaS04. Calculate to '; S03 (includes S03 formed from S02). 15.2 Or, dissolve 0.5 g ofthe sample in 25 mL ofwater, 10 mL pfNH4QH (sp gr 0.90) and HCI in slight excess; dilute to about 150 mL with water and add a piece of aluminum foil which should about cover the bottom of the beaker (being held on the bottom by means of a stirring rod). Heat gently till all lead is precipitated, decant through a filter, pressing the lead sponge with a flattened rod, and washing with hot water. Add to the filtrate a little, bromine water, boil until bromine is expelled, add 15 mL of BaCl2 solution (10 %), let stand on a steam bath for 1 h, filter, wash with hot water, ignite, and weigh as BaS04 (any SrS04 present is not decomposed in this method).9 16. Iron Oxide 16.1 Determine iron oxide in accordance with Section 12 ofMethod D 50, or in a large beaker, treat 20 g ofthe sample with 20 mL of water, 20 mL of HN03 (sp gr, 1.42), and 3 mL Of formaldehyde solution., Warm until all Pb02 is dissolved, dilute with wafer, warm, filter offinsoluble matter, and wash with hpt water. Ignite filter and , Insoluble matter, and evaporate with H2S04 and HF. To filtrate from insoluble matter add 14 mL of H2S04 (1+1), filter off PbS04, and wash. Dissolve the residue from HF and H2S04 in H2S04 and add to the filtrate from PbS04. Dilute to 500 mL and determine iron colorimetrically in an aliquot, using the same amounts of HN03, H2S04, and formaldehyde in the com parison solution.10 Calculate to Fe2Q3. 9 The solubility of BaS04 is increased by the presence of aluminum, chloride. See Skoog, D. A. and West, D. M., Fundamentals ofAnalytical Chemistry, Holt, Rinehart and Winston, Inc., New York, 1969, p. 192. 10 Lunge-Beri, "Chemische-technisch Untersuchungs-Methoden,".VoI 2, p. 95, 6th Ed. 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 Knot revised, either reapproved or withdrawn. Your comments are Invited eithertor 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 lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Raise St,, Philadelphia, PA 19103. _ --- - *4 I**."DUP050296542 Designation: D 50-90 Standard Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing iron and Manganese1 This standard is issued under the fixed designation D SO; 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 rehpproval. This standard has been approvedfor use by agencies of the Department ofDefense to replace Method 714}, 7151 ofFederal Test Method StandardNo. 141. Consult the DoD Index ofSpecifications andStandardsfor the specificyear ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 These test methods cover procedures for the chemical analysis of yellow, orange, red, and brown pigments con taining iron and manganese. The test methods apply specif ically to the following pigments: synthetic hydrated yellow iron oxide, yellow ocher, red arid brown iron oxides, raw and burnt umber, raw and burnt sienna, and Venetian red. 1.2 The analytical procedures appear in the following order: Dry Pigments Sections ASTM Method Refer ences Moisture and Other Volatile Matter Loss on Ignition Coarse Particles Matter Soluble in Water Organic Coloring Matter Iron Oxide Calcium Compounds (Reported as CaO) Sulfates Soluble in Hydrochloric Acid Lead Chromate (in Ochers) Calcium Carbonate (in Venetian Red) Manganese (in Siennas and Umbers) 6 7 8 9 10 11 and 12 13 and 14 15 and 16 17 18 19 and 20 D280 D 185 D 1208 C25 Pigment Pastes in Oil . Pigment Content Moisture and Other Volatile Matter Nonvolatile Matter in Vehicle Moisture by Distillation Coarse Particles and Skins Consistency (Stormer) ` 21 22 23 24 25 26 D 1208 D 1208 D1208 D 185 D 562 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 25 Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime12 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 May 25, 1990. Published July 1990. Originally published as D 50 - 17 T. Last previous edition D 50 - 81. 2 Annual Book ofASTM Standards. Vol 04.01. D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3,4 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D1193 Specification for Reagent Water5 D1208 Test Methods for Common. Properties of Certain Pigments3 E 11 Specification for Wire Cloth Sieves for Testing Purposes2 3. Significance and Use 3.1 These test methods compile in one place, recom mended procedures for analyzing inorganic colored pigv. ments. These pigments are used extensively in paints, and for this reason their compositions are important to the formulators and user. 4. Preparation of Sample 4.1 Mix the sample thoroughly and take a representative portion for analysis. Reduce any lumps or coarse particles to' a fine powder by grinding. Grind extracted pigments to pass a No. 80 (180-pm) sieve (see Specification E 11 for detailed requirements). Discard any skins that do' not pass through the sieve. Mix the finely ground pigment thoroughly. 5. Purity of Reagents 5.1 Purity ofReagents--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. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean Type II reagent 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 11.01 and 06.03. `"Reagent Chemicals, American Society Specifications," Am. Cbem. 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." 22 pppwap DUP050296543 D 50 water conforming to Specification D 1193. DRY PIGMENTS Moisture and Other Volatile Matter 6. Procedure 6.! Determine moisture and other volatile matter in accordance with Method A of Test Methods D 280. S'Sl Loss on Ignition ' * 7. Procedure 7.1 Weigh accurately approximately 1 g of pigment into a previously weighed and ignited porcelain crucible (Note 1). Cover and ignite to constant weight over a bunsen or Meker burner or in an electric furnace at a temperature of approx imately 900C. Cool in a desiccator, weigh, and calculate the percent loss on ignition. This figure may include combined water, carbon dioxide (C02), organic matter, and some sulfuric oxide (S03) if much calcium sulfate (CaS04) is present. The COz may be determined on a separate portion if desired. No t e 1--It is inadvisable to use platinum unless it is known that attacking substances are absent. . 1 Coarse Particles 8. Procedure 8.1 Determine coarse particles in accordance with Test Method D 185. Matter Soluble in Water 9. Procedure 9.1 Determine matter soluble in water in accordance with Test Methods D 1208. Organic Coloring Matter 10. Procedure 10.1 Boil 2 g of the sample with 25 mL ofwater, let settle, and decant the supernatant liquid. Boil the residue with 25 mL of ethyl alcohol (95 %) and decant as before. Boil the residue with'25 mL of 1 N alcoholic sodium hydroxide (NaOH) solution and again decant. Boil another 2-g portion of the sample with 25 mL of chloroform, let settle, and decant the supernatant liquid. If any one of the above solutions is colored, organic coloring matter is indicated (Note 2). If the solutions remain colorless, organic colors are probably absent, but may be tested for by reference to procedures given in standard reference works, taking into account the nature of the pigment involved.7 No t e 2--With this class of pigments indication of presence of an organic color may often be noted by the characteristic odor given off on ignition. Iron Oxide 11. Reagents 11.1 Stannous Chloride Solution (SnCl2-2H20) solve 50 g of SnCl2-2H20 in 300 mL of hydrochloric acid (HQ) (sp gr 1.19) and dilute with water to 500 mL. Keep the clear solution in a tightly stoppered bottle containing some metallic tin. 11.2 Mercuric Chloride Solution (HgCl2)--Prepare a sat urated solution of HgCl2 (60 to 100 g/L). 11.3 Sulfuric-Phosphoric Acid Mixture--Mix 150 mL of sulfuric acid (H2S04) (sp gr 1.84) with 150 mL ofphosphoric acid (H3P04) (85 %) and dilute with water to 1 L. 11.4 Diphenylamine Indicator--Dissolve 1 g of diphenylamine in 100 mL of H2S04 (sp gr 1.84). 11.5 Standard Potassium bichromate Solution (K2Cr207) (Q.1 AQ--Dissolve 4.904 g of K2Cr207 in water and dilute to 1 L. Standardize against the National Bureau of Standards standard sample No. 27 of Sibley iron ore. 11.6 Potassium Fefricyanide Solution (K3Fe(CN)6)--A very dilute solution is most satisfactory. Dissolve approxi mately 0.01 g ofK3Fe(CN)6 in 50 mL of water. This solution must be made fresh when wanted because it does not keep. 12. Procedure 12.1 According to the amount of iron in the pigment, weigh 0.3 to 1.0 g of the pigment and ignite in a porcelain crucible at a duH red heat to destroy organic matter. Transfer to a 400-mL beaker and add 25 mL of HC1 (sp gr 1.19). Cover with a watchglass and digest just short of boiling (80 to 90C) until no dark specks can be seen in the insoluble residue. The addition of a few drops of SnCl2 solution after adding the acid greatly assists dissolving of the iron. When the residue is light in color, the solution of iron may be considered complete. This may take from 15~niin to 1 h, or longer. 12.2 Add 25 to 50 mL of water and heat to gentle boiling (avoid vigorous prolonged boiling). Slowly add SnCl2 solu tion dropwise until the last drop makes the solution colorless or free from any tinge of yellow, then add 1 or 2 drops'in excess. It is best to keep the watchglass on the beaker while adding the SnCl2 solution, with agitation of the hot iron solution after each addition. If too much StiCl2 is. added by mistake, add potassium permanganate. (KMn04) to the solution until a^yellow color appears, then again add SnG2 dropwise until the yellow color just disappears, again adding one or two drops in excess. Dilute with 200 mL of coldwater, then add all at once with vigorous stirring 15 mL of HgQ2 solution. Let stand 3 to 4 min. A slight white precipitate should form. If none, or a heavy grayish precipi tate forms, the determination should be discarded and repeated. 12.3 Add 15 mL ofH2S04-H3P04 mixture and 3 drops of diphenylamine indicator solution. Titrate with K2Cr207 solution, taking the sudden change of the dark green color to a blue-black color as the end point. ' 12.4 If preferred, K3Fe(CN)6 may be used as an external indicator. In this case omit the addition of the H2S04-H3P04 mixture and the diphenylamine indicator. Titrate with the K2Cr207 solution as in 12.3, except toward the end take out a very small drop of the solution being titrated and touch this to a drop of the K3Fe(CN)6 solution, best placed on a paraffined surface. Toward the end point the blue is replaced by a bluish-green coloration, perceptible at the junction of the two solutions. Take as the end point when no trace ofthe DUP050296544 # D 50 bluish-green coloration can be detected. 12.5 Calculation--Calculate the percent of iron oxide (Fe203), A, as fojlows: . A = (FV/S) x 100 (1) where: F -- Fe203 equivalent of the K2Cr207 solution, g/mL, V -- K2Cr207 solution required, mL, and S - sample used, g. tinue the boiling until the precipitate becomes granular. Let stand about 30 min, filter, and wash three times with 20-mL aliquots of hot water until free of ammonium oxalate. 14.3 Place the beaker in which 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) and dilute to about 250 mL. Heat to 90C and titrate at once with KMn04 Calcium Compounds (Reported as CaO) solution. (The temperature of the solution should -not be below 60C when the end point is reached.) 13. Reagents 13.1 Ammonium Oxalate Saturated Solution--Heat to 14.4 Calculation--Calculate the percent of calcium com pounds, A, in terms of CaO, as follows: boiling 5 g powdered ammonium oxalate [(NH4)2C204 H20] A *= (K2c /0.5) x 100 ; (4) and 100 mL of water. Allow to cool. 13.2 Hydrogen Peroxide (H202) (30 %). 13.3 Potassium Permanganate, Standard Solution (KMn04) (0.1 N)--Dissolve 3.16 g of KMn04 in water and dilute to 1 L. Let stand 8 to 14 days,- siphon ofF the clear solution (or filter through a medium porosity fritted disk), where: V.2 -- KMn04 solution required by the specimen, mL, and C = CaO equivalent of the KMn04 solution, g/mL. \, ' Sulfates Soluble in Hydrochloric Acid and standardize against the National Institute of Standards and Technology (NIST) standard sample No. 40 of sodium oxalate (Na2C204) as follows: In a 400-mL beaker dissolve 0.2500 to 0.3000 g of.the NIST Na2C204 in 250 mL of hot water (80 to 90C) and add 15 mL of'H2S04 (1+1). Titrate at 15. Reagent 15.1 Barium Chloride Solution--Dissolve; 117 g of barium chloride (BaCl2-2H20) in water and dilute to 1 L. once with KMn04 solution; stirring the liquid vigorously and continuously. The KMn04 must not be added more rapidly ihari 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 solution shall not be below 6QC by the time the end point has been reached. (More rapid cooling may be prevented by allowing the beaker to stand on a small asbestos-cpvered hot plate during the titration.) The use of a small thermometer (nonmercury type) as a stirring rod is most convenient. Keep the KMn04 solution in a glass-stoppered bottle painted black to keep out light, or in a brown glass bottle stored in a dark 16. Procedure 16.1 Weigh 1 g ofthe sample and add 30 mL of HQ (sp gr 1.19). Boil 10 min, add about 50 mL of water, boil, filter, and wash with hot water. Heat the solution to boiling, add NH4OH in excess, filter, and wash the precipitate several times with hot water. Dissolve the precipitate in hot HC3 (1+1), repredpitate with NH4OH, and wash well with hot water. 16.2 Combine the united filtrates and make distinctly acid with HC1, boil, and add dropwise, while stirring, an excess of place. 13.4 Calculate the calcium oxide (CaO) value of the solution as follows: , C= (Wt X F,) x 0.4185 (2) where: C = CaO equivalent of the KMn04 solution, g/mL, = sodium oxalate used, g, and V, = KMn04 solution required for the titration, mL. BaCl2 solution. Boil about 10 min; The BaS04 precipitate should normally stand for 2 to 4 h before filtering in order to coagulate the precipitate. If the pad-is 'thick gupugh-on the Gooch crucible and filtrate is free of sulfate, then standing may not be necessary. Filter on a Gooch Crucible, and wash with hot wateir. Ignite at 900C, and weigh as barium sBtfate (BaSOJ. 16.3 Calculation--Calculate the percent of S03, A, as follows: 0.4 i 85 = CaO/Na^CL = 56.08/134.01 . (3)14 * * * * * A = i(P x 0.343)/S] x 100 T5) 14. Procedure 14.1 Weigh 2.5 g of sample, transfer to a porcelain crucible, and ignite at a dull red heat to destroy organic matter. Cool, transfer to a 600-mL beaker, and add 100 mL of HC1 (1+1). Digest just short of boiling until no dark specks can be seen in the insoluble residue. Add ammonium hydroxide (NH4OH) (sp gr 0.90) in slight excess and about 2 mL of H202 (30 %). Cool, transfer to a 500-mL graduated flask, and dilute to 500 mL. Mix thoroughly and filter through a dry paper. 14.2 Take 100 mL ofthe filtrate (corresponding to 0.5 g of sample), add a few drops of NH4OH, heat to boiling, and add an excess of saturated ammonium oxalate solution. Con where: P = weight of BaS04, g, and S' = weight of original sample, g. 0.343 = S03/BaS04 = 80.06/233.42 Lead Chromate {in Ochers) 17. Procedure 17.1 Test for lead by any standard method of qualitative analysis. The following method is suggested: Dissolve a small portion of the pigment in cold nitric acid (HN03) (1+5), stirring vigorously. Add a few millilitres of potassium iodide 24 up DUP050296545 D 50 (KI) solution (100 g/L). The appearance of yellow crystals indicates the presence of lead. Calcium Carbonate (in Venetian Red) 18. Procedure 18.1 Determine carbon dioxide (COz) in accordance with Test Methods C 25. 18.2 Calculation--Calculate the percent of calcium car- | bonate (CaC03), A, as follows: ! ' A = [(W, x 2.274)/5] x 100 (6) where: W3 = C02, g, and S = sample used, g. 2.274 = CaC03/C02 = 100.09/44.0 Manganese (in Siennas and Umbers) 19. Reagents 19.1 Standard Potassium Permanganate Solution (KMn04) (1 mL = 0.00035 g Mn)--Dissolve 1 g of KMn04 in 1 L of water. Age and standardize the solution as in Section 13, using one third the quantities of reagents specified therein. Calculate the manganese value of the solution as follows: M-- (WJV3) X 0.165 0) where: M = manganese equivalent of the KMn04 solution, g/ mL, W4 = sodium oxalate used, g, and V3 = KMn04 solution required for the titration, mL. 19.2 Sodium Bismuthate (NaBi03). 19.3 Ferrous Ammonium Sulfate Solution--To 12 g of ferrous ammonium sulfate (Fe(NH4)2(S04)2*6H20) add 25 mL of H2S04 (sp gr 1.84) and 25 mL of H3P04 (85 %) and dilute to 1 L with water. Each day the solution is used run a blank titration against the KMn04 as follows: Measure into a 200-mL Erlenmeyer flask 50 mL of HN03 (1+3), cool, and add about 0.2 g of NaBi03. Dilute with 50 mL of HN03 (3+97), filter by suction through Gooch crucible with a medium porosity fritted disk into a 300-mL Erlenmeyer flask, and wash with 50 mL of HN03 (3 + 97). Run in exactly 25 mL of the ferrous solution and titrate to a faint pink color with the KMn04 solution.20 20. Procedure 20.1 Ignite 1 g of the sample in a porcelain crucible at a dull red heat to destroy organic matter. Transfer to a platinum dish and add 10 mL of water, 4 mL ofH2S04 (sp gr 1.84), 20 mL of HF (48 %), and a few drops of H2S03. Evaporate until the H2S04 fumes freely, cool, and add 25 mL of HN03 (1+3). If no appreciable residue remains, transfer to a 100-mL volumetric flask, using 25 mL of HN03 (1+3) to rinse the dish, dilute to the mark with water, and mix thoroughly. If there is an appreciable residue, filter I through a small qualitative filter paper and wash with water. Ignite the residue in a platinum crucible, and fuse with a little sodium pyrosulfate (Na2S207) or potassium pyrosulfate (K2S207). Dissolve in water, with the addition of a little HN03, add to the main filtrate, and evaporate nearly to dryness. Take up in HN03 (1+3) and transfer to the flask as before. 20.2 Pipet a 10-mL aliquot into a 200-mL Erlenmeyer flask and add 30 mL of water and 10 tnL of HN03 (sp gr 1.42). Add about 0.5 g ofNaBi03 and heat for a few minutes, or until the pink color has disappeared with or without the precipitation of magnesium dioxide (Mn02). Add a few small crystals ofsodium nitrite (NaN02) or potassium nitrite (KN02) to dissolve the MnO? and boil the solution several minutes to expel nitrous oxide fumes (a little anhydrous sodium carbonate (Na2C03) will aid this). Add water to bring the volume up to 50 mL and cool to about 15C.' Add about 0.5 g of bismuthate and shake the flask well. Add 50 mL of HN03 (3+97), filter by suction through an asbestos felt into a 300-mL Erlenmeyer flask, and wash with 50 to 100 mL of the HN03 (3+97). Run in exactly 25 mL of ferrous ammonium sulfate solution and titrate to a faint pink color with KMn04 solution. &'() 3--If 25 mL of ferrous ammonium sulfate solution is not sufficient to decolorize the solution, add a further 10 mL or more as required. Adjust the blank (19.3) accordingly. 20.3 Calculation--Calculate the percent of manganese, A, as follows: A = l(B2 - V4W/WS1 x 100 (8) where: B2 = KMn04 solution required for titration of the blank (18.3), mL, VA = KMnO,, solution required for back-titration of the specimen (19.2), mL, M = manganese equivalent of the KMn04 solution, g/mL, and Ws = sample in the aliquot, g. PIGMENT PASTES IN OIL 21. Pigment Content 21.1 Determine pigment content in accordance with Test Methods D 1208. 22. Moisture and Other Volatile Matter - 22.1 Determine moisture and other volatile matter in accordance with Test Methods D 1208. 23. Nonvolatile Matter in Vehicle 23.1 Subtract the percent pigment content and percent volatile matter from 100 and report as percent vehicle. 24. Moisture by Distillation 24.1 Determine moisture by distillation in accordance with Test Methods D 1208. ' 25. Coarse Particles and Skins 25.1 Determine coarse particles and skins in accordance with Test Methods D 185. 26. Consistency (Stormer) 26.1 Determine consistency in accordance with Test Method D 562. DUP0502 96546 D 50 21. Keywords 27.1 brown pigment (iron and manganese); calcium; col- ored pigment; iron oxide; red pigment; soluble sulfate; yellow pigment The American Society lor Tearing and Materials takes no poaition respecting the validity at 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 IInotrevised, either reapproved or withdrawn. Your comments are invited either for revlslonof 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 mky attend. if you teaI that your comments have not received a fair hearing you should make your views knowh to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. :< . ; ,'f - H- . DUP050296547 Designation: D 79 - 86 American Association state Highway and Transportation Officials Standard AASHTO No.: M124 Standard Specification for Zinc Oxide Pigments1 This standard is issued under the fixed, designation D79; the number immediately following the designation indicates the year of original adoption of, in the case of revision, the year oflasl 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 known as "zinc white" or zinc oxide. The pigments may be purchased in the dry form or. as a paste in oil. *+,---Zinc oxides are used in many industries. For additional information, see Specification D4295 and Test Methods D4315 for descriptions of zinc oxide use in rubber compounding. Jf 2. Referenced Documents $1 2.1 ASTM Standards: v'" D185 Test Methods for Coarse Particles in Pigments, * Pastes, and Paints12 : D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in 1 Pigments3 I D281 Test Method for Oil Absorption of Pigments by JS; Spatula Rub-Out3 D 332 Test Method for Relative Tinting Strength of White i Pigments by Visual Observation3 D1483 Test Method for Oil Absorption of Pigments by Gardner-Coleman Method3 D2745 Test Method for Relative Tinting Strength of White Pigments by Reflectance Measurements3 D3280 Test Methods for Analysis of White Zinc Pigments3 D4295 Classification for Rubber Compounding Materi als--Zinc Oxide4 D4315 Test Methods for Rubber Compounding Mate rial--Zinc Oxide4 E 20 Practice for Particle Size Analysis of Particulate Substances in the Range of 0.2 to 75 pm by Optical Microscopy5 3. Significance and Use * 3.1 Zinc oxide functions as both a chemical and a pigment. It is used in a variety of applications including rubber, paint, reprography, glass, chemicals, etc. In paint, it contributes to mildew protection, ultraviolet absorption, hiding power, and neutralization of acids formed upon oxidation of the paint film. 1 This specification is under the jurisdiction ofASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved April 25, 1986. Published June 1986. Originally published as D 79 - 21 T. Last previous edition D 79 - 80. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vol 09.01. s Annual Book ofASTM Standards. Vol 14.02. 4.Composition and Properties 4.1 Dry Pigment, French Process--In the manufacture of French process zinc oxide, metallic zinc is vaporized, either . in a boiler or a, refining column, and the resulting vapor is burned in a controlled manner in an orifice. The fine particles of zinc oxide are Cooled enough to agglomerate and are collected by a system of fabric bags. French process oxide shall conform to the properties listed in Table 1. 4.2 Dry Pigment, American,Process-~lnJik manufacture of American process zinc oxidie, zinc ore is reduced in the presence of a carbonaceous fuel. The resulting vapor is burned in a combustion chamber, and the fine particles of zinc oxide are cooled enough to agglomerate and are collected by a system of fabric bags. American process oxide shall conform to the properties listed in Table 1. 4.3 Paste in Oil--The paste shall be made by thoroughly grinding the specified pigment with linseed oil. As received it shall not be caked in the container and shall break up readily in oil to form a smooth paint of brushing consistency. The paste shall conform to the following requirements: Pigment, % Linseed oil, % Moisture and other volatile matter, max, % Coarse particles and sidas (total residue retained on a No. 325 (45-jtm) sieve), max, % ofthe dry pigment ^ 80 to 86 14 to 20 0.S 1.5 4.4 In such physical properties as are specified by the purchaser, the pigment shall satisfactorily match a reference sample mutually agreed upon by the purchaser and the seller. The most frequently specified properties are -oil absorption, tinting strength, and particle shape. Appropriate test methods are listed in Section 6. In-the event that-either an acicular type or a nodular (spherical) type* ofzinc oxide is desired, the particle shape shall be determined by examining or photographing microscopic mounts (lOOQx or more) of the sample and the mutually agreed upon standard that are ~ to be prepared as specified in Practice E 20. S. Sampling 5.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing TABLE 1 Composition Zinc oxide, min, % Total sulfur, max, % Moisture and other volatile matter, max, % Total Impurities, Including moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-pra) sieve), max, % French Process 99 0.1 0.5 1.0 0.10 American Process 98.5 0.2 0.5 1.5 0.25 DUP050296548 D 79 between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb, two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 6. Test Methods 6.1 Tests shall be conducted in accordance with the appropriate ASTM test methods, where applicable. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 6.1.1 Coarse Particles--Test Methods D 185. 6.1.2 Moisture in Pigments--Test Methods D 280. 6.1.3 Chemical Analysis of 'Dry Pigments--Methods D 3280. 6.1.4 Oil Absorption of Pigments by Gardner-Colemar, Method--Test Method D 1483. 6.1.5 Oil Absorption of Pigments by Spatula Rub-Out-- Test Method D 281. 6.1.6 Instrumental Tinting Strength of White Pigments-- Test Method D 2745. 6.1.7 Tinting Strength of White Pigments--Test Methoc D332. 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 oi 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 every five years and Ifnot revised, eitherreapproved or withdrawn. Your comments areinvited either tor 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. 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. 28 If DUP050296549 Designation: D 81 - 87 Standard Specification for Basic Carbonate White Lead Pigment1 This standard is issued under the fixed designation D 81; the number immediately following the designation indicates the year of original adoption or.'in the case of revision; the year oflast revision. A number inparentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reappirbval. p. Scope 1.1 This specification covers the material commercially ffcnown as basic carbonate white lead, used as a pigment and i putty. The pigment may be purchased in the dry form or i a paste in oil. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments3 D1208 Test Methods for Common Properties of Certain Pigments3 D1301 Test Methods for Chemical Analysis of White Lead Pigments3 13. Composition and Properties 3.1 Dry Pigment--The pigment shall be free of adulterants and shall contain not more than traces of impurities Iiincident to well-controlled manufacture of high-grade basic tcarbonate white lead. The pigment shall conform to the f following requirements: If Lead carbonate, % Moisture and other volatile matter, max, % - t Total other impurities, max, % f Coarse particles (total residue retained on a No. ! 325 (45-fiir) sieve), max, % 62 to 75 0.7 1.0 1.0 3.2 Paste in Oil--The paste shall be made by thoroughly ; grinding the specified pigment with linseed oil. The paste shall not be caked in the container and shall break up readily in oil to form a smooth paint of brushing consistency. The paste shall conform to the following requirements: Figment, min, % Linseed oil, max, % * Moisture and other volatile matter, max, % Coarse particles and skins (total residue retained on a 89 11 0.7 1.5 No. 325 (45-jim) sieve), max, % of the dry pigment 3.3 Semipaste Containing Volatile Thinner--The semi- 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 D01.31 on Pigment Specifications. Current edition approved May 29, 1987. Published July 1987. Originally published as D 81 - 21 T. Last previous edition D 81 - 80 (1986)!l. 3 Annual Book o]ASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. paste shall be made by thoroughly grinding the specified pigment with a mixture of linseed oil and a small amount of volatile thinner. The semipaste shall not be caked in the container and shall be readily stirred to a uniform mixture which shall mix readily with oil, turpentine, or volatile petroleum spirits to form a smooth paint of brushing consistency. The odor of the semipaste, as taken from the container, while drying or after drying, shall be not abnor mally pungent or disagreeable. The semipaste shall conform to the following requirements: Pigment, min, % Linseed oil, max, % Moisture and other volatile matter, % A Moisture, max, % Coarse particles and skins (total residue retained on a No. 325 (45-pm) sieve), max, % of tbe dry pigment 87.5 10.5 1.5 to 3.0 0.7 1.5 A The volatile matter shall be turpentine, volatile petroleum spirits, or any mixture thereof. 3.4 The color and color strength, when specified, shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except thatJor shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample". 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures not cov ered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 5.1.1 Coarse Particles--Test Methods D 185. 5.1.2 Moisture in Pigment--Test Methods D 280. 5.1.3 Lead Carbonate and Total Other Impurities--Test Methods D 1301. 5.1.4 Pigment, Linseed Oil, and Moisture and Other Volatile Matter in Paste in Oil--Test Methods D 1208. t,t, '1 **> 29 DUP050296550 # D 81 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 Otis 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 any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, either reapproved orwithdrawn. Your comments are Invited either lor revision otthis standard or lor additionalstandards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at $ meeting of the responsible technical dommittee, which you they attend. If you feel that your comments have not received a fair hearing you should make your views known to me ASTM Committee on Standards, 1918 Race St., PhBadaiphia, PA 19103. DUP050296551 Designation: D 83 - 84 (Reapproved 1989) Standard Specification for Red Lead Pigment1 This standard is issued under the fixed designation D 83; 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 reappioval. A superscript epsilon <0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers four grades of red pigment commercially known as red lead. The pigment may be purchased in the dry form or as a paste in oil. 2. Referenced Documents 2.1 ASTM Standards: D49 Test Methods for Chemical Analysis of Red Lead12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 Dry Pigment--The pigment shall be made by roasting litharge or metallic lead, or compounds of lead that yield litharge by heating, and shall consist entirely of oxides of lead, free of adulterants. The four grades of pigment shall conform to the following requirements: True red lead (Pb30), min, %: 85 % grade 95 % grade 97 % grade 98 % grade Total impurities including moisture, water soluble matter, and matter insoluble in a mixture of nitric acid and hydrogen peroxide, max, % Lead monoxide, PbO Coarse particles (total residue retained on a 45-jtm (No. 325) sieve), max, % 85 95 97 98 1.0 remainder 1.0 When mixed as indicated in the following table, the resulting paint, brushed on a smooth vertical iron surface, shall dry hard and elastic without running, streaking, or sagging: Dry red lead Raw linseed oil Turpentine Liquid drier 20 lb (9.1 kg) 5 pt (2.4 L) 2 gills (0.24 L) . 2 gills (0.24 L) 3.2 Paste in Oil--The paste shall be made by thoroughly grinding the specified pigment with linseed oil (Note). The 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.3I on Pigment Specifications. Current edition approved Aug 31,1984. Published December 1984. Originally published as D 83 - 21 T. Last previous edition D 83 - 73 (I984)'1. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. paste as shipped by the seller, and for three months there after, shall not be caked in the container, and shall break up readily in oil to form a smooth paint of brushing consistency. The paste shall conform to the following requirements: Pigment, % Linseed oil, % Moisture and other volatile matter, max, % Coarse particles and skins (total residue retained on a No. 325 (45-jxm) sieve), max, % of the dry pigment 92 to 94 6.0 to 8.0 0.5 15 When mixed as indicated in the following table, the resulting paint, brushed on a smooth, vertical iron surface, shall dry hard and elastic without running, streaking, or sagging: Red lead paste Raw linseed oil Turpentine Liquid drier 20 lb (9.1 kg) 3 pt (1.4 L) 2 gifis (0.24 L) 2 gills (0.24 L) No t e--The storage of paste red lead in places of high temperature should be avoided, as heat accelerates the tendency of this material to cake or harden. Purchasers are cautioned that 85 % grade red lead should not be bought in paste form. The 95 % grade, if made into paste, should be used within a short period of time alter grinding. When pure red lead paste is to be stored for a considerable period oftime, the 97 % or 98 % grade of red lead should be specified. Therefore the manufac turer shall identify the grade ofred lead used in the paste and the date of manufacture. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall. be taken from different packages in the ratio of two samples for .each 10 000 lb (5000Jcg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or afterblending in equal quantities the samples from the production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Chemical Analysis--Methods D 49. 5.1.2 Coarse Particles--Test Methods D 185. 5.1.3 Pigment, Linseed Oil, and Moisture and Other Volatile Matter in Paste in Oil--Test Methods D 1208. T .... .. * w DUP0502 96552 DUP050296553 Designation: D 85 - 87 (Reapproved 1991)e1 Standard Specification for Ochre Pigment1 This standard is issued under the fixed designation D 85; the number immediately following tbe 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 (c) indicates an editorial change since the last revision or reapproval. ./0161 --Keywords were added editorially in July 1991. 1. Scope 1.1 This specification covers ferrous earthy pigment in cluded under the general term "ochre." The pigment may be purchased in the dry form. 2,, Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and. Other Matter Volatile under the Test Conditions) in Pigments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 The pigment shall be a hydrated oxide of iron permeating a siliceous base and shall be free from added impurities and added coloring matter. The pigment shall conform to the following requirements: 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 1.31 on Pigment Specifications. Current edition approved June 26, 1987. Pubb'shed August 1987. Originally published as D 85 - 21. Last previous edition D 85 - 81 (1986)*'. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. Ferric oxide, min, % Calcium oxide, max, % Lead chromate Organic coloring matter Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % 17 5 none none 1.0 1.0 3.2 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken.- At the option ofv the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM methods shall be mutually agreed upon between the purchaser and the seller. ........... 5.2 Chemical Analysis ofDry Figment--Methods D 50. 5.3 Coarse-Particles--Test Methods D 185. 5.4 Mass Color and Tinting Strength--Test Method D 387. 5.5 Volatile Matter--Test Methods D 1208. 5.6 Moisture--Test Methods D 280. .6 Keywords 6.1 ferrous; hydrated iron oxide; ochre; pigment The American Society lor Testing and Materials takes no position respecting the validity cl 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 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 live years and it not revised, either reapproved or withdrawn. Yourcomments are invited either forrevision ofthis standard or.for additional standards and should be addressed td ASTM Headquarters. Your comments will recsive careful consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that yotir comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Face St., Philadelphia, PA 19103. Designation: D 126 - 87 (Reapproved 1991)e1 Standard Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green1 Tbis standard is issued under the fixed designation D 126; 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 hate been approvedfor use by agencies ofthe Department ofDefense to replace Method 7121 ofFederal Test Method StandardNo. 141A. Catsuit the DoD Index ofSpecifications and Standardsfor Ike specific year ofissue which has been adopted by the Department ofDefense. 2 34567Keywords were added editorially in June 1991. .i 1. Scope statements are given in Note 3. - i T 1.1 These test methods cover procedures for the chemical analysis-of yellow, orange, and green pigments containing lead chromate and chromium oxide green. 1.2 The analytical procedures appear in the following order: Sections 89:;9< =>??@AB CDEFGH IJ7KLM N 7OP QRSTUV7WX YZ7[\] Organic Colors and Lakes................................. . Moisture and Other Volatile Matter.............................. Matter Soluble in Water ..:............................ ............... Lead Chromate ........... ........ ................................ .. : r Total Lead................... ;................................... ............., Sulfate....................................................... Carbon Dioxide.................................................. Molybdenum...................................... .............. '......... Extenders'.......................v.V...........'. -- ....................... Calculation of Substances Other than Insoluble Lead Compounds....................................................................... 7 8 9 10 and 11 12 . 16 and 17 18 to 22 23 arid24 15 ^_`a bcdefg hijjk 7lm nopqrop 8DEFGH stuuv Organic Colors and Lakes................. '.............................. Moisture and Other Volatile Matter............. ................... Matter Soluble in Water................... . ..................... ....... Iron Blue ........................................................................ Lead Chromate............................................................... Barium Sulfate and Insoluble Siliceous Material............... Total Lead................................... ................... ....... ......... Sulfate,............................................................ ,............... Calcium Oxide Soluble in Arid.......................................... Extenders............................................................................... Calculation of Insoluble Lead Com pounds ....................................*...........37 25 26. 27- 28 29 and30. 31 32 33 34 and 35 36 wxyz{|}{ ~ h Organic Colors and Lakes....................................................... Moisture and Other Volatile Matter................................... Matter Soluble in Water........................................................ Total Chromium as Chromium Oxide.................................... 38 39 40 41 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. Specific hazard 2. Referenced Documents 2.1 ASTM Standards: ***" D 280 Test Methods foir Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D52I Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)2 D 1013 Test Method'for Determining Total Nitrogen in Resins and Plastics2 - , -. D 1193 Specification for Reagent Water3' , 13Ean1d114 Specification for Wire-Cloth Sieves for'Testing Pur poses4 .. . , 3. Summary of Test Methods 3.1 Chrome Yellow, Chrome Orange, and Molybdate Orange: 3.1.1. .Organic colors and lakes are determined qualita tively by boiling the sample in water, then ethyl alcohol, and finally chloroform. \! . 3.1.2 Moisture and other volatile matter are determined in accordance with Test Method A of Test Methods D 280. 3.1.3 Matter soluble in water is determined by boiling in water and filtering. ' 3.1.4 Lead chromate is determined by dissolving the sample in dilute HQ, filtering and titrating potentio- metrically with FeSO* solution after addition of HGi04. r- 3.1.5 Total lead is determined by precipitation as lead sulfide solution with H2S04 and final precipitation as lead sulfate. 3.1.6 Sulfate is determined by dissolving the sample in acetic add, neutralizing with sodium carbonate, plus addi tion of HC1 to an aliquot followed by addition of BaQ2 to predpitate as barium sulfate. 3.1.7 Carbon dioxide is determined by evolution. 3.1.8 Molybdenum is determined by predpitation as the sulfide, solution in HN03 and H2S04, addition of NH4OH 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 May 29, 1987. Published July 1987. Originally published as D 126 - 22. Last previous edition D 126 - 65 (I981)l. 2 Annual Book cfASTM Standards, Vol 06.02. 3 Annual Book cfASTM Standards, Vols 06.03 and 11.01. * Annual Book cfASTM Standards Vol 14.02. 34 DUP050296555 D 126 Bad H2S04. The solution is reduced in a Jones reductor, pbllected under Fe2(S04)3 solution and titrated with KMn04 lolution. | ,3-1.9 Extenders ar?.either; S i 3.1.9.1 Calcium carbonate, calcium sulfate, magnesium Carbonate pr; . , fa) The compounds in 3.1.9.1 are determined qualitatively jtjy precipitation With ammonium solution. (b) If chromium is present, it is reduced and the lead salts Ived in dissolving solution. Hydroxides and hydrous q^ides are precipitated by addition of HC1 and NIJ4OH and filtered. CaC204 is precipitated with calcium oxalate solution. 1^. ahd. filtered, ashed and weighed as CaO. .Alternatively, the "4 precipitate is dissolved in H2S04 and titrated with KMn04. Mdeatgenrmesiniuamtionisbyd.eptreercmipiniteadtioonhastthhee pfhiltorsaptehatferowmithcaamlcmiuomnium phosphate solution; 3.2 Chromium Oxide Green: 3.2. i Organic .colors and lakes are determined qualita tively hy boiling the sample in water, then ethyl alcohol, and finally choloroform. ri ft* 3.2.2 Moisture and other volatile matter are determined id accordance with Test Method A of Test Methods D 280. , 3.2.3 Matter soluble in water is determined by boiling in water and filteilhg.' 3.2.4 Total chromium as chromium oxide is determined by dissolving the sample in dilute HC1, filtering and titrating potentiometrically with FeS04 solution after addition of HC104. 4. Significance and Use 4.1 These test methods are for analysis designed as an aid in quality of yellow, orange, and green pigments containing lead, .chromate and chromium oxide green. Some sections may ' be applicable tp analysis of these pigments when extracted from whole paints. 5. Purity of Reagents and Water 5.1 Reagents--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. 5.2 Water--Unless otherwise indicated, references to water for Use in the preparation of reagents and in analytical procedures shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6. Preparation of Sample 6.1 Mix the sample thoroughly and take a representative portion for analysis. Reduce any lumps or coarse particles to a fine powder by grinding. Grind extracted pigments to pass a No. 80 (180-pm) sieve (Note 1). Discard any skins that do not pass through the sieve. Thoroughly mix the finely ground pigment and preserve in stoppered and suitably identified bottles or containers. 1--Detailed requirements for this sieve are given in Specifica tion E It. 6.2 Moisten the weighed portions of extracted pigments with a small amount ofsuitable wetting agent (Note 1) before adding reagents for analysis. 2--A 0.1 % solution of sodium dioctylsuccinosulfonate has been found satisfactory. (This material is sold under the trade name of Aerosol OT.) Wetting agents containing mineral salts, sulfates, or sulfonates which may be hydrolyzed to sulfates, should be avoided; the use of alcohol is also undesirable because of its tendency to reduce chromate3s.: . Precaution--As 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 the sample. The wearing of a respirator and rubber or synthetic gloves are recommended. If hexavalent chromium materials come in contact with the skin, wash thoroughly with soap and water. '"Reagent Chemicals, American Chemical Society, Specifications,"--Am. Chem. 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 Nosttand Co., Inc., New York, NY, and the "United States Pharmacopeia." CHROME YELLOW, CHROME ORANGE, AND MOLYBDATE ORANGE ir (Primrose, Lemon, and Medium Yellows; Chrome Oranges; Lead Molybdate or Basic-Lead Chromate; Molybdate Orange) ORGANIC COLORS AND LAKES , 7. Procedure 7.1 Boil 2 g of the sample 2 mufwith 25 mL of water, let settle, and decant the supernatant liquid. Similarly, boil the residue with 25 mL of ethyl alcohol (absolute or 95%) and decant as before. Likewise boil with 25 mL of chloroform and again decant. If any one of the above solutions is colored, organic colors are present. If all solutions remain colorless, organic colors are presumably absent. The presence of organic colors resistant to the above reagents is unlikely, but may be tested for by reference to procedures given in standard reference works.6 MOISTURE AND OTHER VOLATILE MATTER 8. Procedure 8.1 Determine moisture and other volatile matter in accordance with Test Method A of Test Method D 280. 6 Reference may be made to the following: Payne. H. F., "Organic Coatings Technology," Vol U, John Wiley & Sons, Inc., New York, NY, 1961. 35 DU P050296556 MATTER SOLUBLE IN WATER D 126 TOTAL LEAD7 9. Procedure 9.1 Place 2.5 g ofthe sample in a graduated 250-mL flask. Add 100 mL of water and boil for 5 min. Cool, dilute to exactly 250 mL, mix, and allow to settle. Filter die superna tant liquid through a dry paper and discard the first 20 mL. Evaporate 100 mL of the clear filtrate to dryness in a weighed dish, heat for 1 h at 105 to 110'C, cool, and weigh. 9.2 Calculation--Calculate the % of matter soluble in water as follows: Matter soluble in water, % = (R x 2.5 x 1001/5 where: R = weight of residue, and S = specimen weight, g. LEAD CHROMATE7 10. Reagents 10.1 Dissolving Solution--Saturate 1 L of water with NaCl. Filter. Add to the filtered solution 150 mL of water and 100 mL of HC1 (sp gr 1.19). 10.2 Ferrous Sulfate, Standard Solution (0.3 N)--Dis solve 86 g of FeS04-7H20 in 500 mL of water to which 30 mL of H2S04 (sp gr 1.84) has been added with constant stirring. Dilute to 1 L and standardize not more than 6 h before use by potentiometric titration against 0.7-g portions of K.2Cr207. 11. Procedure 11.1 Dissolve 1 g of the sample in 150 mL of the dissolving solution. Agitate for 10 to 15 min, keeping the solution cold until dissolution is complete (Note 4). If dissolution is not complete, filter through fine grade filter paper and wash with three 10-mL portions ofcold dissolving solution. Add 10 mL of HC104 (70 %), dilute to 250 mL, and titrate potentiometrically with FeS04 solution. --Incomplete solution of the pigment is evidence of the possible presence of barium sulfate, silica, silicates, or other acidinsoluble extenders (see Section 1S). Some chrome yellows may contain organic addition agents and will give a turbid solution at this point. Newer chemically resistant-type lead chromate type pigments (silica encapsulated) cannot be decomposed by the procedures described in this method. Pigments of this type may require treatment with strong alkali hydroxide or hydrofluoric acid. Also, if trivalent antimony has been used in manufacturing the product, pentavalent antimony may be present which would interfere in the determination of lead chromate. 11.2 Alternatively, the solution may be reduced by a known excess of FeS04 solution and back-titrated with KMn04 solution in the presence of MnS04, or excess KI may be added and the liberated iodine titrated with Na2S203 solution, using starch indicator. The iodine liberation method is not applicable in the presence of molybdenum. 12. Procedure 12.1 Dissolve 0.5 g of sample as described in Section 11. Add 5 mL of ethyl alcohol (95 % or absolute) and boil until the chromium is reduced, as indicated by a green color. Filter if any insoluble residue is present, retaining the filtrate and washings for the determination. Add NHjOH (sp gr 0.90) to this solution until a faint precipitate begins to form; then add 5 mL of HQ (sp gr 1.19) slowly, dilute to 500 mL, and pass a rapid current of H2S into the solution until precipitation is complete. Settle, filter, and wash with water containing H2S. 12.2 Rinse the precipitate from the filter (Note 5) into a beaker containing 25 mL of HN03 (1+3) and bofl until all PbS has dissolved. Add 10 mL of H2S04 (1+1) and evaporate to strong fumes of S03. Cool and add 50 mL of water and 50 mL of ethyl alcohol (95 %) (Note 6). Let stand 1 hj.then filter on a tarred Gooch crucible. Wash with ethyl alcohol (95 %), dry, ignite at 500 to 600C, and weigh as PbS04. 5--If a trace of sulfide remains on the paper, the stained portion of the paper may be separately treated with bromine water, the paper filtered off, and the filtrate added to the body of the solution. 6--Any sulfur remaining from decomposition of the sulfides may be mechanically removed as a globule of solidified sulfur' at this point. SULFATE7 13. Reagents 13.1 Barium Chloride Solution--Dissolve 117 g of BaCl2'2H20 in water and dilute to 1 L. 13.2 Dissolving Solution--See Section 10.1. 13.3 Sodium Carbonate Solution (saturated)--Prepare a solution containing excess Na2C03 at laboratory tempera ture, and free of S04. Decant the dear solution for use as required. - 14. Procedure . 14.1 Digest 1.25 g of the sample^with 100 mL of dis solving solution at 100*C for 5 min. Add 25 mL of glacial acetic acid and 15 mLof ethyl alcohol and heat gently for 10 min to reduce chromium, as indicated by the green color of the solution. Cool. Neutralize with saturated Na2C03 solu tion and add a slight excess. Transfer to a 250-mL volumetric flask, dilute to the mark with distilled water, and mix. Filter without washing through a dry filter paper, discarding the first 10 to 15 mL. 14.2 Take a 200-mL aliquot of the filtrate, neutralize with HQ (1+1), and add 10 mL excess. Heat to boiling and boil for 5 min. To the gently boiling solution, add 15 mL of BaQ2 solution dropwise with constant stirring. Digest On a steam bath for 2 h. Filter through an ignited tamed Gooch crucible, wash with HC1 (1+99), and finally with hot water. Dry at 105 to 110C, ignite at 900C, and weigh. CARBON DIOXIDE7 7 Sections 23 and 24 under "Calculation of Substances Other than Insoluble Lead Compounds" should be tead carefully before proceeding with the analyses described in Sections 10 to 22. 15. Procedure 15.1 Determine C02 by the evolution method on 2.5 g of m - ... DU P050296557 # D 126 sample, using dilute HN03 free of NO or N02 and I the C02 in soda lime or in KOH solution. MOLYBDENUM7 Reagents | 16.1 Ferric Sulfate Solution--Dissolve 20 g of Fe2(S04)3 (NH4)2S04 24H20 in 200 mL of water to which Sheen added 50 mL of H2S04 (sp gr 1.84) and 20 mL of ?04 (85. %), and dilute to 1 L. 16.2 Jones Redactor--The reductor shall contain at least '''4'35-cm column of amalgamated zinc, prepared by shaking ' 20 to 30-mesh zinc free of iron or carbon with HgCl2 on (20 g/L) in sufficient quantity to produce an .;amalgam containing 1 to 5 % of mercury, and supported by suitable inert pad of asbestos, glass wool, or other inert " material. I 'f 16.3 Potassium Permanganate, Standard Solution (0.1 N)--Dissolve 3.16 g of KMn04 in water and dilute to 1 L. ^ Let stand 8 to 14 days, siphon offthe clear solution (or filter Jgphrough a medium porosity fritted disk), and standardize gigainst the National Bureau of Standards standard sample Jo. 40 ofsodium oxalate (Na2C204) as follows: In a 400-mL (beaker dissolve' 0.2500 to 0.3000 g of the Bureau of Standards sodium oxalate in 250 mL of hot water (80 to 90*C) and add 15 mL of H2S04 (1+1). Titrate at once with KMn04 solution, stirring the liquid vigorously and continu ously. 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 tlropwise with particular care to allow each drop to be fully decolorized before the next is introduced. The solution shall not be below 60C by the time the end point has been 1 reached. (More 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 (non-mercury type) as a stirring rod is most convenient) Keep the KMn04 solution in a glass-stoppered bottle painted black to keep out fight, 'or in a brown glass bottle stored in a dark place.17 17. Procedure 17.1 Dissolve 1 g of the sample as described in Section 11. Add 5 mL of ethyl alcohol (95 % or absolute) and boil until chromium is reduced. Filter if any insoluble residue is present, retaining the filtrate and washings. Add NH4OH (sp gr 0.90) cautiously until a faint precipitate begins to form, then add 15 mL of H2S04 (sp gr 1.84)'and dilute to 300 mL. Heat to boiling, pass in a rapid stream of H2S for 15 min, and dilute with 300 mL of hot water. Pass in H2S for 10 min, boil for 3 min, and cool. Pass in H2S for 10 min, and let | ||i stand at room temperature for 1 h. Filter and wash with H2S04 (1+99) saturated with H2S. till- 17.2 Rinse the sulfide precipitate into the original beaker and add 20 mL ofHN03 (sp gr 1.42) and 5 mL of H2S04 (sp gr 1.84) (see Note 5). Cover and heat to fumes. Cool, add 10 mL of HN03 (sp gr 1.42), and again fume. Repeat this operation if necessary until a light-colored solution is ob tained. Wash the cover and inside Of the beaker and fume again to remove all HN03. Dilute to 200 mL and add NH4OH (1+4) until neutral; then add 10 mL ofH2S04 (sp gr L84). 17.3Cool the solution and reduce by passing through a Jones reductor at a rate not exceeding 100 mL/min, col lecting the effluent under 200 mL of Fe2(S04)3 solution. Titrate with KMn04 solution. A blank determination should also be made. EXTENDERS7 18. General Considerations 18.1 Extenders fall into two groups, depending on their solubility or insolubility in the dissolving solution described in Section 10, as follows: A. Extenders Soluble in Dissolving Solution--Calcium sulfate (gypsum), calcium carbonate (whiting), and magne sium carbonate. B. Extenders Insoluble in Dissolving Solution--Silica, magnesium silicate, and clay (Note 7). 18.2 Extenders of group A may be present if the analysis shows sulfates and carbonates to be in the pigment, and are absent if sulfate and carbonate are absent. Since die latter situation rarely exists, it is advisable to test for the presence of calcium and magnesium to determine if extenders are present Extenders ofgroup B are recognized as an insoluble residue following add solution of the pigment, and may be determined quantitatively if desired, by the method de scribed in Section 31. Extenders of group A, if present, may affect'the calculation of insoluble lead compounds as given in Section 23. Their qualitative or quantitative estimation may be necessary. 7--Some lead chromates may contain zirconium or titanium compounds, some ofwhich are insoluble in the dissolving solution, but are not to be considered as extenders, since they have been added to imprbve the properties of the pigment Qualitative Detection ofExtenders ofGroup A 19. Reagents 19.1 Ammonium Phosphate Solution--Dissolve 100 g of (NH4)2HP04 in water and dilute to 1 L. 20. Procedure 20.1 Dissolve 1 g of the sample as describedin Section 11. Add 5 mL of ethyl alcohol (95 % or absoTute>and'boil Until the chromium isreduced. An insoluble residue at this point denotes the presence of extenders of Group B. Filter if necessary and wash well. 20.2 To the filtrate, add NH4OH (1+4) until just ammoniacal, boil 5 min, and allow to digest in a warm place until the precipitate has coagulated. Filter, washing well with hot water and reserving the filtrate. Dissolve the precipitate on the filter with HQ (1+1), washing back into the original beaker. Reprecipitate, filter, and wash as before' 20.3 Combine the washings, make just acid with HC1 (1+1), and evaporate to a volume of about 250 mL. Add 50 mL of (NH4)2HP04 solution, cool, and add 50 mL of NH4OH (sp gr 0.90). Allow to stand overnight. A precipitate indicates the presence of extenders of Group A. Quantitative Determination ofExtenders of Group A 21. Reagents 21.1 Ammonium Oxalate Solution--Dissolve 30 g of 37 DUP050296558 D 126 ammonium oxalate in water and dilute to 1 L. 21.2 Ammonium Phosphate Solution--See Section 19. 22.Procedure 22.1 If the sample is a chrome yellow or orange use the procedure given in Section 14 for dissolving and reducing chromium. For other chromium pigments heat gently 2 g of sample in a porcelain dish without ignition until iron blue, if present, is just decomposed. Transfer to a beaker and dissolve the lead salts in 150 mL of dissolving solution as described in Section 11. 22.2 Add 20 ml of HC1 (sp gr 1.19) and digest 1 h at lOO'C. Dilute to 300 mL, filter and wash thoroughly. . Add NH4OH (1+4) to the filtrate and washings until just ammoniacal, boil 5 min and allow to digest in a warm place until the hydroxides and hydrous oxides are coagulated. Filter, washing well with diluted water and reserve the filtrate. Redissolve the precipitate with HQ (1+1) washing back into the original beaker. Reprecipitate, filter and wash as before. Combine the washings with, the original filtrate and add 50 mL ofammonium oxalate solution. Filter offthe CaQCV precipitate on quantitative paper. Transfer to a tarred crucible, ash, ignite at 1300C, cool in a desiccator, and weigh as CaO. Alternatively, the washed precipitate may be dissolved in H2S04 (1+1) and the resulting solution titrated hot with 0.1 N KMn04 solution, as described in the Procedure section under Calcium in Test Methods D 521. 22.3 Make the filtrate from the calcium determination slightly acid with HC1 (1+1) and evaporate to 250 mL volume. Add 50 mL of (NH`4)2HP04 solution, cool, and add 50 mL of NH4OH (sp gr 0.90). Allow to stand overnight Filter on suitable quantitative paper, wash with NH40H (1+19), ignite in a platinum crucible at 1050C for 1 h and weigh. Care must be taken to char the paper slowly before igniting. 22.4 Calculation--Calculate the percent of extenders (as oxides) as follows: Calcium oxide, % = weight of CaO x 50 Magnesium oxide, % = weight of Mg2P207 x 18.11 The calculation of the amount of extenders as carbonates or sulfates is described in Section 24. CALCULATION OF SUBSTANCES OTHER THAN INSOLUBLE LEAD COMPOUNDS 23. Calculations Where Extenders Are Absent 23.1 "Insoluble lead compounds" in chrome yellow and chrome orange may consist of PbCr04, PbS04, 2PbC03*Pb(0H)2, PbO, or PbMo04. The first two are characteristic of the chrome yellows, the first, third, and fourth ofthe basic chrome oranges, and the first, second, and last of molybdate oranges. For purpose of determining conformance with specification requirements, where "in soluble lead compounds" are defined as above, make the following calculations If extenders are absent: 23.2 If molybdenum is present, calculate the percent of PbMo04 from the titration of Section 17 as follows: A = PbMo04, % - mL titration x normality of KMn04 x 12.24 23.3 Calculate the percent of PbCr04 from the titration of Section 11 as follows: B = PbCr04, % = mL titration x normality of FeS04 x 10.77 23.4 Calculate the percent of total lead as oxide and the percent of excess PbO from the analysis of Section 12 as follows: C = PbO, % = grams of PbSO, x 147.2 D - excess PbO, % =C-(0.6906 B + 0.6078 A) 23.5 Calculate the sulfate as S03 from the analysis of Section 14 as follows: E -- S03, % = grams of BaS04 X 34.3 23.5.1 If E is equal to or greater than 0.3587 D, the % of PbS04 equals 1.3587 D, and the % total insoluble lead compounds equals A + B + 1.3587 D. 23.5.2 If E is less than 0.3587 D, the percentage of PbS04 equals 3.788 E, and a new excess of PbO is calculated as follows: .F = Excess PbO, % = D -- 2.788 E 23.6 Calculate the percent of C02 from the analysis of Section 15 as follows: G *= C02, % = grams of C02 x 40 23.6.1 If G is equal to or greater than 0.1314 F, the percent of basic lead carbonate (2 PbC03-Pb(0H)2) is 1.1584 F and the percent of total insoluble lead compounds is A + B + 3.788 E + 1.1584 F. 23.6.2 If G is appreciably in excess, extenders are probably present. If G is less than 0.1314 F, the percent of 2 PbC03-Pb(0H)2 is 8.813 G and the exceSS'PbO is: H = Excess PbO, % -- F.~ 7.608 G . 23.62.1 The percent of total insoluble lead compounds is A + B + 3.788 E + 8.813 G + H. 24. Calculations Where Extenders Are Present -- 24.1 Ifextenders are present, calculate, the ,C02 equivalent as follows: -, I = COz equivalent of extenders = CaO, % x 0786 + MgO, %' X~1.100 24.2- If J is less than G, use G -- I as the net C02 for purposes calculating the 2PbCQ3 Pb(OH)2 content oflhe pigment. Total extenders = CaO, % + MgO, % + J 24.3 If I is greater than G, some of the extender is present as CaS04 (Note 8). Calculate the total percent ofextenders as follows: J = C02 equivalent of MgO = MgO % x 1.100 K = C02 present as CaC03 = G -- J -, CaC03, % - 2.73 K L = CaO present as sulfate, % = CaO, % 1.27 K CaS04< % = 2.43 L S03 combined as CaS04, % = 1.43 L 24.3.1 E -- 1.43 L equals the net S03 to be used for calculating the PbS04 content of the pigment. If / is greater 38 -------r-------;------ DUP050296559  D 126 I,;than G, no calculation of2PbC03 -Pb(OH)2 is necessary, and f.i.the excess PbO is given by F. Total extenders, % = 2.100 x MgO, % + 2.73 K + 2.43 L 8--It is impractical to detect by chemical means whether a pigment contains CaCOj and PbS04> or CaS04 and 2PbC03-Pb(0H)2. This calculation assumes the former as more probable. PURE CHROME GREEN AND REDUCED CHROME GREEN ORGANIC COLORS AND LAKES 25. Procedure IS 25.1 Determine organic colors and lakes in accordance with Section 7. MOISTURE AND OTHER VOLATILE MATTER 26. Procedure I 26.1 Determine moisture and other volatile matter in I accordance with Section 8. I MATTER SOLUBLE IN WATER 127. Procedure I 27.1 Determine matter soluble in water in accordance | with Section 9. I IRON BLUE <1 28. Procedure 28.1 Determine the total nitrogen (by the Kjeldahl| Gunning method) (Note 9) on 1 g of the sample, adding 2 g | of FeS04*7H20 before digestion for at least 2)h h. ' 9--For further details refer to Test Method D 1013. 28.2 Calculation--Calculate the percent erf iron blue as ; follows: Iron blue, % = nitrogen, % x 3.4 10--Qualitative tests may be made for other nitrogen-con taining blue pigments. LEAD CHROMATE 29. Reagents 29.1 Ferrous Sulfate, Standard Solution (0.3 N)--See Section 10.2. 29.2 Potassium Permanganate Standard Solution (0.1 N)--Prepare as described in 16.3. Standardization is unnec essary except for the alternative procedure given in Section 30. 30. Procedure 30.1 Mix thoroughly 1 g of sample with at least 10 g of Na202 in a 30-mL pure iron crucible. Heat gently until the fusion is complete; then heat strongly, rotating the crucible with iron tongs (not Nichrome or chromium plate) for a few minutes to ensure complete fusion. Allow to cool; then transfer the crucible and cover to a beaker containing 250 mL of water. When the action has ceased, rinse and remove the crucible and cover, and boil for at least 10 min to destroy excess peroxide. Make just acid with H2S04 (1+1) and add about 35 mL in excess. Add 2.5 mL of 0.1 N KMn04 solution and heat to boiling. Add 10 mL of HC1 (1+4) and boil to reduce manganese and lead as indicated by clearing of the solution. If the solution is not clear after 5 min boiling. add 5 mL of additional HC1 (1+4), and repeat until a clear solution is obtained. Cool and titrate with FeS04 solution on a potentiometric apparatus; or alternatively, add a measured excess ofFeS04 and back-titrate with KMn04 solution in the presence of MnS04. BARIUM SULFATE AND INSOLUBLE SILICEOUS MATERIAL8 31. Procedure 31.1 Heat gently 1 g of sample in a porcelain dish without ignition until the iron blue is just decomposed.- Transfer to a beaker and dissolve the lead salts as described in Section 11, warming if necessary. Filter through a tared Gooch crucible, wash thoroughly, ignite at 600 to 800C, and weigh. 31.2 Calculation---Calculate the percent of BaS04 and insoluble siliceous material as follows: BaS04 and insoluble siliceous material, % -- weight of precipitate X 100 TOTAL LEAD 32. Procedure 32.1 Determine total lead on the filtrate from the deter mination of BaS04 and insoluble matter ^(Section 31) in accordance with the directions of Section 12. SULFATE 33. Procedure 33.1 After decomposition of the iron blue.in 1.25 g of sample as described in Section 31, digesttfae residue with 20 mL of HC1 (sp gr 1.19) at 100C until solution is complete. Add 300 mL of water and heat to boiling. Filter and wash thoroughly. Determine sulfate on the filtrate and washings as described in Section 14. CALCIUM OXIDE SOLUBLE IN ACID 34. Reagents 34.1 Ammonium Oxalate Solution--See 21.1. 35. Procedure 35.1 Decompose 2 g of sample as described in Section 31. Add 20 mL of HQ (sp gr 1.19) and proceed in accordance with 21.1 to the end of the calcium determination. 35.2 Calculation--Calculate the percent of CaO soluble in acid as follows: 8 See Note 7 of Section 18. 39 DUFbS0296S60 # D 126 CaO soluble in acid, % = grams CaO x 50 EXTENDERS 36. Procedure 36.1 The method described, in Sections 3:1, 34, and 35 . suffices for the detection and estimation of all common extenders except MgC03. This may be tested for the filtrate from the CaO determination by the method described-in Section 22. CALCULATION OF INSOLUBLE LEAD COMPOUNDS 37. Procedure 37.1 The insoluble lead compounds may be calculated by the methods of Sectiqns 23 and 24. CHROMIUM OXIDE GREEN ORGANIC COLORS AND LAKES 38. Procedure 38.1 Determine organic colors and lakes in accordance with Section 7. MOISTURE AND OTHER VOLATILE MATTER 39. Procedure . .H ; 39.1 Determine in accordance with Section 8............ MATTER SOLUBLE IN WATER 40. Procedure 40.1 Determine in accordance with Section 9. TOTAL CHROMIUM AS CHROMIUM OXIDE' 41. Procedure 41.1 Using 0.4 g of the sample proceed as in Section 30. 41.2 Calculation--Calculate the percent of chromium as Cr203 as follows: ` Cr203, % -- mL titration X normality of FeS04 X 63.34 42. Precision and Bias 42.1 Data are not available to determine the precision and bias of .these test methods. There are no plans at present to obtain such data. 43. Keywords 43.1 chromium oxide green pigment; green pigment con taining lead chromate and chromium oxide; lead chromate pigment; lead containing pigment; molybdate,pigment; or ange pigment, eontaimng lead chromate and chromium oxide; yellow pigment containing lead chromate and chro mium oxide The American Society for Testing and Materials takes noposition respecting the any patent rights asserted in connection with any item mentioned In this standard. Users oI this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such tights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must bo reviewed every five years and I ttnot revised, either reepproved or withdrawn. Yourcomments are Invited either for revision ofthis standard or lor additional standards j and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible l technical committee, which you may attend. Jf you feel that your comments have not received a fair hearing youchouid make your <! I - viewa known to the ASTM Committee on Standards, 1316 Race St., Philadelphia, PA 19103. ...... DUP050296561 lb Designation: D 153 - 84 (Reapproved 1989),e1 Standard Test Methods for Specific Gravity of Pigments*1 This standard is issued under the fixed designation D 1S3; 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 (e) indicates an editorial change since the last revision or reappiovaL This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4181 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. a Editorial changes were made throughout in March 1989. , Scope 1.1 These test methods cover three procedures for deter- dng the specific gravity of pigments, as follows: |fi Test Method A--For Routine Testing of Several Samples aultaneously. Test Method B--For Tests Requiring Greater Accuracy i Test Method A. Test Method C--For Rapid and Accurate Testing of Single Samples. 1.2 The specific gravity value obtained by these proce dures may be used with the weight of a dry pigment to determine the volume occupied by the pigment in a coating formulation. 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 j the responsibility ofwhoever uses this standard to consult and festablish appropriate safety and health practices and deterf mine the applicability of regulatory limitations prior to use. For specific hazard statements, see Sections 5, 11, and 15. 12. Referenced Document : 2.1 ASTM Standard: ' D1193 Specification for Reagent Water2 3. Purity of Reagents 3.1 Purity of Water--Reference to water shall be under stood to mean reagent water as defined by Type II of Specification D 1193. TEST METHOD A--FOR ROUTINE TESTING OF SEVERAL SAMPLES SIMULTANEOUSLY 4. Apparatus and Materials 4.1 Pycnometer--A pycnometer (Note 1) having a 50-mL capacity. 1--The Weld type with the cap seal on the outside of the neck of the bottle is preferred because there is less danger of trapping air just ' 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 D01.31 on Pigment Specifications. Current edition approved Oct. 26, 1984. Published January 1985. Originally published as D 153 - 23 T. Last previous edition D 153 - 82. 1 Annual Book ofASTM Standards, Vols ll.Oi and 06.03. under the capillary tube than with types having the ground glass seal on the inside of the neck. 4.2 Water Bath, maintained at 25 0.5C and equipped with a stirring device. 4.3 Manometer, open- or closed-tube (see Part / of the apparatus for Test Method C), made of glass tubing 6 mm in diameter, fitted with rubber pressure tubing attached to a T-joint leading to the desiccator and the pump. For the open-tube type 860 mm of mercury shall be used. The difference in levels of the mercury in the manometer when the system is in operation, subtracted from the barometer reading taken at the same time, shall be considered the absolute pressure of the system in millimetres of mercury. 4.4 Desiccator, glass, constructed with heavy walls to withstand a vacuum ofone atmosphere, and with an opening at the side. 4.5 Vacuum Pumps--A laboratory water vacuum-type pump (Note 2), to remove the greater portion of air in the desiccator, and an oil vacuum-type pump, motor-driven, and capable of reducing the absolute pressure of the system to 3 mm. 2--The water vacuum pump may be omitted if the rate of evacuation with the oil pump can be controlled so as to avoid a rapid ebullition of entrapped air and possible loss of specimen. 4.6 Thermometer, having a range frotm.0 to 60C, and graduated in 0,lQ. divisions. 4.7 Weighing Bottle, wide-mouth cylindrical glass (about 30 mm in height and 70 mm in diameter), provided with a ground-glass stopper. 4.8 Immersion Liquid--Kerosine has been found to be a good wetting vehicle for most pigments, and shall be used generally as the immersion liquid. Refined, white kerosine of narrow evaporation and boiling range shall be used. With some pigments that are not wetted well with kerosine, other immersion liquids such as glycerin, ethylene glycol, tetrahydronaphthalene, etc., may be substituted. The liquid must have a low evaporation rate and narrow boiling range, and the same procedure shall be followed as with kerosine. Water is not a preferred liquid because of the possibility of frothing. 5. Hazards 5.1 Before a desiccator is used for the first time, wrap it in a towel and test under an absolute pressure of under 3 mm. Exercise care in handling the desiccator when under vacuum, DUP050296562 # D 153 'M crystalline pigments, about 4 g; for opaque white pigments, 7 1 to 10 g; and for red lead, from 15 to 20 g. Weigh pigments of f a hydroscopic nature from the weighing bottle. | 7.3 Number of Specimens--Run all samples at least in I duplicate. - : j 7.4 Addition of Kerosine--Add enough kerosine to the i pycnometer to form a clear layer approximately '4 in. (6 I mm) above the pigment. When necessary* stir the specimen ! with a polished round-bottom glass rod until completely covered by kerosine, adding more kerosine if necessary. ! FIG. 1 Apparatus for Test Method B Wash' the rod with kerosine, adding the washings to the pycnometer. since a sudden jar may cause it to collapse. 7.5 Removal of.,Occluded Air-^Place the pycnometer in the desiccator. Close the desiccator and attach to the water 6. Standardization of Pycnometer 6.1 Fill the pycnometer with freshly boiled water at 23 to 24C, gradually bring to 25 0.5'C, and then dry and weigh as specified in 7.6. Empty the pycnometer, and clean, dry, and reweigh it. Next fill the pycnometer with kerosine at 23 to 24C, bring to 25' 6.5'C, dry, and weigh as befpre. Calculate the specific gravity, S, ofthe kerosine at 25/25"C as follows: pump until the greater part of the air is removed from the system. Complete this procedure within a period of 5 to 10 min. Gose the system with a. pinchcock and attach , the desiccator to the oil pump for the removal of the small amounts of air given off at the low pressures obtainable .with the oil pump. Use the manometer to indicate whether the oil pump is.giving the.proper vacuum. When the manometer indicates that the absolute pressure is 3 mm and constant, cut off the oil pump for. short periods, taking care that the S = A!M vacuum does not change materially due to leakage. At first where: A = weight of kerosine, g, and B = weight of water, g. bubbles of air rise-from (he pigments very rapidly, then this action gradually decreases and finally stops. The time required for complete removal of air may vary from 30 min to 24 h, depending upon the nature of the pigment. When no 7. Procedure - more bubbles can be seen, it may be assumed , that the occluded air has heen removed and that the pigment, is 7.1 Drying--Dry the pigment, preferably in an electric thoroughly wet with kerosine. Then slowly admit air to the oven, at 105 2"C for2 h.' desiccator by means of the pinchcock, . 7.2 Weighing--Transfer to a clean, dry, weighed 7.6 Filling and Bringing to Temperature--Remove the pycnometer, sufficient sample to form a layer approximately pycnometer from the desiccator, fill with kerosine at 24 to 34 in. (20 mm) deep. For black, blue, and lake pigments of 25C taking, care to add a sufficient quantity to prevent air low specific gravity, use about 1 g of sample; for inert bubbles where the pycnometer is closed, and permit to come DUP050296563 I D 153 9. Precision 9.1 Duplicate determinations by this test method'should not differ by more than 0.02. TEST METHOD B--FOR TESTS REQUIRING GREATER ACCURACY THAN TEST METHOD A 10. Apparatus (see Figs, l and 2) IQA Pycnometer, Water Bath, Manometer, .Vacuum Pump, Thermometer; Weighing Bottle, and Immersion Liq uid--See Section 4; also Fig. 2 (e) and (/). 10.2 Bell Jar, glass, with a two-hole rubber stopper. Into one hole of the stopper shall be fitted a separatory funnel with, a well-ground stopcock (Fig. 1 (c)), extending into the pycnometer. Into the other hole of the stopper.shall be fitted a glass tube, ys^th-.a weltgropnd three-way stopcock (Fig- 2 {d)) and connected with the vacuum pump (Fig. 2 (e)). The bell jar shall rest on a sheet of . rubber,' 'cemented or vulcanized to , a glass or iron plate. With stopcock c closed arid stopcock d open to the pump, the system shall maintain , an absolute pressure of at most 3. mm. A desiccator may be used instead of a.pell jar. 10.3 Bottle, storage,' (Fig. 2 (h)) for kerosine or other' wetting liquid. t Buret: Geissler, straight; glass stopcock, ground accurately. Total capacity lOOmL' Capacity of- bulb 0to75rriL Graduated 75 to 100 mL Subdivisions 0.05 mL Rate of outflow about 2 min Permissible variations: . Capaaty, total ' 0.10-mL Capacity graduated portion 0:03 mL Markings on graduations shall be in conformity with the National Bureau of Standards Circular No. 9. FIG. 3 Buret in Apparatus r to constant temperature at 25 ; 0.5C in the water bath/ Carefully stopper the pycnometer and remove excess kerosine with lens paper. Take the pycnometer out of the'bath, allow to come to room temperature, and weigh. - 8. Calculation 8.1 Calculate the specific gravity; S, of the pigment as follows: s=w- fk D where: Pl = weight of pigment used, g, W = weight of water to fill the pycnometer, g, Kt = weight of kerosine added to the pigment, g, and D = specific gravity of the kerosine. 3 Available from National Institute ofStandards and Technology, Gaithersburg, MD 20899. 11. Hazards ! 11.1 Before a. bell,jar (or desiccator) is used for the first time, tost under.'* vacuum as described in Section 5. 1T.2 Use a buret stopcock, (Fig. 2..(c)) that is well ground and lubricated,with silicone lubricants or use a PTFE-coated ,, stopcock. . 12. Procedure i-2.1 Place the. pycnometer, containing the weighed, dried pigment under the bell jar. Close stopcocks c and d, start the vacuum pump, and then gradually open stopcock d to the pump. When an absolute pressure of 3 mm has been attained and can be maintained, fill the separatory funnel with kerosine, close stopcock d, and gradually open stopcock c, adding sufficient kerosine to cover the pigment. Then stop the pump and release the suction at stopcock d. Finally," fiH the pyenqmefefc with kerosine, and . complete die test as described in 7.6 and Section 8, under Test Method A. 13. Precision . 1:3.1 .Duplicate determinations by this'test method should not differ by more than 0.01. TEST- METHOD C--FOR RAPID AND ACCURATE TESTING OF A SINGLE SPECIMEN 14. Apparatus (see Figs. 2 and 3) 14.1 Buret, 100-mL, with a 75-mL bulb in the upper part, and with the lower part (25 mL) graduated in 0.05-mL divisions (see Fig. 3). 14.2 Flask--A special 100-mL graduated flask (Fig. 2 (b)) with ground-glass stopper. The flask shall be thick enough to withstand an absolute pressure of 1 mm, and shall weigh between 50 and 60 g. The neck ofthe flask shall be graduated in 0.05-mL divisions between the 99 and 100-mL marks. The dimensions of the flask shall be as shown in Fig. 2. 14.3 Stopcocks--A tightly ground stopcock (Fig. 2 (c)) as 43 X. DUP050296564 1 D 153 part of buret, a, and a three-way stopcock (Fig. 2 (d)) zero mark with a piece of capillary tubing. Now close connecting with the vacuum pump, e. To prevent leakage of stopcock d, and carefully open stopcock c, admitting about kerosine use a buret stopcock (Fig. 2 (c)) that is well ground 75 mL of kerosine into the flask. Open stopcock d to the air, and lubricated with silicone lubricant or use a PTFE-coated thus releasing the vacuum in the flask, and fill the flask with stopcock. kerosine to a definite mark on the neck. Read the buret, 14.4 Vacuum Pump--See 4.5; also Fig. 2 (e). In this calling this reading K2 (the volume of the flask). procedure the oil vacuum pump shall be capable of reducing the absolute pressure of the system to 1 mm. 17. Procedure 14.5 Manometer, Thermometer, Weighing Bottle, and 17.1 Clean the flask dry, and weigh. Transfer a quantity of Immersion Liquid-See Section 4; also Fig. 2 (/). the dry pigment to be tested to the flask by means of a clean, j 14.6 Bottle--See 10.3. dry, glass funnel with the stem reaching to the bottom of the bulb. A piece of stiff nickel wire is convenient to push the 15. Hazards powder down the stem. Nearly fill the bulb of the flask with 15.1 The variations that occur under normal conditions the pigment, which, however, shall occupy a volume of less ! in a room do not materially affect the specific gravity of a than 25 mL after all air is expelled. Greater accuracy may be I pigment. However, take care that the temperature of the obtained with a large specimen than with a small one. Wipe liquid after transferring to the flask is approximately the the inside stem as well as the entire outside of the flask with I ;.f same as it was when in the buret 15.2 Since in determining both K2 and V the tip of the a clean piece of dry, lintless cloth. Weigh the flask and pigment, and calculate the weight of pigment by deducting j | buret and bore ofthe stopcock plug are empty, no correction the weight of the empty flask. With the buret clean and dry, j l is to be made; but stopcock c must be so well ground that attach the flask to the evacuating system as shown in Fig. 2. I} under an absolute pressure of 1 mm for 30 min no leakage of After closing stopcocks c and d, start the pump and carefully | kerosine shall take place. The usual sources of error are open stopcock d to the pump. Continue evacuation until the ;} failure to remove all the air from the pigment, and leaks in the system. Use a minimum amount of rubber tubing in the system and, wherever it is used, coat the joints between rubber and glass with a melted mixture of beeswax and rosin. pump maintains an absolute pressure of 1 mm in the flask, or until all the air is removed from the system. Then fill the buret from the top as described in Section 16, close stopcock d, gradually open stopcock c, and add kerosine until the || 15.3 In cleaning the flask of kerosine only, a rinsing two or three times with ether, followed by dry air (dried over pigment is covered. Tap the flask gently to dislodge any air bubbles. Stop the pump, open stopcock d to the air, and fill j| sulfuric acid and calcium chloride), is considered sufficient. the flask up to the same mark as was obtained in determining j| When pigment is also present, remove both pigment and its volume. Designate the volume of kerosine required as V. j kerosine and follow with ether rinses until no more pigment Read the height of the liquid in the buret to the nearest remains. Add some filter pulp (macerated filter paper) and estimated 0.01 mL. water (with or without glass beads), and shake vigorously. 18. Calculation Repeat if necessary. Rinse the flask with reagent water, and 18.1 Calculate the specific gravity, SG, of the pigment as I either dry in an oven, or rinse with alcohol and ether follows: __ followed by dry air. SG = P2/{K2 - V) j 16. Standardization of Apparatus where: I 16.1 Connect the flask to the buret and the pump by P2 = weight of pigment used, g, _ I means of a two-holed rubber stopper. Evacuate the system K2 - volume of kerosine required to fill the flask when with the buret stopcock (Fig. 2 (c)) closed until the pump empty, mL, and maintains an absolute pressure of 1 mm in the flask. Close V - volume of kerosine required to fill the flask when the the three-way stopcock, d, for 30 s, and again open to the pigment is present, mL. pump. There shall be no appreciable change in the mercury levels in the manometer, indicating that the system beyond 19. Precision stopcock d is tight. With the vacuum still maintained, fill the 19.1 Duplicate determinations by this test method should buret from the top with kerosine, adjusting the level to the not differ by more than 0.01. The American Society for Testing endMaterials 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 ofany such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision atany lime by the responsible technical committee and must be reviewed every five years and ifnotrevised, eitherraapproved or withdrawn. Your comments are Invited either for revision ofthis standard ortor additionalstandards snd should be addressed to ASTM Headquarters. Your comments wit! receive ceieiul 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. 44 DUP050296565 Designation: D 185 - 84 (Reapproved 1989)41 Standard Test Methods for Coarse Particles in Pigments, Pastes, and Paints1 This standard is issued under the fixed designation D 183; 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 1 superscript epsilon (i) indicates an editorial change since the last revision or reapproval. I This standard has been approved for useby.agencies ofthe Department ofDefense to replace Methods 4091, 4101 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications andStandardsfor the specific year ofissue which has been adopted by the Department ofDefense. ,, e\ --Editorial changes were made throughout in March 1989. 1. Scope 1.1 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 Purposes12 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-mm) 45-pm (No. 325) sieve conforming to Specification E 11. 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 105 2C, cool, and then 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials arid are the direct responsibility of Subcommittee D0L31 on Pigment Specifications. Current edition approved Oct. 26, 1984. Published December 1984. Originally published as D 185 - 37. Last previous edition D 185 - 78. 2 Annual Bode ofASTM Standards^ Vol 14.02. weigh on an analytical balance, recording the weight to 1 mg. 5.2 Weigh a specimen (25 g for basic carbonate and basic sulfate white leads, 25 g for red lead and mercuric oxide, 2 g for black pigments qf low specific gravity, 3 g for Prussian blues and graphite, and 10 g for all other pigments) of the pigment to be tested oh ah analytical balance to 1 mg. Wet the sieve oh both sides with alcohol and. transfer the' specimen ofjugment to the sieve and wet with alcohol. 5.3 Hold the sieve under a tap delivering about 300 to 500 mL of the wash liquid (water) per minute. By slightly shaking the sieve, the pigment will be rapidly carried through. A soft camel's-hair brush may be used in aiding the operation. If the sieve is held at a slight angle so, that the figment gradually collects at cine 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, ofthe 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-mfn) porcelain dish containing 250 mL of the wash liquid so that the sieve is covered to a depth of about Vi in. Brush the pigment remaining on the sieve with a soft 1-in. (25-inm) camel's-hair brush at the rate of two strokes per second during two periods of l6 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 the1 dish' after every two brushing periods. Continue this operation 'until the wash liquid paSsiiig over the residue and through the Sieve is clear and free from solid particles. When the washing appears fO be complete, collect about 200 mL of the wash liquid, after" passing oyer 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. ' 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 DUP050296566 I05C, cool, and weigh as described in 5.1. Calculate the percent of coarse particles. 6. Procedure for 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 ofthis solution will be sufficient for several tests. 7.3 Crush the pellets between two glass plates approxi mately 12-in. (305-mra) 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-p.m 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 pap.er 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 Darvan No. I available from R.T. Vanderbilt, 30 Winfield St., Norwalk, CT 06855. 8.2 For water-soluble pigments use 10 I g as the : specimen. For pastes in oil, pastes in Japan, and mixed paints use 25 1 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 in Section .4 except that sieves used shall be as follows: 11.1.1 FlatjPaints, a 3-in. (75-mm) 90-pm (No. 170) sieve. 11.1.2 Gloss and Semi-Gloss Paints, a ^3-in. (75-mtrr) 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 maybe 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 1 h, as DUP050296567 escribed in 5.1. Then calculate the percent of coarse articles 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 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 live 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, 1916 Pace St., Philadelphia, PA 19103. 47 DUP050296568 Designation: D 207 - 55 (Reapproved 1987) Standard Specification for Dry Bleached Lac*1 This standard is issued under the fixed designation D 207; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number is 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 specification covers two grades of dry bleached lac, namely, regular and refined. --Dry bleached lac is also known as "bone-dry," "bac-dry," or "kiln-dry" bleached lac. The refined grade is bleached lac from which practically all the wax and insoluble matter has been removed during the process of manufacture. 2. Referenced Document 2.1 ASTM Standard: D 29 Test Methods for Sampling and Testing Lac Resins2 This specification is under thejurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.33 on Varnish and Resins, Including Shellac. Current edition approved Sept. 12, 1955. Published November 193S. Originally published as D 207 - 25. Last previous edition D 207 - 49. 1Annual Book ojASTM Standards, Vol 06.02. 3. Properties 3.1 Dry bleached lac shall conform to the following requirements: Matter insoluble in specified hot solvents, max, % Moisture, max, % Wax, max, % Matter soluble in water, max, % Ash, max, % Rosin Copals Regular 1.0 6.0 5.5 1.0 1.0 none none Refined 0.2 6.0 02 0.3 0.5 none none 4. Test Methods 4,1 The material shall be sampled and the properties enumerated in this specification shall be determined in accordance with Test Methods D 29, TheAmerican Society tor Testing and Meterlals 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 af any time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, either reapproved or withdrawn. Yourcomments are Invited either lorrevision 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 fa/r hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. imm DU P0502 96569 Designation: D 209 - 81 {Reapproved 1989) Standard Specification for Lampblack Pigment1 This standard is issued under the fixed designation D 209; 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 r 1. Scope 1.1 This specification covers the pigment commercially Known as lamp-black. The pigment may be purchased in the dry form or as a paste in oil. p. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D387 Test Method for Color and Strength of Color Pig ments with a Mechanical Muller3 D1208 Test Methods for Common Properties of Certain Pigments3 13. Composition and Properties 3.1 Dry Pigment--The pigment shall be made by burning ! oils or tais in such a manner as to form a deposit of carbon or soot. It shall be high grade in every respect and shall be free from oil, greasy matter, and admixture of any other substance. The pigment shall conform to the following requirements: Ash, max, % Acetone extract, max, % Moisture and other volatile matter, max, % , Coarse particles, (total residue retained on a 45-iim (No. 325) sieve), max, % Tone when diluted with zinc oxide O.S 1.0 3.0 O.S dear-blue-gray 3.2 Paste in Oil--The paste in oil shall be made by 1 This specification is under the jurisdiction of ASTM Commiltee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Aug. 31, 19B1. Published October 1981. Originally published as D 209 - 24. Last previous edition D 209 - 47 (1974). 1 Annual Book ofASTMStandards, Vols06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. thoroughly grinding the specified pigment with linseed oil. As received it shall not be caked in the container and shall break up readily in oil to form a smooth paint of brushing consistency. It shall mix readily in all proportions, without curdling, with linseed oil, turpentine, or volatile petroleum spirits, or any mixture of these substances. The paste shall conform to the following requirements: Pigment, min, % Linseed oD, max, % Moisture and other volatile matter, max, % Coarse particles and skins (total residue retained on a 45-iun (No. 32S) sieve), max, % of the dry pigment 25 7} 0.7 1.0 3.3 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall he within-mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples, shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the Option of the purchaser, the samples may be tested separately or after blending in equal, quantities the samples from the same production unit to form a composite sample. ~- 5. Test Methods 5.1 Tests shall be conducted in accordance -with the following test methods. Test procedures not covered -by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 52 Coarse Particles--Test Methods D 185. . 5.3 Pigment, Linseed Oil, and Moisture and Other Vola tile Matter in Paste in Oil--Test Methods D 1208. 5.4 Mass Color and Tinting Strength--Test Method D 387. 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 ol 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 Ifnotrevised, either reapprovedorwithdrawn. Your comments are Invitedeitherforrevisionofthis 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 feet that your comments have no? received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. mmm 49 mmm m DUP050296570 M||jr Designation: D 21 ~ 81a (ReaPProved 1991 )1 Standard Specification for Bone Black Pigment1 This standard is issued under the fixed designation :D 2I0i the number immediately following the designation indicates the year oforiginal adoption or, in the case ofrevision, the year oflast-revision. A number in parentheses indicates the year ofJast.raapproval. A superscript epsilon (<) indicates an editorial change since the ,-last revision or reapproval, , * --Keywords were added editorially in July ) 991. . 1. SCOP.e .. . 1.1 This specification covers the pigment commercially known as bone black, ivory black, or drop black. The pigment may be purchased in the dry form or as a-paste in oil. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods .for Coarse Particles in Pigments,, Pastes, and Paints2 , . . i ... D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller3 D1208 Test Methods for Common Properties of Certain Pigments3 ! " 3. Composition and Properties > 3.1 Dry Pigment-^The 'pigfneht shall be made by the calcination of bodes, shall be unmixed with`any other substance, and shall conform to the following requirements: Ash (pigment dried at 105`C), %, max Ash insoluble in acids, max, % Acetone extract, max, % .. . Coarse particles (total residue retained'on'a'No. 325 (45-pm) sieve), max, % . ', 88 3.0 2.0 2.0 3.2 Paste id Oil--The paste in :0il shall- be made by thoroughly grinding the specified pigment with linseed oil. As received it shall not be caked in the container and Shall 1 This specification is under the jurisdiction ofASTM Committee D-l on' Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee 001.31 on Pigment Specifications. Current edition approved Aug. 28, 1981. Published October 1981. Originally published as 0210-24.'Last previous edition D'210 - 81. 2 Annua! Book ofASTM Standards, Vols 06.01 and 06.02. ` 3 Annual Book ofASTM Standards, Vol 06.02. break up readily in oil to forth a sifidoth'-pairit of brusliihg4 consistency. It shall mix readily in all proportions,' without curdling, with linseed oil, turpentine, or volatile petroleum , spirits, or any mixture of these substances. The paste shall f conform to the following requirements: Figment, min, % , t -v Linseed oil, max,% .. t i' Coarse particles and skins (total residue retained on a . No. 325 (45-jtm) sieve), max, % of the dry pigment ' ` ' .> ; 0 .45 j 5Si . *1 2.5 I 3.3 The mass color and. chiaractei; of ,the tint and the S tinting strength formed by,g mixture, wifjb a white pigment J shall be within mutually agreed upon limits 6f a standard j acceptable to both the purchaser and the seller. j 4. Sampling -1 4.1 Two samples shall be taken at fandom from different \ packages from each lot, batch;'day's pack, or other unit of prdduction in a shipment. Wheir no markings'distinguishing' I between units of production appear, samples shall be taken''*! froih different packages in the ratfo-of two Samples for each fl 10 000 lb (5000-kg); except that for shipments of less than f 10 000 lb two samples shall be taken. At the optiOti of the | purchaser, the samples may be tested separately or after blending in equal quantities the samples from the., same j production unit tp form a composite Sample. , J 5. Test Methods . 5.1 Tests shall be conducted in-accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. ~ . .. "5.2 Coarse -Particles--Test Methods D 185. ' ,, 5,3, Pigment and. Linseed. Oil in Paste, in Ottr-Jest Methods D1208. < -t 5.4 Mass Color and Tinting Strength--Test Method D 387. f f 6. Keywords '* 6.1 Black pigment; drop black; ivory black; pigment.. The American Society for Testing 'and Materials takes ho position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard arevxpressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely theft own responslbilky. 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 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 Baca St., Philadelphia, PA 19103. 50 ----- r DUP0502 96571 Designation: D 211 - 67 (Reapproved 1989)61 Standard Specification for Chrome Yellow and Chrome Orange Pigments1 This standard is issued under the fixed designation D 213; 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. 1 NoTE^-Hditorial- changes were made throughout in March 1989. This`Specification covers six typds of commercially jpjgfrerlead chromate pigments as follows: i^'-'Type I--Primrose Chrome Yellow, ' >#5^e/?--'Le(tnonChrome:Yeijow'- Type ///--Medium Chrome Yellow, /F^-Light Chrome Orange, *^ta'7ype F--Dark Chrome Orange, ahd ; Sk: Type F/--Chrome Yellow for Green; Rt 1.2 The following hazard caveat applies to the test method portion of this specification only. This standard may involve hazardous materials, operations, and equipment.' This standard does not purport to address all of the safety problems associated with its use. It is the responsibility ofthe yser of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to iiie: ' ' |2. Referenced Documents ' " d.l ASTM Standards; ', D126 Test Methods for Analysis, of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chro mium Oxide Green12 D185 Test Methods for Coarse Particles in Pigments, " Pastes, and Paints3 ' ' ,J ' D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)4 D387 Test Method for Color and. .Strength of Color Pigments With a Mechanical Muller D523 Test Method for Specular Gloss5 6 D562 Test Method for Consistency of Paints Using thp Stormer Viscometer5' D 600 Specification for Liquid Paint Driers4 . D822 Practice for Conducting Tests on Paint and-Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light and Water Exposure Apparatus5 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems5 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee 001.31 on Pigment Specifications. Current edition approved Sept. 8, 1967. Originally published as D 211 - 25T. Last previous edition D 211 - 63 T. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vois 06.01 and 06.02. 4 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 06.01. E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens for Broad-Band Filter Reflectometry5 2.2 FederalSpecification? TT-R-266 Resin, Alkyd; Solutions 3. Composition and Properties , 3.1 The pigments shall be chemical precipitates consisting of normal or basic lead chromates, or mixtures ofthese, with or-without admixtures of other insoluble compounds oflead or other materials used in manufacture to control certain properties. The pigments shall conform to the requirements for composition -as prescribed in Table 1.- 32 The mass color and character of the tint formed by mixture with, a white pigment shall be the same as, and the strength shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and,(he seEer. 3.3 When mutually agreed upon between the purchaser and the seller as being essential to the end use'ofthe pigment, resistance to loss of gloss, chalking, and color change shall be tested as specified in 5.4. The exposed panel shall show no chalking, a loss of not more than 30 % of the original gloss, and a color change no greater than the lightness difference. AL, shown for each pigment type in Table 2. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in-a-shipment. When no markings distinguishing between units of production appear, samples shall be taken 'from different packages'in the ratio of two Simples for each IQ 000 lb ,(4450 kg), except that for shipments of less than i0.000 lb. two samples shall be take. At the option of the purchaser, the samples may be tested separately, or samples from the same production unit may be blended in equal quantities to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following test methods. Test procedures not covered by ASTM methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Chemical Analysis of Dry Pigment--Test Methods D 126. The lead chromate analysis should be conducted in accordance with 11.1 of Test Methods D 126; the procedure 6 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 51 DU P050296572 # D 211 TABLE 1 Requirements for Composition Type 1 Typed Lead chromate (PbCrO.), minx Total matter soluble in water, max % Total of all substances other than Insoluble compounds of lead, max % Moisture and other volatile matter, max % Coarse particles (total residue retained on a 45-pm (No. 325) sieve), max % Organic colors and lakes 50 1.0 8.0. 1.5 1.0 none 65 1.0 10.0 1.5 1.0 none Type III 87 1.0 10.0 1.5 1.0 none Type IV 55 1.0 10.0 18 1.0 none Type V 55 1.0 3.0 18 1.0 none Type VI 75 ~ 1.0 10.0 18 1.0 none TABLE 2 Type 1 II 111 IV V VI Permissible Lightness Difference (At) Pigment AL Primrose chrome yellow Lemon chrome yellow Medium chrome yellow Light chrome orange Dark chrome orange Chrome yellow for green 35 8 6 3 3 6 outlined in is11.2 not applicable. 5.1.2 Coarse Particles--Test Methods D 185. 5.1.3 Mass Color and Tinting Strength--Test Method D 387. 5.1.4 Resistance to Loss of Gloss, Chalking, and Color Change: 5.1.4.1 A test enamel shall be prepared consisting of ingredients conforming to the applicable specifications in the following proportions: Ingredient Pigment under test Alkyd resin vehicle solids, min-4 Total solids, min Mineral spirits Driers Weight Percent 30 to 34 28 60 AC D, E * An alkyd resin solution conforming to Type lit of Federal Specification TT-R-266 is suggested. B See Specification D 235. cAs required to give a Stormer consistency of 100 to ISO g at 200 r/min as prescribed in Test Method D 362. See Gass B in Specification D 600. E As required to obtain set-to-touch in 2 h and dry-hard in S h. 5.1.4.2 The enamel shall have a fineness of grind, asprescribed in Test Method D 1210, of 1.5 mils or less. Apply the enamel to duplicate flat metal panels by spray or applicator to complete hiding and allow to dry 72 h. Measure the gloss at 60 in accordance with Test Method D 523. Measure the directional reflectance of the coating ip accord ance with Test Method E 97. Subject the coated panels for 168 h to accelerated weathering under the conditions pre scribed in Practice D 822. Examine the exposed coating for chalking. Wash the exposed panel under running water with a thoroughly degreased lamb's wool pad to remove scum or dirt. Wipe off water with clean cheesecloth and dry the panel for 2 h. Calculate the loss of gloss from gloss measurements made before and.after exposure. After exposure, determine the directional reflectance for each panel as described in Test Method E97. Calculate the color change or lightnessdifference estimate (AL) as follows: tsL = K(Y2i/2 - T,1'2) where: 7, = luminous directional reflectance ofthe panel measured before exposure, Y2 = reflectance measured after exposure, and K = 100 when the reflectances are expressed as decimal fractions or 10 if reflectances are expressed in percent. The color change for the coating shall be the average obtained for the two panels.7 7 The method of determining the lightness-difference estimate is described in detail in example 4, "Photoelectric Tristimulus Colorimetry with Three Filters," Circular C429, Nat Bureau Standards. The American Society for Testing andMaterials takes no position respecting the valldityaf 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 the responsible technical committee ahd must be reviewed every five years and Ifnotrevised, eitherreapproved or withdrawn. Your comments are Invitedeither for revision 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, 1913 Race St., Philadelphia, PA 19103. DUP050296573 Designation: D 212 - 87 Standard Specification for Chrome Green Pigment1 * 4 5 This standard is issued under the. fixed designation D 212; 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 specification has been approvedfor use by agencies oftheDepartment cfDefense to replace Fed. Spec. TT-P-345. Consult the DoD Index ofSpecifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. |. Scope I 1.1 This specification covers the pigment commercially ^ known as chrome green. The pigment may be purchased in I the dry form or as a paste in oil. 2. Referenced Documents 2.1 ASTM Standards: D126 Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chro mium Oxide Green2 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2,3 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 Dry Pigment--The pigment shall be a precipitated i mixture of lead chromate and iron blue (potassium or ammonium ferriferrocyanide) with or without other insol uble compounds of lead. It shall be free from admixture of any substances other than those added during manufacture, in small amounts up to a total of 7 %, to improve the stability or working properties, or both, of the pigment Extenders and diluents such as barium sulfate, silica, sili cates, calcium carbonate, calcium sulfate, magnesium car f bonate, etc., shall be absent. The pigment shall conform to the following requirements: Of the total lead-* in the pigment, percent present as chromate (PbCr04), min Total matter soluble in water, max, % Moisture and other volatile matter, max, % 70 1.0 4.0 1 This specification is under tbe jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.31 on Pigment Specifications. Current edition approved May 29, 1987. Published My 1987. Originally published as D 212 - 47 (1974). Last previous edition D 212 - 80. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Organic colors or lakes 1.0 none A Calculated as metallic lead. 3.2 Paste in Oil--The paste in oil shall be made by thoroughly grinding the specified pigment with linseed oil. The paste as received shall not be caked in the container and shall break up readily in oil to form a smooth paint of brushing consistency. It shall mix readily in all proportions, without curdling, with linseed oil, turpentine, or volatile petroleum spirits, or any mixture of these substances. The paste shall conform to the following requirements: Figment, min, % Linseed oil, max, % Moisture and other volatile matter, max, % Coarse particles and skins (total residue retained on a No. 325 (45-pm) sieve), max, percent of the dry pigment 70 30 3.0 1.5 3.3 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that ftsr shipments of less than 10 OOO lb-two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures not cov ered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Chemical Analysis of Dry Pigment--Test Methods D 126. 5.1.2 Coarse Particles--Test Methods D 185. 5.1.3 Moisture--Test Methods D 280. 5.1.4 Other Volatile Matter in Paste in Oil--Test Methods D 1208. 5.1.5 Mass Color and Tinting Strength--Test Method D 387. 53 DUP0502 96574 # D 212 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asseitedin 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 Invited eitherfor revision of thisstandard 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 yotir 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. 54 DUP050296575 Designation: D 237 - 57 (Reapproved 1991)' Standard Specification for Orange Shellac and Other Lacs1 This standard is issued under- the fixed designation -D 237; the number immediately foBowing 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 (t) indicates an editorial change since the last revision or reapproval. `'--Keywords were added editorially in January 1991. I Scope ' D29 Test Methods for Sampling and Testing Lac Resins2 1.1 This specification covers three types and four grades pf orange shellac and other lac, as follows: ^ : 1.1.1 Type /, orange shallac, grades A, B, C, and D, : 1.1.2 Type II, button lac, and it 1.1.3 Type III, garnet. lac. I,, 1.2 Stick-lac and seed-lac are not covered by this specifi- fcation. 3. Physical Properties ' 3.1 The material shall conform to the requirements pre scribed in Table 1. --Type II customarily occurs in the form ofcircular disks about 3 in. (76 mm) in diameter and '/in. (3.2 mm) in thickness and is known to the trade as pure button lac. Type III is dark garnet in color and is known to the trade as pure garnet lac. Garnet lac also is manufactured in admixture with rosin and as a dewaxed lac, but these are not covered by this specification. 2. Referenced Document 2.1 ASTM Standard: 4. Test Methods 4.1 The material shall be sampled and the properties enumerated in this specification shall be determined in accordance with Test Methods D 29. 1 This specification 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 1.33 on Polymers and Resins. Current edition approved Sepi. 30, J 957. Published November 1957. Originally published as D.237 - 26. Last previous edition D 237 - 55. 5. Keywords 5.1 lac; orange shellac; shellac 2Annual Book ofASTM Standards, Vol 06.02. TABLE 1 Requirements for Orange Shellac and Other Lacs 4 Type! Type II Type III Grade A Grade B Grade C Grade D Matter insoluble in specified hot solvents, max, % 1,00 125 1.50 3.00 1.00 0.50 Iodine number; max 15.0 15.0 15.0 15.0 16.0 18.0 ~~ Moisture, max, % 2.0 2.0 2.0 2.0 '2.0 ....... - 2.0 Wax, max, % 5.5 5.5 5.5 ' 5.5 '5:5- 3.5 - Orpiment, max, % 0.03 0.03 0.03 0.2 0.03 ' 0.03 Matter soluble in water, max, % 0.5 0.5 0.5 0.5 0.5 0.5 Ash, max, % 1.0 1.0 1.0 1.0 0.5 0.5 Rosin none none ` , none- none none *. Color when specified, the color shall be no darker than that of a sample agreed upon between the seller arid the purchaserA A Attention i6 called to the fact that the seller and the purchaser must agree upon one of the two methods for determining color appearing In Test Methods D 29. 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 pf 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 end 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 additionalstandards and should ba 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 vims known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296576 Designation: D 261 - 75 (Reapproved 1987)1 Standard Specification for Iron Blue Pigment1 This standard is issued under the fixed designation D 26J; 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 tbe year oflast reapproval. A superscript epsilon (e) Indicates an editorial change since the- last revision or reapptovaL l --Section 4.1 was editorially changed in May 1987. 1. Scope 1.1 This specification coven the dry pigment commer cially known as Prussian blue, Chinese blue, Milori:blue, or iron blue. 2. Referenced Documents ' 2.1 ASTM Standards: , D387 Test Method for Color and Strength of Color Pig ments with a Mechanical Muller12 DI135 Test Methods for Chemical Analysis of Blue Pigments2 3. Composition and Properties 3.1 The pigment shall be the blue product formed by the reaction of a solution of iron salts with a ferrocyanide or ferricyanide solution. It shall be free from admixture of any substances other than those added during manufacture, in small amounts up to a total of 5 %, for the purpose of improving the quality or working properties, or both, of the pigment. Extenders, and diluents such as barium sulfate, silica, silicates, calcium carbonate, calcium sulfate, magne sium carbonate, etc., shall be absent. The pigment shall conform to the following requirements: Total matter soluble in water, max, % ' l.Q Moisture, max, % 8.0 Organic colors or lakes none Acidity or alkalinity--the acidity or alkalinity of the aqueous extract, with methyl orange indicator, shall not exceed the chemical equivalent of 0.1 % of sulfuric acid, calculated on the dry-pigment 3.2 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 1 This specification is under the.jurisdictioh ofASTM Committee D-I on Paint and Related Coatings and Materials and is the direct 'responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Oct. 31,1975. Published December 1975. Originally published as D 261 - 27 T. Last previous edition D 261 - 47 (1970). 2 Annual Book ofASTM Standards, Vol 06.02. The physical properties and tests ofiron bine, particularly the tinting strength, are considered a better measure of value than the percentages of chemical constituents.' 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit or production in a shipment. When no markings distinguishing between units or production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SWI), except that for shipments of less than 10 000 lb two samples shall be taken. At (be option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures , not cov ered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.2 Identification---Test Methods D 1135. 5.3 Extenders and Diluents--Test Methods D 1135. 5.4 Total Matter Soluble in Water--Matter soluble in water shall be determined by either of the following methods, as mutually agreed upon between the purchaser and the seller: 5.4.1 Water-Soluble Matter by Extraction--Test Methods D1135. ` 5.4.2 Water-Soluble Salts by Electrical Conductivity-- Test Methods- 1135. -~ 5.5 Moisture ifi Dry Pigment--Moisture shall be deter mined by either ofthe following methods, as mutually agreed upon between the purchaser and the seller: 5.5.1 BrabenderMoisture Tester--Test Methods D 1135. 5(5.2 Toluene Distillation--Test Methods D 1135. 5.6 Organic Colors or Lakes--Test Methods D 1135. 5.7 Mass Color and Tinting Strength--Test Method D 387. The American Society for Testing endMaterials takes no position respecting the validity ofany patent rights ssserted 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 eitherfor 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. DUP060296577 Designation: D 262 - 81 (Reapproved 1987)'el Standard Specification for Ultramarine Blue Pigment1 This standard is issued under the fixed designation D 262; 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 epsiion (<) indicates an editorial change since the last revision or reapproval. el aragraph 4.1 was editorially changed in May 1987. Eft j!3L. Scope 1.1 This specification covers the dry pigment commer- (dally known as ultramarine blue, suitable for use in paints, ' efiamels, lacquers, and similar products. : 2. Referenced Documents ! 2.1 ASTM Standards: 1 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments3 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller3 D1135 Test Methods for Chemical Analysis of Blue * Pigments3 D1208 Test Methods for Common Properties of Certain Pigments3 3i Composition and Properties 3.1 The pigment shall be a manufactured product ob tained by the caldning of mixtures of clays and silicas with sodium salts, sulfur, and carbonaceous material. It shall be a soft, dry, finely ground powder of good blue color, free of admixtures of color substances, and shall conform to the following requirements: 1 This specification is under thejurisdiction ofASTM Committee D-1 on. Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D 01.31 on Pigment Specifications. Iff Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 262 - 41 T. Last previous edition D 262 - 75. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. Matter soluble in water, max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Organic colors or lakes 1.5 4.0 1.0 none 3.2 The mass, color and character of the tint and the tinting strength formed by mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following methods. Test procedures not covered by ASTM methods shall be mutually agreed upon between the pur chaser and the seller. 5.2 Identification--Test Methods D 1135,, 5.3 Matter Soluble in Water--TestMethods D 1135. 5.4 Moistureaitd Other Volatile Matter in Bry Pigment-- Method A of Test Methods D 280 or Test Method D 1208. 5.5 Coarse Particles--Test Methods D 185. 5.6 Organic Colors or Lakes--Section 18 ofTest Methods D 1135. 5.7 Mass Color and Tinting Strength--Test Method D 387. The American Society lor Testing and Materials takes noposition respecting the validity ofanypatent 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 ifnotrevised, either reapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or for additional standards t- and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration al 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. 1' DUP050296578 Designation: D 263 - 75 (Reapproved 1987) Standard Specification for Chrome Oxide Green Pigment1 This standard is issued under the fixed designation D263; 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 dr reapproval. 1. Scope 1.1 This specification covers the dry pigment commer cially known as chrome oxide green. Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-jim) sieve), max, % Organic colors or lakes 0.5 2.0 3,2 The mass color and character of the tint and the f! 2. Referenced Documents tinting strength formed by a, mixture with a white pigipent | 2.1 ASTM Standards: D126 Test Methods for Analysis of Yellow, Orange, and shall be within mutually agreed upon limits of a standard | acceptable to both the purchaser and the seller. J Green Pigments Containing Lead Chromate and Chto- 4. Sampling mium Oxide Green*2 ' D185 Test Methods for Coarse Particles 'in Pigments, Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production ih a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio pf two samples for each 10 000 lb (4540 kg) except that for Shipments of less' than 10 000 lb two samples shall be taken. At the option of the 3. Composition and Properties purchaser, the samples may be, tested separately or .after 3.1 The pigment shall consist of practically .pure chro mium sesqui-oxide (Cr203) without any admixture, and shall blending in equal quantities the samples frpm the same production unit to form a composite sample. : ' conform to the following requirement^: 5. Test Methods Total chromium (calculated as Cr203), rain, % Total matter soluble in water, max,.% 97 5.1 Tests shall be conducted in accordance with the 0,5 following methods where applicable. Test procedures not covered by ASTM test methods shall be mutually agreed ' This specification is under the jurisdiction ofASTM Committee D-1 on Paint upon between the purchaser and the seller.. . I and Related Coatings and Materials and is the direct responsibility of Subcom 5.2 Chromium Content--Test Methods P 126. mittee DO1.31 on Pigment Specifications. 5.3 Total Matter Soluble in Water--Test Methods B 126. Current edition approved Oct 31, 1975. Published December 1975. Originally published as D 263 - 27. Last previous edition D 263 - 46 (1970). 2 Annual Book ofASTM Standards, Vol 06.02. '' 5.4 Moisture Content--Test.Method D 28X). 5.5 Coarse Particles--Test Methods D 185. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 5.6 Organic Colors and Lakes--Test Methods D 126. The American Society for Testing andMaterials takes no position respecting the validityof any patent rights asserted in connection with any item, mentioned in. this standard.Msers oi this standard are expressly advised that determination of the validity of any such patent rights, and th&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 reylewed every five years and . U notrevised, either ^approved or withdrawn. Your comments are invitedeither forrevision of this standard orfor 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. . DUP050296579 Designation: D 267 - 82 (Reapproved 1987)' Standard Specification for Gold Bronze Powder1 This standard is issued upder the fixed designation D 267; 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 reappcoYai. . . --Editorial changes were made throughout in June 1987. Scope Jl.l This specification covers the materials commercially |own as gold bronze, pale gold bronze, and rich gold orize powders. Referenced Documents 1 I2.I ASTMStandards: *' t> 13 Specification forSpirits of Turpentine12 D185 Test Methods for Coarse Particles in Pigments, i Pastes, and Paints3 D480 Test Methods for Sampling and Testing of Flaked y Aluminum Powders and Pastes4 5 $=2.2' U.S. Federal Specification: X TT-V-121h Water-Resisting Spar Varnish3 W ' '' g$3. Composition and Properties Jri3" 3.1 The bronze powder shall be made" from new ingot g-v metals. It shall consist of fine polished flakes containing not ij Ids than 3 % of fatty or oily matter (polishing lubricant) to give good "leafing" properties. ' , ' 3.2 The residue retained on a No: 100 (150-jxm) sieve, | using alcohol as the wash liquid, shall' not exceed 0.2 % (in I accordance withTest MethodsD 185). . 3.3 The powder shall have good "leafing" properties. (By "leafing" is understood the property of forming an appar- 1 This specification is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom- mittee DOl.33 on Pigment Specifications, Current edition approved June 25, 1982. Published October 1982. Originally published as D 267 - 27 T. Last previous edition D 267 - 41 (1975). , 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vials 06.01 and 06.02. A Annual Book ofASTM Standards, Vol 06.02. ; 5 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. ently continuous brilliant film over the entire free surface of a mixture of the powder in a suitable liquid (Note), within 1 min after cessation of stirring the mixture.) In testing for leafing properties the powder shall be mixed in the proportion of 3 to 4 lb (370 to 475 g/L) to aj gallon (3.8 L) of the liquid. As thus mixed it shall also give a free flowing, smooth, continuous coating in accordance with Test Method D 480. --A suitable liquid is made by mixing spar varnish conforming to the U. S. Federal Specification for. W^ter-Resisting Spar Varnish (No. TT-V-121 h) with turpentine conforming to Specification D 13 in such proportions that the mixture will have a viscosity of 0.65 to 0.85 poises (B to C on the Gardner-Holdt scale). 3.4 The gold bronze powder shall be suitable for making gold bronze paint. It shall match in shade and fineness a reference sample mutually agreed upon by the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production,in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments ofJess than 10 000 lb two samples shall be taken. At the> option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to. form a composite sample. 5. Test Methods 5.1 Test shall.be conducted in accordance with the' appropriate methods of the American Society for Testing and Materials, where applicable. Test procedures not covered by ASTM methods shall be. mutually agreed upon between the purchaser and the seller. The American Society tor Testing and Materials takes noposition respecting the validity ofany patent rights asserted in connection with any item mentioned Hi this standard. Uaers of this standard are expressly advised that determination of the validity of any such patent rights, arid the risk tit 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 five years and itnot 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. It you ieel 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. DUP050296580 <1 Designation: D 279 - 87 (Reapproved 1991)ei Standard Test Methods for Bleeding of Pigments1 This standard is issued under the fixed designation D 279; 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 rcapproval These test methods hove been approvedfor use by agencies ofthe Department ofDefense to replace Method 4571.1 ofFederal Test Method Standard No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. Keywords were added editorially in June 1991. 1. Scope 1.1 These test methods cover procedures for determining the bleeding characteristics of dry pigments by direct solvent extraction of the pigment and by overstriping a film with a white coating and observing for the color migration from the base coat containing the pigment. 1.2 This standard does not purport to address all of the safety problems, f'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. Summary of Test Methods 2.1 Test Method A--The pigment is shaken with toluene, filtered, and the filtrate observed for color. 2.2 Test Method B--A coating using the pigment under test is prepared and applied to one half of a panel. A white finish is applied over the dried colored coating and extended to the uncdated portion of the panel. The dried overstripe coating is examined for color migration from the base coat. 3. Significance and Use 3.1 Test Method A determines the amount of color produced when the pigment is in direct contact with a selected solvent such as toluene. It is useful as a rapid, easily conducted test of the general bleeding characteristics of pigments. 3.2 Test Method B determines the amount of color migration into a white film applied over a base coat containing the pigment. It* may give a more practical evaluation of whether a pigment will meet specific require ments for bleed resistance. 3.3 Both Test Method A and Test Method B measure the extent of bleed. TEST METHOD A, DIRECT SOLVENT CONTACT WITH PIGMENT 4. Procedure 4.1 Place 0.50 g of pigment (Note 1) in a 25-mL test tube 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 1.21 on Chemical Analysis of Paints and Faint Materials. Current edition approved May 29, 1987. Published July 1987. Originally published as D 279 - 28 T. Last previous edition D 279 - 73 (1979). and add 20-mL of reagent grade toluene (Note 2). Close with a stopper, shake well for 10 s, and let stand 15 min. Repeat | the 10-s shake and let stand 45 min. ! 1--Additional amounts of pigment , may be used by prior ! agreement lor denser inorganic pigments, A maximum of 1.5 g is recommended for even the dense lead chromate pigments. ' ;i 2--Other solvents may be used, by mutual agreement between ; the parties involved, in place of toluene in a specific pigment bleed j evaluation. j 4.2 Filter through a glass funnel using double filter paper that has first been wet with toluene and collect approxi- ; mately 10 mL offiltrate. Ifthe filtrate is cloudy, refilter to get | a clear filtrate. j 3--In the case of colloidal particles, it may be necessary to centrifuge the filtrate. : 4.3 Hold the test tube containing the filtrate above a white ] background and look down through the filtrate for j coloration caused by pigment Weed. Describe the degree or j severity of bleed according to the following terminology: ' 4.3.1 None--No perceptible color (that is, no Weed). 1 4.3.2 Slight--A fhint but distinct coloration. ~' 1 4.3.3 Moderate--A pronounced but . not severe I coloration. i 4.3.4 Severe--An intense coloration. . 1 TEST METHOD B, WHITE OVERSTRIPE OF A PIGMENTED FILM 1 1 5. Procedure ~ 5.1 Prepare a coating of agreed upon composition, using the pigment under test, and prepare a film of this coating by any method that will give a smooth and uniform film of normal coating thickness (that is, in the range from 2 to 3 mils) (50 to 75 pm) leaving a portion of; the substrate uncoated. Cure the film under conditions appropriate to the end use. For air dry films, dry at room temperature, approximately 25C (77T) for a minimum of 24 h,. 5.2 Pretreatments of the colored coating, such as sanding or solvent wipe, or both, may be used before the overstripe, as agreed upon by the purchaser and seller. 5.3 Overstripe with a white finish of agreed upon compo sition. Ensure that the overstripe film is of uniform thickness and applied at complete hiding; otherwise, color showthrough may be erroneously interpreted as bleed. 5.4 Extend the overstripe film to the uncoated portion of the panel. Dry the overstripe under conditions mutually I I J j DUP050296581 iupon by the involved parties. Examine for color migration from the base coat into lute topcoat. Within 2 h after drying rate the extent of in accordance with tlie scale in Test Method A (4.3). i>cision and Bias The precision and bias are considered to be undeter minable as they will vary with the solvent or solvent blends used in Test Method A and with the type of base coat and type of overstriping used in Test Method B. 7. Keywords < 7.1 bleeding pigments; pigment bleeding test The American Society for Testing aridMaterials takes no positionrespecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressjy 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 and must be reviewed every five years and Ifnot revised, either reapproved orwithdrawn. Yourcomments are Invitedeitherfor revision of thisstandard 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, wltlqh you may attend, if you feet this 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. 61 Designation: D 280 - 81 (Reapproved 1987) Standard Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments1 This standard is issued under the fixed designation D 280; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A Dumber in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These methods hove been approvedfor use by agencies ofthe Department ofDefense to replace Method 4071 offederal Test Method Standard. No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specificyear ofissue which has been adopted by the Department ofDefense, 1. Scope 1.1 These methods cover procedures for determining hygroscopic moisture (and other matter volatile under the test conditions) in pigments. 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 healtk practices and determine the applicability of regulatory limitations prior to use. METHOD A--FOR PIGMENTS THAT DO NOT DECOMPOSE AT 110C 2. Apparatus 2.1 Weighing Bottle, wide-mouth, cylindrical, glass (flat form, about 30 mm in height and about 70 mm in diameter), provided with a ground-in glass stopper. Or, an aluminum moisture dish (about 90 mm in diameter and about 50 mm in depth) with a tightly fitting cover. 2.2 Oven in which a temperature of from 110 2C is maintained. 2.3 Analytical Balance. 3. Procedure 3.1 Weigh accurately the glass weighing bottle and stopper or the aluminum moisture dish with cover. Place a specimen of from 3 to 5 g of the pigment in the clean, dry weighing bottle or in the clean, dry aluminum moisture dish. Insert the stopper (or cover) and weigh to 0.1 mg. Subtract the weight ofthe vessel from the total weight to obtain the weight of sample used in the test. Remove the stopper (or cover) and place it and the bottle (or dish) containing the specimen in an oven that has been previously heated to 110 2C, heat for 2 h at a temperature of 105 to 110"C. Replace the stopper (or cover), cool in a desiccator, and weigh. Calculate the total loss in weight as percent of moisture and other volatile matter. 1 These methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Material. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 280 - 28. Last previous edition D 280 - 75. METHOD B--FOR PIGMENTS THAT DECOMPOSE AT I10C 4. Apparatus 4.1 Weighing Bottle, glass, as described in 2.1. 4.2 Open-Tube Manometer made of glass tubing 6 mm in diameter, filled with mercury to approximately 860 mm, fitted with rubber pressure tubing attached to a T-joint leading to the desiccator and the pump. A suitable lowpressure gage may be used in place of the manometer. The difference in levels of the mercury in the manometer when the system is in operation, subtracted from the barometer reading taken at the same time, gives the pressure ofthe system in millimetres of mercury. 4.3 Desiccator, glass, having a hole at the side or in the cover, constructed with heavy walls to withstand a vacuum of one atmosphere. The hole at the side shall he closed with a one-hole rubber stopper carrying a glass tube with a rubber tube connection and a pinchcock or witlua glass stopcock ground to fit the tubulature. 4.4 Oil Vacuum Pump,2 able to achieve and hold a vacuum of 3 mm. 4.5 Analytical Balance. -- 5. Procedure 5.1 Weigh accurately the glass weighing bottle, and stopper. Place ajspecimen of from 1 to 3 g of the pigment in the clean, dry weighing bottle, insert the stopper and weigh to 0.1 mg. Subtract the weight of the vessel fipm the total weight to obtain the weight of sample used in the test. 5.2 Remove the stopper and place it and the bottle containing the specimen in the desiccator containing fresh, anhydrous magnesium perchlorate.3 Close the desiccator, attach to the pump, and gradually evacuate until the pressure is constant at 3 mm or less (Note 2). dose the pinchcock or stopcock, stop the pump, and let stand at room temperature (70 to 90"F) for 24 h. 5.3 Slowly admit air that has been dried by passage through fresh magnesium perchlorate to the desiccator by means of the pinchcock or stopcock, remove the cover, quickly replace the stopper in the weighing bottle, and weigh. Repeat the evacuations and weighings until the loss in weight does not exceed 0.5 mg in 24 h. Calculate the total loss in 2 The "Hyvac" oil pump is satisfactory. 3 Available from Chemical Suppliera under the name Anhydrous or Dehydrite. 62 DUP050296583 D280 'ght as percent of moisture and other volatile matter (Note 2--Caution should be used in evacuating glass desiccators. The acuum should be applied gradually. Desiccators will maintain a uum for a greater length of time when a thin film of a suitable stopcock lubricant is applied to the ground surfaces. Desiccators when evacuated should be wrapped in towels or covered by other means to preventpos--siTblheisinijsurayntoetmhepiroipcaerlamtoer.thod and the details should be strictly followed. The determination of the true hygroscopic moisture content ofvery finely divided pigments is very difficult, ifnot impossible in some cases. The American Society for Testing anet Materials takes noposition respecting the validity of any patent rights asserted in connection with any ttam mentioned In this standard. Users of this standard are expressly advised (hat determination of the validity ofany 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 live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision 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. 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 RaceSt., Philadelphia, PA 19103. DUP050296584 Designation: D 281 - 84 (Reapproved 1989) Standard Test Method for Oil Absorption of Pigments by Spatula Rub-out1 This standard is issued under the fixed designation D 281; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflastrevision. 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 of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year cfissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the determination of the oil absorption of pigments by the spatula rub-out technique. 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: D234 Specification for Raw Linseed Oil12 D1483 Test Method for Oil Absorption of Pigments by Gardner-Caleman Method3 3. Summary of Test Method 3.1 A stiff, putty-like paste is formed by the dropwise addition of linseed oil to pigment that is being thoroughly rubbed with a spatula. The amount of oil required to produce the end point is used to calculate an oil absorption value. 4. Significance and Use 4.1 The oil absorption value obtained by this test method gives information about the vehicle demand of the pigment when it is used in a pigment paste. Oil absorption values can be used to characterize pigments or batches of a given pigment. 4.2 This test method differs from Test Method D 1483 in that D 1483 involves only a gentle stirring and folding of the pigment, whereas this test method requires a thorough rubbing action. Because the end points are different, the values obtained from the two test methods generally differ. 5. Apparatus and Materials 5.1 Balance, capable of weighing to 0.01 g. 5.2 Dropping Bottle, fitted with ground-in pipet and rubber bulb or buret, graduated in 0.1 -mL divisions. 5.3 Smooth Glass Rub-up Plate or Marble Slab (glass should have a surface similar to Hoover Muller Plates). 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 D01.24 on Physical Properties of Liquid Paints and Paint Materials. Current edition approved Aug. 31,1984. Published December 1984. Originally published as D 281 - 28 T. Last previous edition D 281 - 31 (1980). 2 Annual Book ofASTM Standards, 06.03. 3Annual Book ofASTM Standards, 06.02. 5.4 Spatula, sharp-edged, steel, having a blade of 'h or 3A by 4 in. (15 or 20 mm by 100 mm). 5.5 Oil, linseed, raw, conforming to Specification D 234 except that it shall have an acid number of 3 1. Linseed oil used in comparative tests must have the same acid value. Other liquids, such as refined oil, may be used by mutual agreement. 6. Procedure 6.1 ProcedureA (Weighing Bottle)--Weigh exactly 1 g,, or any multiple thereof (Note 1), of the thoroughly mixed and air dried pigment and place upon a glass plate or marble slab. Weigh to 0.1 g a dropping bottle containing raw linseed oil along with the pipet and rubber bulb. Add the linseed oil gradually, drop by drop (by means of the pipet), to the pigment. After the addition of each drop, thoroughly incor porate the oil by rubbing up with the spatula. The test is complete when exactly enough oil has been incorporated with the pigment to produce a very stiff, putiy-Kke paste, that does not break or separate. Weigh the bottle and oil to 0.1 g and determine by difference the weight of Oil used. --The specimen weight depends upon the specific gravity, fineness, and other characteristics of the pigment. For example, 20 g is taken for white lead, but about 1 g is sufficient for carbon black. Inany event, the specimen size should be large enough so that at least 1 g of oil is required. 6.2 Procedure B (Buret): 6.2.1 Follow Procedure A, except ad&ihe linseed oil from a buret rather than a dropping bottle pipet. Calculate the weight of oil in grams by multiplying the volume oil used by its density (0.93 g/mL). 6.3 It is suggested that when a new pigment is to be tested, a preliminary rub-out be made to determine an approximate end point. Once this is established, the actual determination should he made with a slower addition of oil and a more vigorous rub-out through the critical region, therefore per mitting a more precise assessment of the correct oil absorp tion end point. 7. Calculation 7.1 From the weights of oil and pigment used in the test, calculate the number ofpounds of oil required to exactly wet 100 pounds of pigment or grams of oil per 100 grams of pigment. 8. Report 8.1 Report the oil absorption of the pigment as the number of pounds (grams) of oil required to exactly wet 100 pounds (grams) of pigment. 64 w DUP050296585 1 I D 281 |||9. Precision 9.1.1 Repeatability--Two results obtained by a single operator should be suspect ifthey differ by more than 14.3 % 9.1 On the basis of an interlaboratory study of this test relative. |!jnethod in which one operator in each of five laboratories 9.1.2 Reproducibility--Two results obtained by operators [ tested two grades of zinc oxide covering a small oil absorp- in different laboratories should be considered suspect if they Itjion range by spatula rub-out, the within-laboratory coeffi- differ by more than 38.0 % relative. HLcient of variation was found to be 4.6 % at 10 df and the I between-laboratories coefficient of variation %11.6 at 8 df. 10. Keywords f Based on III used these coefficients, for judging the the following precision of criteria results should at the be 95 % 10.1 rub-out oil absorption; test pigments (general properties); spatula confidence level: 'rt h TheAmerican 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 ofany 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 Ifnot 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. DUP050296586 Designation: D 283 - 84 (Reapproved 1990)*1 Standard Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments1 ' This standard is issued under the fixed designation D 283; the number immediately following; the designation indicates theyear 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 Chdnge'since the last revision or reapproval. ' ' f; These test methods have been approvedfor use by agencies ofthe Department ofDefense to replace Method 7232 qfFederal Test Method Standard No. 141A. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department ofDefense. ` ' . .. %Section 25 was added and the title was changed editorially iri hfay 1990. 1. Scope 1.1 These test methods cover procedures for the chemical analysis of cuprous oxide and copper pigments. 1.2 The analytical procedures appear in the following order: Total Copper Total Reducing Power as Cuprous Oxide Metallic Copper Cuprous Oxide Cupric Oxide Metals Other than Copper Chlorides and Sulfates Acetone-Soluble Matter Water Stability Coarse Particles Coarse Particles Insoluble in Nitric Acid Sections 7 8 and 9 10 and 11 12 13 14 to 16 17 and 18 19 20 21 22 23 1.3 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. Specific hazard statements are given in Section 6. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints*2 D1193 Specification for Reagent Water3 D1208 Test Methods for Common Properties of Certain Pigments4 3. Significance and Use 3.1 This collection of test methods is used by pigment producers and paint manufacturers for process control, product acceptance, and research and development. * These test methods are under the jurisdiction of ASTM Committee D-J on Paint and Related Coatings and Materials, and are the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 26, 1984. Published January 1984. Originally published as D 283-28. Last previous edition D283 -520978)42. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vols 11.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 06.02. 4. Treatment of Sample c 4.1 Grind dry pigineniS; if iumpy or not finely ground, to a fine powder and thoroughly mix (Note 1). Large samples may be thoroughly mixed and a representative portion taken and powdered if lumpy or not finely ground. In all cases thoroughly mix the sample before taking portions for anal ysis. Preserve all samples in dry, dark, airtight and com pletely filled bottles or containers to prevent oxidation. Some commercial copper oxides appear to segregate or oxidize rather easily. Therefore, the thorough mixing of the sample to ensure homogeneity and the rapid handling ofthe sample, when exposed to light and air, are extremely important factors in obtaining accurate results. It is very important that the sample be thoroughly mixed. Some samples of cuprous oxide are not homogeneous so are likely to give trouble when an attempt is made to obtain concordant results. By placing a few grams of a sample on a sheet ofwhite paper and drawing it out with a spatula, it is frequently found that the sample contains coarse particles of black scale, along with small balls of bright red cuprous oxide. Thus, it may be necessary to pass the pigment through a No. 60 (250-pm) sieve, break up any lumps of ground pigment by gentle pressure, and grind any coarse particles failing to pass through the sieve. Since oxidation of slight or even considerable magnitude may take place, these operations sbould be performed quickly, avoiding prolonged grinding and exposure to light and air. 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.5 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. 5.2 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. 5.3 Ammonium Sulfate ((NH4)2S04). 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 Pharmocopeia." 66 * DUP050296587 # D 283 S.4 Nitric Acid (sp gr 1.42)--Concentration nitric acid V$! : fjfe.5 Perchloric Acid (70 %)--Concentrated perchloric arid lliplazards , . |6.1 Warning--Concentrated mineral acids cause burns of . skin, and eyes. Concentrated bases are also, hazardous. li^Avoid contact with skin or eyes. In case of contact immediSl!ljpy flush skin or eyes with plenty, of water. See appropriate IfcA Safety Data Sheets for farther information before ladling dangerous chemicals; ffj.2 Chemicals that have been declared toxic should be posed of as hazardous chemicals and not discharged into a TOTAL COPPER Procedure ` 7.1 Weigh accurately 1,0 g of the sample andtraiisfer to a. JOO-mL electrolytic beaker. AldS` 10 joiL of Coftttentrated. litric acid (HN03) and boil several rdiftufes. Add 10 mL of "ICIO4 (70 %) and; fame for.5 min. Cool,.dilute to a volume fjfapproximately 150 mL, and add 1 mL ofHNOj and 1 g of |(NH4)2so4. k 74 Carefully w^eigh the platinum electrode to 0.1 mg. feiectroplate the copper on a rotating platinum electrode at a. Idtarrent pf 2. A for 2 h. Dilute with .wafer npd continue the Ijelectrolysis for 15 min. When,tfte .deposition is. doriplete,. f reipoye^the electrode, wash with water apd acetone, dry> and I w$gh to <M mg. Save the electrolyte for the determination of % metals ot)ier than`copper ^Section 15)./ , ' , :. ,, 7.3 Calculate, the percent oftqtal'copper, Chi. 9. Procedure 9.1 Weigh accurately (Note 2) 0.15 g of the sample and place in a 250-mL, vented, glass-stoppered Erlenmeyer flask previously filled with carbon dioxide (C02) or other inert gas. Add a few small glass beads and 10 mL of Fed, solution. Heat gently for 15 min, stirring occasionally and maintaining at all times, an atmosphere of C02 or other inert gas. --The use of a 0.4-mL micro beaker for weighing the specimen is- advised. The beaker is Weighed first and the sample introduced into the beaker, the correct weight obtained, and the entire beaker and its contents dropped into the flask. This eliminates errors in weighing caused by brushing the sample from glass balance pans. 9.2 After the.specimen has been dissolved, cool, add 50: mL of distilled, wafer, and titrate at once with 0.1 N ceric ammonium nitrate solution until near the end point. Add 2 drops of orthophenanthroline indicator solution and com plete the titration. A sharp? distinct color change from orange to pale green occurs at the end point. Back-titrate with 0.03 N ferrous ammonium sulfate solution to the orange color. , 9.3 Calculation--Calculate the percent Of total reducing power, A, as cuprbus oxide (Cu20) as follows: ' V,N, - V,N, X 0.07154 x 100 (I) where: --,Ce(NH4)2(No3)6 solution required-to titrate the specimen, mL, = normality of the Ce(NH4)2(No3)fi solution, V2- = Fe(NH4)2(S04)2 solution required for the back- titration, mL, V2 2 = nonttahty of the FeCNH4)2(S04)2 solution, ^ = specimen weight, g, and 0.07154 = equivalent weight of Cu2O/10Q0. TOTAL, REDUCING POWER AS CUPROtJS OXtDE METALLIC COPPER8 8. Reagents 8.1 Ceric Ammonium Nitrate, Standard Solution (0,1 54,826, ,g -of ceric - ammonium nitrate (Ce(NH^)2(rfOj)^ (eithpr,,, reagent ,t^rade !tor _ reference standard purity) with 56 mL, of sulfuric acid ,(HgS04) (f+1). Dissolve the salt and arid,in water, ppql to kqqm, tempera ture, and: dilute to 1 Li Standardize this solution against analyzed bright copper fpil that, has 6een.freed from all oxide cpgting, .. ,7,-,. ; . 8.2 Ferric Chloride Solution--Dissolve 75 g .of ferric chloride (FeCl3-6 H20) in a mixture of 150 mL of hydro chloric arid (HP) (sp gr 1.19) and 400 mL of distilled water. Add 5 mL pf hydrogen peroxide (H2Q2) (30 fo) and boil to remove,the excess. 8.3 Ferrous Ammonium Sulfate, Standard Solution (0,03 N)--Dissolve 12 g of ferrous ammonium- sulfate (Fe(NH4)2(S04)2 6 H20) in 2QQ to 300 mL of water and add 40 mL of H2S04 (sp gr 1.84), while stirring constantly. Dilute to 1 L in a volumetric flask. A few pieces of mossy aluminum may be, added icf stabilize ,the solution. The solution should be restandardized frequently against 0.12V ceric ammonium nitrate solution. 8.4 Orthophenanthroline Indicator Solution-(0.5 % in wa ter)--Orthophenanthroline ferrous complex (ferroin) shall be used, as the indicator. 10. Reagents ,, 10.1 Ceric Ammonium Nitrate, Standard Solution (0.1 A0--See 8.1. ; 10.2 Denatured Alcohol (Formula No. 2B) ` 10.3' Extraction Solution--Add 40 mL ofHC1 (sp gr 1.19) to 1 L of denatured alcohol. Mix thoroughly. Add 40 g of stannous chloride (SnQ2 2H20) and . stir until completely dissolved,., ~ IQ.4 Ferric Chloride Solution--See 8,2. 10.5 Orthophenanthroline Indicator--See 5.4. 11. Procedure 11.1 Add approximately 20 mL of 4-mm diameter glass beads to a 250-mL Phillips beaker (assay flask). Weigh accurately 0.15 g ,pf sample on a tared, glazed paper approximately 'h in. ( 13 mm) square or a small watch glass that will fit into the Phillips `beaker, and transfer the specimen and paper or watch glass to the beaker. 11.2 Add 25 mL of denatured alcohol and swirl vigor ously for approximately 1 min to remove any surface coating 6 This lest method is based on the procedure described by Irvin Baker and R. Stevens Gibbs, "Determination of Metallic Copper in Cuprous Oxide--Cupric Oxide Mixtures," Industrial and Engineering Chemistry, Analytical Edition, Vol U, February 15, 1946, p. 124. DUP050296588 and break up lumps. While swirling the flask, slowly add 100 mL of the extraction solution. 11.3 After the addition of the extraction solution, swirl the flask vigorously for 5 min, adding lumps of dry ice (solid carbon dioxide) (Note 3) continuously during this time to lower the temperature of the solution to approximately -10C. Break up any lumps in the solution with a glass rod or policeman. 11.4 Filter off the metallic copper-cupric oxide residue using a 125-mm close-texture paper, a filter cone to support the paper, and suction (Note 4). Continue the addition ofdry ice to the flask and filter paper during the filtration to keep the solution cold. Wash the flask and filter paper with 150 to 200 mL of denatured alcohol, continuing the use of suction. 3--During the 5-min swirling period approximately 25 to 30 g of dry ice is added in approximately 5-g portions. The initial lumps of dry ice volatilize. rapidly due to the temperature of the solution. Approximately 15 g of dry ice is added in the first 2 min with a subsequent temperature drop to 0C. The remaining 15 g volatilizes more slowly and gradually lowers the temperature to the vicinity of -10C. These directions are not critical, but merely serve as a guide. The solution must be kept very cold in order to obtain correct and reproducible results. During the filtration period, additions ofdry ice to the flask should be continued to keep the solution cold until all of the extraction solution has been filtered. "# 4--In the great majority of cases, the metallic copper-cupric oxide residue is completely retained by the use of a suitable close-texture filter paper. The filtrationis rapid and can be readily completed in 5 min with proper suction. The filtrate should be carefully examined for the presence offinely divided particles ofcopper. In the event that extremely finely divided particles of copper are present and pass through the filter paper, as evidenced by the presence in the filtrate of a reddish color, which may be transient, the following method of filtration should be used: Place a 2S-mm diameter, beveled-edge, perforated porcelain filter disk in a 60, 75-mm diameter glass funnel. Using suction, prepare an asbestos filter pad on the porcelain disk of sufficient thickness and retentiveness to hold the finely divided residue. Wash the asbestos pad several times with denatured alcohol to remove all water from the pad. Filter the metallic copper-cupric oxide residue on this asbestos pad with the suction on at the start ofthe filtration. Keep the solution cold by the addition of dry ice and proceed with washing the residue, transferring it to the original extraction flask, and the subsequent titration as directed in Section 11. 11.5 Transfer the entire residue, filter paper, and beads to the original extraction flask and dissolve the residue in 25 mL of Fed3 solution, keeping an atmosphere of C02 above the sample by addition of dry ice. Heat on a steam bath to dissolve the copper. Add 50 mL of distilled water and 3 drops of orthophenanthroline indicator solution. Titrate with 0.1 N ceric ammonium nitrate solution until the color changes from orange to pale green. 11.6 Calculation--Calculate the percent of metallic copper content, B, as follows: CUPROUS OXIDE 12. Calculation 12.1 Calculate the percent ofcuprous oxide (Cu20), D, as follows: D- A - 2.2525 (3); where: A = total reducing power as cuprous oxide (Section 9), %, and B = metallic copper (Section 11), %. CUPRIC OXIDE 13. Calculation 13.1 Calculate the percent of cupric oxide (CuO), E, as follows: E= $%&7&'()j?*+ ,-,./0 <12 where: F = total copper (Section 7), %, B = metallic copper (Section 11),%, and D -- cuprous oxide (Section 12), %. METALS OTHER THAN COPPER 14. Reagents 14.1 Ceric Ammonium Nitrate, Standard Solution (0.1 N)--See 8.1. 14.2 Diphenylarnine Indicator--Dissolve l g of diphenylamine in 100 mL afHj&VCsp gr 1.84). 14.3 Potassium Ferricyanide Solution (50 g/L)--Dissolve 5 g of potassium ferricyanide (K^Fe(CN)iK m 100 mL of distilled water. Keep tightly stoppered in a dark bottle. 14.4 Potassium Ferrocyanide, Standard Solution (1 mL =* 0.001 g Zn)--Dissolve 5.0 g of potassium ferrocyanide (KtFe(CN)6 3H20) in distilled water and dilute to 1 L. Standardize with analyzed reagent grade zinc prior to use. * J | J 5 15. Procedure 15.1 Filter-the electrolyte from the determination oftotal copper (Section 7). Add 5 mL of H2SQ4 (sp gr l:84>-and evaporate justlto dryness to remove all HCIC>4 and HN03. Add approximately 150 mL of water and neutralize with NH4OH (sp gr 0.90), adding 5 mL in excess. Add 10 g of NH4CI. Boil the solution gently for several minutes and allow the precipitate to settle. Filter through a Close-texture paper, and wash the precipitate with 50 mL of hot NH4CI solution (20 g/L). 15.2 Determination of Iron--Dissolve the precipitate from the filter paper with hot HQ (1+1). Determine iron by the procedure of reduction with SnCl2 solution, followed by addition of HgCl2 and titration with 0.1 N ceric ammonium nitrate solution. 15.2.1 Calculation--Calculate the percent of iron, G, as follows: where: G = tyv, X 0-056 s x 100 (5) V4 - ceric ammonium nitrate solution required to titrate the specimen, mL, Ni - normality ofthe ceric ammonium nitrate solution, and BIWPiwy DUP050296589 # D283 specimen weight (Section 7), g. Determination of Cobalt and Evaporate the |te (see 15.1) to 15 to 20 mL. If the solution is colored, sence of nickel or cobalt, or both, may be indicated. If nt, they must be removed before determining zinc, jjrmined by any standard procedure and reported as snt of cobalt or nickel, or both. .4 Determination of Zinc--Neutralize the solution (see 4) with H2S04 (1+2) and add 15 mL in excess. Dilute to mL with water. Add 10 drops of K,3Fe(CN)6 solution 5 drops of diphenylamine. indicator solution. Heat to and titrate with standard K4Fe(CN)6 solution. A color ;e lirom blue to greenish yellow occurs at the end point i.4.1. Calculation--Calculate the percent of zinc, H, as ows: V.T H= O 100 ere: (6) K4Fe(CN)6 solution required for titration of the spec imen, mL, ?.= zinc equivalent of the K4Fe(CN)6 solution, and == specimen weight (Sectioii 7), g. Report 16.1 Report as percent of metals other than copper the ftal percent of metals determined in accordance With [ection 15. CHLORIDES AND SULFATES Reagents jMj| 47.1 Barium Chloride Solution (100 g/L)--Dissolve 117 g ji^of BaCl2'2H20 in water and dilute to 1 L. 172 Silver Nitrate Solution--Dissolve 5 g of silver nitrate ^(AgN03) in 100 mL of water. 17.3 Sodium Carbonate Solution--Prepare a saturated Jlpjution of sodium carbonate (Na2C03) that is free of both chlorine (Cl) and sulfate (S04). IIP' Procedure 18.1 Weigh accurately approximately 10 g of the sample, add an excess of concentrated HN03, and heat gently until the sample is decomposed. Dilute with water to approxi mately 150 mL. Add an excess of Na2C03 solution (16.3), and bring to a boil. Transfer tb a 500-mL volumetric flask and dilute to the mark with water. Let settle. 18.2 Draw off two separate 50-mL aliquots of the dear solution. Make each slightly add with HN03. 18.3 Determination of Chlorides--To one of the 50-mL aliquots (18.2), add a few drops of AgN03 solution. If no predpitate forms, report no chlorides present. If a precipitate forms, add slowly an excess of AgN03 solution. Heat to boiling after the predpitate has settled, filter through a Gooch crucible, and wash with cold water. Dry at 130"C, cool, and weigh. 18.3.1 Calculation--Calculate the percent of chlorides as Cl, J, as follows: Pi - AgCl, g, and S3 - specimen weight, g. 18.4 Determination ofSulfates--Dilute the second 50-mL aliquot (18.1) to approximately 200 mL. -Add approximately 1 mL ofHC1 (1+1). Heat to boiling and add Slowly an excess (10 mL) of BaCl2 solution. Let settle, filter through a Gboch crucible, and wash. Dry, ignite at fall red heat, cool in a desiccator, and weigh. 18.4.1 Calculation--Calculate the percent of sulfates as S04, K, as follows: where: K= P2 X 0,412 S, x 0.1 x 100 (8) P2 = BaS04, g, and S3 = specimen weight, g. ] ACETONE-SOLUBLE MATTER- 19. Procedure 19.1 Weigh accurately 5.0 g of the well-mixed sample and transfer to a 250-tnL glass' stoppered Erienmeyer flask. Add 100. mL of acetone and shake vigorously for 15 min, Allow to settle, and filter through a double, close-texture paper into a 250-mL Griffin beaker. Wash the flask and paper Well with acetone to remove all acetone-soluble matter. 19.2 Evaporate, the acetone on a water bath to a low volume and transfer to a 15 by 55-mm weighed aluminum moisture dish. Wash out the beaker with a small amount of acetone. Finally evaporate all acetone and heat the residue for 30 min in an oven at 105"C. 19.3 Report the weight of the dried residue as acetonesoluble matter. WATER 20. Procedure 20.1 Determine the water content in accordance with Test Methods D 1208. STABILITY 21. Procedure ~ 21.1 Spread approximately 100 g of the sample on a watch glass and heat in an oven at a temperature of 100F (40C) and approximately 95 % relative humidity for a period of 72 h. Remove from the oven. Note any change in color of the pigment. Determine its total reducing power in accordance with Section 9. 21.2 Determine the percent of moisture on 50 g of the sample remaining from the test described in 18.1 using the distillation method specified in Section 20. 21.3 Calculation--Calculate the percent decrease in total reducing power, L, as follows: where: L = 100 -M L = total reducing power after stability test calculated on dry basis, N = total reducing power after stability test as determined in 21.1, aud M= moisture (21.2), %. DUP050296590 where: L = ~jj~ x 100 (10) L = decrease in total reducing power (from stability test), % and A - total reducing power before stability test as calculated in 9.3. COARSE PARTICLES 22. Procedure 22.1 Determine the percent of coarse particles on a 25-g specimen as described in Test Methods D 185 using both a No. 200 (75-pm) and a No. 325 (45-pm) sieve. COARSE PARTICLES INSOLUBLE IN NITRIC ACID 23. Procedure 23. i Transfer the residue retained on a No. 200 (75-pm) sieve to a beaker, add 50 mL of HN03 (1+3), and boil for 5' min. Cool and filter through a tared Gooch crucible, previously washed with HN03 (1+3), or a fiitted-glass filter of appropriate porosity. Wash the insoluble residue on the filter with hot water. Dry the crucible or fritted-glass filteand contents at 105 to 110C and weigh. 23.2 Calculation--Calculate the percent of coarse parti-' cles insoluble in nitric acid, T, as follows: T = |xl00 (II) where: R = weight of residue, g, and S = weight of original specimen, g. 24. Precision 24.1 Precision data are not available at this time. When ' available the appropriate precision statements will be added. 25. Keywords 25.1 chemical analysis; copper pigments; cuprous oxide, pigments 77ie American Society for Testing end Materials takes 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 of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any thpeby the responsible technicalcommittee and must be reviewed every thre years and knot revised, either reapprovedor withdrawn. Yourcomments are Invited either forrevision 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 fee/ that your comments have not received a fair hearing you should make Yoor views known to the ASTM Committee on Standards,-1916 Race St., Philadelphia, PA 19103. 70 lip*.......................... DU P050296591 Designation: D 284 - 88 e r Standard Test Methods for Chemical Analysis of Mercuric Oxide Pigment1 This standard is issued under the fixed designation D 234; 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 ft) indicates an editorial change since the last revision or reapproval. '.'Hi. Scope fjjj? 1.1 These test methods cover procedures for the chemical mnalysis of mercuric oxide pigment. * 1 1 This standard may involve hazardous materials, oper- \ions, and equipment. This standard does not purport to ddress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish vpropriate safety and health, practices and determine the iplicability ofregulatory limitations prior to use. A specific iazard statement is given in the Note of 11.1. ^.Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water12 , D1208 Test Methods for Common Properties of Certain Pigments3 *$. Significance and Use 3.1 These test methods are intended as a quick and |reliable procedure for measuring purity of mercuric oxide |pigment to determine if it meets purity standards as agreed jtipon between the producer and the consumer. f4. Purity of Reagents and Materials 4.1 Reagent grade chemicals shall be used in all tests. lUnless otherwise indicated, it is intended that all reagents llhall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, vhere such specifications are available.4 Other grades may be Jused, provided it is first ascertained that the reagent is of (sufficiently high purity to permit its use without lessening the |faccuracy of the determination. [t. 4.2 Unless otherwise indicated, references to water shall |be understood to mean reagent water conforming to Type II I of Specification D 1193. it: 15. Preparation of Sample | 5.1 If the sample is large, mix it thoroughly before taking I a representative portion. Grind the representative portion to 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 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 31, 1988. Published December 1988. Originally published as D 284 - 28 T. Last previous edition D 284 - 74 (1987)'1. 2 Annual Book ofASTM Standards. Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.02. 4 "Reagent Chemicals, American Chemical Society Specifications" Am. Chem. 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 Nostraad Company, Inc., New York, NY, and the "United States Pharmacopeia." a fine powder and thoroughly mix before taking portions for analysis. Keep the sample in a stoppered glass bottle. 6. Precision 6.1 Repeatability and reproducibility are believed to be well within the limits usually obtained on similar chemical test methods, but no actual figures on precision are available. ALKALINITY OR ACIDITY 7. Procedure 7.1 Determine alkalinity or acidity in accordance with Test Methods D 1208. T344 5689;8= 8. Procedure 8.1 Examine a representative specimen of the dry mer curic oxide under a microscope for the presence of free mercury. TOTAL MERCURY 9. Reagents and Materials 9.1 Ammonium Thiocyanate, Standard Solution (1 mL = 0.012 g Hg)--Dissolve 9g of ammonium thiocyanate (NH4CNS) in water and dilute to 1 L. Standardize the solution against mercury, as follows: Weigh to 0.1 mg about 4.6 g of mercury, and dissolve it in 40 mL of warm HN03 (1+1). Dilute to 200 mL with wafer and add KMnO,, solution (50-g/L) dropwise until the pink color persists for 5 min in order to ensure the absence of nitrous acid (HN02) and monovalent mercury. Add FeS04 solution (50 g/L) dropwise to destroy excess permanganate. Add 4 mL of ferric ammonium sulfate indicator solution, and titrate with the NH4CNS solution. 9.2 Calculate the mercury equivalent M of the NH4CNS solution, in grams per millilitre, as follows: M -- WJV) where: Wt -- mercury used, g, and V, -- NH4CNS solution required for titration, g. 9.3 Ferric Ammonium Sulfate Indicator Solution--Dis solve enough feme ammonium sulfate (Fe2(SQ4)3 (NH4)2S04 24H20) in water to make a saturated solution at room temperature and add HN03 (sp gr 1.42) dropwise to bleach the brown color of the solution. About 30 g of ferric ammonium sulfate per 100 mL of water will be required for the saturated solution. 71 DUP050296592 D284 9.4 Ferrous Sulfate Solution (50 g/L)--Dissolve 5g of ferrous sulfate (FeS04 7HzO) in water and dilute to 100 mL. 9.5 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (NHOj). 9.6 Nitric Acid (1+1)--Mix 1 volume of HN03 .(sp gr I. 42) with 1 volume of water. This acid must be free of nitrous acid (HN02). .. 9.7 Potassium Permanganate Solution (50 g/L)--Dissolve 5 g of potassium permanganate (KMn04) in water and dilute to 100 mL. 10. Procedure 10.1 Weigh to 1 mg about 0.5 g of the sample, previously dried for 1 h at 150C into a 750-mL Erlenmeyer flask. Add 40 mL of;HN03 (1+1), and warm gently until the specimen is dissolved. , 10.2 Dilute to 200 mL with water, and add 4 mL of ferric , ammonium sulfate indicator solution. Titrate with 0.1 N NH4CNS solution until a distinct pink color persists after vigorous shaking. II. Calculation 11.1 Calculate the percent of mercury P as follows:' P=[(V2x M)/SJ x 100 where: V2 = NH4CNS solution required for titration of the spec. ii imen.-mL ij M = mercury equivalent of the NH4CNS solution, g/mL and S' = dried specimen, g. ASH 12. Procedure 12.1 Ignite 2.0 gofa dry specimen in a weighed porcelain 1 crucible or dish under a well-ventilated hood. (Warning-- See Note) Cool and weigh the residue. Calculate the percent 1 of ash. , Note: Warning--The fumes are poisonous. * INDEX TERMS ' : 13. Index Terms 1' s| 13.1 These Test Methods are indexed under the following 1 terms: mercuric oxide; pigments--mercuric oxide. 1 The American Society for Testing and Materials takes noposition respecting the validity ofanypatent rights asserted In connection with any Item mentioned in this standerd. 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 andmust be reviewed every five years and footrevved, eitherreapproved orwithdrawn. Yourcommenta era invited either for revision ofthis standard orforadditionalstandards and should be addressed to ASTM Headquarters. Your comments wllf recelva careful consideration at a meeting ol 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 Race St., Philadelphia, PA 19103. ` t: . 1. - ' . mu. > ippssw ' I 1.. i;.1,!TM.!,'!!! DUP050296593 Designation: D 301 - 89 Federation of Societies for Paint Technology Standard No. Cs-2-58 Standard Test Methods for Soluble Cellulose Nitrate1 This standard is issued under the fixed designation D 3D1; 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 cope These test methods cover the material known as ble cellulose nitrate (also known as soluble nitrocellui), which is shipped wet in conformance with regulations be Interstate Commerce Commission. The test methods appear in the following sections: Sections j Samples iTest rogen bility and Appearance ofSolution ility |uene Dilution 5 to 7 4 20 and 21 8 to 10 19 II to 13 22 to 24 14 to 18 1.3 This standard may involve hazardous materials, oper|iions, and equipment. This standard does not purport to mdress ail ofthe safety problems associated with its use. It is ffe responsibility of the user of this standard to establish Appropriate safety and health practices and determine the 7pplicability of regulatory limitations prior to use. For Hie hazard statements, see Notes 2 through 5. . Referenced Documents 2.1 ASTM Standards: D 302 Specification for Ethyl Acetate (85 to 88 Percent Grade)12 D303 Specification for n-Butyl Acetate (90 to 92% Grade)3 D 362 Specification for Industrial Grade Toluene2 D1343 Test Method for Viscosity ofCellulose Derivatives by Ball-Drop Method4 E 1 Specification for ASTM Thermometers5 3. Sampling 3.1 Samples shall be taken from not less than 10 % (at least two barrels) of each lot or batch in the shipment In sampling the barrels, two samples of approximately 1 pt (0.5 dm3) each shall be taken from two well-separated points at least 1 ft (0.3 m) beneath the surface of the material in the barrel. These samples shall then be composited to represent each lot or batch in the shipment. 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 D01.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D301 -29. Last previous edition D301 -72(1983). 2 Annual Book ofASTM Standards, Vol 06.03. 2 Discontinued, see 1986 Annua! Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 06.02. 5 Annua! Book ofASTM Standards, Vols 05.03 and 14.03. 3.2 The samples shall meet the following requirements: 3.2.1 Appearance--The cellulose nitrate shall not be dis colored and shall be free oflumps and foreign matter, such as charred particles. 3.2.2 Ash--Ash content shall not exceed 0.30 %, calcu lated on the basis of dry-weight soluble cellulose nitrate. 3.2.3 Nitrogen--The percent nitrogen, calculated on the basis of dry-weight soluble cellulose nitrate, shall be within the limits agreed upon by the purchaser and the manufac turer for the particular type of soluble cellulose nitrate. 3.2.4 Stability--The stability as determined by the 134.5 C test shall be not less than 25 min. 3.2.5 Viscosity--The viscosity shall be within the limits agreed upon by the purchaser and the manufacturer for the particular type of soluble cellulose nitrate. 3.2.6 Solubility and Appearance of the Solution--The solubility and appearance of the sample shall be equal to the reference standard for the particular type of soluble cellulose nitrate. 3.2.7 Film Test--The film test of the sample shall be equal to that ofthe reference standard for the particular type of soluble cellulose nitrate. 3.2.8 Toluene Dilution Test--The toluene dilution value of the sample shall be equivalent to that"of the reference standard for the particular type of soluble cellulose nitrate. DRYING SAMPLES 4. Procedure 4.1 Soluble cellulose nitrate is a flammable material, the degree of flammability varying with the extent and nature^of the wetting medium. Cellulose nitrate is always wet with water or alcohol in commercial handling, shipping, and_ storage, in which condition it presents no unusual hazard. Dry cellulose nitrate, if ignited by fire, spark, or static electricity, bums very rapidly. Samples of dry cellulose nitrate must not be stored at any time. Dry only that portion required for immediate test. Wet the excess material and the samples left after testing with water and dispose of by burning on a safe burning ground. 4.2 Dry small quantities required for ash and nitrogen tests by spreading in a thin layer on a tray at room temperature for 12 to 16 h, followed by oven-drying in crucibles or weighing bottles 1 h at 100 to 105C. The oven used for drying cellulose nitrate should have the latch removed. Wear a face mask (see 9.2) when the oven is opened after samples have been heated. 4.3 Dry larger quantities of water-wet material required for viscosity and toluene dilution tests, or a small quantity for stability tests, by blowing warm compressed air (at a temperature of 60 to 65C, and a pressure of 40 to 60 psi 73 DUP050296594 (275 to 415 kPa)) through the sample placed in a cylindrical holder with a screen over one end for % to 1 h. Provide the compressed air line with a safety plug (Note 1) of Wood's metal, which melts at 70 to 75'C, so the air will be diverted from the sample if a temperature of 70"C is exceeded. >@AB I--Information on the availability of a suitable fitsible plug assembly may be obtained from ASTM Headquarters. 4.4 If the material is alcohol-wet, it is necessary to modify the drying procedure. After placing the required amount of cellulose nitrate in the cylindrical holder, pour in sufficient distilled OrTron-free water, to fill it Allow the bulk of the liquid to drain off. Then dry by blowing warm air through the holder aS described in 4.3. ASH 5. Significance and Use 5.1 Ash accounts for the nonsoluble, nonfilin forming portion df the polymer. It may affect solution clarity and film properties. 6. Procedure 6.1 Dry the cellulose nitrate as described in 4.2 and place a specimen of approximately 2.0. g in a tared and .ignited, crucible. After drying at 100 to 105C for ' 1 h, cool in a desiccator and weigh accurately. Moisten the specimen w` 20 to 30 drops of ACS grade HN03 (sp gr 1.42) and heat o a steam bath until the specimen is decomposed to a gum mass. If necessary to complete the decomposition, a several additional dropsr of HN03 at intervals. Then heat t crucible slowly over a bunsen burner or in an electric furna until all volatile matter is driven off. Finally, ignite at re heat to constant weight, cool, and weigh. 7. Calculation 7.1 Calculate the percent ash as follows: Ash, % - (wt of ash/wt ofdry sample)' x 100 NITROGEN 8. Significance and Use 8.1 The nature and strength of solvent systems required! for cellulose nitrate are dependent upon the nitrogen coto l tent. Mismatches of solvent with nitrogen level cafr result in i poor solution quality and colloid and gel formation. 9. Apparatus 9.1 Nitrometer--Use the duPont Nitrometer, which is illustrated in Figs. 1 to 4. 9.2 Face Mask--A. face mask, so constructed that a heavy i i l5il; CDEFG1 in. = 25.4 mm. FIG. t General Assembly of Apparatus for Nitrogen Determination 74 DUP050296595 W&8& D 301 being held at the same height. Then seal the compensating tube using a small blowpipe flame. 10.2.2 As a preferred alternative, nitrogen may be used in place of air. 10.2.3 Place in weighing bottles 0.95 0.05-g portions of ACS grade KN03 that has been recrystallized twice from distilled water and ground to pass a No. 100 (150-pm) sieve. Dry the specimens 2 to 3 h at 135 to 150C. Stopper the bottles, cool in a desiccator, and weigh accurately. Transfer the KN03 to the cup of the reaction bulb and weigh the weighing bottle to obtain tlie weight of sample used. Add 1.0 mL of water and stir the mixture in the cup with a small glass stirring rod to liberate the entrained bubbles of air; work the undissolved crystals into the lower part of the cup, keeping them below the surface of the solution. It is not necessary that the KN03 dissolve before drawing it into the reaction bulb. Make sure the lowerstopcock is open; then admit the mixture to the bulb by a series of quick openings ofthe upper stopcock, in the meantime, keeping the crystals below the surface of the liquid. In this way, all but a small amount of the KN03 may be run into the bulb. Rinse the cup with a IMPORTANT* JtI CALIBRATE IN THIS PORTION SO THAT MERCURY MENISCUS HIJKI L MM NO PQR SWILL BE THUS AT THE 14.01 MARK I S 7 7 to 240.36cc.AT 20*C IMPORTANT . MAKE STRONG, ANO TAP&R CRAPUAUL' AS SHOWN, BEGINNING h VS* BELOW STOPCOCK. COUNTERSUNK. - -More--Cl 'In.- * 25.4 mti.* FIG. 2 Measuring Tube for Nitrogen Determination * pibee of cellulose acetate sheeting protects the fate. ' TUVW 2: Precaution--The cellulSse acetate mask , must be worn during the generation and measurement of the gas as a precaution in. case ofan explosion. 10. Procedure 10.1 Calibrate the measuring tube accurately in the usual manner, using mercury as the calibfating liquid.. J0.2 Standardize the apparatus as follows: . 10.2.1 Fill the compensating, measuring, and reaction tubes and their rubber connections with mercury. Run 20 to 30 ml of H2S04 (ACS grade, 94.5 0.5 %) into the reaction bulb through the cup at the top and admit about 210 mL of air. Close the stopcocks, shake the bulb well, and allow to stand overnight. This desiccates the air which is then run into the compensating tube until the mercury is about on a level with the 12.50 % mark- on the measuring tube, the two tubes XYZ[\1 ia = 25.4 inm. FIG. 3 Reaction Bulb DUP050296596 D 301 Brazed to Under abcde1 in. - 25.4 ram. FIG. 5 Copper Bath for Stability Test j FIG. 4 Compensating Tube second 1.0-mL portion of water; then repeat with a third 1.0-mL portion (3 mL in all). This should be sufficient to dissolve all remaining particles of KN03 in the cup. Transfer 25 mL of the H2S04 (94.5 0.5 %), divided in several portions, to the cup, and subsequently to the bulb by lowering the reservoir slightly and opening and closing the upper stopcock, care being taken that no air enters even the bore hole in the stopcock. There must always be a slight suction when introducing the specimen, the wash water, and the acid, but never enough to cause air to be sucked into the reaction bulb. The quantities of water and H2S04 used should be constant. Then with the bottom stopcock still open, lower the reservoir bulb to give reduced pressure in the reaction bulb and gently shake the reaction bulb to start the decomposition. 10.3 After the evolution of NO has become slow (Pre caution, see Note 3), lower the reservoir bulb until all but 25 mL of the mercury in the reaction bulb is withdrawn, close the bottom stopcock, and shake the reaction bulb vigorously for 5 min. ]^_` 3: Precaution--It is extremely important that the bottom stopcock be left open until the major part of the decomposition has occurred; otherwise, sudden evolution of gas will burst the bulb, scattering acid and glass. 10.4 When the reaction is completed, allow the gas to cool for 20 min; then transfer the gas to a measuring tube. By means of the leveling device make careful adjustment of the mercury levels so that the mercury in .the measuring tube is at the 13.85 % mark (the theoretical percent nitrogen in KNOa) if an "exactly 1.000-g specimen was used, or a proportional reading if less was used. Paste strip of paper on the compensating tube at the level of the" mercury, and the standardization is completed. It is advisable to make several check determinations, preferably on different days, to ensure accurate standardization. Determinations should check within 0.01 %. 10.5 Dry the cellulose nitrate as described in 4.2 and place a specimen of 1.0 to 1.2 g in a weighing bottle. After drying at 100 to 105C for l h, stopper, cool in a desiccator, and weigh accurately. Transfer the specimen to the cup, of the decomposition bulb; then reweigh the empty bottle to get the weight of the specimen by difference. Add 5 to fO mL of H2S04 (94.5 0.5 %) to the cup and stir the mixture with a small stirring rod. Lower the mercury reservoir and then, with the lower stopcock open, draw the mixture in by opening the upper stopcock. Take care that no air is drawn in. Rinse the cup of the decomposing bulb several times with H2S04, using a total of 25 mL for dissolving and rinsing. Complete the determination in accordance with the proce- 1 I ! 76 DUP050296597 # D301 cation E 1. The thermometer should be fitted with a cork stopper and placed in an empty glass tube in the bath. 12.8 Methyl Violet Test Paper? FIG. 6 Brass Condenser for Stability Test Apparatus ure described in 10.2 for Standardisation of the apparatus, and take a'reading after adjusting the level rifthe mercury in $he reading tube to the mark on the compensating tube. The reading divided by the weight of the specimen gives the 'percent nitrogen. STABILITY filj. Significance and Use : ft? 11.1 Nitrocellulose stability is measured by-detecting the evolution of nitrogen oxides under elevated temperature. The results are not necessarily a predictor of shelf life. 12. Apparatus 12.1 Copper Bath--Copper bath with copper or brass condenser, as shown in Figs. 5 and 6. These baths are usually made to hold 13 to 15 test tubes. To aid in heat transfer, add 15 to 25 mL of mineral oil to each copper vyeH, in order to fill the space between the glass tube and the well. To maintain the. bath at a temperature of 134.5 0.5C, fill to within 3 ini (76 mm) of the top with a mixture consisting of ten parts of a commercial ethylene glycol solution (auto mobile radiator antifreeze containing a corrosion inhibitor) and one part of water. Adjust the temperature of the boiling liquid in the bath to 134.5 0.5C by adding more glycol or water, as necessary. 12.2 Test Tubes--Heat-resistant glass6 tubes, with an out side diameter of 18 mm, a wall thickness of L5 mm, and a length of 290 mm. 12.3 Heater--An electric hot plate for heating the bath. 12.4 Face Mask--See 9.2. 12.5 Gloves--A pair of heavy gloves. 12.6 Pincers--Long pincers for handling the test tubes. 12.7 Thermometer--An ASTM Stability Test Thermom eter having a range from 130 to 140<'C and conforming to the requirements for Thermometer 26C as prescribed in Specifi 7 13. Procedure 13.1 Conduct the test in a room that is free of acid fumes. fghi 4: Precaution--It is important that the operator wear the cellulose acetate mask and heavy gloves and the tubes be handled with long pincers. 13.2 Dry the sample as described in 4.2. Weigh duplicate specimens of 2.5 0.1 g into test tubes and press the specimens down so that they occupy the lower 2 in. (51 mm) of the tubes; then swab out all cellulose nitrate particles adhering to the inside wall of the tubes. Crease a piece (20 by 70 mm) of normal methyl violet test paper for one half its length; then insert it in the tube .with the uncreased portion downward, until the lower edge is 1 in. above the top of the specimen. The papa? must remain in this portion throughout the test. Stopper die tube With a cork provided with hole or notch 4 mm in diameter. Place the tube, without jarring, in' the heating bath maintained at 134.5 0.5C. Beginning at the end of the first 20 min, inspect the tube at S-min intervals by lifting the tube until the methyl,violet paper, but not the cellulose nitrate, is visible above the surface of the bath. The end point is reached when the entire test paper changes in color to salmon pink. For example, if the color is not completely changed at 20 min but iS completely changed at 25 min, record the stability of the specimen as 25 min. jklm 5: Precaution--As asafety measure, immerse the specimen in cold water immediately upon completion of the test.-- VISCOSITY 14. Significance and Use 14. i Coating and lacquer formulations are based- on percent solids in.a solvent system. Viscosity is a determining factor in limiting the percent solids in a given solvent system. 15. Solutions Required 15, f Determine viscosity by dissolving the cellulose ni trate, dried as described in 4:3, according to a standard formula (Table 1) and noting the time for a steel ball to fall through a measured depth of the solution at 25<>C. Use formula A for types designated as 5 s or over. Use formula B for types designated as 'h and % s,. Use formula C for types designated as `A s and 30 to 35 cp. Cellulose nitrate will dissolve more quickly if it is first wet with alcohol and toluene and the mixture then allowed to stand a few minutes before, the ethyl acetate is added. Completely dissolve the sample in the solvent mixture by agitating in a tightly closed bottle. ' - 16. Viscosity Determination 16.1 Measure the viscosity, using the apparatus and fol lowing the procedure described in Test Method D 1343. 6 Borosilicaie glass has been found satisfactory for this purpose. 7 The norma] methyl violet test papers are available from the Naval Powder Factory, Indian Head, MD. DUP050296598 D 301 17. Report 17.1 Report the results in seconds (Note 6) for a Vn-in. (2.4-mm) steel ball (density 7.7 0.1) and a 2.00 0.02-in. (50.8 0.5-mm) drop. The viscosity value shall be prefixed with the letter A, B, or C, corresponding to the formula of the solution employed. nopq 6--Results in seconds for a %2-in. steel ball may be converted to poises as follows: n - 0.560 (a -- b) t where: n - viscosity at the specified temperature: P. a = ball density, g/mL, b = solution,density, g/mL, and t - time of Ml, s. 18. Precision and Bias 18.1 Precision--The coefficient, of variation between two results.obtained by a single analyst is estimated to be.2.6 % at 10 dfl Two results should be considered suspect, ifthey differ by more than 7 %. 18.2 Bias--No statement on bias can be made at this time as no material is available to serve as a standard. SOLUBILITY AND APPEARANCE OF SOLUTION 19. Procedure 19.1 Compare either formula A, B, or C (Table 1) with a freshly-prepared standard solution of the same type of soluble cellulose nitrate of the same formula. Make the comparison in small vials and note the color, turbidity, "grain," and "flock." TABLE 1 Solutions for Viscosity and Film Tests Formula A Formula B Formula c Ingredients: Soluble cellulose nitrate (dried). weight percent Complete^ denatured ethyl alcohol (188 to 190 proof), weight percent Toluene,'' weight percent Ethyl acetate,8 weight percent Density of solution at 25C (g/mL) 12.2 22.0 48.3 17.5 0.90 20.0 20.0 44.0 16.0 0.93 25.0 18.75 41.25 15.0 0.97 * Toluene conforming to Specification O 382. 8 Ethyl acetate conforming to Specification 0 302. FILM TEST 20. Significance and Use 20.1 The quality of a lacquer or other surface finish is dependent upon clarity and gloss of the dry film. This test method can reveal potential impurities and flaws in applied finishes. 21. Procedure 21.1 Dilute formula A, B, or C (Table 1) with an equal volume ofnormal butyl acetate and pour the solution beside a freshly prepared standard solution of the same type of soluble cellulose nitrate and of the same formula, on a clean glass plate. Allow to dry in a nearly vertical position in a dust-free atmosphere. Compare the specimen with the standard for undissolved particles, which indicate unnitrated cellulose or impurities, and for poor flow and poor gloss. TOLUENE DILUTION 22. Significance and Use 22.1 This test method can ascertain whether cellulose nitrate of a given percent nitrogen is contaminated with material of a significantly different nitrogen content. Such cross contamination may adversely affect solution and film quality. 23. Procedure 23.1 Prepare a solution containing 12.2 weight percent of cellulose nitrate dried as described in 4.3, and 87.8 weight percent of butyl acetate conforming to Specification D 303. To 50 mL of this solution in a stoppered bottle add'toluene, conforming to Specification D 362 in small quantities from a buret, shaking well after each addition, ~- 24. Calculation and Report 24.1 Report as the dilution value the volume of toluene required to effect the first permanent separation of cellulose nitrate, calculated as a percent by volume of the original solution, as follows: ' Dilution value = (mL toluene x~100)/50 ,- = mL toluene X 2 rstu 7--Large quantities of butyl acetate and toluene should be reserved for this test to avoid posable variation betweep different loti The test should be ran at 25"C. The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights assertedin 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 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 ba reviewed every five years and Ifnotrevised, 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. ' 78 DU P050296599 Designation: D 305 - 84 (Reapproved 1990)' Standard Test Method for. Solvent-Extractable Material in Black Pigments1 This standard is issued under the fixed designation D 305; 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. l vwxyzSection 9 was added editorially in May 1990. Scope "Id This test method covers the determination of the olvent-extractable material in black pigments such as rbon black, lampblack, and bone black. 11.2 This standard does not purport to address the safety problems associated with its use. It- is the responsibility, ofthe per of this standard to establish appropriate safety and ealth practices and determine the applicability ofregulatory ^imitations prior to use. Smm. Outside Diameter, Approx^ 50mm:----->f*----- 50mm.------ * \ Referenced Document 2.1 ASTM Standard: D 329 Specification for Acetone21 ., Significance and Use 3.1 This test method is used by black pigment producers j|rid users for product acceptance. i1' ft. Apparatus p 4.1 Extraction Apparatus, consisting of a flask, siphon prop, and a condenser similar to the apparatus shown in' either Fig. 1 or Fig. 2. ; {|}~ 1--A Sophlet apparatus may be used as an alternative, 4.2 Extraction Thimbles--The thimble must be made of ' greaseless paper and be of correct size to fill the selected apparatus. |f! 2--Tbe recommended thimble size for each of the apparatus shown in Fig. I is listed below; r Fig. I Fig. 2 Height ,, Inside diameter -- Outside diameter 70 ram 28 mm 30 mm 62 mm 22 mm 24 mm ` 4.3 The thimbles are available in various heights and $ widths with two thickness levels, single thickness or double * thickness. Single-thickness thimbles are recommended for this extraction procedure. . S. Reagents and Material 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended 80mm. FIG. 1 Extraction Apparatus 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 he 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 Solvent--Acetone and benzene are the most com monly used solvents (see Specification D329); however, other solvents may be used as agreed upon. 5.3 Glass Wool. 6. Procedure 6.1 Weight approximately 10 g of pigment (moisture-free) 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 D01.2I on Chemical Analysis of Paints and Paint Materials. Current edition approved Aug 31, [984. Published October 1984. Originally | published as D 303 - 29 T. Last previous edition D 305 - 72 (1978). 2 Annual Book ofASTM Standards, Vol 06.03. 1 "Reagent Chemicals, American Chemical Society Specifcations," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not lisled by the American Chemical Society, sec "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co.. Inc., New York, NY, and the "United States Pharmacopeia." 79 DUP050296600 D 305 cup. Add 200 to 250 mL of the solvent to the previously dried flask. 6.2 When using acetone as the extraction solvent, extract continuously for 4 h, heating at a rate such that the time required to fill and empty the siphon cup will not exceed 8 min. With other solvents extract for 16 h. Nora 3--If particles of carbon have escaped from the cup into the extraction liquid,' filter the liquid, wash the paper with solvent, and return the total filtrate to the extraction flask, prior to continuing with 6.3. 6.3 Transfer quantitatively the extract solution to a 400mL beaker that has been weighed to the nearest 0.1 g, and evaporate off the solvent on a steam bath or plate. Remove the beaker from the bath or hot plate just before the last trace of the solvent disappears. Dry the dish for 1 h at 105C (221 F). Cool and weigh to the nearest 0.1 g. , 7. Calculation 7.1 Calculate the percent extractable material, E, to the nearest 0.05 % as follows: v ' E= t(R - B)/(S - fV}] x 100 where: R = weight of extractable material and weighed dish, g, B = weight of weighed dish, g, S -- weight of thimble and specimen, g, and W = weight of thimble, g. FIG. 2 Extraction Apparatus into a weighed thimble and record the weight to 0.1 g. For pigments with high apparent density (bone black, iron oxides, etc.) a 40-g saihple is recommended. Plug the open end of the thimble with glass wool and place in the siphon 8. Precision 8.1 Precision data are not available at this time. When they are available the appropriate precision statements will be added. ' 9. Keywords 9.1 black pigment; solvent extractable The American Society for Testing andMaterials takes no position respecting the Validity ct any patent rights asserted In connection with any Item mentioned in this stenderd. Users of this standard are expressly advised that determination of the validityof. any such patent rights, and this risk ol infringement ofsuch rights, are entirely their own responsibility... This standard is subject to revision atany time by the responsible technical committee andmust be reviewed every five'fears and ifnot revised, either reapproved or withdrawn. Yourcomments are invited either for revistonof 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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Rawe st., Philadelphia,'PA 19103. 80 m DUP050296601 17. Report FILM TEST 17.1 Report the results in seconds (Note 6) for a %a-in. 20. Significance and Use (2.4-mm) steel ball (density 7.7 0.1) and a 2.00 0.02-in. (50.8 0.5-mm) drop. The viscosity value shall be prefixed 20.1 The quality of a lacquer or other surface finish is with the letter A, B, or C, corresponding to the formula of dependent upon clarity and gloss of the dry film. This test j the solution employed. method can reveal potential impurities and flaws in applied finishes. 6--Results in seconds for a Vst-in. steel bail may be converted to poises as follows: 21. Procedure n = 0.560 (a - b) t where: n = viscosity at the specified temperature, P, a = ball density, g/mL, b = solution, density, g/mL, and t - time offall, s. 18. Precision and Bias 18.1 Precision--The coefficient of variation between two results.obtained by a single analyst is estimated to be. 2.6 % at 1.0 df. Tvyo results should be considered suspect, ifthey differ by more than 7 %. 18.2 Bias--No statement on bias can be made at this time as no material is available to serve as a standard. SOLUBILITY AND APPEARANCE OF SOLUTION 19. Procedure 19.1 Compare either formula A, p, or C (Table 1) with a freshly-prepared standard solution of the same type of soluble cellulose nitrate of the same formula. Make the comparison in small vials and note the color, turbidity, "grain," and "flock." TABLE 1 Solutions for Viscosity and Film Tests 21.1 Dilute formula A, B, or C (Table 1) with an equal volume of normal butyl acetate and pour the solution beside a freshly prepared standard solution of the same type of soluble cellulose nitrate and of the same formula, on a dean glass plate. Allow to dry in a nearly vertical position in a dust-free atmosphere. Compare the specimen with the standard for undissolved particles, which indicate unnitrated cellulose or impurities, and for poor flow and poor gloss. TOLUENE DILUTION 22. Significance and Use 22.1 This test method can ascertain whether cellulose nitrate of a given percent nitrogen is contaminated with material of a significantly different nitrogen content Such cross contamination may adversely affect solution and film quality. 23. Procedure 23.1 Prepare a solution containing 12.2 weight percent of cellulose nitrate dried as described in 4.3, and 87.8 weight percent of butyl acetate conforming to Specification D 303. To 50 mL ofthis solution in a stoppered bottle add'toluene, conforming to Specification D 362 in small quantities from a buret, shaking well after each addition.. 1 Formula A Ingredients: Soluble cellulose nitrate (dried). weight percent Completely denatured ethyl alcohol (188 to 190 proof), weight percent Toluene/ weight percent Ethyl acetate,8 weight percent Density of solution at 25C (g/mL) 12.2 22.0 48.3 17.5 0.90 A Toluene conforming to Specification D 362. " Ethyl acetate conforming to Specification P 302. Formula B 20.0 20.0 44.0 16.0 0.93 Formula C 25.0 18.75 41.25 15.0 0.97 24. Calculation and Report 24.1 Report as the dilution value the volume of toluene required to effect the first permanent separation of cellulose nitrate, calculated as a percent by volume of the original solution, as follows: ` Dilution value = (mL toluene xT00.)/50' ' ----- . = mL toluene X 2 7--Large quantities of butyl acetate and toluene should be reserved for this test to avoid possible variation between different lots. The test should be run at 25"C. 77ie American Society for Testing and Materials takas no position respecting the validity ofanypatent rights assertedIn 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 rlek of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any tlma by the responsible technical committee and must be reviewed every live years and ifnotrevised, either reapproved or withdrawn. Your comments are Invitedeither 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 lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Raoe St., Philadelphia, PA 19103. If DUP050296602 Designation; D 305 - 84 (Reapproved 1990)**1 Standard Test Methodor Solvent-Extractable Material in Black Pigments1 This standard is issued under the fixed designation D 30S; 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. <l --Section 9 was added editorially in May 1990. This test method covers the determination of the it-extractable material in black pigments such as bon black, lampblack, and bone black. This standard does not purport to address the safety blems associated with its use. It-is the responsibility.ofthe of this standard to establish appropriate safety and hlth practices and determine the applicability ofregulatory Citations prior to use. f Referenced Document 2.1 ASTM Standard: D329 Specification for Acetone" ^Significance and Use 3.1 This test method is used by black pigment producers nd users for product acceptance. Apparatus 4.1 Extraction Apparatus, consisting of a flask, siphon 1 cup, and a condenser similar to the apparatus shown in' either Fig. 1 or Fig. 2. 1--A Sophlet apparatus may be used as an alternative. 4.2 Extraction Thimbles--The thimble must be-made of greaseless paper and be of correct size to fill the selected apparatus. 2--The recommended thimble size for each of the apparatus shown in Fig. 1 is listed below: Height Inside diameter Outside diameter Fig. 1 70 mm 28 mm 30 mm Fig. 2 62 mm 22 mm 24 mm 4.3 The thimbles are available in various heights and widths with two thickness levels, single thickness or double thickness. Single-thickness thimbles are recommended for this extraction procedure. S. Reagents and Material 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.3 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 Solvent--Acetone and benzene are the most com monly used solvents (see Specification D 329); however, other solvents may be used as agreed upon. 5.3 Glass Wool. 6. Procedure 6.1 Weight approximately 10 g of pigment (moisture-free) * 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 Aug. 31, 1984. Published October 1984. Originally published as D 305 - 29 T. Last previous edition D 305 - 72 (1978). 1 Annual Book ofASTM Standards, Vol 06.03. J 44Reagent 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.** DUP050296603 Designation: D 332 - 87 (Reapproved 1991)1 Standard Test Method for Relative Tinting Strength of White Pigments by Visual Observation1 This standard is issued under the fixed designation D 332; 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 sincethe last revision Or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4222 cfFederal Test Method Standard No. 141A. Consult the DoD Index qfSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. Keywords were added editorially in August' 1991. i|cope If This test method describes the procedure for detergHlg die relative tinting strength of white pigments by. "^ assessment of blue tints. t|.2 This test method is applicable only for comparing the |kpigment with a reference standard of the same type' and fide. 1--ASTM Test Method D 2745 describes a procedure for sfu' m**' ental evaluation ofblack tinted samples. -A.3This standard does not purport to address all of the,, I0ty problems, if any, associated with its use. It is the Responsibility ofthe user ofthis standard to establish appro* mate safety and health practices and determinerhe applica bility ofregulatory limitations prior,to use. , . 2. Referenced Documents 2.1 ASTM Standards: 1 D262 Specification for Ultramarine Blue Pigmeiit2 D2745 Test Method for Relative Tinting Strength of White Pigments by Reflectance Measurements2 3. Summary of Test Method 3.1 Specified amounts of white pigment and blue tinting ligment are dispersed together in oil using a glass hand IjiuUer or an .automatic muller. Both the test and standard jgigments are treated identically. The pastes are drawn-down together on a panel and visually assessed for tinting strength. obtain a numerical rating T>f tinting strength, dispersions iwith the standard white pigment and more or less of the e" tinting pigment are made until the lightness of the test |>igment paste is matched. The weight ofthe tinting pigment ' is used to calculate relative tinting strength. 4 `4. Significance and Use 4.1 This test method is used as a referee method and for quality control. The vehicle (oil) for preparing the disper sions and the tinting pigment (ultramarine blue) are specified 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 1301.26 on Optical Properties. Current edition approved Nov. 27, 1987. Published January 19S8. Originally published as D 332 - 31 T. Last previous edition D 332 - 64 (1930). * Annual Book ofASTM Standards, Vol 06.02. but other vehicles and tinting pigments can be used. Any such changes in the test method must be agreed upon between the purchaser and the seller. 4.2 The results obtained with a muller dp not necessarily agree with an industrial situation where different dispersing conditions ;exist. However, dispersing with a muller is a fast and relatively inexpensive way of testing tinting strength for routine quality control, 5. Apparatus 5.1 Balance, laboratory-type, sensitive to 0.1 mg, equip ped with a counterbalanced watch glass. 5.2 Buret, 1-mL capacity, stopcock controlled, graduated in 0.1-mL divisions, or other suitable dispensing apparatus with a delivery accurate to 0.05 mL. 5.3 Glass Hand Muller--A weighted glass hand muller. with beyeled edge having a total weight of 15 lb (6.8 kg) and a grinding face of from 23A to 3 in. (70 to 75 mm) in diameter. The face shall be free of blowholes and other imperfections and kept roughened by lightly grinding_with No. 303 optical emery, or its equivalent, and turpentine. 5.4 Rubbing Surface--A ground glass plate, at least 14fey 20 in. (35$ by 510 mm), the surface of which is kept roughened by lightly grinding with No. 303 optical emery, or its equivalent,-and turpentine. 5.5 Automatic Muller, automatic,3 equipped with a weight that exerts a permanent 50-lbf (220-N) force and an addi tional weight exerting a 50-lbf making a total of 100-lbf (445-N). The two glass plates shall be kept sharp by removing from the machine and grinding them face-to-face with No. 303 optical emery or equivalent, and water. 5.6 Spatula--A flexible spatula having a chromium- plated or plastic blade 3 to 6 in. (75 to ISO mm) long. 5.7 Panels of bright tin, glass, or white-lacquered card board. ., 5.8 Scraper--A French scraper or stiff scraping knife having a blade that is about 3 or 4 in. (75 to 100 mm) wide with a straight edge. 6. Materials 6.1 Tinting Material--Ultramarine blue conforming to 3 A muller supplied by Hoover Color Corp., P. O. Box 218, Hiwassee, VA 24347, has been found satisfactory for this purpose. 81 DUP050296604 D 332 TABLE 1 Quantities of Materials for Tinting Strength Tests pastes, on the top side only, for relative lightness of tint; Pigment Type White Lead Zinc oxide Zinc oxide, leaded Titanium dioxide (anatase) (rutile) Weighted Pigment, g, 2 2 2 .2 . -2 Weight of the sample is lighter than the reference standard it has greater, Ultramarine Amount of Blue Timing Oil, mL PigrneBt. g ; . u-trj- 04! " 0.5 0.2 0.7 0.2 0.S ;i- tinting stsrai^lL. 4fae.. from % reference standard ii lightness of tint, and if a numerical `ra!fing!'is d?p:ed,'pfepafe^dther (fastis: Of' the reference standard white pigment usings different. amounts of the tinting material. Make a draw-down ofthe sample paste with each standard asdescribed in 7.3. Select the draw-down in r ,- OA - -.. :* 1.0 . 0:4- -, 0.8 . . =.,. . . is - ,. 'yf^lch t^ie'-staijphird' pigitient paste; faost clt^eliy. matches the . teirt pigment pastei in lightness. Use,-the weight of tinting ', ^aterihl .in this ..method to calculate the tinting strength off Specification D 262',ot# grade agreed fipohioythe puxpKas^. /',th .test pigment),, ".'. and the seller. 6.2 Oil--Refined linseed oil with an add number of. 8. Procedure B--Automatic Muller approximately 4. 8.1 In,-order to mhiimize. the,,effect-of the difference in \ 6.3 Reference Standard--A standard' white pigment "of the ~ grindingDfthe area near the center ofthe plates as compared same type and grade as the pigment to be tested, as agreed to the area, near the periphery of the plates, draw two upon between the purchaser and the seUer. ' '" > i's*4 concentric circles under the base plate ofthe muller in such at jj way-tha^.they sbpw clearly through tbp pjate. ,.Thf5 circles 7. Procedure A--Glass Hand Muller ; n, cap bg,cu5awn e|th^r on a paper ins^e<J un|pr.'(he,plat^,,p|. 7:1 Wdgh 2` guftoe'stahdardwliite pigmeht- hfad' the amount o`f ultrarfiartne1 blue listed in Table t to 2 mg. Trafisfer the weighed portions of white-and blu^pigmetrts tbthe ground-glass irihtei Add the toiiohiif of oil ^^ecified'ih Table 1 from the buret (Note). Be sure-to allow the buret to ` drain to its true level because variations in the amount of oil decrease the precision of the test. Work the pigments arid oil into' a paste with the'spatuli;'then nib'up'fe paste-frith the g|ass hand rauller, spreading ft over ariareiM-tb '4 in: (75 to 100 fhfii-)5Wide and frorii l-2`to;15'Wl(-305 tO;3S0 Mm) long. In counting the rtibsy one Stroke and'Ohe stroke*back' is considered one rub. Allow-the Mullef,tel travel;ttp!^ie;side ahd back thd other ideVitwisting it`'slightly aT theitop`alid Mavra" directly on the bottom of the"j>late. The inner',circle) should be, in,. (6,3 mm):in;diampter' ,ansi",tlie.opiteE circle l^i-3 .inxjj) in 4iaroe^er. ' :,r.- ; ., 8.2 Carefully weigh the pigment as described ini $4*, transferring the pigment to the, base plate Of (he. muller. Ada the oil arid' wOrk*the j)igrnpnt;aiid dl into a pMe:,ptfr fae, spatula. Distribute the paste within me area between*the two , concentric circles on:theplate;vdose`to&:muller* and add a { 50-lb (23'--kg)-weight (to make atotal weight of 160 lb (45 *kg? j pressing the plates together Carry put three `Mulling Stages of- 1 50 revolutions each, collecting the' paste from. both-.-plates^ with the spatula after each stage, spreading it around the path. on the lower plate and wiping the spatula on the upper plate, bottom of each Stroke. Afler*each!2S irubs With thetoulTef, "pick dp" the paste with the spdtulsPl^^sdrapiftg the fat of the Muller and-gathering'the paste On the Slab into a ntotind;' 8.3 Continue the treatment of the paste of the test and standardpigBjents asdeseribed-.in 12, 7.3, and;7,4;' v Repeatunfil the paste has beerigiven 100 rubs/' - 2-^W.here `the r'$Itm| paste ls t6p;'flui4prtgg. .thick for' mulling, ilfiwt' the quantity of oil to'give a wearable paktie Ws prepay a 'fisw poster itk-uiling as before. Report thb 'amount ofoil feed. - 9. Calculation''' l' '' / "J: rh-e-.. - -a1!'-- - 1 i-t!-'-- 9.1 Calculate the tinting strength Of the sample as follows: TS**(/Ai-d'TJ- 'f j' 7.2 work 2 g of the test pigfaeni'ln, exactly.the same mapner .as prescribed in 7.1,for the stgridptri', uapthe same ainouht.bf finting mateiial'^hddifi ,, J. .... , 7.3 Spread, the paste, (trie.standard gnd. test(Rigtnentsin \yhere: '__ " ; '. ' ...' TS * tiiititi^!sttori^th of the tdsit pigment, lbf (Or N),"' .'*' < A ; freight of* tinting Material used with^standrird to give `'`dbudii^ oFifafiig, parallel, contigjuoiis ^ectapgRl^r argg? .Qij,,pdiiel,- eapii' about,firi. (25 mm)'wide.grid 2, i& (50^ Minl^pii^. ,tlse, f " scraper to smooth ,the surface'.of-the pastes '(herq gelled "draty-d,owns") by drawing tfie. scraper lightly over the pastes Ifi. Precision apd Bias / . , to give a straight and even line 0(903(4$ between tpera. Keep tfie drayra-downs sufficiently`tfiici/((i ofiipto the panel. ' ` '* ' .......... 10.1 The precision-and bias are .to be determined.. 11. Keywords 3. ' , > 7.4, Immediately examine .the draw-doiyns pf .tjie two 11 ..1- riptiag. strength; white'{figment strength. The American Socldy for Testing and Materials tafres no pos/f/on respecting,thg validity, g) any patent rights essprtetf.ln.Gpnnection with any Item mentioned in this standard. Usets il`tH& standard are expressly ddvTseil that determination ot'the validity vt any such patent rights, and the risk of Infringement of sucp rights, are entirely their own responsibility. .... This standardJssup/edt to nUUOn atany timeby the responsible technical committee and must bereviewedevery five years and' if not revised, either reapproved or withdrewn. Your comments are Invited either torrevision ofthis standard or for additionaldafdards and should be addressed to ASTM Headquarters. Yqur comments will receive careful consideration at a meeting ot 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 AsfhfCdrrfmlttae on StShdards, lilBRace St., Philadelphia, PA1$i03: ' ... 82; . DUP050296605 Designation: D 360 - 89 Standard Specification for Shellac Varnishes1 , This standardis issued under the fixed desigiiatioti p 360; the numher'injme^teljf following the desigt^tidn indictites the year of original adoption or, in the case of revision, the year of.last revision; \ number in pareptlgses indicates thte year of last reappnwal. A' superscript epsilon () indicates an editorial change' since the"last revision or reapproval'.1 " 1 ' pScope |.l This specification covers shellac varnish consisting of olution or "cut" of a specified type and grade of dry lac |jn in specially denatured alcohol. Ninety-five percent (190 pof) ethyl alcohol, specially denatured according to Forula No. 1 of the U. S. Bureau of Internal Revenue, is the BfVent most commonly used. However, other specially hatured alcohols and proprietary solvents are also used for i purpose. 1 Referenced Documents |i?2.1 ASTM Standard: E.D29 Test Methods for Sampling and Testing Lac Resins12 if- D 207 Specification for Dry Bleached Lac2 D 237 Specification for Orange Shellac and Other Lacs2 Types, Grades, and Bodies 3.1 This specification covers two grades, A and B, of orange shellac varnish and two grades, regular and refined, of pleached lac varnish. Each type and grade may be furnished in very light, light, medium, heavy, very heavy, or extra ^ Heavy body varnish, as specified. ft. Color I 4.1 The color of shellac varnish shall be no darker than Ithe color of a standard varnish of the same nonvolatile [matter content mutually agreed upon between the purchaser |and the seller. | 1--Attention is called to the fact that the purchaser and the seller must agree upon one of the two methods for determining color [ appearing in Test Methods D 29. ;5. Drying Time 5.1 Shellac varnish shall dry. hard in 1 h. Shellac varnishes having a body greater than that for a light body varnish shall be thinned to the nonvolatile matter content of a light body 1 This specification is under the jurisdiction of the ASTM Committee D-l on Punt and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally published as D 360 - 33. Last previous edition D 360 - 73( 1981). 2 Annual Book ofASTM Standards, Vol 06.02. varnish. Special conditions for this test may be made by mutual agreement between the purchaser and the seller. 6. Body and Cut 6.1 The body and cut of the respective types and grades shall be based on the percent of nonvolatile matter, and shall conform to the following minimum requirements: Nonvolatile Matter, min, Orange, Grades A and B Bleached, Regular and Refined Very tight body (3-lb (1.4-kg) cut) varnish Light body (4-lb (L8-kg) cut) varnish Medium body (4.5-Ib (2.0-kg) cut) varnish Heavy body (5-lb (2.3-kg) cut) varnish Very heavy body (6-lb (2.7-kg) cut) varnish Extra heavy body (8-lb (3.6-kg) cut) varnish 28.5 35.0 37.5 40.0 44.0 51.0 28.0 34.5 37.0 39.5 43.5 50.5 2--The term "cut" is defined as the number-ofpounds of dry lac resin (containing only that amount of moisture acceptable for proper cutting with the solvent to ensure a satisfactory varnish) that were added to 1 gal (3.8 L) of specified solvent in manufacturing the varnish. Allowance has, therefore, been made for 2 % maximum moisture and other volatile matter and 3 % insoluble matter in orange shellac, and for 6 % moisture and other volatile matter in bleached lac, in arrivin& at a minimum value. Varnishes of the above specified bodies or "cuts" should accordingly conform to the respective minimum requirements specified for nonvolatile matter. 7. Properties of Dry Lac - - . - . 7.1 The nonvolatile matter in the varnish shall conform to the Properties section of Specification D 207 and Table 1 of Specification D 235. .. 8. Packaging and Marking 8.1 Shellac varnish shall be packaged in standard com mercial containers ofthe type and size mutually agreed upon between the purchaser and the seller. The label of the container shall show the type, grade, body or cut, and date of manufacture of the varnish contained therein. 9. Test Methods 9.1 The sampling and methods of testing shall be con ducted in accordance with -Test Methods D 29. 83 DUP050296606  D 360 The American Society for Testing andMaterials takes 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 ol any such patent rights, and the risk ol Infringement of such rights, are entirely thetr own responsibility. This standard Is subject to revision atany 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 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, 1918 Rape St., Philadelphia, PA 19103. 84 7k DUP050296607 Designation: D 365 - 84 (Reapproved 1989)61 Standard Test Methods for Soluble Nitrocellulose Base Solutions1 git This standard is,issued under the fixed designation D 365; the number immediately following Ihe 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. --Editorial changes were made throughout, including the title, in March 1989.__________ ________________________ 3 pope These test methods cover the testing of soluble nitroiose base solutions that are made by dispersing various i and concentrations of soluble nitrocellulose (cellulose |te) in various solvent mixtures. This standard may involve hazardous materials, oper|k and equipment. This standard does not purport to fess all ofthe safety problems associated with its use. It is 1responsibility of the user of this standard to establish fppriate safety and health practices and determine the miCability of regulatory limitations prior to use. For hazard statements see Section 11. eferenced Documents ASTM Standards: > 301 Test Methods for Soluble Cellulose Nitrate12 jj&fc>333 Test Methods for Clear and Pigmented Lacquers3 Sp3`il93 Specification for Reagent Water4 jffD 1200 Test Method for Visdosity by Ford Viscosity Cup3 B 300 Practice for Sampling Industrial Chemicals5 jr/i3. Significance and Use '3.1 Since the desired specifications and compositions of stv soluble nitrocellulose base solutions vary greatly, these , .ndthods are used to establish whether limits that shall be as ^.agreed upon between the producer and the user have been Wet. Sampling 4.1 Select the sampling method from those listed in Practice E 300. CONSISTENCY (VISCOSITY) 5. Consistency Tests 5.1 For Consistencies from 3 to 500 s--Determine the Jconsistency by falling-ball consistency test described in ' Method D 301 for those solutions having a consistency from 13 to 500 s when tested in that apparatus. 1 These methods are under the jurisdiction of ASTM Committee D*1 on Paint and Related Coatings and Materials and are the direct responsibilities of Subcommittee D01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Oct. 26, 1984, Published January 1985. Originally published as D 365 - 33. Last previous edition D 365 - 79. 2 Annual Bonk ofASTM Standards, Vol 06.02, 3Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01, 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 5.2 For Consistencies Less than 3 s--Determine the consistency by Test Method D 1200 For those solutions having a consistency of less than 3 s when tested in the falling-ball apparatus referred to in 5.1. 5.3 For Consistencies over 500 s--Determine the consis tency using the apparatus and procedure described in Sec tions 6 and 7 for those solutions having a consistency greater than 500 s when tested in the falling-ball apparatus referred to in 5.1. 6. Apparatus 6.1 The consistency test apparatus, shown in Fig. 1, shall consist of the following: 6.1.1 Glass Tube (preferably heat-resistant glass),6 2 V32 in. (50 1.5 mm) in inside diameter and 10 in. (255 mm) in length, with marks 5 Vis in. (177 1 mm) apart, the upper one being 3 in. (75 nun) from the top of the tube. 1,--The. steel ball can be removed (in order .to.leave the same material in the tube for a check run) by removing the lower stopper. However, a small air bubble is usually introduced in this way. It is preferable to invert the tube, removing the guide to get the ball out. It is often necessary to put a few drops of solvent in the guide lip to loosen it from the tube on account of the solution drying at the edge of the tube. When the latter method is used for removing the ball, a larger bubble traverses the tube .than when the former method is used, but a large bubble moves sufficiently fast, even in a very viscous solution, to escape at the top in a few minutes, whereas small bubbles take hours to escape. 6.1.2 Steel Ball, 0.625 0.001 in. (15.88 0.02 mm) in diameter, and weighing 16.536 0.10 g. 6.1.3 Aluminum Guide Cone of light gage aluminum (approximately 0.02 in. (0.5 mm) in thickness) as shown in Fig. 1. The orifice of the guide cone shall be Vs"in. (22 mm) in diameter, the conical portion 1 in. (25 mm) in height, the cylindrical portion Vz in. (12.7 mm) in height, and the outside diameter shall be slightly under 2 in. (50 mm) so as to fit snugly into the viscosity tube. 6.1.4 Stoppers, made preferably of rubber and covered with tin foil. 7. Procedure 7.1 Fill the tube in any convenient manner whereby bubbles do not form and no appreciable amount ofsolvent is lost. One method is to immerse the lower end of the open tube in the solution and to apply suction at the upper end of the tube. In this manner the tube can be filled in from 5 to 10 s without the introduction of air bubbles or an appreciable 6 Borosilicate glass is satisfactory for this purpose. 85 DUP050296608 D365 FIG. 1 Apparatus for Consistency (Viscosity) Test of Solutions Having Consistencies over 500 s loss of solvent. Close the bottom of the tube with a stopper covered with tin foil. Push the aluminum guide cone slowly into the top of the tube and insert a stopper covered with tin foil into the top of-the guide.. 7.2 Bring the tube and its contents to a temperature of 25 O.TC by placing in a suitable bath. Allow at least 30 min for the solution to reach temperature equilibrium. For accurate measurements keep the tube during the determina tion either in a thermostat or suspended within a consider-, ably larger cylinder of water at the specified temperature. 7.3 Remove the upper stopper only long enough to place the ball in the center of die tube; this can be done conveniently with crucible tongs. The principal value of the guide cone is to retard the ball sufficiently at the start of its fall so that the solution will close over the ball and hot leave on the top of the ball a large "trailer bubble." If the guide is not used a big trailer bubble usually accompanies the ball, retarding its fall and, if the bubble is off center on the ball,' pulling the latter away from the center of the tube. 7.4 Measure the time of fall in seconds from the instant the bottom of the ball is level with the upper reference mark on the tube until it reaches the lower mark on the tube. ' ' NONVOLATILE MATTER 8. Procedure 8.1 Determine the percent of nonvolatile matter in ac cordance with the procedure described in the Nonvolatile Matter section of Test Methods D 333. observations) in similar bottles for turbidity, hair, grain, and , insoluble matter. ' DEPTH OF COLOR- 10. Apparatus 10.1 The apparatus used for the preparation of the color standards and for the depth of color determinations shall consist of the following: 10.1.1 Light--Source of transmitted light. ` 2--Not absolutely necessary but will increase accuracy and be more convenient. 10.1.2 Bottles, three dozen 2-oz (60 mL) screw-cap, square, glass. 10.1.3 Flasks* several, 1-L, volumetric. .10.1.4 Burets, two, 50-mJL. 10.1.5 Analytical Balance, 10.1.6 Colorimeter--Dubosq colorimeter (see Note 2). 10.1.7 Color Glass--Yellow glass about 25 mm square and 10 mm thick.7 8 11. Reagents and Materials 11.1 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 Chem ical Society, where such specifications are available.^ 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. 11.2 Purity of Water--Unless otherwise,indicated, refer ences to water shall be understood to mean reagent water as defined by Type III of Specification D 11 $3. 11.3 Potassium Chloroplatinate, (K2PtCl6). 3: Warning--This material is hazardous. Carefully review Material Safety Data Sheets supplied by manufacturers for handling and first aid instruction. - 11.4 Cobait Chloride (CoCl2 6H20). (Warning--See Note 3.). 11.5 Hydrochloric Acid (sp gr i. 79)--Concentrated hy drochloric acid (HC1). (Warning--See Note 3.) 11.6 Caramel (sugar coloring). 11.7 Phenol. (Warning--See Note 3.) 12. Preparation of Color Standards 12.1 Platinum-Cobalt Color Standards--Prepare the plat inum-cobalt color standards as follows: Weigh out on an analytical balance exactly 1.245 g of K2PtCl6 and 1.000 g of crystallized cobalt chloride (CoCl2"6H20). Dissolve in dis tilled water, add 100 mL of HC1 (sp gr 1.19), and dilute to 1000 mL with distilled water. This solution is color standard No. 10.9 Prepare color standards Nos. 1 to 10, inclusive, by APPEARANCE OF SOLUTION 9. Procedure 9.1 Compare the appearance of the soluble nitrocellulose base solution with a reference standard agreed upon between the purchaser and the seller (both the reference standard and sample solutions shall be thoroughly agitated before making 7 Corning glass, signal yellow No. 330 has been found satisfactory and is available from the Corning Class Works, Coming, NY. 8 "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 Nostrand Co., Inc., New York, NY., and the "United States Pharmacopeia." 9 This solution has an assigned value of 500 on the Hazen color scale (see American Chemical Journal, Vol XIV, p. 300). 86 -.... V DUP050296609 # D365 TABLE 1 Plpiatlnum-Cobalt s -Color Standards f" No. 1 No. 2 ir No. 3 No. 4 No. 5 No. 6 < No. 7 , No. 8 No. 9 No. 10 Platinum-Cobalt Color Standards Quantity of No. 10 Color Standard, mL Quantity of Distilled Water, mL S 45 10 40 15 35 20 30 25 25 30 20 35 15 40 10 45 5 60 0 ^Irately measuring from burets directly into the square ggk (60-mL) bottles the quantities shown in Table 1 of the m P0 color standard and distilled water. After preparation nhe color standards seal the bottles with corks and paraffin rfaiymk putting on the screw caps. The platinum-cobait color ^'dards are permanent for approximately six months, ke the color standards from No. 12 to No. 500, inclusive, a caramel solution, but the color is based on the mum-cobalt color standard. j|2i2 Caramel Color Standards--Prepare the caramel 5r standards as follows: Dilute caramel (sugar coloring) in le ratio of about 1 mL of caramel to 100 mL of distilled Iter in a glass vessel. Add 0.5 % phenol and agitate Roughly. Adjust the concentration of'this solution so that j56r it is diluted in the ratio of 1 mL of solution to 49 mL of tilled water, to which has been added 0.5 % phenol, the gllition will match color No. 10 of.the platinum-cobalt color idard. This caramel solution before dilution is color No. 30 (Note 4). Prepare color standards No. 12 to No. 500, J Kclusive, by accurately measuring-from burets directly into }|ie square 2-oz (60-mL) bottles the quantities shown in |Table 2 of color No. 500' caramel standard and distilled water to which has been added 0.5 % phenol.. After prepara tion of the color standards, seal the bottles with corks and paraffin before putting on the screw caps. All of the caramel pfe color standards are permanent for approximately one month but should be checked' semi-monthly if frequently used. TABLE 2 Caramel Color Standards No. 12 No. 15 No. 20 No. 25 No. 30 No. 35 No. 40 No. 45 No. 50 No. 60 No. 70 No. 75 No. 80 No. 90 No. 100 No. 125 No. 150 No. 175 No. 200 No. 250 No. 300 No. 350 No. 400 No. 450 No. 500 Caramel Color Standards Quantity of No. 500 Caramel Color Standard, mL Quantity of Distilled Water plus Phenol, mL 1.2 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 6.0 7.0 7.5 8.0 9.0 10.0 12.5 15.0 17.5 20.0 25.0 30.0 35.0 40.0 45.0 50.0 48.8 48.5 48.0 47.5 47.0 46.5 46.0 45.5 45.0 44.0 43.0 42.5 42.0 41.0 40.0 37:5 35.0 32.5 30.0 25.0 20.0 15.0 10.0 5.0 0.0 4--It is more convenient to check the caramel color standard No. 500 against a colored glass that has been previously standardized against the platinum-cobalt color standard; a piece of signal yellow glass (see 10.1.7) about 25 mm square by 10 mm thick may be standardized and used as a check on the caramel solution. This must be done by use of a colorimeter. 13. Procedure 13.1 Fill a square 2-oz (60-mL) glass bottle with the material to be tested and match this against one of the color standards using either direct daylight or indirect artificial transmitted light, the latter being preferred. The number of the color standard matched is die depth of color oftthe material. 14. Precision and Bias 14.1 The precision and bias of these-test methods-is-as described for. each pf the separate methods cited if available. The American Society lor Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned In thle 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 Is subject to revision at any time by the responsible technical committee end must be reviewed every five years and Ifnotrevised, either reapproved orwithdrawn. Your comments are invited either for revision ol this standard orforadditional 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. DUP050296610 Designation; D 387 - 86 Standard Test Method for Color and Strength of Color Pigments with a Mephanical Muller1 This standard is issued under the fixed designation D 387; 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 iast 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 4220.1, 422! ofFederal Test Method Standard-No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year of issue which hits been adopted by the Department ofDefense. 1. Scope 1.1 This test method is intended to be used to compare the color and strength of a pigment under test with a reference standard of the same type and grade. 1.2 This test method does not apply to white pigments. i--Test Method D 3022 is similar to this test method, but it utilizes a. miniature sandmill rather than a mechanical mulier, to disperse die color pigment Test Method D 332and Test Method D 2745 are similar to this test method, but they are intended for use with white pigments, rather than color pigments: 1.3 This standard may involve hazardous materials, oper ations, arid 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. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D 332 Test Method for Relative Tinting Strength of White Pigments by Visual Observation12 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials3 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D2745 Test Method for Relative Tintitig Strength of White Pigments by Reflective Measurements2 D3022 Test Method for Color and Strength of Color Pigments by Use of a Miniature Sandmill2 D3964 Practice for Selection of Coating Specimens for Appearance Measurements4 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry3 E 308 Test Method for Computing the Colors of Objects by Using the CIE System5 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 DO1.26 on Optical Properties. Current edition approved Aug. 26, 1986. Published October 1986. Originally published as D 387 - 34 T. Last previous edition D 387 - 81. 1 Annual Book ofASTM Standards, Vol 06.02. 5 Annual Book ofASTM Standards, Vol 06.01 and 14.02. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vol 14.02. 3. Summary of Test Method , 3.1. Pigments are dispersed , in a suitable vehicle vtjth a mechanical mulier. Test arid standard pigments are treated identically. Opaque drawdowns are made from the disper sions and compared, either visually or instrumentally, for color and strength differences. ' 4. Significance and Use 4.1 Color and tinting strength are the most important properties of a color pigment. This test method provides a means of testing these properties for quality,control. ; 4.2 This test method is intended as a referee method so that such matters as the vehicle,for preparing the dispersions and the white for making tints , have been suggested. How ever,,,other vehicles and whites may be suitable, few quality control purposes, and changes in this test method are aliowed'by agreement between the parties to a test. ,^ 4.3 It is assumed that the most exact comparison of mass color add tinting, strength occurs when the pigment is completely dispersed. By followihg the procedure described m Annex Al, the conditions for achieving the maximum practical degree of dispersion with a mechanical mulier may be determined. Color and strength tests should be carried out under these conditions. 4.4 The results obtained with a mechanical mulier do not necessarily correlate directly with an industrial situation where different dispersing conditionsvexist. However, disper sion with a mechanical mulier is a quick and inexpensive way oftesting the color and strength of a pigment for routine quality control. .~ 5. Apparatus 5.1 Balances--(]) A balance sensitive to 10 mg and (2) an analytical balance sensitive to 1.0 mg. 5.2 Muller, Mechanical,s equipped with, ground-glass plates to which a variable but known force may be added in 50-lbf (220-N) increments. The driven glass plate shall have a speed of rotation of between 70 and 120 rpm and-, the apparatus shall have an arrangement for pre-setting the number of revolutions in multiples of 50. 5.3 Rubbing Surfaces--The rubbing surfaces of the ground glass plates shall be kept sharp by removing them from the mulier and grinding them face-to-face with No. 303 optical emery, or its equivalent, and water. A satisfactory mulier is supplied by the Hoover Color Corp., 13 Cordier St, Irvington, NJ 07111. DUP050296611 D 387 jSvfBm Small Glass Slab or other nonabsorbent material, HjaMtfele for weighing and mixing pigment pastes. .Spatula--A flexible spatula having a 3 to 6-in. (75 to am) blade. i Paper Charts,7 white with a black band and a surface vious to paint liquids. Film Applicator, at least 3 in. (75 mm) wide with a Jjiyearanee of 4 mils (100 pm) to produce wet films about 2 ' 'Kjils (50 pm) thick. Color-Measuring Instrument, meeting the requirejljfSnts of Method D 2244. faterials pi Reference Standard--A. standard pigment of the same | and grade as the pigment to be tested, as agreed upon Veen the purchaser and the seller. '.2 Vehicle--A solvent-free vehicle, such as No. 1 lithojgjphic varnish, with 0.8 % each of cobalt and manganese %is (6 % types). 6.3 White Tinting Paste--A white paint compatible with i dispersion vehicle, such as 57 parts of rutile titanium ||ide dispersed in 43 parts of the vehicle described in 6.2. 3--Because the choice of vehicle and white tinting pigment JSjy affect the results, they should be agreed upon between the jgfBfaiaser and the seller. Hazards aBj.7.1 Some pigments may be potentially toxic and therefore i ^Hrould be handled with care, .Obtain specific precautions the manufacturer or supplier. jjjp7.2 "Many solvents and paint vehicles present explosion, je, and toxicity hazards, and they should accordingly be Handled with care. Again, obtain specific precautions from pb manufacturer or supplier. |p. Dispersing Conditions 5|i.*.l The conditions for dispersing the pigment on the jphechanical muller should be such that the maximum tinting jPfreQgth is developed. For each pigment and each dispersing wehicle the development of tinting strength by the mechanJfcal muller is influenced by the force applied, the number of revolutions, the mass of the pigment, and the mass of the vehicle. The conditions for obtaining the maximum tinting Jstrength with the mechanical muller can be determined by | following the procedure in Annex Al. 8.2 If these conditions are known for a particular pigment f with a particular vehicle, or if the purchaser and seller agree upon a particular set of conditions, there is no need to carry out the procedure in Annex Al. 9. Dispersion Procedure 9.1 Decide, by agreement or by experimentation, as discussed in Section 8, the following dispersing conditions: 9.1.1 Force applied to the muller plates; 9.1.2 Number of revolutions; 7 White chans with a black band are preferred forjudging opacity. Satisfactory charts are available from the Morest Co., 2 JI Centre St., New York, NY 10073, and the Leneta Co., P.O. Box 576, Ho-Ho-Kus, NJ 07423. * Satisfactory film applicators are available from Bird and Son, Walpole, MA |J 02031 and Precision Gage & Tool Co., 28 Volkenand Ave., Dayton, OH 45410. 9.1.3 Mass of the pigment; and 9.1.4 Mass of the vehicle. 9.2Applying these decisions, prepare a dispersion of the reference standard pigment. We v; onto a glass slab to within 2 mg, the appropriate quantities of the standard pigment and the dispersing vehicle. Mix the pigment and vehicle together thoroughly with the spatula and transfer the mixture to the lower plate ofthe muller. Spread the mixture in a path approximately 100 mm wide and hallway between the center and rim ofthe lower plate, and clean the spatula as much as possible by wiping it on the upper plate of the muller. Close the plates and carry out the mulling stages of 50 revolutions; after each stage collect the paste from both plates with the spatula and spread it around the 100-mm path on the lower plate, wiping the spatula on the upper plate as before. When the mulling has been carried out for the prescribed number of revolutions, collect the paste and store it Clean the glass slab, the muller plates, and the spatula, and repeat the procedure with exactly the same quantities of the test sample and vehicle. Collect the paste from this sample and store it. Clean the glass slab, the muller plates, and the spatula. 4--The most common sources of error in this procedure are inaccurate weighing, incomplete transfer of the pigment and vehicle mixture, and contamination of the plates by previous samples. 10. Masstone Color Procedure 10.1 Draw down a portion of the test and standard pastes in juxtaposition on a paper chart over a vacuum-drawdown plate or other suitable plane surface with the film applicator. Make sure that the coating is opaque. 10.2 Immediately compare the colors visually while still wet, using Practice D 1729, and record the results. Set the drawdowns aside in a dust-free area to dry. When dry repeat the visual color difference evaluation and record the results. See Practice D 3964. 10.3 If desired, evaluate the color difference instrumen- tally using Method D 2244, and report the color difference in units as agreed upon between the purchaser and seller. 5--Wet color difference evaluations ujay not agree with dry color difference evaluations because ofsuch phenomena as flooding and flocculation. In the case of a difference between the wet and dry evaluations, the purchaser and the seller should agree upon which condition is the standard. .- 6--Color difference measurements ofwet paints may require a special adapter to protect the instrument from fouling. Because color difference-measuring instruments differ widely in their design, the user may have to develop his own adapter. 11. Tint Color Procedure 11.1 Determine by calculation the amount of white pig ment paste that must be added to 0.5 g of the color pigment paste so that the mixture contains 1 part of dry color pigment to 10 parts of dry white pigment. For stronger or weaker pigments this ratio may be adjusted accordingly, for ex ample, 1:20 or 1:5, respectively. 11.2 Weigh 500 2 mg of the standard color pigment paste onto a glass slab. Then weigh the amount of white pigment paste determined in 11.1, and place it next to the color pigment paste on the glass slab. Thoroughly mix the two pastes together with the spatula until a uniform color is observed. 89 DUP050296612 4!fo D 387 il .3 Prepare a tint mixture of the test color pigment paste and the white pigment paste on a separate glass slab by the procedure described in 11.2. 11 'A Draw a portion of the test and standard tint pastes down in juxtaposition on a paper chart as in 10.1. Evaluate the color difference visually as in 10.2 and, if desired, instrumeritaliy as iri` 10.3. Clean the Spatula blade and glass slabs. 12. Calculation of Tinting Strength 12;1 If the colors of the test tint paste; and the standard tint paste are visually the same, the tinting strength ofthe test pigment is equal to that of the standard pigment, and the relative tinting strength of the test pigment is 100 %. However, ifthe test and standard colors are not the same, the difference may be due to tinting strength or hue (shade). 12.2 To determine the relative tinting strength of the test pigment, repeat the operations of Section .11, but this, time use an amount of the test pigment paste that is estimated to give the closest color match .to the standard pigment paste. Repeat this procedure until satisfied that the closest color match has been obtained. At this point any residual, color difference between the test.and the standard pigments is attributed to a shade difference, rather than a strength difference. Note and record this shade difference. 12.3 Calculate the relative tinting strength of the test pigment by . dividing the .mass of the standard paste by the mass of the test paste, used to obtain the closest color match;: multiply by 10G to express the result in percent, 12.4 If desired, the relative tinting strength of the sample pigment can be calculated from instrumental measurements (see Test Method E 97 or Practice E 308) using the following equation: TS = [(1 - RJ2/2R,,]u/[(l - RJ*/2RJ, (D where: TS = tinting strength of test pigment, R,, = measured reflectafrt factor (as a decimal), T = aligned tinting strength of standard, usually 100 %, and subscripts "u" and "s" refer to the test and standard pigments, respectively. 12.4.1 For use the lowest reflectance value measured in the range 420 to 680 dm with a spectrophotometer or abridged spectrophotometer. This method of calculation- is not valid when any tristimolus value or filter colorimeter reading is substituted for Rx unless it can be demonstrated that with such a substitution the function (1 - Ra)2/2R^ still H varies linearly with concentration for the pigments beh_ tested over the range of concentrations of interest. Because the use of different parameters may give significantly dif ferent results for the tinting strength, the choice of the parameter to be used as R^, shall be agreed on- between the purchaser and the seller. 7--This method is not applicable to metatiieric specimens, or to specimens exhibiting large shade differences, or to specimens differing" in strength by more than about 30 %. 13. Report 13.1 Report the following information: 13.1.1 Type and identification of the test pigment, refer ence standard pigment, wftite tinting pigment, and dispersing vehicle. ' ,. 13.1.2 Mass ratio ofpigment to vehicle, and for tints mass ratio of color pigment mass to white pigment. 13.1.3 Manufacturer and model number of the mechan ical muller employed. 13.1.4*Total force applied to the muller plates and totaj number of revolutions. 13.1.5 Results of the visual evaluation of the color differ ence (masstone and tint) in accordance with Practice D 1729. 13.1.6 If an instrument was used to evaluate the color difference, the results of the instrumental evaluation in accordance with Method D 2244. 13.1.7 Relative tintfng strength and method by which it was determined (visual br instrumental). Also, for the instrumental method, the parameter used as the measure of Rin. . 13.1.'8 Anydeviation, by agreement or otherwise, from, the test procedure described above. 14. Precision 14.1 The precision of this test method depends on several factors such as the type of pigment, the level of tinting, and the magnitude and direction of the color difference. This; point is illustrated by the results in Table 1(a), which contains the between-laboratories standard deviations, ob tained in an .interlaboratory study involving five different laboratories and four different pigments. The dispersing conditions used to obtain these results are ligted in Table 2. 14.2 Table 1(b) lists the maximum acceptable differences, calculated at the 95 % confidence level from the results in Table 1(a). s TABLE 1(a) Between-Laboratories Standard Deviations (or Various Color Difference* and Timing Strength13 Parameters Pigment Type Masstone Color Ab 7 L" AE Tint Color &a Ab AL TmtingStrength Y 7H Yellow Iron Oxide BON Red Molybdate Orange Phthalocyanine Green0 0.10 0.46 0.22 . 0.42 0.12 0.37 0.20 0.28 0.09 0.14 0.06 0.11 0.29 0.6S 1.43 0.51 0.13 0.20 0.19 0.08 0.29 0.31 0.07 0.24 0.11 0.12 0.05 0.14 0.25 0.07 0.13 Q.21 2.0 2.2 3.0 0.7 1.8 1.10.5 0i8 0.8 1.6 1.8 2.6 V 0.7 2.5 1.0 1.8 90 DUP050296613 # D 387 TABLE 1(b) Maximum Acceptable Differences for Various Color Difference4 and Tinting Strength8 Parameters p. Pigment Type IP VeBow Iron OxidB Bj BON Red P Molybdate Orange jfi; Pthalocyanine Green0 Masstone Color Aa Ob OL AE 0.28 1.30 0.62 1.19 0.34 1.05 0.57 0.79 0.25 0.40 0.17 0.31 0.82 1.84 4.04 144 Tint Color Aa Ob ' AL AE 0.37 0.57 0.54 023 0.82 0.88 0.20 0.68 0.31 0.34 0.14 0.40 0.71 0.20 0.37 0.59 Tinting Strength y> 7 R V 5.7 6.2 8.5 2.0 2.0 5.1 3.1 7.1 1.4 2.3 1.7 2.8 4.5 5.1 7.4 5.1 * Color difference values were calculated with ths CIE 1976 L'a'b' (CIELAB) equation. 3 Tinting strengths were calculated four different ways with the equation In 12.2: Y, based on Y tristimulus value: T, based on lowest tristirrulus value; R, based on t reflectance factor between 420 nm and 6B0 nm; and V, based on visual observation. " Severe bronzing occurred with the masstone of this pigment (more in the batch than the standard), which probably affected the color difference measurements made } different types of instruhients. ` I#? K \ : , jEfrfc . Pigment type. *- njm.,.' Force applied to the muller plates, lb (N) ilittn:.. Total number of revolutions - - IfepL,. Mass of color pigment, g .*>' Mass of dispersing vehicle, g Pthalocyanine Green 100(440) 400 (8 x 50) 0.75 1.8 Yellow iron Oxide 100 (440) 100(2 X 50) 1.0 1.7 BON Red 100 (440) 200 (4 x 50) 0.6 1.4 Molybdate Orange . 100(440) 100(2 X 50) 2.0 1.0 - kbit ANNEX (Mandatory Information) , .t lii;. Al. DISPERSING CONDITIONS FOR MAXIMUM TINTING STRENGTH "A 1.1 The following describes a test method for deter mining the conditions for achieving the maximum level of tinting strength with the mechanical muller. " ' ^,A1,2 Determine the appropriate ratio of color pigment to. jijispersing vehicle by. performing the following operations: Tare off the weight of a glass slab on a balance. Weigh LOO 0.01 g of the standard pigment on to the glass slab. Add dispersing vehicle to the pigment in small amounts and mix them together with the spatula. Keep1 adding the vehicle and mixing the paste until the pigment is completely wetted and a workable paste is-obtained. At'this point the consistency of the paste should be such that a dab of the paste will drop from the spatula when it is gently tapped with the finger. Weigh the paste, and subtract the mass of the pigment to determine the mass of the vehicle. Calculate the pigment to vehicle mass ratio. Repeat the bperatiohs described above for the test pigment. I A1.3 Detehnine the appropriate amount of pigment to use by estimating, to within 0T2 mL, the volume of that paste prepared in A 1.2 that has the smallest pigment-to-vehicie mass ratio. Calculate the masses of pigment and vehicle needed, to give a paste having; a volume of about 2.0 mL. Round the amount of pigment down and the amount of N; vehicle up to the nearest 0.1 g. A 1.4 Apply 100 lbf (440 N) to the muller plates and prepare a tint ofthe standard pigment in accordance with the procedure in Sections 9 and 11. Use the amounts ofthe color pigment and dispersing vehicle determined in A1.3 and mull the paste for 100 revolutions in two stages of 50 revolutions . each. . Al .5 Prepare three more specimens from the same sample following the procedure described in A 1.4, but mull these specimens, in stages of 50 revolutions, for 200, 300, and 400 revolutions, respectively. A1.6 Compare each of the four specimens, one to the other, for tinting strength using one ofthe methods described in Section 12, and determine the minimum number, of revolutions necessary to achieve full tinting strength. If the tinting strength is still developing - after 400 revolutions, repeat A1.4 to_A1.6 with 50 lbf (220 N) more force on the mechanical muller plates. A1.7 Record the appropriate amounts of pigment and vehicle (by A1.3), the force Applied to the mechanical muller plates and the minimum number of revolutions required for maximum tinting strength. A 1.8 Table 2 lists, as examples, the dispersing conditions used in the interlaboratory study that established the preci sion given in Tables 1(a) and 1(b). The vehicle used was No. 1 lithographic varnish with 0.8 % each of cobalt and manga nese driers (6 % types). -a 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 stapdard 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 ateinvitedeither for revision 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, 1916 Race St., Philadelphia, PA 19103. 91 DUP050296614 Designation: D 411 - 83 (Reapproved 1987) Standard Methods of Testing Shellac Used for Electrical Insulation1 This standard is issued under the fixed designation D 411; 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 methods cover tests for shellac in the dry or powdered form to be used for electrical insulating purposes.' 1.2 The values stated in inch-pound units are to be regarded as the standard. The SI equivalents of inch-pound units may be approximate. 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 ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 29 Test Methods for Sampling and Testing Lac Resins12 E 1 Specification for ASTM Thermometers3 3. Genera] Tests 3.1 Each of the following tests shall be made in accord ance with the procedures described in Test Methods D 29: 3.2 Sampling, 3:3 Insoluble Matter, 3.4 Iodine Number, 3.5 Moisture Content, 3.6 Wax, 3.7 Ash, and 3.8 Orpiment (Native arsenic trisulfide). POLYMERIZATION TIME 4. Significance and Use 4.1 Polymerization time provides a measure of time during which shellac retains its plasticity and flow properties at the specified temperature before gelling or polymerizing to the tough rubbery insoluble Torm. This test is important in determining the quality of different lots, useful shelf-life, batch uniformity, and processing characteristics of shellac. 5. Apparatus 5.1 Test Tubes and Wire Rack--Two 18-mm (%-in.) outside diameter glass test tubes, supported by a wire rack to a depth of 100 mm (4 in.) when placed in an oil bath. The 1 These methods are under the jurisdiction of ASTM Committee D-9 on Electrical and Electronic Insulating Materials and are the direct responsibility of Subcommittee D09.O1 on Electrical Insulating Varnishes, Powders, and Encapsu lating Compounds. Current edition approved May 27, 1983. Published July 1983. Originally published as D 4H - 35 T. Last previous edition D411 - 73. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 14.03. test tubes must be supported and maintained in a vertical position. The rack shall be constructed so as to permit free circulation of oil around the test tubes. 5.2 Oil Bath--An oil bath of such construction as to permit the maintaining of a test temperature of 150 PC (300 2F). It is essential to use a mechanical stirring device in the oil bath to maintain a uniform temperature. The oil used shall be a mineral oil, or its equivalent, having a Saybolt Universal viscosity of approximately 150 St (0.015 m2/s) at 100'C (212T). 5.3 Oil Bath Heater--A thermostatically controlled heater capable of maintaining the oil bath temperature within the specified limits. 5.4 Glass Rod--A smooth glass rod about 3 mm (0.12 in.) in diameter and approximately 200 mm (8 in.) long. The end of the glass rod which is to be immersed in the shellac shall be fire polished to a smooth round end. t--A smooth glass rod about 5 mm (0.2 in.) in diameter and approximately 200 mm (8 in.) long with an indicator mark at the top to indicate movement may be used, flatten slightly the diameter of the glass rod for approximately 3 mm (0.12 in.) length at the end which is immersed in the shellac. The purpose ofthe flattened'rod is to provide a more positive feel of the twist lack and rubbery character at the end point. If this alternative is used, it must be specified in the report. 5.5 Thermometer, suitable to indicate the test tempera ture. 5.6 Stopwatch, suitable to indicate elapsed time in-minutes and seconds. 6. Conditioning 6.1 Roll samples of shellac on clean paper, mix.well, and then carefully dry as. described in 6.2 before testing. 6.2 For each shellac to be tested, evenly spread 9 0.1 g of the prepared shellac in a flat bottom dish about 50 mm (2 in.) in diameter. Desiccate over anhydrous calcium chloride (CaClJ for 24 h at room temperature or dry in a wellventilated convection oven at a temperature of 41 2C (105 4F) for approximately 16 h (or overnight). 6.3 After drying, immediately transfer the. sample to a clean, dry, tightly stoppered bottle, and allow to cool. Do not open the bottle except when a specimen is being removed for test. 7. Test Specimens 7.1 Each test specimen shall consist of 4 0.01 g samples of dried shellac as specified in 6.2. 7.2 Test two specimens of each shellac sample. 8. Procedure 8.1 Transfer a specimen of shellac from the stoppered ; j 92 PSWPWf* DUP050296615 D 411 : to the 18-mm (%-in.) glass test tube. Insert the tube fhold securely in a vertical position in the test rack. Place ; in the oil bath having a test temperature of 150 (300 2F) maintained throughout the test. Record the time when the test tube enters the oil bath. Il3. Using the glass rod, stir the specimen gently for up to the first 3 min of the test so that the shellac melts rapidly. It js essential that there be no stirring after, the first 3-min riod. ... 8.4 At the end of each minute thereafter, give the glass rod ' i"sligl?t twist (turning approximately 90). In.the early stages ||pe test, and before the polymerization point is reached, p glass rod will remain in the position to which it has been joined. When, however, the shellac takes, on. a rubbery set, ' ire will be a definite turning or twisting back of the rod jiwing the 90 twist. This is the end point. t O --In the early stages of the test there may be a tendency for glass rod to move back slowly after twisting with the.-fingers. This- . t movement should not be confused with the definite "twist-back" ";eryed when the end point is reached. . ... . W Polymerization Time : 9.1 Record the elapsed time in minutes, from the time of ntry of the specimen into the bath and including the 3-min Stirring period, until the first "twist-back" of the glass rod is |hoted, as the polymerization time. /UrtO. Report ft 10.1 The report shall include the following: ; f 10.2 The polymerization time to the nearest 1 min for each specimen, and '' 10.3 The average of the values in 10.2. FLOW TEST 11. Summary of Methods ' 1J..1- These tests, determine, the flpw of shellac when subjected to 100 ,iC,(212. 2F) under the, CQpditipns of test, specified, herein. These methods .consist,pf melting a sample of ground shellac in a, graduated test .tube.and then tilting the tube to the specified angle while maintained at 100 1G (212 2F) in order .tp permit the shellac to . flow down the tube. 11.2 Two methods are,.provided as follows:. 11.2.1 Method A--In this method the time, required for the shellac, to flow specified distances along the test tube is observed, and 11.2.2 Method B--In this method the total, distance the shellac flows along the test tube in a specified time is observed. 12. Significance and Use 12.1 The rate at which shellac flows down an inclined plane under standard conditions can be used to determine the flow variation that occurs between different types, grades, or lots of shellac. 12.2 Flow tests are sensitive to atmospheric conditions; the flow being greater under humid conditions and less if desiccated. It is essential to carry out the test as quickly as possible so as to minimize the errors due to the effects of atmospheric conditions. 13. Apparatus 13.1 Method A--A suitable form of testing apparatus for use in Method A is shown and described in the Annex. 13.2 Method B--A suitable form of testing apparatus for use in Method B is shown and described in the Annex. Any apparatus that will provide for accurately maintaining the required test temperature and the required positions of the test,tubes may be used in Method B. 14; Test'Specimens 14.1.Each test specimen shall'consist of 2 0.1 g of shellac, Coarsely ground (approximately^ to pass a No. 20 sieve). The specimens' shall be well spread out in a shallow vessel and placed in a desiccator over a saturated solution of sodium dichromate with an excess ofsolid salt and left in this atmosphere (52 % relative humidity) at room temperature for at least 24 h. The specimens shall be tested immediately upon removal frcim the desiccator. ' 14.2 Two specimens shall be tested. 15. Preparation of Specimens 15.1 The two specimens of shellac shall be placed in separate glass test tubes with care being taken that the specimen in each tube is at the bottom and that none of the powdered shellac adheres to the walls of the glass tube. The top level of the, dry' shellac in-each tube shall be read on the millimetre graduated scale. The tubes containing the speci mens shallthen be clamped in place in the testing fixture (see Section 13 and Fig. A 1.1). ~ T 5.2'The' testing fixture, with the glass test tubes in a vertical position, shall be inserted in the oil bath maintained at the testtemperature of 100 1C (212 2F). - 1 15.3 The top surface of the specimen in each tube should be level and at right angle? to the walls of the.tube. 15.4 .The,specimens ?hall be allowed to me}t for 3 min., - _. : METHOD A : 16. Procedure 16.1 At'the end of the 3-min melting period, place each tesi tube at i an angle of 15" from the horizontal, with the corked ends down (see 13.1 and Fig. A 1.2), and with the breather tube extending above the level ofthe oil bath. Make the change from the vertical position to the flow position as quickly as possible. With the oil bath maintained at the test temperature of 100. 1C (212 2F), record the total time required for-the shellac in each tube to flow from the initial level of the shellac to each centimetre marking along the tube. Discontinue the test in each tube when the flow is 9 cm (3.5 in.) or the total time is 20 min. 17. Report 17.1 The report of tests by Method A shall include the following: 17.2 Time required for each centimetre distance of flow for each specimen. DUP050296616 17.3 Plot of curve showing the data reported in 17.2 with time plotted as abscissas and flow, in centimetres, as ordi nates, 17.4 Angle of the test tubes during the flow period, and 17.5 Atmospheric temperature and humidity of the labo ratory. METHOD B 18. Procedure 18.1 At the end of the 3-min melting period, place each test tube at an angle of 15 from the horizontal, with the corked ends down (see 18.2 and Fig. A 1.2) and with the breather tube extending above the level ofthe oil bath. Make the change from the vertical position to the flow position as quickly as possible. With the oil bath maintained at the test temperature of 100 1C (212 2F), allow the test tubes to remain in the bath in this position for exactly 12 min. 18.2 Remove the test tubes immediately, place, in a vertical position, cool, wipe, and measure the flow of the shellac in each tube by reading the distance between the initial point (18.1) and the end of the flow tongue. Disregard the "feather" at the very tip of the tongue. 3--This "feather," caused by separation of wax from the shellac, is more noticeable with some shellacs than with others. It can * readily be distinguished from the main body of shellac as it is always of a different color. "1 19. Report 19.1 The report of tests hy Method B shall include the following: 19.2 Flow expressed in millimetres for each specimen, 19.3 Average of the values in 19.2, : 19.4 Angle of the test tube during the flow periods, and 1 19.5 Atmospheric temperature and humidity of the labo-' 'I ratory. '<j | i!( 20. Precision and Bias 20.1 Shellac is a naturally occurring resin and its chemical ,i and physical properties are highly variable, and dependent ' J upon a number of factors. A standard reference material has not been established. 20.2 Because of the unavailability of round-robin data, no ; statement can be made as to the precision and bias of these j methods for determining polymerization time and flow of \ shellac. ANNEX (Mandatory Information) Al. DESCRIPTION OF APPARATUS FOR DETERMINING THE FLOW OF SHELLAC A1.1 The apparatus shown in Figs. A1.1 and A1.2 consist blocks, and held in position by coil springs H, attached to of the following: disks C. , Al.1.1 Test Tubes--Two test tubes, A, of the following Al.1.3 Oil Bath--A metal bath E, heated by a bunsen types should be used: burner or an electric immersion heater. Oil having a Saybolt A 1.1.1.1 For use with Method A, the tubes should be Universal viscosity of approximately 150 s at 212T (100C) preferably a red-lined, heat-resistant glass, 13 cm in length, is suitable. Glycerol or a clear oif should be used where visual 2.5 cm in outside diameter, and 1.5 mm in wall thickness. observations during the flowing peribd are required as in They should be graduated in 5-mm divisions beginning Method A. It is essential to use a mechanical stirring device 1.1-cm from the outside bottom and extending upward to F, tb~ maintain a uniformly distributed-temperature. The use I' 100 mm. Every 10-mm line should be numbered. These tubes are to be used for holding the specimen, S. of a glass tank or container with an immersion heater is required for Method A, where it is desired to observe the flow during the test and to record the time ..for the shellac A1.1.1.2 For use with Method B, plain heat-resistant glass specimen to flow various stated distances. For Method B any tubes 12.5 cm in length and.2.5 cm in outside diameter. suitable container may be used. The test tubes should be stoppered with tightly fitting A. 1.1.4 Thermometer--A thermometer G, to indicate the t corks through which extend small breather tubes, B. test temperature. The ASTM Partial Immersion Thermom A l. 1.2 Support--A fixture C for holding the glass tubes in eter graduated in either Celsius or Fahrenheit degrees as the correct position. This consists of two disks, of brass specified, the range being -5 to +300C or +20 to +580F, supported as a pendulum as indicated. The disks are free to and conforming to the requirements for Thermometer 2C or turn on the supporting shaft and are held in the desired 2F respectively, as prescribed in Specification E I, is satisfac position by the pin D. The tubes are supported on narrow V tory for this purpose. 94 ww DUP050296617 The American Society lor Testing and Materials takes no position respecting the validity of anypatent rights asserted tn 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 that 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 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. 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 Pace St., Philadelphia, PA 19103. DUP050296618 Designation: D 444 - 88 Standard Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow)1 This standard is issued under the fixed designation D 444; 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 ieapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 7211 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. 1. Scope 1.1 These test methods cover procedures for the chemical analysis of the pigment known commercially as "zinc yellow" or "zinc chromate yellow," 1.2 The analytical procedures appear in the following order: Moisture and Other: Volatile Matter Combined Water Chromium: Dichromate Method Thiosulfate Method Zinc: Hydroxyquinoline Method Ferrocyanide Method Alkaline Salts Sulfates Chlorides Matter Insoluble in Dilute Acetic Add Coarse Particles Sections 9 to 11 9, 12, and 13 9, 14, and 13 9, 16, and 17 18 and 19 20 and 21 22 and 23 24 25 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 ofregulatory limitations prior to use.. 2. Referenced Documents 2.1 ASTM Standards: D 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 D478 Specification for Zinc Yellow (Zinc Chromate)3 D 1193 Specification for Reagent Water4 E 11 Specification for Wire-Cloth Sieves for Testing Purposes5 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 D 01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 31, 1988. Published December 19SS. Originally published as D 444 - 37. Last previous edition D 444 - 81( I987)el. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 14.02. E 50 Practices for Apparatus, Reagents, and Safety Pre cautions for Chemical Analysis of Metals6 . -c 3. Significance and Use 3.1 This lest method has been developed to standardize the chemical analysis of zinc chromate yellow pigment and to provide alternate methods of analysis for chromium and zinc. 4. Preparation of Sample 4.1 Mix the laboratory sample thoroughly. Take a suffi cient quantity for the chemical analyses and pass it through a 180-pm (No. 80) sieve, grinding in a mortar if necessary. 1--Detailed requirements for this sieve are given in Specifica tion E 11. 5. Reagents 5.1 Purity of Reagents--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.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. 5.2 Purity of Water--Unless otherwise indicated,'refer ences to water-fbr use in the preparation of reagents and in analytical procedures shall conform to Type II reagent water, in Specification D 1193. - 6. Precision 6.1 Precision statements have not been established. MOISTURE AND OTHER VOLATILE MATTER 7. Procedure 7.1 Determine moisture and other volatile matter in accordance with Test Method A of Test Method D 280. 6 Annual Book ofASTM Standards, Vol 03.05. 7 "Reagent Chemicals, American Chemical Society Specifications," Am. Chens. 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." 96 mg ~i,_____ DUP050296619 D 444 COMBINED WATER |||ocediire |F$| Weigh to 0.1 mg 3 g of the oven-dried material from determination of moisture and other volatile matter tes 2 and 3), and place in a porcelain boat. Introduce the with the charge into a refractory combustion tube in an ically-heated combustion furnace of the type used for [etermination of carbon in steel by direct combustion 4). Place the boat at the center of the combustion tube plained at a temperature of 1000C 'for 4 h. Draw a tnt of pure dry air or dry nitrogen through the tube to the evolved moisture into a previously weighed irption tube containing' anhydrous magnesium Shlorate (Mg(C104)2) or other efficient desiccant. The '! increase of the absorption tube represents the "cornwater." 2--Loss on ignition of the pigment does not suffice for the ' nination of combined water in zinc yellow. 3--If the pigment contains an organic treating agent, first ove this treating agent by washing with ether or chloroform. iNoii 4--See Apparatus No. 1 for the determination of total carbon lldireet combustion as described in Practices E 50. SPECIMEN SOLUTION FOR DETERMINATION OF CHROMIUM AND ZINC ^Procedure Jp9.1 Weigh to; 0.1 mg about a 4-g specimen and mix with gpinL of cold sulfuric acid (H2S04)( 1+5). It should dissolve ly at this stage (Note 5). Dilute the solution to 500 jftlL in a. volumetric flask. ( 5--A cloudy solution may result if the pigment contains a surface-treating agent. In this case, it usually can be cleared by cooling in pit ice-bath and filtering through a medium porosity fritted disk. If the Mution is not clarified by this treatment, extract a portion of the original sample with a solvent such as chloroform before the analysis is begun. r CHROMIUM BY THE DICHROMATE TEST METHOD fO. Reagents 10.1 Ferrous Ammonium Sulfate Solution--Dissolve 80 g of ferrous ammonium sulfate (FeS04 (NH4)2S04 6H20) in 50 mL of H2S04 (sp gr 1.84) and enough water to make 1 L of solution. Mix thoroughly.before use. This solution is 4pproximately 0.2 N. 10.2 Ortho-Phenanthroline Indicator Solution--0.5 % in water. 10.3 Potassium Dichromate, Standard Solution (0.1 N)--Dissolve 4.9035 g of dried potassium dichromate (K2Cr207) in water and dilute to 1 L in a volumetric flask.11 11. Procedure 11.1 Pipet 50 mL ofthe solution ofthe specimen (Section 7) into a 600-mL beaker. Add 200 to 250 mL of water and SO mL of H2S04 (sp gr 1.84). Cool to 35C or below. 11.2 Add an excess of ferrous ammonium sulfate solution and back-titrate with 0.1 N K2Cr207 solution, using orthophenanthroline indicator. Carry out a blank titration of the same amount of ferrous ammonium sulfate solution at the same time and in the same manner. 11.3 Calculation--Calculate the percent of chromium C as Cr03, as follows: C = (5, - K,)?/, x 0.03334/S, x 100 where; Bi = K2Cr207 solution required for titration of the blank, ruL, Vx = K2Cr207 solution required for back-titration of the specimen, mL, Nx = normality of the K2Cr207 solution, and = specimen in the aliquot used, g. 0.03334 = milliequivaients weight of Crb3. 11.4 Alternatively, the solution of the specimen may be titrated directly with the ferrous ammonium sulfate solution, using an electrometric titration assembly to detect the end point. Standardize the ferrous solution against K2Cr207. CHROMIUM BY THE THIOSULFATE TEST METHOD 12. Reagents 12.1 Potassium Iodide Solution (150 g/L)--Dissolve 150 g of potassium iodide (KI) in water and dilute to 1 L. . 12.2 Sodium Tkiosidfate, Standard Solution (0.1 N)-- Dissolve 24.8 g of sodium thiosulfate of (Na^Oj-5^0) in 1 L of freshly boiled and cooled water contained in a sterile glass bottle. If sulfur precipitates during preparation or upon subsequent use, discard the solution and prepare a new one. Standardize against iodine. 12.3 Starch Indicator Solution--Stir up 2 to 3 g of potato starch with 100 mL salicylic add solution (1 %), and boil the mixture until the starch is practically dissolved, then dilute to 1 L with water. 13. Procedure 13.1 Pipet a 25-mL aliquot of the solution of the spec imen (Section 9) into a 500-mL glass-stoppered Erlenmeyer iodimetric flask or other suitable glass-stoppered bottle containing 200-mL of H2S04 (1+39). Add 20 mL of KI solution (150 g/L), stopper, and allow the solution to stand for approximately 5 min. - 13.2 Titrate the liberated iodine with 0.1 N Na2S203 solution at room temperature until the reddish brown iodine color becomes quite faint Add 5 mL of starch solution and continue the titration until the final color change becomes pale green with no blue tinge. Titrate this final titration by swirling the flask at least three times after each addition of the Na2S203 solution, being sure that there is no further color change, especially at the final stage of the titration. The green end point is definite and sharp. 13.3 Calculation--Calculate the percent of chromium C as Cr03 as follows: C - l(V2N2 X 0.03334)/52] x 100 where: V2 - Na2S203 solution required for titration of the spec imen, mL N2 = normality of the Na2S2P3 solution, and S2 = specimen in the aliquot used, g. 97 DUP050296620 444 ZINC BY THE HYDROXYQUINOLINE TEST METHOD (Suitable if No Interfering Substances Are Present) 14. Reagents 14.1 Acetone Solution of 8-Hydroxyquinoline (50 g/L)-- Dissolve 5 g of 8-hydroxyquinoline in 100 mL of acetone. 15. Procedure 15.1 Pipet 50 mL of the solution of the specimen (Section 9) into a 250-mL beaker and dilute to 100 mL with water. Add 5 to 10 g of ammonium chloride (NH4CI) and heat to boilipg.. Add a slight excess of ammonium hydroxide (NH4OH) and let stand a few minutes to allow any precipi tate to coagulate. Filter through an ashless, rapid paper into ft 400-mL beaker and wash. 15.2 Heat the filtrate to boiling and add 5 mL of NH4OH (sp gr 0.90). Add dropwise 10 mL of the acetone solution of 8-hydroxyquinoline (Note 6): Let stand 10 to 20 min and filter through a medium-porosity sintered-glass crucible. Wash well with water. --The reagent is used in acetone solution rather than alcohol solution to eliminate the danger of reducing some of the chromate by alcohol. Avoid adding an excess Of reagent andTengthy boiling after its addition. Ten millilitres of hydroxyquinoline (50 g/L) is sufficient for a normal zinc yellow. The solution can be tested for complete precipita tion, but since the reagent itself is rather insoluble, the results may be misleading. The insoluble reagent will dissolve in a hot solution and also in an excess of alcohol or acetone, whereas the zinc oxyquinolate will' not. 15.3 Dry the precipitate at 16$C for at least 2 h and weigh as zinc oxyquinolate. 15.4 Calculation--Calculate the percent zinc A as zinc oxide (ZnO), as follows: A = [(Px 0.2303)/53] X 100 where: P = zinc oxyquinolate, g, and S3 < > specimen in aliquot used, g. 0.2303 = ZnO/zittc oxyquinolate = 81.38/353.37 ZINC BY THE FERRQCYANIDE TEST METH9D 16. Reagents 16.1 Methyl Orange Indicator Solution--Dissolve 0.1 g of methyl orange in 100 mL of water. 16.2 Potassium Ferrocyaniie, Standard Solution--Dis solve 22 g of potassium ferrocyanide (K4Fe(CN)6'3H20) in water and dilute to 1 L. To standardize, transfer 0.2 g of metallic zinc or freshly ignited ZnO to a 400-mL beaker. Dissolve in 10 mL of hydrochloric acid (HC1, sp gr 1.19) and 20 mL of water. Drop in a small piece of litmus paper, add ammonium hydroxide (NH4OH) until slightly alkaline, then add HCl until just acid, and then 3 mL.more of HC1, 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 solution shows a brown tinge after standing 1 min. Do not allow the temper ature of the solution to fall below 70C during the titration. Run a blank using the same amounts of reagents and water as in the standardization. The standardization must be made under the same conditions of temperature, volume, and acidity as obtained when the specimen is titrated. Calculate the strength of the K4Fe(CN)6 solution in terms of grains of zinc as follows: Z = W/(V3 -- B2) where: :! Z = zinc equivalent of the K^FefCNJg solution, g/mL,, ' W = zinc used (or equivalent to the ZnO used), g, sf V3 = K4Fe(CN)6 solution, required for titration of the standard, g, and B2 = K^FefCbOe solution required for titration of the blank, mL. ' 16.3 Thyniol Blue Indicator Solution (0.5 g/LJ--Dissolve 0.1 g of thymol blue indicator in 200-niL of methanol, ethanol, or isopropariol. ' 16.4 Uranyl Acetate Indicator Solution (50 g/L)--Dis solve 5 g ofU02(C2H302)2 H20 in water made slightly acid with acetic acid and dilute to 100 mL. '` 17. Procedure 17.1 lUpet 50 ipL ofthe solution ofthe specunen (Section 9) into a 400-mL beaker. Add 35 mL of H2S04 (.1+5) and 3 to 4 drops of thymol blue indicator solution. First add NH4OH (sp gr 0.90) and finally NH4OH (1+10) until the color of the indicator changes to a salmon shade-interme diate between pink add yellow. This gives a pH ofabout 2.4. Dilute the solution to 300 mL and heat to just under boiling. Pass in H2S at a moderate rate for 40 min. Allow the precipitate to settle for-1 h arid filter. Wash'the filter ten times with water saturated with hydrogen sulfide gas'(H2S). 17.2 Dissolve the precipitate in hot HC1 (1+3) and wash the filter paper well with hot water. Boil out the H2S, neutralize to methyl orange with NH4OH, and dilute to 300 mL. Add 2 gofNH4Cl and 3 mL of HQ (sp gr 1.19), and heat to boiling, - .> 17.3 Titrate the hot solution with K4Fe(CN)6 solution (16.2), using uranyl acetate as an external indicator on aspot plate or 1 to 2 drops of ferrous ammonium sulfate solutiori as an internal indicator. 17.4 Calculation--Calculate the percent zinc A as ZnO, as follows: -- ... - ..A** (K4Z/S4) x 100. . .. where: ` : .- . , t. VA = K4Fe(CN),5 solution required for titration of the spec imen, mL, ' : Z = ZnO equivalent of the K4Fe(CN)6 solution, g/riiL, and? S4 = specimen in the aliquot used, g. ALKALINE SALTS 18. Reagents . 18.1 Gelatin Solution (0.2 g/L)--Dissolve 0.2 g of low-ash gelatin in water and dilute to 1 L. 18.2 Lead Acetate Solution (100 g/L)--Dissolve 117 g of Pb(C2H302:)2 3H20 in water and dilute to 1 L. 19. Procedure 19.1 Dissolve exactly 1 g (Note 7) of a specimen in 10 mL of acetic acid (1+1) and add 25 mL of water. Heat until dissolved. Dilute to 250 mL and heat to hailing. Add 20 mL oflead acetate solution (100 g/L) and allow the precipitate to 98 DUP050296621 A D 444 s V' f Filter and.wash the precipitate with hot water. 10--The.acetic acid is necessary to minimize the tendency of B 7--The specimen should riot be greater than 1 g because above loss in alkali metals due to adsoiption on the precipitate becomes e. sulfate to form an inner complex with the trivalent chromium. It is necessary that the solution stand overnight to ensure the precipitation of all the sulfate. |,2 Saturate the filtrate with hydrogen sulfide (H2S) for in. Add 10 mL df gelatin solution (0.2 g/L) and stir fously. Filter and wash with H2S water acidified with a 21.3 Dry the precipitate in an oven, and ignite at 900"C to constant weight. Weigh as barium sulfate (BaSC>4). 11--If the wet precipitate has a yellow appearance, all the ops of H2S04 (1+1). , |.3 Add 5 mL of H2S04 (1+1) to the .filtrate and boil to ||ume of50 mL. Transfer to a silica dish and evaporate to , Ignite gently. chromate was not previously reduced. The results will be high and the specimen should be discarded. Greater attention should then be given to the reduction of the chromium. A slight greenish color cannot be avoided but does not indicate a serious error. \A Leach the residue with hot distilled water, transfer- 21.4 Calculation--Calculate the percent sulfates E as Jthe entire contents of .the silica dish to a: small beaker, sulfur trioxide (S03), as follows: pte with H2S for about 15 min (Note 8). Add 10 mL of h solution (0.2 g/L) and stir vigorously. Filter and wash Precipitate with H2S water, catching the filtrate in a tared la dish. pfdTE 8--A second treatment with H2S is necessary because some of jjieavy petals pass through to. the alkali metal filtrate. 9.5 Add about 2 mL of H2S04 (1+1) to the filtrate, feorate to dryness, and again ignite gently. During the Jtion process add small -portions' of solid ammonium fbonate ((NH4)2C03). Cool in a desiccator ahd weigh. (9.6 Test the residue for calcium. If present, determine E = [(P2 x 0.343)/^] x 100 where: P2 = BaSO* g, and S6 = sample used, g. CHLORIDES 22. Reagent 22.1 Silver Nitrate Solution (17 g/L)--Dissolve 17.0 g of AgNG3 in water and dilute to 1 L. j amount, calculate to.calciium sulfate (C&S04), and deduct iin the weight of the ignited residue. , .. Jfl9.7 Calculation--Calculate the percent of alkaline salts ||as potassium oxide (K20), as follows: ... D = [(R - W2) x 0.541)/53] X 100 there: = ignited residue (see 16.5), g, V2 -- CaS04 (if any) (see 16.6), g, and $ = sample used, g. 23. Procedure 23.1 Weigh a 10-g specimen into a 600-mL beaker. Add 200 mL of water and 50 mL of nitric acid (HN03) (2+3). Warm just enough io dissolve the specimen. Filter to remove insoluble material. Add a slight excess ofAgNQ3 solution (17 g/L) (Note 12). Boil for 5 min and let stand for about 2 h. 12--If care is exercised in adding but a slight excess of AgN03 solution, no silver chromate (Ag2CrO+) will form. About 10 to 15 mL of AgN03 solution (17 g/L) is usually not too much. SULFATES |p. Reagent 20.1 Barium Chloride Solution (100 g/L)--Dissolve 117 g 3aCl2 - H20 in water and dilute to 1 L. I ,f21. Procedure | 21.1 For this determination take about 20 g of Type I igment or about 5 g of Type II pigment as defined in Ipecification D478. Weigh the-specimen into a 1-L beaker. |\dd 75 mL of HQ (sp gr 1.19). Boil the solution under a TM hood until the rapid evolution of chlorine has subsided. Add 5 mL of methyl alcohol and boil to a volume of about 35 mL - ((Note 9). Add 25 mL of HC1 and continue boiling. Add 5 mL of methyl alcohol and again boil to a volume ofabout 35 mL. 23.2 If no crystals of Ag2Cr04 are present, filter at room temperature through a tared, fine-porosity sintered-glass crucible, using suction. Wash the precipitate free of AgNG3 with HN03 (1+99). To be sure that an excess' ofAgN03 was used, test the filtrate by adding a few dfOps of HQ (2+3). Dry the precipitate at 105 2C for 2 h, cool, and weigh as silver chloride (AgQ). 23.3 If crystals of Ag2Cr04 are present (Note-13), filter the solution through a fine-porosity sintered-glass crucible and discard the filtrate containing most of the chromium. Dis solve the AgQ precipitate by pouring 100 mL of hot ammonium hydroxide (NH4OH) (1+5) slowly through the crucible while applying gentle suction. Catch the filtrate in a clean flask, taking care not to lose any ofit. Wash with a few millilitres of HN03 (sp gr 1.42) and then with a little more NH4OH (1+5). 9--If the volume is reduced below 35 mL, a precipitate may form that will not dissolve upon dilution. It is imperative, however, that all the chromium be reduced. 13--Silver chromate is difficult to dissolve completely by washing with dilute HN03; hence, in such cases, it is necessary to dissolve in NH40H and reprecipitate. 21.2 Dilute the solution to 400 mL with water. If the ' solution is not clear at this point, filter it Heat to boiling and add 50 mL of glacial acetic acid. Add 10 mL of BaCl2 solution (100 g/L) dropwise, while stirring. Boil for 30 min and allow to stand overnight (Note 10). Filter through a tared Gooch crucible and wash with hot water. 23.4 Transfer the solution to a beaker and make it faintly acid by adjusting with either HN03 (1+5) or NH40H (1+5) as required. Add a few drops of AgN03 solution (17 g/L) and boil for 5 min. Let stand at least 2 h in a dark place. Filter through a tared, fine-porosity sintered-glass crucible, using suction. 99 DUP050296622 i D444 23.5 Wash the precipitate free of AgN03 with HN03 (1+99), and dry at 105 2"C for 2 h. Cool and weigh as AgCl. 23.6 Calculation--Calculate the percent chlorides E as chlorine, as follows: E = [(P3 x 0.247)/S'7] x 100 where: Pi = AgCl, g, S7 -- specimen used, g, and 0.247 = Cl/AgCl = 34.45/143.32. MATTER INSOLUBLE IN DILUTE ACETIC ACID 24. Procedure 24.1 Weigh to 0.1 mg about a 10-g specimen (Note 14) and place in a 600-mL beaker. Add 300 mL of acetic acid (1+9). Heat the mixture to 80C and maintain at 80 5C, while stirring, until nothing further dissolves. Filter while hot through a tared Gooch crucible. Wash the insoluble residue on the filter with hot water. 14--If the pigment contains an organic treating agent, first, remove this treating agent by washing with ether or chloroform. 24.2 Dry the crucible at 105 2C and weigh. 24.3 Calculation--Calculate the percent of matter insol. uble in acetic acid (1+9).Fas follows: F = {Rx/S%) x 100 where: R, -- residue, g, and Ss -- specimen used, g. COARSE PARTICLES 25. Procedure 25.1 Determine the percent of coarse particles in die pigment as received, in accordance with Test Methods D 185. INDEX TERMS 26. Index Terms 26.1 These test methods are indexed under the following terms: zinc chromate; pigments--zinc chromate. . The American Society for Testing and Materials takes no position respecting the validity ofanypatent rightsasserted 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 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 he reviewed every live years end ifnot revised, either reapproved or withdrawn. Yourcomments are Invitedeither torrevision 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. 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. 1 too DUP050296623 Designation: D 475 - 67 (Reapproved 1989} Standard Specification for Pure Para Red Toner Pigment*1 This standard is issued under the luted designation D 475; 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. yjeope Type I Type H _JT This specification covers the red pigment commer- M known as pure para red toner: It is available in two Type I, light, and Type II, dark. HSfnPjieferenced Document A ( .. 1 ijpff-l ASTM Standard: ' P970 Test Methods for fara Red. and TolUidine Red ftfigments2 ' Ash, max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on a 45-|im (No.325) sieve), max, % Solubility in chloroform Resistance to .acids Resistance to alkalis Identity test 3.0 1.0 1.5 complete to pass test to pass test to pass test 3.0 1.0 1.5 to pass test equal to standard to pass test 3.3 The mass color and character of the tint formed by Composition and Properties |.S Dry Pigment: ah 1 Type /--The pigment shall be in a soft dry form and ..consist of para red toner, light (1 -(p-nitro-phenyl|)-2-naphthol) free of any substrate. .1.2 Type II--The pigment shall be in a soft dry form itshall consist of para red toner, light (l-( p-nitro-phenyle)r2-naphthol) mixed with a small quantity of l-(ppo-phenyl-azo)-2-naphthoh7-sulfonic acid free of any sub ate. . - , |3.2 The pigments shall conform to the following requireents: mixture with a white pigment shall be the same as, and the strength not less than, that of a reference sample fnutually agreed upon by the purchaser and the seller. r 4. Sampling 4.1 Two samples shall betaken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be' taken from different packages in the ratio of two samples for each 10 000 lb (5 000 kg), except that for shipments of less than 10 000 lb two samples shall be taken.. At the option of the purchaser, the samples may be tested separately, or after blending in equal quantities the samples from the same JpifThj* specification is under thejurisdiction of ASTM Committee D-l on Paint production unit to form a composite sample. ,,^pd Related Coatings and Materials and is the direct responsibility of Subcom- }^mil;ee.D0I.31 on Pigment Specifications. 5. Test Methods , .- Iff Current edition approved Nov. 30, 1967. Originally published as D 475 - 38 T. "1st previous edition D 475 - 49. 11 Annual Book ofASTM Standards, Vol P6.02. 5.1 Tests shall be conducted in accordance with Test Methods D 970. [M,:S ; * The American Society ion Testing andMaterials takes no position respecting the validity ofany patent rights, ssserted in connection with any item mentioned in this standard. Users,ol this standard are expressly advised'tMrdetermlnatkm of the validity of any such patent rights, and fha risk of infringement of such rights, are entirely their own responsibility. This standardis subject to revision at any time by the responsible technical committee andmust be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Yourcomments are Invitedeitherforrevision 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 19103. DUP050296624 <1 Designation: D 476 - 84 (Reapproved 1989) i Standard Specification for Titanium Dioxide Pigments1 This standard is issued under the fixed designation D 476; 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 icapprovaj. 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 This specification covers four types of titanium di oxide pigments: 1.1.1 Type I--Anatase, free chalking. 1.1.2 Type //--Rutile, medium chalk resistant (low). 1.1.3 Type Ilf--Rutile, medium chalk resistant (high). 1.1.4 Type IV--Rutile, highly chalk resistant. 2. Referenced Documents 2.1 ASTM Standards: D34 Practice for Chemical Analysis of White Pigments12 D153 Test Methods for Specific Gravity of Pigments2 D185 Test Methods for Coarse Particles in Pigments, Pastes, , and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D1394 Test Methods for Chemical Analysis of White Titanium Pigments2 D2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance ofthe Leachate of the Pigment2 D3720 Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments by X-Ray Diffraction2 3. Composition and Properties 3.1 Titanium Dioxide Pigments,4 shall conform to the requirements for composition prescribed in Table 1. They shall be chemically prepared pigments consisting of anatase or rutile titanium dioxide with or without modifications with water-insoluble oxides of aluminum, silicon, zinc, eta, or other agents; these reagent materials are introduced specifi cally to improve those properties for which the pigment is used. The titanium dioxide pigments shall be free of ex 1 This specification is underthe jurisdiction ofASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Nov. 14, 1984. Published January 1984. Originally published as D 476 - 38. Last previous edition D 476 - 73 <1979). 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 4 The Titanium Dioxide pigments specified by type in 3.1 are indexed by type in the National Paint and Coatings Association, Raw Materials Index, Pigment Section. tenders such as barium sulfate, clay, magnesium silicate, whiting, etc. 3.2 The desired properties of the pigment, other than as herein indicated, shall be subject to mutual agreement between the purchaser and the seller and shall be based on a satisfactory match between the submitted pigment sample and a previously agreed upon reference sample (see 5.1.6). 4. Sampling j I 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or as a composite sample formed by blending in equal quantities the samples from the same production unit. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. -- 5.1.1 Chemical Analysis--Practice D 34 or Test Methods D1394. ' .- 5.1.2 Specific Gravity--Test Methods D.153; . 5.1.3 Coarse Particles--Test MethodsD 185. 5.1.4 Moisture--Test Method D 280. 5.1.5 Matter Soluble fn Water, Specific Resistance--Test Method D 2448. The measured specific resistance of the aqueous leachage from the pigment is an index of water- soluble salts. 5.1.6 Chalk Resistance--It is recommended that pur- chaser arid seller agree upon standards and methods of test suitable for their requirements (see 3.2). Comparison in a good quality exterior air-dry alkyd enamel (trade sales or industrial) and exposure in Florida at 45' facing south are recommended. Chalking differences are minimized by less durable vehicles and required exposure times are prolonged by more durable vehicles. Once the reference sample agreed upon by the purchaser and seller has qualified, subsequent shipments of that product may be compared with the reference sample by a mutually agreed upon accelerated weathering test. I ! ; 1 J1 1 j 1 1 102 DUP050296625 D 476 TABLE 1 Requirements for Composition of Titanium Dioxide Pigments Typel Type II Type III Type IV Hr AnataseA Free Chalking Rutile--Medium Chalk Resistant Rutile--Medium Chalk Resistant Rutile--Highly Chalk Resistant 1%. ||fypteal Paint Applications white exterior house paints; interior uses SfeldemO,). min, % jljjjjpte In water, specific resistance, 94 5000 low-medium % PVC enamels and lacquers 92 5000 medium-high % PVC enamels; alkyd and emulsion flat wall paints 80 3000 exterior coatings requiring excellent durability and gloss retention 80 3000 fjTard other volatile matter (loss at r3vflOC), max, %B rijrarity 'oartteles (total residue retained on a If(No. 32S) sieve), max, % 0.7 3.8 to 4.0 0.2 0.7 4.0 to 4,3 0.2 1.5 3.6 to 4.3 0.2 1.5 3.6 to 4.3 0.2 ndltioned overnight at 50 % relative humidity at 25"C (for referee purposes only), p permissible for water dispersible types only. 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 ol 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 reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Yourcomments ere invitedeither lor 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 malm your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. DUP050296626 Last ASTM Designation: D 477 - 78 Standard Specification for Zinc Sulfide Figments This specification covers dnc sulfide pigments. ,i:. Formerly under the jurisdiction' of Committee D-l On Paint and Related Coatings and Materials, this specification was discontinued in 1988. \V 104 T DU P050296627 Designation: D 478 - 86 (Reapproved 1991)1 Standard Specification for Zinc Yellow (Zinc Chromate) Pigments41 1 This standard is issued under the fixed designation D 478; the number immediately following the designation indicates the yedr 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. 41 --Keywords were added editorially in July 1991. Scope This specification covers the pigments commercially [Evil as zinc yellow (zinc chromate). p2 Two types are included: |.2.1 Type /-High-purity, low sulfate and chloride con- p.2.2 Type //--Regular grade. IReferenced Documents iSLl ASTMStandards: fD185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2 |D 387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller3 D 444 Test Methods for Chemical Analysis of Zinc Yellow |i Pigment (Zinc Chromate Yellow)3 Significance and Use 3.1 Zinc yellow is used in rust-inhibiting protective coatS tags and metal primers for ferrous and non-ferrous metals. ; 4. Composition and Properties '4 ' 4.1 Dry Pigment--The pigment shall be a reaction precipfl? itate of soluble chromates and a suitable zinc compound and shall be free of extenders, carbonates, and organic color in I* any form. The pigment shall conform to the requirements for composition prescribed in Table 1. 4.2 The mass color and character of the tint and the x tinting strength formed by a mixture with a white pigment H shall be within mutually agreed upon limits of a standard I acceptable to both the purchaser and the seller. 4 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint ,;nd Related Coatings and Materials and is the direct responsibility of Subcom mittee DO! .31 on Pigment Specifications. Current edition approved April 25, 1986. Published June 1986. Originally ; published as D 478-38 T. Last previous edition D478-49(1981)*'. * 2 Annual Book ofASTMStandards, Vols 06.01 and 06.02. i..' 3 Annual Bock ofASTM Standards, Vol 06.02. rV 5. Sampling 5.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 6. Test Methods 6.1 Tests shall be conducted in accordance with the following ASTM test methods: 6.2 Chemical Analysis--Test Methods D 444. 6.3 Coarse Particles--Test Methods D 185. 6.4 Mass Color and Tinting Strength--Test Method D 387. 7. Keywords s. 7.1 chromatic; inhibitor metal primer, pigment; zinc chromate; zinc yellow TABLE 1 Composition Requirements Zinc (calculated as ZnO), % Chromium (calculated as CrCy, min, % Sulfates (calculated as SO3), max, % Chlorides (calculated is Cl), max, % Alkaline salts (calculated as KjCr), max, % Matter Insoluble In acetic add (1+9)at 80"C, max,* Moisture and other volatile matter, max, % Coarse particles (total residue retained on No. 325 (45-pm) sieve), max, X Type 1 35 to 40 41 ----- 0.20 0.10 13 0.3 1.0 1.0 Type 11 35 to 40 4t ' 3.0* 0.8* 13 ' 0.3 1.0 1.0 * The maximum percent of sulfates or chlorides given in the table for Type II pigment apply if only one or the other is present (for this purpose amounts of less than 0.05 % shall be disregarded). If both sulfates and chlorides are present, the sum of the percentages of each divided by Its respective maximum permissible percentage (3.0 for S03 and 0.8 for Cl) shall not exceed 1.0. For example, If a sample contains 1.8 % SO3 (0.6 of the maximum for sulfates) and 0.3 % chlorides (0.4 of the maximum for chlorides), the sample just conforms to the maximum requirements of the specification in this respect DUP050296628 # D 478 Tha 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 ol 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 dnet revised, eitherreapprovedorwithdrawn. Your comments are Invitedeither for revision 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 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 St., Philadelphia, PA 191P3. i DUP050296629 Designation: D 480 - 88 Standard Test Methods for Sampling and Testing of Flaked Aluminum Powders and |ir Pastes1 This standard is issued under the fixed designation D 480; 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 yearofiast reapproval. A superscript epsilon (e) 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 Method 4451.1. 7233 ofFederal Test MethodStandard No. 141. Consult the DoD Index qfSpecifications andStandardsfor the specific year ofissue which has been adopted by the Department ofDefense. ;> Hope These test methods cover procedures for sampling, Sative analysis, and physical testing of flaked aluminum |ers and pastes (leafing and nonleafing) for coatings. k These test methods apply equally- to leafing and leafing flaked aluminum powders and, pastes; except v: noted to the contrary. Sf Tfc standard may involve hazardous materials, operTp- and equipment. This standard does not purport to pess all ofthe safety problems associated with its use. It is. f responsibility of the user of this standard to establish |mpriate safety and health practices and determine the liability of regulatory limitations prior to use. For a ific hazard statement, see Note 1. ,.f . Referenced Documents ASTM Standards: * 185 Test Methods for Coarse Particles in Pigments, r Pastes, and Paints12 e||ff)235 Specification for Mineral Spirits (Petroleum Rjfjfir: Spirits) (Hydrocarbon Drycleaning Solvent)3 ijP*fp 329 Specification for Acetone3 *jjdlP,'9i62 Specification for Aluminum Powder-and'Paste tipi' Pigments for Paints4 5 BED.398Q Practice for Interlaboratory Testing of. Paint and t| "Related Materials2 IE-11 Specification for Wire-Cloth Sieves for Testing pLfPurposes3 . ; IE 34 Test Methods for Chemical Analysis of Aluminum and Aluminum Alloys6 * / E 607 Test Method for Optical Emission Spectrometric Analysis of Aluminum and Aluminum Alloys by the Point-to-Plane Technique; Nitrogen Atmosphere?. E 691 Practice for Conducting an Interlaboratory . Study to Determine the Precision of a Test Method8 1 These test methods are under the jurisdiction of ASTM Committee D-l on Huint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.31 on Pigment Specifications; Current edition approved July 29,1988. Published December 1988. Originally published as D 480 - 38. Last previous edition D 480 - 70 (1976). 3 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 06.03. "Annual Book qfASTM Standards, Vol 06.02. 5 Annual Book ofASTM Standards, Vol 14.02,: 6 Annual Book ofASTM Standards, Vol 03.05. 1 Annual Book ofASTM Standards, Vol 03.06. `Annual Book ofASTM Standards, Vols 06.03 and 14.02. 3. Significance and Use 3.1 Flaked aluminum pigments are produced in a variety of forms. These test methods allow the user to determine the applicability of a given product to this use.! 4. Sampling 4.1 Sampling is subject to mutual agreement between the seller and die purchaser. Place each sample in a cleati, dry metal or glass container which shall be nearly filled, then close with a tight cover, seal, mark, and send to the laboratory for testing. 4.2 When requested, duplicate samples may be taken from the same container and delivered to the seller, and the inspector may take a third set of samples to hold for test in case of disagreement.- 5. Qualitative Analysis 5.1 Significance and-Use--This test method determines if there are chemical- impurities, other than fatty and oily matter, as specified in Specification D962, to ensure the absence of fillers or extender pigments. 5.2 Procedure: . -- 5.2.1 TotalImpurities--Determine the total impurities by weight in accordance with Test Methods E 34 and E 607 or by atomic absorption. - 5.2.3 Total d/nw/nam-r-Determine the total aluminum . by weight difference with elemental impurities"in accordance with 5.2.1. 6. Leafing Properties 6.1 The leafing tea conditions specified are selected arbitrarily, and even though the numerical leafing value obtained by this test method appears to be low, the pigment may give substantially perfect leafing under the conditions of practical application in a paint. 6.2 Significance and Use--This leafing test method has been established to determine the percent of leafed alu minum flakes at the surface of a simulated paint formula to ensure a bright metallic luster. Minimum leafing character istics must conform to Specification D 962. 6.3 Apparatus: 6.3.1 Leafing Spatula, nonmagnetic, stainless steel spatula having the following dimensions: Length of blade min, in. (mm) 5.5 (139.7) Width of blade, in. (mm) 0.540 0.002 (13.72 0.05) Thickness of blade, in. (mm): DUP050296630 to mm from tip 100 mm from tip Shape of tip 0.013 0.003 (0.33 0.08) 0.038 0.004 (0.97 0.10) rounded or straight The surface of the spatula shall be polished with 3/0 emery or silicon carbide metallographic paper wet with mineral spirits; polishing shall be repeated for 1-min intervals until a consistent minimum leafing result is obtained in a typical leafing test. 6.3.2 Test Tube, 6 in. (152 mm) in length by 0.75 in. (19.0 mm) in diameter. 6.3.3 Glass Cylinder, 8 in. (203 mm) in length and 1.5 to 2.0 in. (38.1 to 50.8 mm) in inside diameter. A stopper shall be used and the spatula shall be attached to the stopper so as to hang vertically in the cylinder with the tip about 1 in. (25 mm) from the bottom. 6.4 Reagents: 6.4.1 Coumarone-Idene Resin--The form commercially known as "chipped" and having the following properties; Softening point, C Specific gravity Add value, max Cloud point, C, max 109 to 117 1.12 to 1.16 0.5 -7 6.4.2 Petroleum Spirits--Conforming to Specification D 235 and having the following additional properties: Specific gravity at 60F (16C) Surface tension at 70`F (21C), N/m, min Kauri butanol value Aniline point, *F (C) 0.800 to 0.810 24.5 42 to 44 105 to 115 (40 to 45) 6.5 Preparation of Leaf-Testing Vehicle--Prepare solu tion by dissolving 30.0 g of resin, in the form of small chips, in 100 mL ofpetroleum spirits, while heating gently at about 140F (60C). The specific gravity of the solution shall be between 0.877 and 0.881 at 60F (16C). Allow the solution to settle and retain the clear portion for use. 6.6 Aliquot--Unless otherwise specified, the aliquot weight shall be as follows: Classification ASTM Designation Class Aliquot Weight, g Flaked aluminum powder Aluminum paste D 962, Type I D 962, Type 2 A 1.0 B 1.0 C 2.0 A 1.5 B 1.5 C 3.0 6:7 Procedure--Perform the test at a room temperature of 25 2C. Place approximately 5 mL of the leaf-testing vehicle in the glass cylinder and cover with a watch glass. Transfer 25.0 1.0 mL of the vehicle to a clean container. Weigh the required aliquot of aluminum powder or paste to the nearest 0.01 g and transfer to a small dish. Add about 2.5 mL of the 25-mL quantity of vehicle and mix to a stiff paste with a spatula or small stiff brush. Add approximately 5 mL more of the vehicle and stir to a smooth mixture, then add the remainder of the vehicle and continue stirring to obtain complete dispersion. Transfer the mixture to the test tube to give a depth of about 110 mm when the specified spatula is immersed. Avoid formation of bubbles. Dip the spatula to the bottom of the mixture and rotate it gently through an arc of about 90 for 10 s. Withdraw the spatula at a uniform rate of about 2 in. (50 mm)/s. The spatula should not touch the wall of the test tube above the liquid level. Immediately suspend the spatula vertically in the glass cylinder with leafing liquid in it and allow to remain for 3 min. Measure the height of immersion and the height of complete leafing on both sides of the spatula, measuring to the bottom of the meniscus in each case. Clean the spatula by rinsing it in petroleum spirits and wipe dry with a clean cloth. Stir (do not shake) the mixture in the test tube and repeat the determination. 6.8 Calculation--Calculate the leafing value L as follows: L = A/B X 100 -- AX 100/15 where: A = height of complete leafing, in. (mm), and B = height of immersion, in. (mm). 7. Coarse Particles f 7.1 This section provides two test methods for deter mining the percent residue retained on a sieve by wet screening techniques. 7.2 Significance and Use--These procedures determine the percent of coarse particles present in aluminum pigments to ensure a smooth appearance, as required in Specification D 962. 7.3 Procedure A: 7.3.1 Aluminum Powder--Fill two "straight wall" containers not less than 12 in. (305 mm) in diameter to a depth of not less than 4 in. (102 mm) with petroleum spirits, and fill a third similar container to a depth of not less than 3 in. (76 mm) with acetone. The petroleum spirits used for the test shall conform to Specification D 235, and the acetone shall conform to Specification D 329. Weigh-5 g of the aliquot, transfer to a 250-mL beaker, and add in small portions a total of about 150 mL of petroleum spirits, mixing thor oughly to a uniform consistency after each addition. Clamp a standard sieve 8 in. (203 mm) in diameter conforming to Specification Ell, just above the level of the petroleum spirits in the first container and pour the specimen OH the sieve, using a 45-pm (No. 325) sieve for Classes A, B, and C powder and in addition a 150-p.m (No. 100)sieve for'Class C powder. Rinse the beaker with clear petroleum spirits and transfer the rinsings to the sieve. Holding the sieve at a slight angle to prevent air lock, shake it backward and forward working die sieve alternately just under and just above the level of the liquid with rotation, avoiding spillage from the screen, at a rate of approximately 60 to 100 cpm. It is important that the material be thoroughly sieved in each container. After the bulk of the aliquot has passed through the sieve (usually about 2 min) repeat the procedure in the second container for about 2 min. When it is evident that practically none ofthe residue on the sieve is passing through it, repeat the procedure in the acetone container for about 2 to 3 min until nothing more passes through the sieve. Rinse the sides of the sieve with a small stream of acetone, and collect the residue at one side of the sieve. Transfer the residue to a dried and weighed aluminum cup or small evaporating dish with a small stream of acetone, using not less than 15 to 25 mL. Place the aluminum cup or dish in an oven, evaporate to dryness at 105 to 100C, and continue heating at this temperature for 15 min. | I j j j j J 1 jf J J [ ; 1 108 DUP050296631 # D 480 sg 1: Warning--Do not close the door of the oven while evapo:acetone, as there is danger of explosion or flash of acetone Wi-Aluminum Paste--Determine the percent of coarse ]|in accordance with the procedure described in 7.3.1 jpt5-|tm (No. 325) sieve for Classes A, B, and C paste iition a 150-pm (No. 100) sieve for Class C paste, p Calculation--Calculate the weight percent of the ' fietained on the sieve R from the increase in weight as R = [(A/W)X CF\ x 100 pyliht of dried residue, g, ^correction factor (1.0 for NIST sieves), and Eg aliquot weight, g. fejhTE 2--A correction factor shall be applied in the case of sieves Id in thetest that have not been certified by the National Institute of inilards and Technology. Sieves having a correction factor above 1.2 jliiow 0.8 should not be used. The correction factor may be calculated (jpllows: Determine the coarse particles ofan aliquot on a master sieve ! by the National Institute of Standards and Technology foi ls the procedure described in 7.3.1. Sieve the same aliquot on the jpni sieve by the same procedure. Calculate the correction factor, " i follows: CF = X/Y | i= weight of residue on the NIST sieve, g, and , weight of residue on the unknown screen, g. ||4 Procedure B--Test in accordance with Test Methods 185 to determine conformance of flaked aluminum powand pastes to Specification D 235. |asily Extracted Fatty and Oily Matter gc< 1 Easily extracted fatty and oily matter is determined by j| following arbitrary test method. Details of the test ggeedure shall be strictly followed. Significance and Use--This test method determines , percent , of easily extracted fatty and oily matter in aum pigments in accordance with Specification D 962. >J| Procedure: V .. , '` ' S. 1 Aluminum Powder--Weigh accurately (to within |01 g) approximately 2 g of the aliquot Transfer to a 3-mL volumetric flask and add about 50 mL of redistilled conforming to Specification D 329. Heat the mix- ; to boiling while occasionally agitating. Cool, fill to the 200-mL mark with acetone, and mix. Allow the mixture to settle. Draw off approximately one half of the supernatant liquid and filter through dry paper. Discard the first 10 mL of the filtrate. Transfer 100 mL of the dear filtrate to a weighed dish. Evaporate the acetone at a temperature not above 75C. Heat the dish for 15 min in an oven at 105 to 110C. Cool and weigh the amount of fatty oily matter. 8.3,2 Aluminum Paste--Determine the percent of easily extracted fatty and oily matter in aluminum paste in accordance with the procedure described in 8.3.1. 8.4 Calculation--Calculate the weight percent offatty and oily matter P as follows: F- [2 x (A/W)\ x 100 where: A -- weight of residue in 100 mL of acetone, g, and W -- weight of aliquot, g. 9. Nonvolatile Matter 9.1 Determine the percent of nonvolatile matter in alu minum paste consisting of aluminum, fatty acids, additives, and their inter-reaction products. 9.2 Significance and Use--This test method determines the combined percent of aluminum and other nonvolatile matter, such as fatty adds and their inter-reaction products, in aluminum pigments and their conformance with Specifi cation D 962. 9.3 Procedure--Aluminum Paste and Powder--Weigh into an evaporating dish 5 g of paste or powder to within 0:01 g. Evaporate in an oven at a temperature of 105 to 110"C for 3 h. Cool to room temperature and weigh. 9.4 Calculation--Calculate the weight percent of nonvol atile matter NV as follows: NV=A/Wx 100 " where: A = weight of residue, g, and W -- weight of aliquot, g. -- 10. Precision and Bias 10.1 Precision and Bias--Determinejn accordance with Practices D 3980 and E 691. '. ' ' 11. Index Terms 11.1 These test methods are indexed under the following terms: flaked powders; leafing properties; aluminum powders and pastes. 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 potent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject tb revision atany time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, eitherreapprovedor 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 flaceSL, Philadelphia, PA 19103. DUP050296632 i Designation: D 520 - 84 (Reapproved 1989) Standard Specification'for Zinc Dust Pigment1 This standard is issued under the fixed designation D S20; 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 reapptoval. li Scope 1.1 This specification covers two types of zinc dust, for use as a pigment in paints. Type I is a general grade. Type II is a high-purity grade. 2. Referenced Documents 2.1 ASTM Standards: B 214 Test Method for Sieve Analysis of Granular Metal Powders12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D521 Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)4 E 40 Test Methods for Chemical Analysis of Slab Zinc (Spelter)5 . 3. Composition and Properties 3.1 The pigments shall consist substantially of metallic zinc and shall conform to the requirements for composition prescribed in Table 1. .. 3.2 In such physical properties as are specified by the purchaser, the pigment shall satisfactorily match a reference sample mutually agreed upon between the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing 1 This specification is under the jurisdiction ofASTM Committee D-l on Faint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.51 on Figment Specifications. Current edition approved Aug. 3t, 1984. Published December 1984, Originally published as D 520 - 39 T. Last previous edition D 520 - 83. 2 AnnualBook ofASTM Standards, fol 02.05. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 4 Annual Book ofASTM Standards, Vol 06.02. 5 Annual Book ofASTM Standards, Vol 03.05. TABLE 1 Requirements for Composition Total zinc, calculated as Zn, min, % Metallic zinc, min, % Material other than metallic zinc, ZnQ, and admixed CaO, where applicable max % Calcium, calculated as CaO, max, % Lead, calculated as Pb, max, % Iron, calculated as Fe, max, % Cadmium, calculated as Cd, max, % Chlorine, calculated as Cl, max, % Sulfur, calculated as SOa, max, % Moistureend other volatile matter, max, % Oily or fatty matter, or both, max, 56 Zinc oxide (ZnO), max, % Coarse particles, max, %: Total residue retained on a 150-um (No. 100) sieve Total residue retained on a 75-um (No. 200} sieve Total residue retained on a 45-um {No. 325) sieve Type 1 97.5 94.0 0*75 0.7 0.10 . 6.0 none 4.0 Type II 98.0 94.0 . 0.7 0.01 0.02 0.01 0.01 0.01 0.10 0.05 remainder 0.1 0.8 3.0 between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb, two samples shall be taken. At-the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. _ 5. Test Methods 5.1 Tests sbhll be conducted in accordance with the following ASTM test methods. Test procedures npt cpvered by. these ASTMtest methods shall be mutually agreed upon between the purchaser and the seller. ' 5.1.1 Total and Metallic Zinc--Methods Et52i . 5.1.2 Lead, Cadmium, arid Iran--Sections 8, 18.2, and 22, respectively, of Methods E40. 5.1.3 Oily or Fatty Matter, or Both--Methods D 521. 5.1.4 Coarse Panicles--Test Method B214 or Test Methods D 185. . 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 tevisad, 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 oi 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. 110 DU P050296633 Designation: D 521 - 90 Standard Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)1 This standard is issued under the fixed designation D 521; 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. Scope These test methods cover procedures for the chemical pjsis of metallic zinc powder in the form commercially rtbtvn as zinc dust for use as a pigment in paints. _2 The analytical procedures appear in the following ds er: Sections future and Other Volatile Matter ^particles [erSolubie in.Hexane lie Zinc Oxide 7 S 9 and 10 . 11 and 12 13 and 14 15 16 and 17 . 18 19 20 21 and 22 23 and 24 Jjfe'2 This standard does not purport to address the safety ffimtems associated with its use. It is the responsibility ofthe . ' of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory ^initiations prior to use. Referenced Documents fisil ASTM Standards: p 214 Test Method for Sieve Analysis of Granular Metal || Powders12 . jbl85 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 SD280 Test Methods for Hygroscopic Moisture {and Other Matter Volatile Under the Test Conditions) in Pig ments4 D1193 Specification for Reagent Water5 E 40 Test Methods' for Chemical Analysis of Slab Zinc (Spelter)6 aft. E 68 Polarographic Determination of Lead and Cadmium in Zinc7 . Significance and Use 3.1 These test methods compile procedures which can be 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paim and Related Coatings and Materials and are the direct responsibility of BSubcommittee DO 1.21 on Chemical Analysis of Paim and Paint Materials. ||s Current edition approved May 25, 1990. Published July 1990. Originally Ippublished as D 521 - 39 T. Last previous edition D 521 -81. I-. 2 Annual Book ofASTM Standards, Vol 02.05. If 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. It' 4 Annual Book ofASTM Standards, Vol 06.02. If 5 Annual Book ofASTM Standards, Vol 06.03. 1' 6 Annual Book ofASTM Standards, Vol 03.05. 7 Discontinued--See 1979 Annual Book ofASTM Standards, Part 12. used to check the composition of purity of metallic zinc powder. This information is useful to both the formulator and users. 4. Treatment of Sample 4.1 Store the laboratory sample in a tightly stoppered bottle to protect it from oxidation. Mix the whole sample thoroughly before taking, portions for analysis. 5. Purity of Reagents 5.1 Purity of Reagents--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.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. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D1193. 6. Precision 6.1 Precision statements have not been established. MOISTURE AND OTHER VOLATILE MATTER 7. Procedure 7.1 Determine moisture and other volatile matter in accordance with Method A of Test Methods D 280, except heat the sample for only 1 h. COARSE PARTICLES _ 8. Procedure 8.1 Determine the percent of coarse particles in ifie pigment in accordance with Test Methods D 185 or B 214. " MATTER SOLUBLE IN HEXANE 9. Reagent 9.1 Hexane--Pure hexane or commercial hexane or pe troleum ether of boiling point not higher than 75'C. Redistill before using. 10. Procedure 10.1 Place 100 g of the pigment in an extraction thimble 5 "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." 111 DUP05Q296634 D521 in a Soxhlet extraction apparatus. Record the tare weight of the receiving flask. Charge the flask with a suitable volume of hexane and extract the sample for 4 h, subjecting the specimen to not less than 20 extractions in this time. Make a blank determination at the same time. 10.2 Remove the receiving flask, evaporate or distfll off the hexane on a steam bath, and dry the flask at 105 2"C for 1 h. Cool and weigh. 10.3 Calculate the percent of matter soluble in hexane, allowing for any material found in the blank. B2 K4Fe(CN)6 solution required for titration of t| blank, mL, Z = zinc equivalent of the K4Fe(CN)6 solution, g/mL, and St = sample used, g. METALLIC ZINC ; I--Sections 12 and 13 cover a rapid method for determining! metallic zinc, intended for routine analysis. The results are inclined to be. * somewhat low, and for highest accuracy and particularly for referee tests, : the hydrogen evolution method should be used.9 if TOTAL ZINC 11. Reagents I. 1.1 Potassium Ferrocyanide, Standard Solution--Dis solve 22 g of potassium ferrocyanide (K^FefCNjg 3H20) in water and dilute to 1 L. To standardize, transfer 0.2 g of metallic zinc or freshly ignited zinc oxide (ZnO) to a 400-mL beaker. Dissolve in 10 mL of hydrochloric add (HQ), sp gr 1.19 and 20 mL of water. Drop in a small piece of litmus paper, add ammonium hydroxide (NH4OH) until slightly alkaline, then add HC1 until just acid, and then 3 mL more of HC1. 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 solution shows a brown tinge after standing 1 min. Do not allow the temperature of the solution to fall below 70C during the titration. Run a blink using the same amounts of reagents and water as in the standardization. The standard ization must be made under the same conditions oftemper ature, volume, and acidity as obtained when the sample is titrated. Calculate the strength of the K4pe(CN)6 solution in terms of grams of zinc as follows: Z=W/(V,-B) (1) where: Z = zinc equivalent of the KJFeCCN),; solution, g/mL, W = zinc used (or equivalent to the ZnO used), g, Vl = IQFefCNJe solution required for titration of the standard, mL, and B = K4Fe(CN)6 solution required for titration of the blank, mL. II. 2 Uranyl Nitrate Indicator Solution--Dissolve 5 g of uranyl nitrate (tJ02(N03)2 6H20) in 100' mL of water. 12. Procedure 12.1 Transfer 0.25 g of the sample to a 400-mL beaker, moisten with alcohol, and dissolve in 10 mL of HQ (sp gr 1.19) and 20 mL of water. 12.2 Continue with the procedure used in standardizing the JCtFefCNlg solution as described in 10.1, beginning with the addition of the litmus paper and the adjustment of the acidity with NH4OH and HC1. 12.3 Calculation--Calculate the percent of total zinc, T, as follows: T=[(V2- B2)Z/S,} x 100 (2) where: V2 = K4Fe(CN)6 solution required for titration of the specimen, mL, 13. Reagents 13.1 Ferric Chloride Solution--Prepare a solution con taining 20 g of ferric chloride (FeCl3-6H.20) and 20 mL of' 20 % sodium acetate (NaC2H302) solution per 100 mL. It is advisable to make up only one day's supply at a time (50 mL are required for each determination). 13.2 Potassium Permanganate, Standard Solution (0.1 N, 1 mL *= 0.008 g Ti02)--Dissolve 3.16 g of KMn04 in water and dilute to 1 L. Let stand 8 to 14 days, siphon off-the clear solution (or filter through a medium porosity fritted disk),, and standardize against the National Institute of Standards and Technology (NIST) standard chemical No. 40 of sodium oxalate (Na^O,,) as follows: In a 400-mL beaker dissolved 0.2500 to 0.3000 g ofthe NIST sodium oxalate in 250 mL of hot water (80 to 90Q and add 15 mL of 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 solution shall not be below 60C by the time the end point has been reached. (More rapid cooling may be pre vented by allowing the beaker to stand on a small hot plate during the titration. The use of a small nonmercury type thermometer as a stirring rod is most convenient.) Keep the KMn04 solution in a glass-stoppered bottle painted black to keep out light, or in a brown glass bottle stored in a dark place. 13.3 Sodium Acetate Solution (200 g/L)--Dissolve 200 g ofiodium acetate (NaQHjO^ or 332 g of NaC2H302 3H20, in water and dilute to 1 L. 13.4 Zimmerman-Reinkardt Solution--Prepare a solu tion containing 67 g of manganese sulfate (MnSO4-4H20) 130 mL of H2S04 (p gr 1.84), and 138 mL of phosphoric acid (#i3P04) (85 %) per L. 14. Procedure 14.1 Weigh 0.2 g of the sample, transfer immediately to a dry, 600-mL heavy-wall Erlenmeyer flask, and add 50 mL of the FeCl3 solution. Tightly stopper the flask and agitate constantly for approximately 15 min. As soon as the zinc dust is all dissolved, add 50 mL of the ZimmermanReinhardt solution and 250 mL of water. Titrate with 0.1 N KMn04 solution. 'Wilson, L. A., "The Evaluation of Zinc Dust: A Proposed Method of Analysis," Proceedings, ASTEA, Am, Soc. Testing and Mats., Vol IS, Part II, 1918. p. 220. 112 it < | \y ' i <" I ! * 4 1 ' i , ^ rl iji (; l/j, ' 1 I* jf ` V ] DUP050296635 p--If preferred, the redueed iron may be titrated with 0.1 N g.dichromate (K2Cr207) solution, using sodium diphenylamine lin the presence of phosphoric acid (H3P04) as an internal |f : |iblank--Make a blank determination, following the rocedure and using the same amounts of all reagents Ufithe titration. (The blank is usually 0.1 to 0.2 mL of i04 solution.) 'alculation--Calculate the percent of metallic zinc, iws: If Af=[(K3- B3)(N . 0.0327J/SJ X 100 (3) life.- r.. p KMn04 solution required for titration of the spec if- imen, mL, | = KMn04 solution required for titration of the I blank, mL, = normality of the KMn04 solution, l = sample used, g, and |27 = milliequivalent weight of Zn. ZINC OXIDE Calculation 5.1 Calculate the percent of zinc oxide (ZnO), Z, as allows: Z = (A - C) X 1.2447 (4) tsre: jMotal zinc, % (Section 10), and ^ metallic zinc, % (Section 12). CALCIUM Reagents 16.1 Ammonium Oxalate, Saturated Solution--Mix 50 g fammonium oxalate and 1 L of water. 16.2 Ammonium Oxalate Solution (10 g/L)--Dissolve 10 (ammonium oxalate in water and dilute to 1 L. p6.3 Potassium Permanganate, Standard Solution (0.1 -See 13.2. |. Procedure |p7.1 Transfer 10 g of the sample, weighed to 0.1 g, to a 1-mL beaker. Dissolve in 30 mL of HQ (1+1), keeping the faker covered. Dilute to 200 mL. The solution at this point hould be clear and transparent. Neutralize with NH4OH. Some zinc, because ofits high concentration, will precipitate as hydroxide at this point.) Add NH4OH (sp gr 0.90) f jji'dropwise, stirring until die solution becomes clear. Heat r nearly to boiling and add 75 mL of saturated ammonium S 11;ovalate solution. Boil until the precipitate assumes a dense crystalline appearance. Allow to settle on a steam bath for 20 inin and then cool. Filter on close-grained paper and wash live times with a cold ammonium oxalate solution (10 g/L). If 17.2 Carefully dissolve the precipitate from the filter |paper, using alternately hot HC1 (1+3) and hot water. Catch in a clean 400-mL beaker, dilute (if necessary) to a volume of PTlfbout 250 mL, and add 25 mL of saturated ammonium * 1? 10KoIthoff, 1. M. and Sandell, E. B., Textbook of Quantitative Inorganic Analysis, 1945, p. 608. oxalate solution. Bring to a boil, and add NH4OH in slight excess. Boil until the precipitate becomes crystalline and dense. Let stand 1 h on a steam bath. Allow to cool. Filter and wash with small amounts of hot water until all ammo nium oxalate is removed. 17.3 Remove the paper from the funnel and spread it out on the inside of a 600-mL beaker above 300 mL of warm water to which has been added 20 mL of H2S04 (1+1). Rinse the precipitate off the paper with water from a wash bottle and warm the solution to 80C. Titrate at this temperature with KMn04 solution. As soon as a persistent pink end point is obtained, drop the paper into the liquid, rinse the side of the beaker, and quickly complete the titration. 17.4 Calculation--Calculate the percent of calcium, C, as CaO, as follows: C = [( VaN x o 2804)/S3] x 100 (5) where: V4 = KMn04 solution required for titration of the sample, mL, N = normality of the KMn04 solution, and S3 -- specimen used, g. LEAD 18. Procedure 18.1 Determine the lead content in accordance with Section 6 of Test Methods E 40. 3--Lead may also be determined in accordance with Test Method E68. ' IRON 19. Procedure 19.1 Determine the iron content in accordance with Section 22 of Test Method E 40. CADMIUM 20. Procedure 20.1 Determine the cadmium content in accordance with 18.1 and 18.3 of Test Method E 40. 4--Cadmium may also be determined in accordance with Test Method E 68. CHLORINE 21. Reagents 21.1 Silver Nitrate Solution (3.5 g/L)--Dissolve 3.5 g of silver nitrate (AgN03) in water and dilute to 1 L. 21.2 Sodium Chloride, Standard Solution (0.01 N)-- Dissolve 0.5850 g of pure sodium chloride (NaCl) in water and dilute to 1 L. 22. Procedure 22.1 Transfer 1.000 g of the sample to a 200-mL electro lytic beaker. Add 20 mL of water and then cautiously add 5 mL of nitric acid (HN03) (sp gr 1.42). Cover with a watch glass and heat on a steam bath with frequent stirring for 5 min, or until a dear solution results. Add 70 mL of water and cool to room temperature. 22.2 To the specimen and to a blank (prepared in similar fashion) add 5.0 mL ofAgN03 solution (3.5 g/L) and stir. To f DUP05Q296636 D 521 the blank, add dropwise from a 10-mL buret, with thorough mixing, enough NaCl solution to develop a turbidity matching that of the sample. Keep the contents of both beakers well stirred and view against a black background in equal illumination. ., 22.3 Calculation--Calculate the percept of chlorine, C, as follows: C = 0.035 V} (6) where Vs - 0.01 iVNaQ solution .added to the blank, mL.. 'SULFUR ' 23. Reagents *< 23.1 Barium Chloride Solution {\00 g/L)--Dissolve 117 g of barium chloride (BaCl2-2H20) in water and dilute to l L. 23.2 Bromine Water (saturated). 24, Procedure 24.1 Transfer 20 g ofthe specimen, weighed to the nearest 0.1 g, to a 600-mL beaker. Cover the sample with 50 mL of saturated bromine water and then cautiously add HN03 (sp gr 1.42) until solution is complete. 24.2 Add 1 g of anhydrous sodium carbonate (Na2C03) and boil down until salts just begin to separate, then add 75 mL of HC1 (sp gr 1.19) and again boil down until salts begin to separate. Repeat this operation and,'finally,'dilute to 100 mL, heat until solution is complete, and filter into a 400-mL beaker through close-texture paper. 24.3 Wash the paper with hot water, make the filtrate* alkaline with NH4OH, and then just acid with HC1. Heat to boiling and hold at boiling temperature at least 5 to 10^nnni to drive out C02 then slowly add with stirring 5 mL ofBaQaf solution. Allow to stand at least 5 h (preferably overnight).-1 24.4 Filter on a weighed Gooch crucible, wash free from - chlorides!with hot water, dry, and ignite carefully at 900"C. Cool and weigh. The difference between the original and/! final weight is BaSQ4. , , ? 24.5 Blank--!Make a blank deterfnination, following the; same procedure and using the same amounts of all reagents. 24.6 Calculation--Calculate the percent of sulfur, S, as (I follows: S = [tF, - B,,) X 0.1374)/S4J X 100" (7) ;; where: , :r W1 =BaS04, g, B4 = correction for blank, g, . S4 = sample used, g, and 0.1374 = S/BaS04 = 32.06/233.42. 25. Keywords 25.1 calcium; chlorine; potassium ferrocyanide; zinc dust; ` zinc powder : TheAmerican Society for Testing andMaterials,takes no position respecting the validity ofanypatent rights asserted in connection wifh any item mentioned in this standard. Users oithls stendard are expressly advised that determination of the valldity 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 andmust be reviewed every five years and Itnotrevised, either reapprovedor withdrawn. Your comments are invitedeither for revision ofthis standard or for additionalstandards and should be addressed to ASTM Heedquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you they attend, if you feel that your comments have not received a fair hearing you should make your viaws known to the ASTM Committee on Standards! 1916 Race SL, Philadelphia, PA 19103. I "''`'..MW- DUP050296637 r Designation: 0 561 - 82 (Reapproved 1989) Sir*Hi n Si" Standard Specification for Carbon Black Pigment for Paint1 This standard is issued under the fixed designation D 561; 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. f This specification covers the pigment commercially i' as carbon black, which is suitable for use in the jnfocture ofprotective or decorative coatings. P need Documents USTM Standards: Test Method for Solvent-Extractable Material in tCkPignients? ' ' ' P'Tesf Method for Color and Strength of Color Pig* |fents with a Mechanical Mullei*2i, S06! Test Method for Carbon Black--Ash Content3 109 Test Method for Carbon Black--Heating Loss3 If5l4 Test Method for Carbon Black--Sieve Residue3 Composition and Properties Sjhe pigment shall be made by burning natural gas i| I) or oil (Type ill), in such a. manner as to, fprm a jgjirof carbon. It shall be free of adulterants and be in the f of-powder r. dustless pellets and shall conform to the iltrements specified in Table 1, . ' I'M The mass color and character of the tint and tinting (ength formed by a mixture with a white pigment shall be jjjjithin mutually agreed upon limits of a standard acceptable Ijaboth the purchaser and the seller when tested in accord- " cepwith Test Method D 387,' '- ViuiB 1--For the tinting strength test a ratio of 100 parts of white to JEsbnt of black is usually suitable. , IV. T( specification, is under thejurisdiction of ASTM Committee D-l on Paint ffi Reiated Coatings and Materials and is the direct responsibility of Subcomrtittoc f)01.31 on Pigment Specifications. * Current edition approved Oct 29, 1982. Published February 1983. Originally ; Stfj-ublished asD5Si -40. Last previous edition D56I -77. i, 2 Annual Book ofASTM Standards, Vol 06.02. Annual Book ofASTM Standards, Voi'09.0). .4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a, shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10' 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples stall be taken; 4.2 At . the option of the purchaser, the samples may be tested separately or, after blending the samples from the . same production unit in equal quantities, tested as a com posite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not.covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Solvent Extractable Material--Test Method D 305. 5.1.2 Color and Tinting Strength--Test Method D 387. 5.1.3 Carbon Black--Ash Content--Test Method D 1506. 5.1.4 Heating Loss--Test Method D 1509. 5.1.5 Sieve Residue--Test Method D 1514. TABLE 1 Composition and Properties Typel Type II ASTty Test Method Ash, max, * Acetone extract, max, % Moisture (toss at 105C) max, % Coarse particles (totalpgsrdue / retained op.45-jipv (No. 325) screen, max), % Organic dyes 0.2* 0.5* 8.0 0.2 ! 1.0* 1.0* 8.5'-- 02 . D1506 " D305 DM09 ~ .; D.1514 none none - 050 * When mutually agreed upon by die pirrchaser'and the seller, higher maximum ash and acetone extract values may be allowed if final product requirements necessitate the use of additional treating agents. u It may be necessary for the purchaser and the seller to agree upon a higher maximum moisture content in higlvcolor black. Higivccilor blacks are very hygroscopic and should be protected against moisture during storage. TheAmerican Society for Testing and Materials takes no position respecting the validity ot anypatent rights asserted In connection with any Item mentioned th 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 reepproved 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, 1318 Race St., Philadelphia, PA 19103. DUP050296638 # D 563 ed, using the alcohol-benzene wash solution for ing the precipitate and washing the reaction flask. |the precipitate with successive portions of alcohol;e wash solution until a few millilitres of washings :ed in a second suction flask are no longer alkaline to ijpbthalein. (Normally about 75 mL of wash solution is desired, proceed as follows: Dissolve the weighed precipi tate in about 50 mL of distilled water that has been neutralized to phenolphthalein. Add 3 to 4 drops of phenolphthalein indicator solution, and if the solution is alkaline, titrate with 0.1 N HC1. icient.) Do not allow air to be drawn through the as they are hygroscopic. Finally pour 2S4nL of ether ie crucible and draw through the precipitate with the suction. Wipe the outer surface of the crucible with a clean Ifead place in a gravity convection oven at 60C for 1 h 3). Cool to room temperature in a desiccator, and 7. Calculation 7.1 Calculate the percent of phthalic anhydride A in the specimen as follows: 0.1382 A = [((/'- K) x 0.5136)/$] X 100 where: *8 *3--The precipitate is the alcoholate (C6H4(COOH)2 KOH)), and the alcohol of crystallization will be slowly driven off "ploaged heating. It is safe, however, to dry the alcoholate at jumperstores up to 60'C for as long as 1 h. K =. correction for K2C03 (if determined), g, V - HCI used for titration (see 6.5), mL, N = normality of HQ, P = potassium alcohol phthalate (see 6.5), g, and S = specimen used, g. ^i' Correction for Carbonates--Coprecipitation of potas- | carbonate (K2C03) with the' potassium alcohol 5 may be a source ofe'rror. Ifa correction for K2C03 8. Precision and Bias 8.1 Precision and bias are being determined. tt I! The American Society for Testing end Materials fates no position respecting the validity of anypatent rights assertedIn 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. ?.i' ' ' Tits standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and It notrevised, eitherreapprgved or withdrawn. Yourcomments are Invited ethertorrevision of thisstandard orforadditionalstandards and should be addressed to ASJM Headquarters. Your comments will receive caretul 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. 117 DUP050296639 Designation: D 602 - 81 (Reapproved 1991}1 Standard Specification for Barium Sulfate Pigments1 This standard is issued under the fixed designation D 602; the number immediately following the designation indicates (he year of original adoption or, in the case ofrevision, the year of last 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. !"#$il --Keywords were added editorially in July 1991. iisf 1. Scope 1.1 This specification covers the barium sulfate pigments commercially known as barytes and blanc fixe. 2. Referenced Documents 2.1 ASTM Standards: D 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments3 D715 Test Methods for Analysis of Barium Sulfate Pigment3 D1208 Test Methods for Common Properties of Certain Pigments3 , 3. Composition and Properties 3.1 The pigment shall consist of barium sulfate (BaS04) without any admixture of other materials in the case ofblanc fixe, and without any admixture of other materials not naturally occurring in the barite ore in the case of barytes, and which conform to the following requirements: Barytes Blanc Fixe Barium sulfate, min, % Ferric oxide, max, % pH, min 94 0.05 3.5 97 0.02 3.5 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materialstand is the direct responsibility of Subcom mittee DO1.31 on Pigment Specifications. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 602 - 41 T. Last previous edition D 602 - 42 (1975). 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 5 Annual Book ofASTM Standards, Vol 06.02. Barytes Blanc Fixe Matter soluble in water, max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on No. 325 (45-pm sieve), max, % Free silica (quartz, clays, or other foreign mate rials), max, % .0.2 0.5 0.5 2.0 0.2 0.5 0.5 2.0 . 3.2 In such physical properties as are specified by the purchaser, the pigment shall, satisfactorily match a reference 1 sample mutually agreed upon by the purchaser and the :j seller. 1 4. Sampling .I 4.1 Two samples shall be taken at random from different I packages from each lot, batch, day's pack, or other unit of I production in a shipment. When no markings distinguishing 1 between units of production appear, samples shall be taken I from different packages in the ratio of two samples of each | 10 000 lb (5000 kg), except that for shipments of less than ..i 10 000 lb two samples shall be taken. At the option of the 1 purchaser, the samples may be tested-separately or after j blending in equal quantities the samples from the same f production unit to form a composite sample. i 5. Test Methods -- ; 5.1 Tests shall be conducted in accordance with the ! following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. ~ 5.2 Coarse-Particles in Pigment--Test Methods D 185. 53 Moisture--Test Methods D 280. 5.4 Barium Sulfate, Ferric Oxide, and Free Silica--Test Methods D 715. 5.5 Hydrogen Ion Concentration and Matter Soluble in Water--Test Methods D 1208. 6. Keywords 6.1 barium sulfate; barytes; blanc fixe; pigments The Ameriosn 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 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, it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, t91B Race St,, Philadelphia, PA 19103. 118 DU P050296640 Designation: D 603 - 66 (Reapproved 1989) Standard Specification for Aluminum Silicate Pigments (Hydrous)1 This standard is issued under the fixed designation D 603; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearof Iasi revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval; ' ' pcope Jl This specification covers the white pigments that gsist substantially of natural hydrous aluminum silicate12 ithe 1:1 layer type), and are restricted to those minerals jjch conform to die chemical limits prescribed herein and |ch can be suitably processed to what is commercially i as paint pigment quality. I Referenced Documents !.l ASTM Standards: Test Method for Oil Absorption of Pigments by Spatula Rub-Out3 Method for Particle-Size Analysis of Soils4 ID 718 Test Methods for Analysis of Aluminum Silicate r Pigment3 D1208 Test Methods for Common Properties of Certain Pigments3 D1483 Test Method fbr Oil Absorption of Pigments by Gardner-Coleman Method3 D 2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment3 :E 70 Test Method for pH of Aqueous Solution with the Glass Electrode5 |. Composition of Properties , 3.1 Preparation--The pigment shall be made by grinding, Silling, washing, purifying size-fractionating, or otherwise irocessing, natural hydrous aluminum silicates, and shall conform to the composition requirements (weight percent) liven in Table 1. 3.2 pH--The pH of a water slurry ofthe pigment shall be ) within a range as agreed upon between the purchaser and the teller. 3.3 Water-Soluble Matter--,sThe water-soluble matter `shall be not more than 0.50 %. 3.4 Wet-Sieve Residue--The pigment shall contain no * more than 0.5 % wet-sieve residue retained on a 45-jrm (No, 325) sieve ("grit" or "coarse particles'1) except as may be agreed upon by the purchaser and the seller. 3.5 Color--The color (brightness, reflectance) shall con- 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint , tnd Related Coatings and Materials and is the direct responsibility of Subcom|-*f mittee D0I.31 on Pigment Specifications. Current edition approved Sept. 20, 1966. Originally issued 1941. Replaces |D603 - 42 (1955). 2 Synonymous terms are china clay and kaolinite. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 04.08. 5 Annual Book ofASTM Standards, Vol 15.05, TABLE 1 Pigment Composition Requirements AiumiriUm oxide, A1203, % Silicon dioxide. Si02, Si Iron oxide, Fe203, % Titanium dioxides'TlOj, 5S Calcium oxide, CaO, % Sodium oxide, Na^, % . Potassium oxide, K20, % Other oxides, % Free moisture (10SC), % Loss on ignition (1000C), % Ideal 39.50 46, ,5.4 1356 Typical 38.8 45.4 0.3 1.5 0.1 0.1 0.1 trace .. 13.8 Range 37 to A2a 48 tO`43B v.. A Permitting up to 5 % 8 Permitting up to 5 % AI3O3. for example as allophane. SIO:, ter example as quartz. Max 0.5 2.0 0.2 0.3 2.0 0.1 1.0 15.0 form to the following requirements: 3.5.1 The color shall be equal, within agreed upon toler ances, to that of a reference standard agreed upon between the purchaser and the seller, or 3.5.2 The color shall be not less than a guaranteed minimum expressed as percent reflectance of standard iUuminant C at 457 nm compared to a freshly smoked standard magnesium oxide surface by means of an accepted integrating sphere reflectance spectrophotometer6 or a monochromatic reflectance meter,6 or 3.5.3 The color shall be specified by actual determination of dominant wavelength, hue, and spectral efficiency as can be calculated from the tristimulus integration of the reflec tance curve. 3.6 Oil Absorption--The oil absorption shall be equal, within agreed upon tolerances, to that of a reference standard agreed upon between the purchaser and the seller. 3.7 Aluminum., silicate pigments may be furnished in several types or grades whose various properties are de pendent in part on average size or particle size, distribution about the average, or both. The particle size shall be equal within agreed upon tolerances to that of a reference standard agreed upon between the purchaser and the seller. 4. Number of Tests 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after 6 The General Electric Reflectance Spectrophotometer and the General Electric Reflectanoe Meter, respectively, have been found satisfactory for this puipose. 119 DUP050296641 production unit to form a composite sample. S. Test Methods 5.1 Tests shall be conducted in accordance with The appropriate ASTM test methods, where applicable. Test procedures not covered by ASTM: test methods shall be agreed upon between the purchaser and the seller, except as . follows: 5.1.1 Hydrogen Jon Concentration (pH)--Prepare a 5.1.3 Coarse Particle*--Test Methods D 718. 5.1.4 Oil Absorption--Test Method D 281 or D 1483. 5.1.5 Particle Size Distribution--Method D 422. 5.1.6 Chemical Analysis--Test Method D 718. The American Society for Testing andMaterials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned In thisstandard. Users of this standard are expressly advised that determination of the validity of anysuch patent rights, and the risk of Infringement of such rightst 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 . Ifnotrevised, either reapproved or withdrawn. Yourcomments are Invited either for revision ofthis standard or foradditionalstandards 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, 1916 Pace St., Philadelphia, PA 19103. t 120 DUP050296642 Designation: D 604 - 81 (Reapproved 1989) Standard Specification for Diatomaceous Silica Pigment1 This standard is issued under the fixed designation D 604; 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 last revision or reapprovaL iallllpfiis specification covers two types of diatomaceous ifegments for use in paints: , Jy Type A--Standard fineness for general paint use. Hff',2 Type B--Extra fine, for special uses. 1--Silica pigments originating from crystalline rocks or sands jjenot covered by this,specification. JffiSjfoTE 2--For additional information, see Test Methods D 719. ;r . iferenced Documents 1 ASTM Standards: JS&5 Test Methods for Coarse Particles in Pigments, Pastes, and Paints*2 5719 Test Methods for Analysis of Diatomaceous Silica Pigment3 H208 Test Methods for Common Properties of Certain igments3 Composition and Properties |.l The pigment shall be a diatomaceous silica especially . duced by chemical, heat, and grading processes, and |cted for use in paints and shall conform to the following tturements: * This specification is under the jurisdiction of ASTM Committee D-l on Faint ^Related Coatings and Materials and is the direct responsibility of Subcom- |fteh D0l.3l on Figment Specifications. - Current edition approved Oct 30,1981. Published December 1981. Originally bed as D 604 - 41 T. Last previous edition D 604 - 42 (1975). 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. f ' 1Annual Book ofASTM Standards, Vol 06.02. Loss on ignition, max., % Matter soluble in HQ (14-2), max, % Moisture and other volatile matter, max, % Volume of settled pigment in petroleum spirits after 1 h, min, mL: Type A Type B Coarse particles (total residue retained on a 45-pm (No. 325) sieve), %: Type A Type B 1.0 3.0 1.0 35 25 5.0 to 15.0 f.O max 3.2 The color shall be within mutually agreed upon limits of a reference sample acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb. two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after^ blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Test shall be conducted in accordance with the following ASTM test methods, where applicable. Test proce dures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.2 Coarse Particles--Test Methods D185. . 5.3 Loss on Ignition and Moisture--Test Methods D1208. ..._ fci The American Society tor Testing and Materials takes no position respecting the validity ofanypatent rights asserted In connexion, with any Item mentioned In this standard. Users ofthis standard are expressly advised that determination ol the validity of any sitoh 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 ofthis standardor 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 Hace St., Philadelphia, PA 19103. 121 DU P0502 96643 Designation: D 605 - 82 (Reapproved 1989) Standard Specification for Magnesium Silicate Pigment (Talc)1 This standard, is issued under the fixed designation D 605; 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 (i) indicates an editorial change since the last revision or reapproval . : This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Fed. Spec. TT-P-403A. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 3.2 Color--The color shall be equal, within agreed upoi 1.1 This specification covers pigments that Consist sub stantially of natural hydrous magnesium silicate, and is restricted to those minerals that, conform to the chemical limits prescribed herein and can be suitably processed to what is commercially known as paint pigment quality. 1.2 The following hazard caveat applies to the test method portion of this specification only! This standard may involve Hazardous materials, operations, and equipment. This standard does not purport to address all of the Safety problems associated with its use. It is the responsibility ofthe user of this standard to, establish appropriate safety and healthpractices and determine the applicability ofregulatory lirrtitations prior, to use. tolerances, to . that of a reference ; sample agreed upoi between the purchaser and the seller. 3.3 Coarse Particles--The pigment shall contain no mor than 2 % of coarse particles, retained on-'a 4S-pm (Not 325 sieve except as may be agreed upon between the purchase and the seller. 3.4 Water-Soluble Matter--The pigment shall contain n> more than 1 % water-soluble matter except as may be agreei upon between the purchaser and the seller. 3.5 Oil. Absorption--The oil absorption shall be equa within agreed upon tolerances, to that of a reference sampl agreed upon between the purchaser, and the seller. - 3.6 Consistency--When Consistency is included ip th purchaser's specification, it shall be , equal, within Igree 2. Referenced'Documents upon tolerances, to that of a reference sample agreed upo 2.1 ASTMStandards: -5 *. D280 Test Methods for Hygroscopic Moisture (and Other- . Matter Volatile Under the Test Conditions) in Pigments2 D281 Test Method for Oil Absorption of Pigments aby- between the purchaser and the seller. 3.7 Fineness--The paint fineness shall be equal, withi agreed upon tolerances, to that of a reference Sample agree upon between the purchaser and the seller. Spatula Rub-Out2' 4. Sampling D 562 Test Method for Consistency of Paints Using the Stormer Viscometer3 D7I7 Test Methods for Analysis of Magnesium Silicate Pigment2 D1208 Test Methods for Common Properties of Certain 4.1 Two samples shall be taken at random from differet packages from each lot, batch, day's pack, or other unit c production in a shipment. When no markings distinguish^ between, units of production appear, samples shall be take Pigments2 ' ' ' ' D1210 Test Method'fqr Fineness of Dispersion of Pig from different packages in the ratio of two samples for ,eac 10000 lb (5000 kg); except that for shipments of less tha ifii-ir ment-Vehicle Systems3 It: 3. Composition and Properties 10 000 lb, two' samples shall be -taken. At die option of th purchaser, the samples may be tested separately or aftf blending in equal quantities, the samples from the sarr f! 3.1 The pigment shall be made by grinding or otherwise, production unit form a composite sample. processing natural, hydrous magnesium silicate aad shall 5: Test Methods conform to the following requirements: Weight % 5.1 Tests, shall, be conducted in accordance with tl following ASTM,test methods, where applicable. Test proa nun dures not covered by ASTM test methods'shall be mutual! Combined magnesium and calcium sili cates (MgO plus Si02 plus CaO) Calcium oxide (CaO) 88 agreed upon between the purchaser and' the seller. 5.1.1 Color, Composition, and Coarse Particles--Te Aluminum and iron oxides (R203) Methods D 717. Loss on ignition Moisture and other volatile material 5.1.2 Water-Soluble Matter and Loss on Ignition--Te Methods D 1208. 5.1.3 Oil Absorption---Jest Method D281. 1 This specification is under thejurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom- 5.1.4 Consistency--Use the pigment to prepare a mixtu: according to the following directions: Weigh 78 g of petn leum spirits and 80 g of linseed oil (viscosity, 21 to 24 P; ac number, 4 to 8) into a pint can and thoroughly mix with spatula. Weigh in 160 g of magnesium silicate and stir with spatula to wet all lumps. Stir with a motor-driven propelle DUP0502 96644  0 605 ter for 5 min at approximately 800 r/min. Weigh in pitional 180 g of linseed oil and stir an additional 2 min he electric stirrer. Determine the consistency in accordf&Jce with Test Method D 562. 5.1.5 Fineness--Test Method D 1210. The test mixture may be the same as that used for the consistency test. 5.1.6 Moisture--Test Methods D 280. The American Society lor Testing and Materials takes no position respecting the validity of anypatent rights asserted In connection with any item mentioned.ln this standard. Users of this standard-are expressly advised that detarmlnatlonof the validity of any such patent rights, and the risk of Infringement ofsuchrights, are entirely their own responsibility. This standardJS subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Your comments are Invited either forrevision ofthis standardor for.additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting cf 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., PhUadelphle, PA 19103. Tv-fe. DUP050296645 Designation: D 607 - 82 (Reapproved 1987}61 Standard Specification for Wet Ground Mica Pigments1 This standard is issued under the fixed designation D 607; 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 qfthe Department of Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year cfissue which has been adopted by the Department ofDefense. *' Nora--Paragraph 4.1 was changed editorially in May 1987. 1. Scope 1.1 This specification covers two types of finely divided muscovite mica, commercially known as wet ground mica, suitable for use in the manufacture of protective coatings. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under Test Conditions) in Pigment3 D716 Test Methods for Evaluating Mica Pigment3 D1208 Test Methods for Common Properties of Certain Pigments3 3. Composition and Properties 3.1 The pigments shall be made by wet grinding musco vite mica and shall conform to the requirements for proper ties prescribed as follows: Types A Regular 326 M Grade B Fine Grade Apparent density, max, lb/ft3 (g/cm5) 12.0 (0.2) 12.0 (0.2) 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved June 25, 1982. Published August 1982. Originally published as O 106 - 41 T. Last previous edition D 106 - 75. 2 Annual Book ofASTM Standards, Vois 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. Types A Regular 325 M Grade B Fine Grade i Moisture and other volatile matter, max, weight % Grit, max, weight % Coarse particles, max, weight %\ Total residue retained on a No. 140 (106-gm) sieve Total residue retained on a No. 325 (45-itm) sieve Ignition loss, max, weight % (dry basis) 0.5 0.5 0.1 12.0 5.0 0.5 0.5 0.01 3.0 5.0 3.2 The color shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different j packages from each lot, batch, day's pack, or other unit of j production in a shipment. When no markings distinguishing ! between units of production appear; samples shall be taken st from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite_sample. _ 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM methods. Test procedures not covered by ASTM methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Apparent Density--Test Method D 716. 5.1.2 Moisture--Test Method D 280. 5.1.3 Grit--Test Method D 716. 5.1.4 Coarse Particles--Test Method D 185. 5.1.5 Ignition Loss--Test Method D 1208. The American Society for Testing and Materials takes rto position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users ol this standard are expressly advised that determination of die validity of any such patent rights, and the risk ol 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 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, 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. 124 DUP050296646 Designation: D 656 - 87 Standard Specification for Pure Toluidine Red Toner1 This standard is issued' under the fixed designation D 6$6; 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 () indicates an editorial change since the last revision or reapproval.: This specification has been approvedfor use by agencies ofthe Department ofDefense to replace Fed. Spec. TT-P-455. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofisstie which has been adopted by the Department 6fDefense. Scope 1,1 This specification covers, the red pigment1 commeriy known as pure toluidine red toner. The pigment may i purchased in the dry form or as a paste in oil. Referenced Documents |il ASTM Standards; 5185 Test Methods for'Coarse Particles in Pigments, Pastes, and Paints2 . . 5280 Test Methods for Hygroscopic Moisture (arid Other Matter Volatile Under the Test- Conditions) in if--'Pigments3 If 387 Test Method for Color and Strength offColor ^Pigments with a Mechanical Muller3 97.0 Test- Methods for Pam Red and Toluidine Red Pigments3 | Composition and Properties 0.1 Dry Pigment--The pigment shall consist of toluidine Jdjtpner (l-(2-nitro-p-tolylazo)-2-naphthol) with or without &nixture witli a small quantity of (l-fS-nitro-p-methoxyJliehyl-a2o)-2-haphthol). It shall be free of any substrate and pfiail conform to the following requirements: ' ' ! *'this specification is under thti jurisdiction ofASTM Committee D-1 on Paint Sfo Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment-Specifications. , ^ " Current edition approved June 26, 1987. Published. August 1987, Originally Cfeuutilished as D 656 - 42 T. Last previous edition D 656-81. %Annual Book OfASTM Standards, Vqis 06.0 land 06.02. < 5 Annual Book ofASTM Slandanjs, Vpl 06.02. >i Ash, max, % Moisture and other volatile matter, max, % Coarse particles (total residue remined on a No. 325 (45-jtm) sieve), max, % ParanitranUine red Solubility in chioroform Resistance to acids and alkalis Identity test 1.0 1.0 1.0 none' complete to pass test to pass test 3;2 The mass color and character of the. tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4. F Two samples shall be taken at random from different packages from each lot, batch, day's pack, or Other uhit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound of SI), except that for shipments of less thaii 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, of after blending in equal quantities the samples-from the same production unit to form a composite sample. 5. Test Methods 5.1. Tests shall be conducted in accordance with the appropriate test methods. T.est procedures not covered by ASTM methods shall be mutually, agreed upon between the purchaser and the seller. 5.2 Coarse Particles--Test Methods D1;85.,, 5.3 Moisture-^-Test Methods 280. 5.4 Color and Tint--Test Method D 387. 5.5 Solubility--'test Methods D 970. 7 5.6, Identity---Test Methods 970. . . 5.7 v4s/i--Test Methods D 970. ` '~ , The American Society for Testing end Materials takes no position respecting the'validity otanypatent 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;ar6 entirely their own responsibility. ihiS 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 commentsare invitedeither for revision of thisstandard 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. 125 m DUP050296647 Designation: D 715 - 86 (Reapproved 1991)1 Standard Test Methods for Analysis of Barium Sulfate Pigment1 This standard is issued under the fixed designation D71S; the number immediately following the designatiop indicates the year of original adoption or, in the ease of revision, the year of last revision. A number in parentheses indicates the year oflast teapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. &')* --Keywords were added editorially in January 1991, and Specification E 832 replaced Specification D 1100. 1. Scope 1.1 These test methods cover the analysis of barium sulfate pigment. 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: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 D 1193 Specification for Reagent Water4 D 1208 Test Methods for Common Properties of Certain Pigments3 E 832 Specification for Laboratory Piter Papers5 3. Significance and Use 3.1 These test methods are used to determine the purity of barium sulfate and to determine the concentration bf known impurities. This information is useful to producers and users as an aid in the'manufacture of coatings. 4. Purity of Reagents 4.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications df 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 1 These test methods are under the jurisdiction of ASTM Committee DJ on Paint and Related Coatings and Materials and are the direct responsibility of Committee DO).21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Sept. 26,1986, Published November 1986, Originally published as D 715-43. Last previous edition D 715 - 75 (1981)*1. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vois 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 14.02. 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 Roan, D. Van Nostrand Co., Inc., New York, NY, and the "United Stales Pharmacopeia." accuracy of the determination. 4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. BARIUM SULFATE 5. Reagents 5.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH): 5.2 Ammonium Sulfate ((NH4)2S04). 5.3 Hydrochloric Acid (sp gr 1:19)--Concentrated hydro chloric acid (HC1). 5.4 Hydrochloric Acid (1+1)--Mix equal volumes of con centrated HQ (sp gr 1.19) and water. 5.5 Methyl Red Indicator Solution--Dissolve 0.2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol. 5.7 Sodium Carbonate Solution (30 g/L)--Dissolve 30 g of Na2C03 in water and dilute to 1 L. ' 6. Procedure 6.1 Weigh to 0.1 mg approximately 0.5 g of the sample into a platinum crucible, add 3 g of Na2C03, mix thoroughly, and fuse until the melt is clear. Allow the melt to cool and then leach in a platinum dish with hot water until it is entirely disintegrated. Filter on a close-texture paperiand wash thoroughly with hot Na2CD3 solution (30 g/L). 6.2 Transfer the filter paper containing the insoluble carbonates to_a 250-mL beaker and acidify with concentrated HC1 (sp gr 1.19). Wash the fusion crucible with HC1 (sp gr 1.19) so that no barium is lost. Boil the solution, filter into a 600-mL beaker, and wash well with water. Add methyl red indicator solution, and add NH4OH (sp gr 0.90) until the solution is slightly alkaline. Add 6 mL of HQ (1+1), and dilute to 300 mL. 6.3 Heat the solution to boiling, and add 5 g of (NH4)2S04 dissolved in 40 mL of water; If low-grade material is being analyzed, the (NH4)2S04 solution should be added drop by drop from a buret to minimize inclusion. If the barytes is a rather pure product (95 to 99 % Ba$04), this is not necessary, since the only nonvolatile constituents of the solution will be barium salts. Allow the precipitate of BaS04 to digest for 4 h or overnight, and filter through a close-texture paper. Wash the precipitate with as little cold water as possible (consistent with the purity of the precipi tate), ignite in an oxidizing atmosphere, and weigh as BaS04. 1 j j j 7. Calculation 7.1 Calculate the percent of BaS04 as follows: 126 mmmmpPRfglS I DUP050296648 It # D 715 BaS04, % = (P/S, ) x 100 BaSQ4, g, and = sample used, g. FERRIC OXIDE apparatus *ffl Colorimetric Apparatus- -Nessler type, or pther sim< 100-mL colorimetric tubes. Jpeagents ' K,1 Ammonium Thiocyanate Solution (76.1 g/L)--Disl|e 76 g of ammonium thiocyanate (NH,,CNS) in water M dilute to 1 L. m2 Iron, Standard Solution (100 mL = 0.00002 g Fe)-- |ite and divide a ferric solution of known iron content so jo obtain 0.4 mg of iron. Dilute the solution to 2 L with jFjjwter containing 200 mL of iron-free H2S04. 9.3 Potassium Permanganate Sohaion (0.1 g/L)--DisMve 0.1 g of potassium permanganate (KMn04) in water fid dilute to 1 L. 19.4 Standard Color Solution--Mix thoroughly 10 parts m volume of NH4CNS and 90 parts by volume of standard Bon solution (100 mL = 0.02 mg Fe). One hundred jpllilitres of the solution will thus contain 0.000018 mg of fe. d 9.5 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid p2so4). 9.6 Sulfuric Acid (1+1)--Carefully mix 1 volume of oncentrated H2S04 (sp gr 1.84) with 1 volume of water. 10. Procedure 110.1 Dissolve the soluble portion of a 1-g specimen in *2S04 (1+1), filter, and wash, keeping the volume of the iilution under 100 mL. Oxidize any iron present in the Bltrate by adding potassium permanganate (KMn04) until a jfaint pink color is obtained. Dilute the solution to 100 mL pnd pour into a buret graduated in 0.1-mL divisions. | 10.2 Pour 100 mL of the standard color solution into a llOO-mL colorimetric tube. Into a second colorimetric tube gfpour 10 mL of concentrated H2S04 (sp gr 1.84) and 10 mL pof NH4CNS, dilute to 60 or 70 mL and then add the test polution from the buret until the depth of color thus Iproduced on dilution to 100 mL exactly matches that of the iistandard. Record the number-of millilitres required. |11. Calculation I 11.1 Calculate the percent of Fe203 as follows: i Fe203, % = [(/ X 1.4298)/52] X 100 I where: I / = iron in standard, g, Fe2Q3 _ 159.694 Fe2 111.694: i S2 = sample used, g. HYDROGEN ION CONCENTRATION ` 12. Procedure 12.1 Determine the pH in accordance with Test Methods MATTER SOLUBLE IN WATER 13. Procedure 13.1 Determine the amount of water soluble material present in accordance with Test Methods D 1208. MOISTURE AND OTHER VOLATILE MATTER 14. Procedure 14.1 Determine the moisture and other volatile matter in accordance with Test Method D 280. COARSE PARTICLES (Total Residue Retained on No. 325 (45-ym) Sieve) 15. Procedure 15.1 Determine the coarse particles' in accordance with Test Methods D 185. FREE SILICA 16. Reagent 16.1 Heavy Liquid (sp gr 2.9)--Dissolve 4 parts by weight of potassium iodide (KI) in 6 parts of warm water, and add, while stirring constantly, 5 parts of mercuric iodide (Hgl2). Evaporate over a hot plate or gas flame, protected by screen cloth, until a light crystalline scum forms. Cool, and filter through heavy paper. The solution will be a clear, deep, amber color of about 3.2 specific gravity. All filter washings showing a yellow color should be saved and evaporated. Determine the 3.2 specific gravity accurately by means of a specific gravity bottle, and correct the solution to a specific gravity of 2.9 at room temperature by adding water. Prepare approximately 200 mL of the solution. 17. Procedure 17.1 Carefully weigh 10 g of the finely ground dry barium sulfate pigment and transfer to a carefully dried 125"-tnL clear glass separatory funnel of the long narrow type. Add 100 mL of the heavy liquid (sp gr 2.9), stopper, and shake well to liberate any air bubbles that might adhere to the particles, and also to break up all agglomerates. Set the separatory funnel aside and allow to stand in a perpendicular position for 2 h, or for a sufficient time for the particles to rise or sink. -' 17.2 Draw off the heavy particles through the stopcock into a beaker along with 75 mL of the liquid. Add 50 mL of fresh heavy liquid (sp gr 2.9) to the float particles and liquid remaining in the separatory funnel and repeat the procedure as described in 17.1. 17.3 Draw off the heavy particles along with:75 mL of the liquid and add to those drawn off in accordance with 17.1, leaving the float particles in the funnel. Wash the particles remaining in the funnel with fresh heavy liquid (sp gr 2.9), filter through a No. 2/0 paper (see Specification E 832), and wash free of solution with warm water. 17.4 Transfer the filter paper and silica to an ignition cup, dry, and ignite carefully in an electric furnace or over a flame to keep mechanical loss at a minimum. Weigh the floated material, and transfer to a tared platinum dish or crucible. Add 20 mL of hydrofluoric acid (HF) and 3 drops of H2S04 (1+1), evaporate to dryness, and ignite carefully to expel all w DUP050296649 D 715 fumes. Cool and weigh. The loss in weight represents the free silica in the floated material. 18. Calculation 18.1 Calculate the percent of free Si02 as follows: Free Si02, % = (A/S3) x 100 where: A = Si02, g,and S3 = sample used, g. 19. Precision and Bias 19.1 The precision and bias of these test methods has not been determined. 20. Keywords 20.1 analysis of pigment; barium sulfate; barium sulfate content; barium sulfate pigment; ferric oxide ip barium sulfate; free silica in barium sulfate | The American Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection 1 with any Item mentioned In this,standard. Users of this standard are expressly advised that determination of the validity of any such J patent rights, and the ri3k of Infringement o! such rights, are entirely thek 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. Veor 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 responslbte technical committee, which you may attend. It you feat that your comments have hot received a fair hearing you should make yeur ' vlewsknown to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.' \ DUP050296650 * Designation: D 716 - 86 (Reapproved 1991)i'i Standard Test Methods for Evaluating Mica Pigment1 This standard is issued under the fixed designation D 716; 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 (e) indicates an editorial change since the last revision or reappraval. +,-/0Keywords were added editorially in January 1991. Scope 1.1 These test methods cover the evaluation of mica _ment. 1.2 This standard does not purport to address dll of the ety problems associated with its use. It is the responsibility .the user ofthis standard to establish appropriate safety and fdlth practices and determine the applicability ofregulatory filiations prior to use. * f, Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2 D280 Test Methods for Hygroscopic Moisture (and'Other Matter; Volatile Under die Test Conditions) in Pig ments3 Ell Specification for WireiCloth Sieves for Testing Pur poses4 13. Significance and Use 3.1 These test methods are used to determine apparent density ofmica pigments and the grit level. This information is significant to the user of mica pigments for inclusion in coatings. . APPARENT DENSITY 4. Apparatus 4.1 Volumeter3--A Scott volumeter or similar apparatus modified as follows: The screen used shall conform to the requirements of a No. 40 (425-pm) sieve as prescribed in Specification Ell. The funnel below the screen shall be replaced by a conical funnel having a bottom opening 1 in. (25 mm) in diameter. It may be found necessary to replace the top glass baffle with one that is longer to ensure that all of the sifted mica is caught. * 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 DOi.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Sept. 26,1986. Published November 1986. Originally published as D 716- 43. Last previous edition D 7J6- 75<198I)*,< 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vo! 06.02. 4 Annual Book ofASTM Standards, Vol 14.0Z 5 The volumeter is no longer generally available. As of June 1986 only one supplier, Sargent Welch Co., Skokie, IL, was known. The device is Scott-Schaeffer and White Volumeter listed on p. 932 of Catalog No. 133 (1985-86). 5. Procedure 5.1 Transfer convenient quantities of the mica pigment to the funnel of the modified volumeter and brush the pigment through the screen with a camel-hair brush until the receiver is slightly more than full. Scrape off the excess and weigh the pigment. Care must be taken not to jar the apparatus during the procedure. 6. Calculation 6.1 Calculate the apparent density of the mica pigment and convert to pounds per cubic foot. 7. Report 711 Report the mean of three determinations as the apparent density of the mica pigment. 8. Reproducibility of Results 8.1 The mean of the three determinations should check within 5 %. MOISTURE AND OTHER VOLATILE MATTER 9. Procedure 9.1 Determine the moisture and other volatile matter in accordance with Test Methods D 280. GRIT -10. Apparatus 10.1 Beaker, 600-mL, low-form. * 10.2 Metal Tubing--An L-shape metal tube (Fig. 1) lA in. (6.4 mm) in outside diameter with a foot 1 ip. (25 mm) lH length. The foot of the tube shall be drilled to 0.173 in. (4.4 mm) (No. 17 drill) in inside diameter for a depth of 'A in. (12.7 mm). The tube shall be placed in the beaker with the long arm in the vertical position, and the foot of the L parallel to the bottom of the beaker and perpendicular to the radius of the bottom at a point such that there is about Vifi-iu. (1.5-mm) clearance between the tubing and both the bottom and side ofthe beaker. The center of the foot shall be placed 90 from the lip of the beaker. 11. Procedure 11.1 Transfer 10 g of the sample to the 600-mL beaker, add 100 mL of water, and swirl the beaker until the mica is dispersed. Insert the metal tubing into the beaker as de scribed in 10.2 and connect the upper end to a water faucet. Regulate the flow ofwater by a constant head to a rate of 800 mL/min over the lip of the beaker. When the eiutriation has 129 OUp05029665i Tube Drilled to 0.113'diom. Wo.riDrill)for in Depth FIG. 1 Grit Test Apparatus progressed so that the body ofthe water in the beaker is clear, stop the flow, and lower lie water level to prevent spilling. 11.2 Swirl the beaker again to bring the remaining mica pigment into suspension and repeat the elutriation procedure as described in 11.1 three times. After final clearing, decant part of the water, and filter the residue. Transfer the paper and residue to a weighed crucible, and ash slowly, cool, and weigh. 12. Calculation 12.1 Calculate the percent grit, G, as follows: G, % = [(A - B)/S] x 100 15. Procedure , 15.1 Compare pastes made byjrubbing a standard mica pigment and standard ^inc oxide, mutually agreed upon by the purchaser gndihe seller, in linseed oil with a similar pake using the sample to be tested. Rub 9 g of zinc oxide, and 3 g ofmica pigment on a glass plate with a glass muiler of rubber spatula to avoid staining, with 4 mL of bleached linseed oil. Spread the pastes adjacenfly on a clear glass plate and determine the color by viewing the spreadouts on the glass. 16. Precision and Bias 16.1 Insufficient data are available to develop acceptable precision and bias statements. The information presented in Section 8 (Reproducibility of Resiilts)'was obtained in j.943, apd no documentation is currently available. The informa tion will remain in Section 8. 17. Keywords 17.1 grit, detection in mica pigment; mica pigment, analysis of; pigment . The American Society for Testing and Materials takes no position respecting the validity of.any patent rights asserted fn 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 infrlngemsnt of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must bs reviewed every.liueyears and It notrevised, either reapprovedor withdrawn. Your commentsare invited either forrevision ofthfs standard orfor additional standards and should be addressed toASTM Headquarters. Your comments will receive carefaroonslderation 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. ,, map* 130 DUP050296652 Designation: D 717 - 86 (Reapproved 1991)'ei Standard Test Methods for Analysis of Magnesium Siiicate Pigment1 This standard is issued under the fixed designation D 717; 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 theulast revision or reapproval. 12345' fi Keywords were added editorially in January 1991. cope These test methods cover the analysis of magnesium ate pigment. 1 This standard does not purport to address the safety Jems associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety and ith practices and determine the applicability ofregulatory Motions prior to use. '- Referenced Documents ASTM Standards: t> 234 Specification for Raw Linseed Oil12 |D 280 Test Methods for Hygroscopic Moisture (and Other p Matter Volatile Under the Test.Conditions),in PigI' ments3 ' p718 Test Methods,jfpr Analysis of Aluminum Silicate |r 'Pigment3 . ; b 1193 Specification for Reagent Water4 * D1208 Test Methods for Common Properties of Certain P- Pigments3 D2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of , the Pigment3 ' E 97 Test Method for Directional Reflectance Factor, ... 45-degO-deg, of Opaque Specimens by Broad-Barn! ' Filter Refleptometry3 3. Significance and Use 3.1 These test methods may.be used to confirm the stated Sip2, CaO, and MgO content of magnesium silicate for quality control, ... -. 4, Purity of Reagents 4.1 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 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! .21 on Chemical Analysis ofPaints and Paint Materials. , Current edition approved April 25, 1986. Published June 1986. Originally published as D 717 - 43. Last previous edition D 717 - 73 (1979)'2. 3 Annual Book ofASTM Standards, Vol 06.03. 3 Annudl Book ofASTM Standards, Vol 06.02. 4 Annual-Book ofASTM Standards. Vols 06.03 and U .01. 3 Annual Pook qfASTM Standards, Vols 06.01 and. 14.02. 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. 4.2 Unless otherwise indicated* references to water shall be understood to mean Type II of Specification D 1193. 5. Apparatus 5.1 Platinum Crucible. 5.2 Electric Furnace, capable of 1200'C. SILICON DIOXIDE 6. Reagents 6.1 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 6.2 Hydrochloric Acid (1+20)--Mix 1 volume of concen trated hydrochloric acid (HC1, sp gr 1.19) with 20 volumes of water. 6.3 HydrofluoricAcid (48 %)--Concentrated hydrofluoric acid (HF). 6.4 Sodium Carbonate (Na2C03). 6.5 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04).; 7. Procedure 7.1 Transfer 1 g of the sample weighed to 0.1 mg, to a platinum crucible and fuse with 5 g of Nabobs'uii& Sw' entire contents of the crucible are in a molten state. Continue heating for 20 min. Keep a close-fitting platinumcover on the crucible during the fusion. When the fusion is complete, allow the crucible and contents to cool, and transfer to a 600-mL porcelain casserole containing 200 mL of water (Note 1). Boil until the melt is disintegrated. 6789 1--If, during the cooling period, the. crucible is partially immersed several times in cold water to chill the outer portions of the melt, the subsequent removal of the melt is facilitated. Do not allow the water to enter the Crucible while the contents are hot to avoid spattering. 7.2 Remove crucible and lid, being careful to scrub and rinse out any adhering particles ofthe melt. Carefully acidify the contents of the casserole with concentrated HC1 (sp gr 6 "Reagent Chemicals, American Chemical Society Specification," Am. Chem ical Sac., 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 Nostrasd Co., Inc., New York, NY, and the "United States Pharmacopeia." 131 D 717 1.19); introduce the HC1 in small portions, keeping a watch glass over the crucible to avoid loss by spattering. Add 30 mL of HC1 in excess and evaporate to dryness on a steam bath; take care to break up any crusts that form. When the material appears completely dry, and no odor of HC1 can be detected, remove the casserole from the steam bath, and allow to cool. 7.3 Wash down the sides of the casserole with 20 mL of HC1 (sp gr 1.19) and then with water. Repeat the evaporation as described in 7.2, then bake for 1 h in an oven at 105C. Cool the residue, drench with 25 mL of HC1 (sp gr 1.19), add 175 mL of water, and warm, while stirring, until all soluble salts are dissolved. Filter off the silica on a dose-texture paper, wash five times- with HC1 (1+20), wash five times with hot water, and reserve the filtrate for determination of other oxides (Section 9). , 7.4 Transfer the paper and washed silica to a clean platinum crucible, ignite, first gently until the filter paper is consumed, and then at 12C0"C for 20 min, cool, and weigh. Moisten the residue with water, add 5 drops of H2S04 (sp gr 1.84), and 15 mL of HF, Evaporate to dryness on a steam bath, heat gently until H2S04 has been expelled, and ignite at 1200C for 5 min. Cool and weigh. The loss in weight represents the Si02. 8. Calculation 8.1 Calculate the percent of silica as follows: Si02, % - (P/S) x 100 where: P -- Si02, g, and S = sample used, g. AMMONIUM HYDROXIDE GROUP (Alumina and Iron Oxide) 9. Reagents 9.1 Ammonium Chloride Solution (2 g/100 mL)--Dis solve 2 g of ammonium chloride (NH4C1) in 100 mL of water. 9.2 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). .9.3 Hydrochloric Acid (1+3)--Mix 1 volume of concen trated HQ (sp gr 1.19) with 3 volumes of water. 9.4 Methyl Red Indicator Solution--Dissolve 0,2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol. 9.5 Potassium Pyrosulfate (K2S2b7). 10. Procedure 10.1 If an appreciable residue remains after the treatment with HF in accordance with 7.4, fuse the residue with a small amount of K2S207 until it is dissolved. Leach the pyrosulfate. melt out ofthe crucible with water and combine the solution with the filtrate reserved in accordance with 7.3. 10.2 Using the methyl red indicator solution, neutralize the combined solutions from the silica determination with NH4OH and add an excess of 2 drops. Bring to a boil adding NH4OH 1 drop at a time if necessary to maintain a slight alkalinity. Allow the precipitate to settle (not more than 5 min) and filter. Wash four times with hot NH4Cl solution. 10.3 Set aside the filtrate and transfer the precipitate and filter paper to the same beaker in which the first precipitation was effected. Dissolve the precipitate with 40 mL of hot HC1 (1+3), dilute the solution to about 100 mL, and reprecipitate the hydroxides as described in 10.2., Filter and wash the precipitate four times with hot NH4C1. Combine the filtrate and washings with the filtrate set aside and reserve for the determination of CaO (Section 10). 10.4 Race the precipitate in a weighed platinum crucible, heat slowly until the papers are charred, and finally ignite to constant weight at 1050 to llOO'C with care to prevent reduction. Cool and weigh as R203 (aluminum and iron oxides). 11. Calculation 11.1 Calculate the percent of R203 as follows: R203, % = (P2/S) x 100 where: Pz = R203, g, and S = sample used, g. CALCIUM OXIDE 12. Reagents 12.1 Ammonium Hydroxide (1+1)--Mix l volume of concentrated NH4OH (sp gr 0.90) with 1 volume of water. 12.2 Ammonium Oxalate Solution--((NH^QCVH^O), saturated. 12.3 Ammonium Oxalate Solution (1 g/L)--Dilute 1.0 g of ammonium oxalate (CNH4)2C204'H20) in 1 L of water. 12.4 Hydrochloric Acid 11+3)--See 9.3. 12.5 Hydrochloric Acid (1+1)--Mix 1 volume of concen trated hydrochloric acid (HC1, sp gr 1.19) With 1 volume of water. ,, 12.6 Methyl Red Indicator Solution--See 9.4. 13. Procedure 13.1 Acidify the combined filtrates obtained in the precip itations ofthe ammonium hydroxide group (Section 10) with HQ and evaporate them to a volume of abgut 300 mL. Add 5 mL of HQ (1+1), a few drops of methyl red indicator solution, and 30 mL of warm ammonium oxalate solution (saturated). Heat the solution to 70 to 80C and add NH40H (1+1) dropwise while stirring, until the color changes from red to yellow. Allow the solution to stand without further heating for 1 h (no longer) with occasioiial stirring during the first 30 min. Filter and wash moderately with cold dilute ammonium oxalate solution. Reserve the filtrate and washings. 13.2 Transfer the precipitate and filter paper to the beaker in which the precipitate was effected. Dissolve the oxalate in 40 mL ofhot HQ (1+3) and macerate the filter paper. Dilute to 200 mL with water; add a few drops of methyl red indicator solution and 5 mL of ammonium oxalate solution (saturated). Heat the solution nearly to boiling, and precipi tate calcium oxalate again by neutralizing the acid solution with NH4OH as described in 13.1. Allow the solution to stand 1 to 2 h and wash as before. Combine the filtrate with that already obtained and reserve for the determination of MgO (Section 16). 13.3 Dry the precipitate in a weighed covered platinum crucible. Char the paper without inflaming, bum the carbon at as low a temperature as possible, and, finally, heat with the 132 UP050296654 # D 717 tightly covered in an electric furnace or over a blast at a temperature of 1100 to 1200C. Cool in a itor and weigh as CaO. Repeat the ignition to a it weight, ilculation pi Calculate the percent of CaO as follows: CaO, % = (P3JS) x 100 re: : CaO, g, and = sample used, g. MAGNESIUM OXIDE where: P4 - Mg2P207, g, and 5 = sample used, g. molecular weight 0,2 MgO _ 2 x 40.32 _ ^ molecular weight Mg2P207 222.60 -- 17.2 Consider the sum of MgO, CaO, and Si02 as combined magnesium and calcium silicate. LOSS ON IGNITION 18. Procedure 18.1 Determine the loss on ignition in accordance with Test Methods D 1208. l Ammonium Hydroxide (sp gr 0.90)--Concentrated onium hydroxide (NH4OH). .2 Ammonium Hydroxide (5+95)--Mix 5 volumes of ntrated NH4OH (sp gr 0.90) with 95 volumes of water, |f5.3 Diammonium Phosphate Solution (250 g/L)--Dis[ye 250 g of diammonium phosphate (NH^HPO,, in hugh water to yield 1 L of solution. 15.4 Hydrochloric Acid (1+3)--See 9.3. Procedure 16.1 Acidify the filtrates reserved in the determination of .0 (Section 13) with HC1 and concentrate to about 400 ,. Add to this solution about 50 mL of (NH4)2HP04 (250 ,) and if the solution becomes alkaline, add HQ (1+3) to geep the solution acidic. Cool the solution by placing the :er in a cold water trough or in a tray of ice water. After ioling add NKLjOH drop by drop, while stirring constantly, til the crystalline magnesium ammonium phosphate beins to form, and then in moderate excess (5 to 10 % of the "volume of the solution), the stirring being continued for several minutes. Set the solution aside for at least 8 h in a , cool atmosphere. i 16.2 Filter the solution on a close-texture paper and wash (frith NH4OH (5+95). Unfold the filter paper and, using hot Water, wash the precipitate into the beaker in which the precipitation was effected. Rinse the filter paper with hot HQ (1+3) and again with hot water; if necessary add more hot HC1 (1+3) to dissolve the precipitate. Dilute the solution |lo about 250 mL, add 1 mL of (NH4)2HP04 solution, and I then add concentrated NH4OH drop by drop, while stirring ^constantly, until the precipitate is again formed as described ,in the NH4OH is in moderate excess. Cool and allow to stand for about 4 h. 16.3 Filter the solution on a close-texture paper and wash six times with NH40H (5+95). Transfer the precipitate wrapped in the moist paper to a weighed platinum or porcelain crucible, slowly char the paper without allowing it to ignite and carefully bum off the carbon over a gradually increasing flame which shall never heat the crucible to more than the faintest red. Finally ignite at 1000 to 1100C to constant weight, taking care to avoid melting the pyrophosphate. 17. Calculation 17.1 Calculate the percent of MgO to 0.1 as follows: MgO, % [(P4 X 0.3623)/S] x 100 MOISTURE AND OTHER VOLATILE MATTER 19. Procedure 19.1 Determine the moisture and other volatile matter by Test Methods D 280. COARSE PARTICLES (Total Residue Retained on a No. 32S (45-|J.m) Sieve) 20. Procedure 20.1 Determine the coarse particles in accordance with Test Methods D 718, except that the specimen weight should be adjusted to provide appropriate sensitivity for the residual weight determination.. Any difficulty encountered in wettingout, the specimen can be overcome by prewetting with a 50+50 mixture of acetone or alcohol and water. MATTER SOLUBLE IN WATER 21. Procedure 21.1 Determine the matter soluble in water by Test Method D 2448 or alternatively by Test Methods D 1208, COLOR 22. Standard Pigment __ 22.1 Standard Extender Pigment. 22.2 Standard Zinc Oxide. 23. Procedure 23.1 Carefully weigh out the proportions of the standard extender pigment and standard zinc oxide mutually agreed upon, and rub up to a fairly stiff paste with a glass muller on a glass plate or stone slab with raw linseed oil conforming to Specification D 234. Note the volume of the oil required. Prepare a similar paste with the sample, using the same weight of pigment, volume of oil, and number of strokes.of the glass muller as used in the preparation of the paste of the standard pigments. Spread the pastes adjacently on a micro scope slide, draw a scraper lightly across them so as to present them on an even plane, and judge the color immediately. 24. Dry Brightness 24.1 The test sample and reference sample shall be prepared into suitable smooth, dry, packed surfaces in DUP050296655 # D 717 accordance with accepted practice and tested for reflectance using the green filter in accordance with Test Method E 97. PRECISION 25. Precision and Bias 25.1 Data are not available to determine the precision and bias of these test methods. There are no plans at present to obtain such information. The methods have been in use for; several years and are considered acceptable. 26. Keywords 26.1 calcium oxide in magnesium silicate; magnesium oxide in magnesium silicate; magnesium silicate pigment, analysis of; silicon dioxide, analysis of The American Society for Testing and Materials takes no position respecting the validity of any patent 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 of such rights, ere entirely their own responsibility. This standard is subject to revision at any tinie by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Your comments are invited either for revision ofthis standard or foradditional standardsand 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. jj 134 pn B DUP050296656 Designation: D 718 - 86 (Reapproved 1991)',<1 Standard Test Methods for Analysis of Aluminum Silicate Pigment1 This standard is issued under the fixed designation D 718; 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. :;<=fl --Keywords were added editorially in January 1991. ^IPCOpe These test methods cover the analysis of aluminum ate pigment. lj.2 This standard does not purport to address the safety Iitlems associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety , and j$th practices and determine the applicability ofregulatory mtations prior to use. ^Referenced Documents jg.1 ASTM Standards: m) 234 Specification for Raw Linseed Oil2 |b 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 |P717 Test Methods for Analysis of Magnesium Silicate Pigment3 1193 Specification for Reagent Water4 ID 1208 Test Methods for Common Properties of Certain i Pigments3 ; D2448 Test Methods for Water-Soluble Salts in Pigments by Measuring the Specific Resistance ofthe Leachate of the Pigment3 Ell Specification for Wire-Cloth Sieves for Testing Purposes5 Up. Significance and Use ,3.1 These test methods may be used to confirm the stated f aluminum oxide and SiOz content of aluminum silicate for Equality control. 1 4. Purity of Reagents * 4.1 Reagent gracle chemicals shall be used in all tests, jp 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,6 1 These test methods are under the jurisdiction of ASTM Committee D-J on Paint and Related Coatings and Materials and arc the direct responsibility of Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved April 25, 1986. Published June 1986. Originally published as D 718 - 43. Last previous edition D 718 - 73 (1979)ei. 2 Annual Book, ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 14.02. 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." where such specifications are available. 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 Unless otherwise indicated, references to water shall be understood to mean Type II of Specification D 1193. 5. Apparatus 5.1 Platinum Crucible. 5.2 Electric furnace (or gas burner), capable of 1050 to llOO'C. 5.3 Volumetricflask, 100 and 250 mL. 5.4 Colorimeter, with transmission range from 400 to 550 am. 5.5 High Silica Crucible. SILICON DIOXIDE 6. Procedure 6.1 Determine the silicon dioxide content in accordance with Test Methods D 717. ALUMINUM OXIDE 7. Reagents 7.1 Ammonium Acetate (20 %)--Dissolve 200 g of am monium acetate (NH4C2H302) in 1 L of distilled water. 7.2 Ammonium Chloride Solution (20 g/L)--Dissolve-20 g ofammonium chloride (NH4G) in water and dilute to 1 L. 7.3 Ammonium Hydroxide (sp gr fr90)--Concentrated, ammonium hydroxide (NH4OH). , 7.4 Diphenylamine Indicator Solution (1 g/100 mL)-- Dissolve 1 g of diphenylamine in 100 mL of concentrated sulfuric acid (H2S04, sp gr 1.84). 7.5 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 7.6 Hydrochloric Acid (1+3)--Mix 1 volume of concen trated HC1 (sp gr 1.19) with 3 volumes of water. 7.7 Hydrofluoric Acid (48 %)-i-Concentrated hydrofluoric add (HF). 7.8 Hydrogen Peroxide (H202, 3 %, freshly prepared)-^ Mix 1 volume of H202 (30 %) with 9 volumes of distilled water. 7.9 Hydroxylamine Hydrochloride (10 %)--Dissolve 10 g of NH2OH HC1 in 100 mL of distilled water. Prepare fresh weekly. 7.10 Iron Standard--Dissolve 0.1 g of analytical grade iron wire in 10 mL of HC1 (1 + 1) and dilute to 1 L. Each millilitre contains 0.1 mg of Fe. 7.11 Mercuric Chloride Solution (HgGy, saturated. w MS* DUP050296657 D 718 7.12 Methyl Red Indicator Solution--Dissolve 0.2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol. 7.13 Potassium Dichromate, Standard Solution (0.05 N)--Dissolve 2.457 g of potassium dichromate (K2Cr207) in water and dilute to 1 L. Standardize against National Bureau of Standards' standard sample No. 27b of Sibley iron ore, using such an amount as to give approximately the same titration as the sample to be analyzed. 7.14 Phosphoric Acid (H3P04, 85 %)--Concentrated phosphoric acid. 7.15 Potassium Pyrosulfate (K2S207). 7.16 o-Phenanthroline (0.1 %)--Dissolve 1.0 g of o-phenanthroline in 1 L of hot distilled water. ` 7.17 Stannous Chloride Solution (5 g/100 mL)--Dissolve 5 g of stannous chloride (SnCl3, 2H20); in 10 mL of concentrated HC1 (sp gr 1.19) and dilute to 100 mL with water. Add scraps of iron-ftee granulated tin;'and boil until the solution is clear. Keep the solution in a dosed dropping bottle containing metallic tin. 7.18 Sulfuric Acid (1+1)--Add carefully 1 volume of concentrated sulfuric add (H2S04, sp gr 1.84) to 1 volume of distilled water. 7.19 Sulfuric Acid (1+9)--Add carefully 1 volume of concentrated H2S04 (sp gr 1.84) to 9 volumes of distilled water. 8. Procedure 8.1 If an appreciable residue remains after the treatment with HF in accordance with 7.4 ofTest Methods D 717, fuse the residue with a small amount of K2S207 until it is dissolved. Leach the pyrosulfate melt out,ofthe crucible with water and combine the solution with the filtrate reserved in, accordance with 7.3 or Test Methods D 717. 8.2 Bring the volume of the combined solution to 250 mL, and, if necessary, add HQ in order to ensure a total of 10 to 15 mL of HQ, add a few drops of methyl red indicator solution, and heat to boiling Add concentrated NH4OH (sp gr 0.90) dropwise until 1 drop changes the color of the solution to a distinct yellow. Reheat the solution containing the precipitated hydroxides to boiling, boil for 1 or 2 min,, and filter. Wash the precipitate once by decantation and then slightly on the filter with hot NH4C1. 8.3 Transfer the precipitate and paper to the original beaker in which the precipitation was made. Dissolve the precipitate in hot HQ (ld-3), dilute to 100 mL, and precipitate again as described in 8:2. After filtering, wash the precipitate ten times with small portions of hot NH4C1 solution. Transfer the precipitate to a weighed platinum crucible, heat slowly until the paper is charred, and finally ignite to constant weight at 1050 to 1100C in mi electric furnace or over a burner, taking care to avoid reduction. Weigh the precipitate as A1203 + Ti02 + Fe^. 8.4 Fuse the combined oxides from 8.3 with 9 to 10 g of K2S20? in a platinum crucible, starting at low temperature and increasing the heat gradually until the oxides have all dissolved; Take up the melt with 5 mL of H2S04 (1+1) in 150 mL of water and warm to effect solution. Transfer the solution to a 250-rnL volumetric flask, dilute to volume, and mix well. Reserve for Ti02 and Fe203 determinations. 8.5 Determine the percent of Ti02 as follows; Pipet an aliquot containing 0.2 to 3.0 mg of Ti02 into a 100-mL volumetric flask. For samples containing 0.5 to 3 % TiOj,*-*; 20-mL aliquot is suitable. Add 5 mL of H202 (3 %), dilute to volume with H2S04 (1+9) and mix well. Obtain the colorimetric reading in a suitable colorimeter using a filter, with transmission limits of400 to 450 nm or at 410 nm with a prism or grating spectrometer. Compare the readings to curve plotted from a set of Ti02 standards similarly treated* and read on the same instrument. 8.6 Determine the percent of Fe203 as follows: Pipet a 25-mL aliquot into a 100-mL volumetric flask. Add the * following in the order given, mixing well after each addition- 2 mL of NH2OH-HQ (10%), 10 mL of NH4C2H302 (20 %), and 10 mL of o-phenanthroline (0.1 %). Roll a small piece of Congo red paper into a ball and introduce into the flask. Add concentrated NTLOH dropwise until indicator turns red and 1 drop in excess. Dilute to volume' and let 1 stand for 10 to 20 min. Obtain the colorimetric reading in a. suitable Colorimeter using a filter with transmission limits 485 to 550 nm, or at 510 nin with a prism or grating spectrometer. Compare the readings to a curve plotted from a set of Fe203 standards similarly treated and read on the same instrument. 4 8.7 Alternatively the Fe203 may be determined by titration as follows: Fuse 1 g of sample with 10 g of K2S207 in a high-silica < crucible starting at low temperature and increasing the heat gradually until the crucible glows with a dull red color and decomposition is judged to be complete. Leach the melt with 10 mL of concentrated HQ in 100 mL ofwater and digest at low heat to disintegrate the cake. Filter and wash free ofchlorides with hot water. Save filtrate. Ignite. the insoluble residue in a platinum crucible. Treat with 5 mL of H2S04 (1+1) and IS mL of HF (48.%), and heat until flumes of H2S04 appear. Bring the residue into solution with the addition of a few drops more of H2S04 (1+1) and combine the solution with the bulk of the iron. Add 5 mL of HQ to the combined solutions and evaporate to 50-mL volume. 8.8 To the hot solution add SnCl2 solution, dropwise, while stirring, .until the solution is decolorized, and then add 2 to 3 drops more. Cool the solution to room temperature, wash down the Inside of the beaker with water, and add at one stroke 10 mL of cool HgCl2 solution (saturated). Stir the solution vigorously for 1 min, add 5 mL of phosphoric add (85 %) and 3 drops of diphenylamine, indicator solution. Titrate with 0.057VK2Cr207 solution to an intense deep-blue end point that remains unchanged on further addition of K2Cr207 solution. 8.9 Calculate the percent of Fe203 as follows: Fe2Q3 % " [(Ar x V X 0.0798)/S\ x 100 where: ; S = sample used, g, V = K2Cr207, mL, and N -- normality of the K2Cr207. 8.10 Calculate the percent of A1203 as follows: A12Oj > % = lOOiP/S) - C where: P = weight of combined oxides A1203 + TiOa + Fe203, S' = specimen weight, g, and C = Fe203 + Ti02, %. 136 DUP050296658 LOSS ON IGNITION ijcedure lltDetermine loss on ignition in accordance with Test lods D 1208. MOISTURE AND OTHER VOLATILE MATTER Procedure '10.1 Determine moisture and other volatile matter in '^accotdahce with Test Methods D 280. COARSE PARTICLES (Total Residue Retained on a No. 325 (45-tun) Sieve) JpApparatus '"li;i Sieve--A No. 325 (45-pm) 3-in. (76.nidi) diameter pfifgii form sieve conforming to Specification Eil, shall be S* ,L IL2 Stirring Apparatus,'1 consisting of: ^' 11.2.1 Mixing Cup--A stainless steel cup, about 7 in. i!78 mm) deep, and slightly tapered from an outside Ipmeter at the top of about 4 in. (102 mm) to about 2% in. I7O mm) at the bottom, such as is characteristic of a usual Kalted-milk type mixing cup. | 11.2.2 Mechanically Operated Stirring Device, in which a suitably mounted electric motor turns a vertical shaft at a Speed of not less than 10 000 r/min without load. The shaft ihall be equipped with a replaceable stirring button not more ilhan 1 in. (25 mm) in diameter, and of such length that the tirring button shall operate not less than % in. (19.0 min) Inor more than l`A in. (38 mm) above, the bottpm of the [dispersion cup. A common malted milk-type mixer of high quality meets this specification. |12. Procedure f 12.1 Dry a No. 325 (45-p.m) sieve in an oven at 105 i 2C, cool, and weigh accurately. Transfer. 100 0.5 g of the (`.specimen to the mixing clip containing approximately 250 [.nili of water to which Has been added about 2-drops of0.5 % [solution sodium silicate,78 and stir for about 10 min at high I speed. Pour the resulting slurry slowly through the sieve and 7 The Hamilton Beach Mixer or equivalent has proven satisfactory for this purpose. 8 "CP Brand sodium silicate, manufactured by the Philadelphia Quartz Co., Public Ledger Building, Independence Square, Philadelphia, PA, or equivalent Has been found satisfactory for this purpose. wash out the mixing cup carefully (a polyethylene squeezetype wash bottle is very convenient) to ensure complete transfer of the specimen to the sieve. Spray the sieve surface gently with a low pressure fan-shaped spray (tap water at about 5 psig (30 kPa) back pressure) arid continue washing until all the pigment has been washed through and the water passing the sieve is clear. Dry the sieve for 1 h at 105 to 110C, cool and weigh. 12.2 Calculation: Percent of coarse particles = (increase in weight of sieve/specimen weight) X 100) MATTER SOLUBLE IN WATER 13.' Procedure 13.1.Determine the matter soluble in water by Test Method. D 2448. COLOR 14. Standard Pigment 14.1 Standard Extender Pigment. 14.2 Standard Zinc Oxide. . 15. Procedure 15.1 Carefully weigh out the proportion of the standard extender pigment and standard zinc oxide ,mutually agreed upon, and rub up to a fairly stiffpaste with a glass muller on a glass plate or stone slab with raw linseed oil conforming to Specification D 234. Note the volume of the oil required. Prepare a similar paste with the sample using the same weight of pigment, volume of oil, and number of strokes of the glass muller as used in the preparation ofthe paste of the standard pigments. Spread the pastes adjacently on a micro scope slide, draw a scraper lightly across them to . present them on an even plane, and judge the color immediately. PRECISION AND BIAS 16. Precision and Bias 16.1 Data are not available to determine the precision and bias of these methods. There are no plans at present to obtain such information. The methods have been in use for several years and are considered acceptable. 17. Keywords 17.1 aluminum oxide in aluminum silicate pigment; alu minum silicate pigment, analysis of; pigment, aluminum silicate 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 entirsly 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, either reapproved or withdrawn. Your comments are invitedeither for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters: Your comments wSI receive careful consideration at a meeting of the responsible technlcal'committea, 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. 137 DUP050296659 Designation: D 719 - 91 Standard Teat Methods for Analysis of Diatomaceous Silica Pigment1 This standard is issued under the fixed designation D 719; 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 These test methods cover the analysis of diatomaceous silica pigment. 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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D 234 Specification for Raw Linseed Oil3 D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)3 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments4 D1208 Test Methods for Common Properties of Certain Pigments4 MATTER SOLUBLE IN HYDROCHLORIC ACID . 6. Procedure 6.1 Transfer about 2 g (weighed to 0.1 mg) oif the dried material (Section 3) to a 150-mL flask or beaker. Add 45 mL of hydrophlpric acid (HC1, 1+2) and boil for 5 min. Add 50 mL of water and boil for 5 min. Filter .through a previously dried and weighed Gooch crucible. Wash the insoluble residue on the filter with hot water until free of chlorides and then with methanol. Dry the crucible and contents at L05 2'C for 2 hi ..................... 7. Calculation 7.1 Calculate the percent of matter soluble iii HQ as follows: ' Matter soluble in HC1, % = [(5 - R)/S]x 100 - where: S = sample used, g, and R=redue, g. . , ' VOLUME OF SETTLING IN PETROLEUM SPIRITS 3. Significance and Use 8. Procedure I 3.1 These test methods are used to determine the purity and some physical properties ofdiatomaceous silica pigment. The information is significant to pigment producers and coatings manufacture. 8.1 Transfer 3 g of the sample to a 100-mL, glassstoppered, graduated cylinder. Add mineral spirits, con forming to Specification D235 until a total volume of 10,0 mL is obtained. Disperse the mixture by invertingthe cylinder 50 times, and then allow to, stand for 1 fa. Read the volume of fhe settled pigment. --. , . , MOISTURE AND OTHER VOLATILE MATTER 4. Procedure 4.1 Determine the moisture and other volatile matter by 9. Standard Pigments si: Test Methods D 280. 9.1 Standard Extender Pigment. 9.2 Standard Zinc Oxide. LOSS ON IGNITION 5. Procedure 5.1 Determine the loss on ignition in accordance with Test Methods D 1208. 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 May 15, 1991. Published July 1991. Originally published as D 719 - 43 T. Last previous edition D 719 - 86. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book qfASTM Standards, Vol 06.02. 10. Procedure iO.l Carefully weigh out the proportions of the standard extender pigment and standard zinc oxide mutually agreed upon, and rub up to a fairly stiff paste with a glass muller on a glass plate or stone slab with raw linseed oil conforming to Specification D 234. Note the volume of ..oil required. Prepare a similar paste with the sample, using the same weight of pigment, volume of oil, and number of strokes of the glass muller as used in the preparation ofthe paste ofthe standard pigments. Spread the pastes adjacently on a micro scope slide, draw a scraper lightly across them so as to present them on an even plane, and judge the color immediately. 138 BlWil^ ........... .... W DUP0502 96660 D 719 COARSE PARTICLES |1 Determine the percent of coarse particles in accordiwith Test Methods P 185. 12. Precision and Bias 12.1 Precision and bias for these test methods have not been determined. . 13. Keywords , 13.1 diatomaceous silica pigment, analysis of; pigment, diatomaceous silica The American Society for Testing and Materials takes no position respecting the validity bf 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 tights, 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 areinvited either forrevision ofthis standard or for additionalstandards and should baaddressed 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 view? known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. DUP050296661 Designation: D 763 - 81 (Reapproved 1988)1 Standard Specification for Raw and Burnt Umber Pigments1 This standard is issued under the fixed designation D 763; 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 ieapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. f1 ?@ABCEditorial changes were made throughout, including the title, in May 1988. 1. Scope 1.1 This specification covers the pigments commercially known as raw umber and burnt umber. 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 Dry Pigments--The pigments shall conform to the following requirements: 3.1.1 Raw Umber--The pigment shall be in a soft, dry form and shall be a hydrated oxide of iron (together with such manganese that is naturally associated with it) perme ating a siliceous base and shall be free of admixtures of other substances except carbon pigments. The pigment shall con form to the requirements for composition prescribed in Table 1. 3.1.2 Burnt Umber--The pigment shall be produced by the calcination of raw umber and shall be free of admixtures of other substances except carbon pigments. The pigment shall conform to the requirements for composition prescribed in Table 1. 3.2 Paste in Oil--For both raw and burnt umber, the paste in oil shall be made by thoroughly grinding the pigment with linseed oil (with or without a small amount of volatile thinner) together with (where necessary) small amounts of wetting or dispersing agents to produce a paste or semipaste of satisfactory consistency. As received, it shall not 1 This specification is under the jurisdiction of ASTM Committee D-t on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.31 on Pigment Specifications. Current edition approved March 2, 1981. Published May 1981. Originally pubtished as D 763 - 44 T. Last previous edition D 763 - 48 (1974). 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. be caked in the container and shall break up readily in linseed oil to form a smooth paint of brushing consistency. It shall mix readily in all proportions, without curdling, with linseed oil, turpentine, or volatile petroleum spirits, or any mixture of these substances. The paste shall conform to the following requirements; Pigment, min, % Nonvolatile vehicle, min, % Moisture by distillation, max, % Coarse particles and skins (total residue retained on a No. 32$ (45-pm sieve), max, % of dry pigment 55 30 2.0 1.0 3.3 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 5.2 Chemical Analysis ofDry Pigment--Methods D 50. TABLE 1 Requirements for Composition of Raw and Burnt Umber Raw Burnt Umber Umber Iron oxide (Fe203), min, 56 Calcium compounds (as CaO), max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Organic colors, max, % 37 5.0 5.0 2.0 none 42 5.0 5.0 2.0 none 140 DUP050296662 # D 763 isture in Paste in Oil--Test Method D 280, except iple shall be weighed instead of measured and the be expressed as weight percentage instead of 'oarse Particles--Test Methods D 185. 5.5 Pigment and Linseed Oil in Paste in Oil--Test Methods D 1208. 5.6 Mass Color and Tinting Strength--Test Method D 387. ' The American Society tor Testing andMaterials takes noposition respecting,the validity of any patent rights asserted In,contraction with any Item mentioned In this standard. Users ot this standard are expressly advised that determination of the validity irf 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 technicalcommittee and must be reviewed every five.y'ears and Ifnot revised, eitherreapproved or withdrawn. Yourcomments are Invited either forrevision ofthis standardorfor 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 nearing you should make your views known to the ASTM Committee on Standards, 1919 Race St, Philadelphia, PA 19103. 141 DU P050296663 Designation: D 765 - 87 (Reapproved 1991)' 1 Standard Specification for Raw and Burnt Sienna Pigments1 This standard is issued .under the fixed designation D 765; the number immediately following the designation indicates the year of originafadoption 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 reapprovai. D EFGH--keywords were added editorially in July 1991. 1. Scope TABLE 1 Requirements for Composition of Raw and Burnt 1.1 This specification covers the pigments commercially Sienna known as raw sienna and burnt sienna. Raw Sienna Burnt Sienna 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 Iron oxide {Fo2Ofi, min, % Calcium compounds (as CaO) max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Organic colors, max, % 38 5.0 4.0 2.0 none 40 5.0 4.0 2.0 none D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D280 Test Methods of Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig linseed oil, turpentine, or volatile petroleum spirits, or any mixture of these substances. The paste shall conform to the following requirements: ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigment, min, % Nonvolatile vehicle, min, of vehicle Moisture by distillation, max, % Coaise particles and skins (total residue retained on a No. 325 <45-)tm) sieve), max, % of dry pigment 60 SO 2.0 1.0 Pigments2 ti ;` ' i 3. Composition and Properties 3.3 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard 3.1 Dry Pigments--The pigments shall conform to the acceptable to both the purchaser and the seller. . 11 following requirements: 3.1.1 Raw Sienna--The pigment shall be in a soft, dry 4. Sampling form and shall be a hydrated oxide of iron permeating a 4.1 Two samples shall be taken at random from different siliceous base. The pigment shall conform to the require packages from each lot, batch, day's pack, or other unit of ments for composition prescribed in Table 1. production in a shipment. When no markings distinguishing 3.1.2 Burnt Sienna--The pigment shall be produced by between units of production appear^samples shall,be. taken the calcination of raw sienna and shall conform to the from different packages in the ratio of two-samples for each 5 requirements for composition prescribed in Table 1. tons (inch-pound or SI), except that for shipments of less 3.2 Paste in Oil--For both raw and burnt sienna, the than 10 000 lb two samples shall be taken. At the option of paste in oil shall be made by thoroughly grinding the pig the purchaser, the samples may be tested separately or after ment with linseed oil (with or without a small amount of blending in equal quantities the samples from the same volatile thinner) together with (where necessary) small production unit to form a composite sample. amounts ofwetting or dispersing agents to produce a paste or 5. Test Methods sa iipi fcis semipaste of satisfactory consistency. As received, it shall not be caked in the container and shall break up readily in linseed oil to form a smooth paint of brushing consistency. It shall mix readily in all proportions, without curdling, with 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures not cov ered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 5.1.1 Total Iron Oxide, Calcium Compound, and Organic ImI 1 This specification is under the jurisdiction of ASTM Committee D-I on Paint Coloring Matter--Methods D 50. and Related Coatings and Materials and is the direct responsibility of Subcom 5.1.2 Coarse Particles--Methods D 185. mittee DOI.3J on Pigment Specifications. Current edition approved June 26, 1987. Published August 1987. Originally published as D 765 - 44. Last previous edition D 765 - 80. 2 Annual Book ofASTM Standards, Vol 06.02. 5.1.3 Pigment and Linseed Oil in Paste in Oil---Test Methods D 1208. 5.1.4 Moisture in Paste in Oil--Test Methods D280, 3 Annual Book ofASTM Standards, Vois 06.01 and 06.02. except that the sample shall be weighed instead of measured DUP050296664 # D 765 fje results shall be expressed as percentage by weight glcf TOlume. . ,,^ . , ^5 Mass Color and Tinting Strength--Test Method 6. Keywords 6.1 burnt sienna; iron; manganese; pigment; raw sienna The American Society tor Testing endMaterials takes no position 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 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 end Ifnotrevised, 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 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 it., Philadelphia, PA 19103. DUP050296665 Designation: D 768 - 81 (Reapproved 1987)'fi Standard Specification for Yellow Iron Oxide Hydrated1 This standard is issued under the fixed designationD 788; 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 specification has bbeii approvedfor rise by ageiicibs ofthe DepartmentcfDefense toYefihtce Fed. Spec. TT-P-4SS: Consult the DoD Index ofSpecifications and Standardsfor the specific pear ofissue which has btfeh adopted by the Department ofDefense. i IJKLMEditorial changes were made throughout id.June 1987. ,u 1. Scope 1.1 This specification covers the pigment commercially known as yellow iron oxide, hydrated. 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D 1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 The pigment shall be a manufactured yellow iron oxide obtained by chemical reaction. It shall be a soft, finely powdered pigment, free of admixtures of other substances and shall conform to the following requirements: Total hydrated oxide of iron, min, % Total oxide of iron,'4 min, % Loss on ignition,'4 max, % Moisture and other volatile matter, max, % Water soluble matter, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Hydrogen ion concentration (pH value) 93 83 13 1.0 0.50 0.5 4.5 to 8.0 * Total hydrated oxide of iron shall be the sum of iron oxide and loss on ignition. Loss on ignition shall be calculated on the dry material. 3.2 Paste in Oil--The paste in oil shall be made by thoroughly grinding the specified pigment with linseed oil (with or without a small amount of volatile thinner) together with (where necessary) small amounts of wetting or dis persing agents to a semipaste or fluid type consistency. As received, it shall not be caked in the container and shall 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved March 2, 1981. Published May 1981. Originally published as D 768 - 44T. Last previous edition D 768 - 47 (1974). 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards. Vols 06.01 and 06.02. break up readily in oil to form a smooth paint of brushing consistency. It shall mix readily in all porportions, without curdling, with linseed oil, turpentine, or volatile petroleum [ spirits, or any mixtures of these substances. The paste shall conform to the following requirements: Figment, min, % Nonvolatile vehicle, min, % of vehicle Moisture by distillation, max, % Coarse particles and skins (total residue retained on a No. 325 (45-jun) sieve), max, percent of the dry pigment Consistency by the Stormer viscometer: At shearing rate of 100 revolutions/30 s, min, g At shearing rate of 100 revolutions/35 s, max, g 55 80 2.0 1.0 700'4 1200* A Equivalent to a rating of 125 Krebs* Units. B Equivalent to a rating of 145 Krebs* Units. 3.3 The mass color character of the tint and the tinting' strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of S standard acceptable to both the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment When namarkings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 General--Tests shall be conducted in accordance.with the appropriate ASTM test methods. Test procedures'not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Chemical Analysis--Methods D 50. 5.1.2 Coarse Particles in Pigments--Test Method D 185. 5.1.3 Moisture in Pigments--Test Method D 280. 5.1.4 Water Soluble Matter--Test Method D 1208. 5.1.5 Hydrogen Ion Concentration--Test Method D 1208. 5.1.6 Pigment and Linseed Oil in Paste in Oil--Test Methods D 1208. 144 DUP050296666 # D 768 The American Society tor Testing and Materials takes noposition respecting the validity ofanypatent 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 r This standard Is subject to revision at any time by the responsible technical ct Ifnot revised, eitherreapproved orwithdrawn. Your comments are Invited eHher for revision ofthis standardorforadditionalstandards and should be addressed to ASTM Headquarters. Your comments wlH 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 vlewa known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. DU P0502 96667 Designation: D 769 - 87 (Reapproved 1991)*1 StandairdSpecificationJor Black Synthetic Iron Oxide1 This standard is issued under the fixed designation D 769; the dumber immediately foUowing tbe designation indicates the year of original adoption or, in the case ofrevision, the-year ofla-st revision. Anumber in parentheses indicates the-ycar of last icapprovah A superscript epsilon (e) indicates an editorial change since the last revision, or reappmyal. NOPQR** Keywords were added editorially in July 1991. 1. Scope 1.1 This specification covers the pigment commercially known as black synthetic iron oxide. 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese2 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions} in Pig ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D 1208 Test Methods for Common Properties of Certain Pigments2 D 3872 Test Method for Ferrous Iron in Iron Oxides2 3. Composition and Properties 3.1 The pigment shall be a manufactured ferrous-ferric oxide obtained by chemical reaction. It shall be a soft dry finely powdered pigment, free of admixtures of other sub stances and shall conform to the following requirements: Total ferrous and ferric oxide, min % Ferrous oxide (FeO), min, % Water-soluble matter, max, % Moisture and other volatile matter, max, % Coarse particles (total residue retained on a No. 32$ (45-jun) sieve), max, % Hydrogen ion concentration (pH value) 93 20 0.5 1.0 0.5 4.5 to 8.5 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved May 29, 1987. Published July 1987. Originally published as D 769 - 44. Last previous edition D 769 - 81. 2Annual Book ofASTM Standards, Vol 06.02. 1 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3.2 The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. I 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Total Iron Oxides--Methods D 50. 5.1.2 Ferrous Iron in Iron Oxides--Test Method D 3872. 5.1.3 Water Soluble Matter, Maximum, Percent--Test Methods D 1208. 5.1.4 Moisture and Other Volatile Matter; Maximum, Percent--Test Methods D 280. .. ` ' 5.1.5 Coarse Particles (Total Residue Retained on a 325-mesh sieve {45 p.m), Maximum, Percent--Test Methods D 185. 5.1.6 Hydrogen Ion Concentration (pH value)--Test Methods D 1208. 5.1.7 Mass Color and Tinting Strength--Test Method D387. 6. Keywords 6.1 iron oxide; manganese; pigment The American Society tor Testing and Materials takes noposition respecting the validity ol anypatentrights 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 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 five years end ifnot revised, either reapprwed or withdrawn. Yourcomments are invited either lor revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive oaretul consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your commems have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Baca St., Philadelphia, PA 19103. 1,46 DUP050296668 Designation: D 784 - 83 (Reapproved 1987) Standard Specification for Orange Shellac and Other Indian Lacs for Electrical Insulation1 This standard is issued under the fixed designation D 784; 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 r- superscript epsilon (<) indicates an editorial changesincethelast revision or reapproval. fScope ' ' 1.1"This specification ''covers'"the6 requirements, and', hqds. of test for three types and four grades of orange Sc anci other lacs, as follows: 1.1.1 Type /--Orange Flake Shellac, Grades A, B, C, and 1.1.2 Type //--Button Lac, and 1.1.3 Type ///-^Garnet Lac. L2 Stick-lac and seed-lac are not covered by this" spedfi- ition. . <t,. , .. 1.3 The values stated , in. inch-pound .units , are to he led as the'standard. The metric equivalents of inch- ___units may be approximate. ' ". ' 1.4 This standard may involve hazardous materials, oper- ions, and equipment. This standard does not purport to Idress all ofthe safety problems associated with its use. It is responsibility ofwhoever uses this standard to consult and ablish appropriate safety and health practices and deter- iine the applicability ofregulatory limitations prior to use. , Referenced Documents 2.1 ASTM Standards: D29 Test Methods for Sampling and Testing Lac Resins12 D411 Test Methods for Shellac Used for Electrical Insulation3 1 This specification is under the jurisdiction of ASTM Committee D-9 on Electrical mid Electronic Insulating Materials and is the direct responsibility of Subcommittee D09.01 on Electrical Insulating Varnishes, Powders, and Encapsu- i ialing Compounds. Current edition approved May 27, 1983. Published July 1983. Originally published as D 784 -61. Last previous edition D 784 - 61 (1975). 2 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vols 06.02 and 10.01. Description of Materials ' " 3.1 Type I is the commercial rosin-free grade of orange flake shellac. Type II customarily occurs in the form of circular disks about 76'tniri (3 in.) in diameter and 3.nmi (V* in.) in thickness and is known to the trade as pure buttori lac. Type III is dark garnet in color and is known to the trade as pure garnet lac. Garnet lac is also manufactured in admix ture wi$i r^sin. and'as a dewaxed lac, but these are not covered by this specificatiom-. 4. Ordering Information 4;1 Orders for material covered by this specification shall include the following: ' 4;2 Lot numBer ^.Supplier's dfesigtiation,. 4.3 Type and graded 4.4 Quantity in each bag or container, and 4.5 Total quantity. 5. Properties 5.1 The material shall conform to the requirements pre scribed in Table 1. 6. Test Methods 6.1 Determine the material sampled and the properties enumerated in this specification in accordance with Test Methods D 29 and Methods D 411. 7. Packaging and Package Marking 7.1 Packaging and marking shall be as agreed upon between the purchaser and the supplier.__ 8. Certification 8.1 When specified in the purchase order or contract, a producer's or supplier's certification shall be furnished to the purchaser that the material complies with the requirements of tins specification. A report of the test results shall be furnished when specified in the purchase order or contract. DUP050296669 D 784 TABLE 1 Requirements far Orange Shellac and Other Lacs Grade A Typel Grade B Grade C Grade D Type 1 Type ill Matter insoluble in specified hot solvents, max, % Iodine number, max Moisture, max, % Wax, max, S Orpiment, max, * (native arsenic trisulfide) Matter soluble in water, max, % Ash, max, % Rosin Color Polymerization time at 150 1C Flow test at 100 1C 1.00 15.0 2.0 5.5 0.03 0.5 1.0 none 1.25 1.50 3.00 1.00 0.50 ' 15.0. 15.0 15.0 15.0 18.0 1 2.0 2.0 2.0 2.0 20 | 5.5 5.5 5.5 5.5 3.5 I 0.03 0.03 0.2 0.03 0.03 0.5 0.5 0.5 0.5 0.5 1.0 Id) 1.0 0.5 0.5 none none none none when specified, the color shall be no darker than that of a sample agreed upon by the purchaser and the sefler when specified, shafi be within the maximum-minimum range agreed upon by the purchaser and the seller .f when specified, shall be within the maxImum-mWmum range agreed upon by the purchaser and the seder4 * Attention is celled to the tact that the purchaser and the seller must agree upon one of the two methods far determining {1} color tor Type 1, appearing in Method; D 2? and (2) flow test In Methods D 411. . . TheAmerican Society lor Tasting andMaterials lakes no position respecting the validity ofany patent rights assertedIn connection with any Kern 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 ifnot revised, eitherreapproved or Withdrawn. Yourcomments are Invited ehher 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 emend, if you feel that your comments hairs not receiired a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296670 Designation: D 817 - 91 Standard Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate1 ' i This standard is issued under the fixed designation D 817; the Dumber 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 ,, , ope These test methods cover procedures for the testing of ose acetate propionates and acetate butyrates. These p may vary widely in composition and properties, so !n of the procedures can be used only in the ranges of Jpcisition where they are suitable. i2rThe test procedures appear in the following sections: . . i Sections T.Propionyl or Butyryl Contents-.......;............... 28 to 37 1 Content, Apparent............. ............................... 18 to 27 .Free......................'................................ 12 to 17 .............................................................................. 7 to 10 ` b'rand Haze..................... ............. ............ . ................. 77 toil Stability.................................................................. 57 to 65 `-oxyl Content........................................................... 38 to <14 ^:xyl Content, Primary............................................. 46 to 50 irisic Viscosity' ............... .................... -......... .. ' 67 to 7i gsture Content............................................................ 5 to 6 r or Sulfhle Content ............................................... 51 to 56 aty............................................................................. 74 to,75 'ting Viscosity Number................................. tfMb71 _ ^3 This standard does not purport to qddress the safety zblems, if any, associated with its use. It is the respoMity of the user of this standard to establish appropriate ifety and health practices and determine the applicability of datory limitations prior to use. It?:: Referenced Documents fkl ASTM Standard: ' \ .D.6i8 Practice for. Conditioning plastics and Electrical Jnsulating Mateiials for Testing21 ... iff D1343 Test Methpd for Viscosity ,of Cellulose Derivatives, by Ball-Drop Method3 , . D 2929 Test Methpd for Sulfur Content of Cellulosic Materials by X-Ray Ruore^peuce3 . Reagents, ' > 3.1: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 1 These test methods ate under the jurisdiction of ASTM CJommitjee D-l on Paint and Related Coatings and Materials and are tbe direct responsibility of Subcommittee D0I.36 on Cellulose and Cellulose Derivatives. Current edition approved Feb. 22, 1991. Published: April 1991. Originally published as D 817 -44T. Last previous edition Q 817-72 (1983). ^ Annua! Book ofASTM Standards, Voi 08.01. 3 Annual Book ofASTM Standards, Vd 06.02. 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., 4. Conditioning 4.1 Conditioning--Condition the test specimens at 23 2C (73.4 3.6'F) and'50 5 percent'relative humidity for not less than 40 h prior to test in accordance with Procedure A of Methods D 618, for those tests where conditioning is required. In cases of disagreement, the tolerances shall be 1C (1.8F) and 2 percent relative humidity. ,, 4.2 Test Conditions--Conduct tests in the Standard Lab oratory Atmosphere of23 2C (73.4 3.6F) apd 50 5 % relative humidity, unless otherwise specified in the'test methods. Iri cases of disagreements, the tolerances shall be 1C (1.8F) and 2 % relativfe humidity. ' MOISTURE CONTENT 5v'Procedure 1 5.1 Tratisfdr about 5 g 'of the sample to a -fared, Tbw, wide-form weighing bottle and weigh to the nearest 0.001 g. Dry in an oven for 2 h at 105' 3C. Remove the bottle from the oven, cover, cool in a desiccator, and weigh. 6. Calculation ; , 6,1 Calculate the percentage of moisture as follows: Moisture, % = (A/B) x 1Q0 - - '. Wherfe: : ` A '== weight loss' on heating^ g,! and B = sample used, g. V: .. * (1) '' '' ASHT 7. Significance and Use 7.1 Ash content gives an estimate of the inorganic content of cellulose ester samples. The presence of high levels of inorganic content (ash) can be detrimental to tfie melt stability and optical- clarity of a cellulose ester in "melt processing or act as a potential source of insolubles when the ester is used iir solution1. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical 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 Nostrand Co., Itic., New York, N.Y., and the "United States Pharmacopeia." . 149 DUP050296671 D 817 8. Procedure 8.1 Dry the sample for 2 h at 1Q5 3C and weigh 10 to 50 g, to the nearest 0.01 to 0.1 g, depending on its ash content and the accuracy desired. Bum directly over a flame in a 100-mL tared platinum crucible that has been heated to constant weight and weighed to the nearest 0.1 mg. Add the sample in portions if more than 10 g is taken. The sample should bum gently and the portions should be added as the flame subsides. Continue heating with a burner only as long as the residue bums with a flame. Transfer the crucible to a muffle furnace and heat at 550 to 600C for 3 h, or longer if required, to bum all the carbon. Allow the crucible to cool and then transfer it, while still warm, to a desiccator. When the crucible has cooled fo room temperature, weigh accu rately to the nearest 0.1 mg. 9. Calculation 9.1 Calculate the percentage of ash as follows: Ash, % = (A/B) x 100 where: A " aSh, g, and' B = sample used, g. (2) 10. Precision and Bias 10.1 No statement on bias can be made as no reference material is available as a standard. FREE ACIDITY 11. Significance and Use 11.1 Free acidity is a measure of unesterified organic acid in the ester. The presence of high levels of free acid is potentially detrimental to melt processing of the ester and can impact the odor of the ester. 12. Reagents 12.1 Acetone, neutral. 12.2 Methyl Red Indicator Solution (0.4 g/L)--Dissolve 0.1 g of methyl red in 3.72 mt of 0.1000 N NaOH solution and dilute to 250 mL with water. Filter if necessary. 12.3 Phenolphthalein Indicator Solution (1 g/100 mL)-- Dissolve 1 g phenolphthalein in 100 mL of ethyl alcohol (95%). 12.4 Sodium Hydroxide, Standard Solution (0.01 N)--Prepare and standardize a 0.01 N solution of sodium hydroxide (NaOH). Test Method A--For Samples Containing Not More than About 30 % Propionyl or Butyryl 13. Procedure 13.1 Shake 5 g of the sample, corrected for moisture content if necessary, in a 250-mL Erlenmeyer flask with 150 mL of freshly boiled, cold water. Stopper the flask and allow it to stand for 3 h. Filter off the cellulose ester and wash it with water. Titrate the combined filtrate and washings with 0.01 N NaOH solution, using phenolphthalein indicator solution. 13.2 Run a blank determination on the water, using the same volume as was used in extracting the sample. 14. Calculation 14.1 Calculate the percentage ofacidity as free acetic as follows: Free acetic acid, % -- {[(A -- B)C x 0.06]/IV} x 100 where: A = NaOH solution used to titrate the sample, mL, B = NaOH solution used to titrate the blank, mL, C = normality of the NaOH solution, and W = sample used, g. Test Method B--For Samples Containing More than About 7% Propionyl or Butyryl and Particularly Suitablefor Samples Containing More than 30 % Propionyl or Butyryl 15. Procedure 15.1 Dissolve 10.0 g ofthe. sample, corrected for moisture content if necessary, in 200 mL df neutral acetone plus 2ft1 mL of water. When completely dissolved, add' 50 mL of water and shake well to precipitate the ester in a finely divided form. Add 3 drops of methyl red indicator solution and titrate to a lemon-yellow end point and 0.01 N NaOH solution. 15.2 Make a blank determination on the reagents. 16. Calculation 16.1 Calculate the free acid content as acetic acid as directed in Section 14. 17. Precision and Bias 17.1 No statement on bias can be made as no reference material is available as a standard. APPARENT ACETYL CONTENT 18. Scope 18.1 The test methods described in the following sections 20 to 26 cover the determination of the saponification_yalue of the sample calculated as percentage of apparent acetyl, equivalent weight 43. This value is required in the calcula tion of acetyl and propionyl or butyryl contents in 36.1. 18.2 The test method used should.he specified or.agfeed upon. The choice depends on the propfonyl or butyryl content and the physical condition ofthe sample. Ordinarily, Test Method A is recommended for samples having less than about 35 % propionyl or biityryl and Test Method B for samples having more than that amount. 19. Significance and Use 19.1 Apparent acetyl content is a measure of the saponi fication value of the ester. Apparent acetyl value is required in the calculation ofacetyl, propionyl, and butyryl content in 36.1. Test Method A--For Samples Containing Less than About 35 % Propionyl or Biayryl 20. Apparatus 20.1 Weighing Bottle, glass-stoppered, 15-mL capacity, 25-mm diameter by 50 mm high. 20.2 Tray, copper or aluminum, approximately 137 mm (5% in.) square, containing 25 compartments 25 mm (1 in.) square. Each compartment shall have the correct dimensions 150 DUP050296672 D 817 strongly'recommended. Solution is more rapid, titrations are more rapid, and the end point can be approached direcily and without a back STUVtitration. 3--It is important to correct all 1.0 N H2SO,, buret readings for temperature and buret corrections. 23. Calculation 23.1 Calculate the percentage by weight pf acetyl as follows: Acetyl, % = {[(Z> ~C)Na - (B - A]Nb+ P] X 0.04305}/^x IpO P= (GH x. 1000)/204.2 (Note 4) (4) where: A - NaOH solution required for titration of the sample, mL, B - NaOH solution required for titration ofthe! blank, mL, Nb = normality of the NaOH solution, C . = H2SO4 required for titration of the sample, mL D = H2S04 required for titration of the blank, mL, Na = normality of the H2S04, r P = milliequivalents of potassium acid phthalate, G = potassium acid phthalate used, g, H = purity factor for potassium acid phthalate, and W = sample used, g. WXYZ [\When equal volumes of alkali or acid are.added to samples and blank, these amounts cancel out. Thus only the amounts of each added in the titration enter into the calculations. Use of potassium acid phthalate in the blank is recommended. When it is not used, the-term F drops out of the equation. ' Test Method B--.For Cellulose Ester? Containing More than 30 % Propionyl or Butyryl, by Varying the Reagents5 24. Reagents 24.1 Acetone-Alcohol Mixture--Mix equal' volumes of acetone and methyl alcohol. 24.2 Hydrochloric Acidf, Standard (0.5 AO-^-Prepare' and standardize a 6.5 N solution of hydrochloric acid (HCI). 24.3 Phenolpfithalein Indicator Solution (1 g/100 mL)-- Dissolve 1 g of phjenolphthalein in 100 mL of ethyl alcohol (95%).. ; 24.4 Pyridine - Alcohol Mixture--Mix equal volumes of pyridine and methyl alcohol. 24.5 Sodium. Hydroxide. Aqueous Solution (20 g/L)-- Dissolve 20 g of sodium hydroxide (NaOH) in water and dilute to 1 L with water. 24.6 Sodium Hydroxide^ Methanol Solution (20 g/L)-- Dissolve 20 g of NaOH iri 20 mL of water and dilute to 1 L with methyl alcohol. , ., 25. Procedure 25.1 Dry the sample for 2 h at i05 3C andcool in a desiccator. Weigh 0.5-g portions of the sample to the nearest 0.Q05 g and; transfer to 250-mL glass-stoppered Erlenmeyer flasks. Dissolve each sample in 100 mL of appropriate solvent (see 25.2 and 25.3) and prepare at least two blanks, which shall be carried through aU steps of the procedure. 25.2 Samples Containing 30 to 45% Propiptiyl or Butyryl--Dissolve in 100 mL of the acetone-alcohol mixj ture. Add water and aqueous NaOH solution from a buretqj pipet in the following order and swirl the contents of thi flask vigorously during all additio'ns: 10 mL of NaOif| solution, 10 mL of water, 10 mL ofNaOH solution, 5 mL.<sj$ water, 20 mL ofNaOH solution, and 5 mL of water. StoppeJ and allow to stand at room temperature for 16 to 24 h. 25.3 Samples Containing More than 45 % Propionyl a-1 Butyryl--Dissolve in 100 mL of the pyridine-alcohol mix ture. Add 30 mL of the methanol solution of NaOH from a ! pipet or buret slowly, with swirling. Add 20 mL of water slowly in about 2-mL portions, with' swirling, and swirl the! flask until the solution becomes turbid. Stopper and allow to stand overnight at room temperature. j 25.4 Back-titrate the excess NaOH with 0.5/VHC1 just to the disappearance of color,, using phenolphthalein indicator.! solution. J 26. Calculation .1 - .26.1 Calculate the apparent acetyl content as follows: ... | ' Apparent acetyl, % = {[(/l B)N,, x 0.04305]/x 100 (5) I where: A = HCI required for titrationof the blank,mL, B = HCI required for titrationof the sample,mL, Na = normality of the HCI, and 'u. W = sample used, g. 1 1 j 1 j 27. Precision and Bias I 27.1 No statement oh bias can be made as no reference 1 material is available as a standard. 1 ACETYL AND PROPIQNYL OR BUTYRYLCONTENTS 1 28. Scope '' `' | 28.1 The test methods described in the Mowing Sections | 30 to 36 cover the determination of acetyl and propionyl or ! butyryl contents of cellulose mixed esters by calculation from the apparent acetyl content, determined in accordance ; with Sections 18 to 26, and the molar ratio pf acetyl and 1 propioifyi or biltyryl, determined im.accordance \yitbSet- * tions 30 to 35. The molar ratio ofacetyfand propionyl or blityryl is determihed by saponifying, acidifying,' vacuum distilling off the mixture of acids, add ^determining the distribution ratio of the acids between n-butyl acetate and water. The distribution ratios are also determihed for acetic, propioniCi and butyric acids, using samples of knpwn high purity, and the' molar ratio of the acids in the sample is calculated from these values.6 :. . 28.2 The saponification conditions are varied depending on the propionyl or butyryl content of'the sample. Usp Procedure A (Section 32) for samples containing less, than about 35 % propionyl or butyryl, and use Procedure B (Section 33). for samples containing more than that amount. 28.3 Analyses for combined acetic, propionic, and butyric acids may be done by gas chromatographic methods. Diffi- 5 Malm. C.J., Genung, L. B., Williams, R. F., Jr., and Pile, M. A., "Analysis of Cellulose Derivatives: Total Acyl in Cellulose Organic Esters by Saponification in Solution," Industrial and Engineiring Chemistry, Analytical Edition, IENAA, Vol 16, 1944, pp. 501-504. 6Malm', C. J., Nadeau, G. F., and Genung, L. B.,' "Analysis of Cellulose Derivatives: Analysis of Cellulose Mixed Esters by the Partition Method," Industrial ami Engineering Chemistry, Analytical Edition, IENAA, Vo[. 14, 1942, pp. 292-297. TTsis reference may be consulted for application to other mixed esters and to three-component mixtures. 152 DUP050296673 D 817 stoppered opening, F, for adding extra water during the distillation. A water bath, G, for heating the sample and a cooling bath, H, for cooling the receiver shall be provided. Pi* K (5 '<&A--Flask containing sample (500-mL, round-bottom). mkll--Capillary inlet tube. 2--Kjeldehl distilling head. {-Condenser. -Receiver (500-mL distilling 8ask). |rOpenlng for adding water. -Water bath for heating sample. ^-Coding bath for receiver. Side arm, connected to vacuum line. 1 Vacuum Distillation Apparatus for Mixed-Ester Analysis ;ulties encountered include ghosting in the columns, variaion of factors with composition, and inconsistencies in the |se of pure acids as standards. When such methods are used pr this purpose, they shall be cross checked with the "following partition method using suitable check batches to ptablish accuracy. f 29. Significance and Use 29.1 Acetyl and propionyl or butyryl content is a measure jfbf the amount of each of these acids esterified onto the fcellulose backbone of the polymer. The amount of substitu tion of these esters has a very strong effect on the polymer's Isolubility and physical properties. |30. Apparatus | . 30.1 Vacuum Distillation Apparatus--The vacuum distil|lation apparatus shown in Fig. 1 will be required. The ' 500-mL round-bottom flask. A, shall be fitted with a stopper icarrying a very small capillary inlet tube, B, and a Kjeldahl (distilling head, C. The Kjeldahl distilling head shall be gconnected to a vertical condenser, D, having an outlet tube flong enough to reach within 76.2 mm (3 in.) ofthe bottom of i the 500-mL distilling flask, E, used as a receiver. The | Kjeldahl distilling head shall be equipped with a funnel or 31. Reagents 31.1 Acetic, Propionic, and Butyric Acids--Acetic, propionic, and butyric acids of tested purity. 31.2 Bromcresol Green Indicator Solution (0.4 g/L)--Grind 0.1 g of tetrabromo-wz-cresolsulfOnphthalein in a mortar with 14.3 mL of0.01 TV NaOH solution and dilute to 250 mL. 31.3 n-Butyl Acetate--Prepare n-butyl acetate for use as an extraction solvent, free of acidity and water and con taining not more than 2 % butyl alcohol. Check for acidity by shaking 60 mL ofthe -butyl acetate with 30 mL ofwater in a 125-mL separatory funnel for about 1 min. Allow to settle, draw off the water layer, and titrate with 0.1 N NaOH solution, using phenolpbthalein as the indicator, If this requires more than 0.02 mL of 0.1 TV NaOH solution, the butyl acetate should be purified or a correction for acidity applied to each titration. 31.4 Ethyl Alcohol;formula 2B, 3A, or 30 (denatured). 31.5 Phosphoric Acid (1 + 14)--Dilute 68 mL of phos phoric acid (H3PO4, 85 %) to 1 L with water. Titrate the NaOH solution (20 g/L) with this acid to a yellow end point, using bromcresol green indicator solution, and calculate the volume of the acid (approximately 50 mL) required for 100 mL of the NaOH solution. 31.6 Sodium Hydroxide Solution (20 g/L)--Dissolve 20 g of sodium hydroxide (NaOH) in water and dilute to 1 L. 31.7 Sodium Hydroxide, Standard Solution (0.1 N)-- Prepare arid standardize a 0.1 TV solution of NaOH. Isolation ofthe Mixed Adds 32. Procedure A--For Samples Containing Less than Abput 35 % Propionyl or Butyryl 32.1 Heat duplicate 3-g portions of the sample, riot especially dried nor accurately weighed, with 100 mL of NaOH solution (20 g/L) in 500-mL, round-bottom, chemi cally resistant glass flasks in a water bath at 40C for 48 to 72 h. At the end of this time add the required amount (approximately 50 mL) of H3P04 (1+14) to. each flask to form monosodium phosphate, which liberates the organic acids from their sodium salts. 32.2 Assemble the vacuum distillation apparatus as illus trated in Fig. 1. Heat the 500-mL round-bottom flask containing the sample in a water bath, and vacuum-distill the acid solutions to dryness, allowing a small -stream of air bubbles to enter to avoid bumping. Keep the receiver cooled to 0C. Add 25 mL of water to the residue in each flask and again distill to dryness. Repeat the distillation to dryness with a second 25-mL portion of water. ]^_` 5--In this operation it is not necessary to work with quantita tive accuracy at all stages, but it is necessary to obtain water solutions of the acids in the same ratios as they occur in the esters. The volume of the distillate and rinsings is usually 200 to 250 mL, which in the majority of cases automatically adjusts the acidity of the distillate to 0.06 to 0.12 N, the range desired for subsequent extractions. 32.3 Continue as directed in Section 34. DU P050296674 33. Procedure B--For Samples Containing More than About 35 % Propionyl or Butyryl 33.1 Weigh duplicate 3-g samples, not especially dried nor accurately weighed, into 500-mL round-bottom flasks and add 100 mL of Formula 2B, 3A, or 30 denatured ethyl alcohol and 100 mL ofNaOH solution (20 g/L) to each flask. Allow the samples to stand stoppered at room temperature for 48 to 72 h. At the end of this period, filter off the regenerated cellulose, collecting ,the filtrates in 500-mL round-bottom flasks. 33.2 Assemble the vacuum-distillation apparatus as illus trated in Fig. 1. Heat-the flasks in the water bath and vacuum-distill off all die alcohol. After.distilling to dryness, release the vacuum, rinse out the distillation heads, con densers, and receivers, and discard the distillates and rins ings. 33.3 Add the required amount, about 50 mL, of H3P04 (1 +14) to form monosodium phosphate, which liberates the organic acids from their sodium salts. Also add 100 mL of water to each flask and reassemble the distillation apparatus. Vacuum-distill the volatile acids as described in 32.2. - 33.4 Continue as directed in Section 34. , Determination ofthe Molar Ratios ofthe Acids, 34. Procedure 34.1 Titrate a 25-mL portion of the distillate (32.2) with 0.1 N NaOH solution, using phenolphthalein as the indi cator. Designate the volume of NaOH splution required as M. Shake 30 mL ofthe distillate in a small separatory funnel with 15 mL of n-butyl acetate. Measure these volumes accurately using pipets. and burets. Shake the mixture thoroughly for 1 min, allow the layers to separate for 2 min, and draw off the aqueous (lower) layer. Pipet out 25 mL of the solution and titrate with 0.1 /VNaOH solution (Note 6). Designate the volume of NaOH solution required as Mu Calculate K, the percentage partition ratio of the acids in the distillate, as follows: K=(.M',/M)X 100 (6) abcd 6--It should be kept in mind that ail these determination'are ratios and not quantitative; however, accuracy of duplication is very important. All measurements, must be made as exactly as those made by standardizations of the solutions. and equipment 34.2 In the same manner determine,the distribution ratios for acetic, propionic, and butyric adds. Dilute a sample of each acid of tested purity with water to give an approxi mately 0.1 If solution. Titrate 25-mL portions and extract 30-mL portions, following exactly the same procedure as used for the mixtures (34.1). Calculate the partition ratios for the pure acids, as decimal fractions, as follows (Note 7); k -- MtfM (7) where: ka = distribution ratio for acetic'acid under the conditions described, kp = distribution ratio for propionic acid under the condi tions described, and kb = distribution ratio for butyric acid under the conditions described. efgh 7--The constants must be checked occasionally and must be determined by each operator for each supply of butyl acetate. Blanks should be run on the butyl acetate, since it may develop acidity on standing, particularly if it contains a little water. AH measurements ' should be made with good pipets or burets and extreme care and cleanliness observed during the whole operation. The accuracy of the procedure can be checked by testing an acid mixture of knowt) composition. 35. Calculation 35.1 Calculate the molar ratios of acetic and propionic or butyric acids in the mixed adds as follows (Note 8): P=(mka- K)/(ka-kp) A=m-P B = (100fc,, - K)i{ka - kb) A = 100 -- B where: P = percentage of propionic acid, mol, B = percentage of butyric acid, mol, A = percentage of acetic add, mol, K = percentage distribution ratio of the acids in the distil late (34.1), ka = distribution ratio of acetic acid (34.2), kp = distribution ratio of propionic acid (34.2), and kb = distribution ratio of butyric add (34.2). ifgh 8--In order to evaluate two unknowns, two simultaneous algebraic equations involving the two unknown quantities are necessary. In the case of a binary acid mixture, the sum of the mol percentages of the adds present represents the total acidity, or 100 %. If A and B represent the mole percentages of Acetic and butyrifc acids, respectively: A + B= 100 Ak,, + Bkb -- K _ ; (12) " (13). The distribution ratios ka and kb are known and refer to the pure individual adds, whereas the distribution ratio K refers to the binary mixture. By solving these equations for B, the equations given in this section may be derived. Calculation ofAcetyl, Propionyl, and Butyryl Contents -- S 36. Calculation ,j 36.1 Calculate the percentages by weight' of :acetyl, j propionyl, and butyryl as follows: - .j Acetyl, %=ACim (14) ! Propionyl, % = (PC/100) X (57/43) (15) i Butyryl, % = (BC/100) X (71/43)> (16) where: -- A -- percentage of acetic add (Section 35), mol, P = percentage of propionic add (Section 35), mol, B -- percentage of butyric add (Section 35), mol, and C = percentages by weight of apparent acetyl (Sections 23 and 26). | 1 j J 36.2 Hydroxyl can be measured precisely, particularly at high degrees of esterification (Sections 38 to 44). It is therefore sometimes advantageous to base the calculation of weight percentages of acetyl, propionyl; and butyryl on hydroxyl content rather than on apparent acetyl as in 36.1. The equations for this calculation are as follows: j ' j For cellulose acetate propionates: Acetyl, % = 9.15^4(31.5 - A)/(786 -A) (17) Propionyl, % = 2.93P(31.5 - ft)/(786 - A) (18) 1 DUP050296675 i t i D 817 40. Significance and Use 40.1 Hydroxyl content is a measure of the free hydroxyl on the cellulose backbone of the polymer. Hydroxyl content has a strong effect on the polymer's solubility and physical properties. Hydroxyl content also impacts the propensity for this polymer to crosslink with various crosslinking agents. Acetyl, % = 4.884(31.5 - /j )/jkkl -A) ' Butyryl, % - 8.055(31,5- A)/(443 - A) (19) (20) Inhere, in addition to the definitions of terms in 36.1: h = weight percentage of hydroxyl (Section 44). mnop q--This calculation involves the assumption that there are I'exactly three hydroxyls, free plus esterified, for each aahydroglucose unit iof cellulose. $7. Precision and Bias .37.1 No statement,on bias can be made as no reference material is available as a standard., r stuvwxty'z{|}~|} 38. Scope 38.1 This test method is,applicable to pyridine-soluble J cellulose esters and is especially useful when the hydroxyl content is low. (Samples containing plasticizer may be analyzed directly by this test method because the plasticizer is removed during washing of the carbanilate). 39. Summary of Test Method 39.1 Hydroxyl in cellulose esters is determined by reac tion with phenyl isocyanate in pyridine solution under anhydrous conditions to form the carbanilate derivative. The derivative is then analyzed for its carbanilate content by ultraviolet absorption. 41. Apparatus 41.1 Spectrophotometer,379 complete with hydrogen light source and a set of four 1.00-cm quartz cells or an equally suitable apparatus. The wavelength calibration, as checked against a mercury lamp, shall be within the manufacturer's tolerances. As a further check, measure the density of a potassium chromate (K2Cr04) solution prepared as follows: Dissolve 0.0400 g of K2Cr04 or 0.0303 g of potassium dichromate (K2Cr207) in 0.05 N potassium hydroxide (KOH) solution and dilute to 1 L in a volumetric flask with 0.05 N KOH solution. Using the hydrogen lamp measure the absorbance at 280 nm of a silica cell filled with the K2Cr04 solution and also of the same cell, filled with water. The absorbance of the solution minus that of the blank shall be 0.723 0.023. 41.2 Bottles, 112-g (4-oz), with screw caps, for washing the samples. 41.3 Special Reflux Tubes for the carbanilation, con structed as follows (see Fig. 2): Make a test tube approxi mately 20 by 150 mm from the outer part ofa standard-taper 24/40 ground-glass joint by closing the open end in a blast lamp. Draw the tubing on the inner joint to a constriction just above the joint. Cut the glass at the point and seal on a short length of 8-mm tubing to provide a bearing for a glass stirrer. Make a stirrer of 4-mm glass rod with a semicircle at right angles to the shaft at the bottom and small enough to fit into the test tube. When properly constructed this unit acts as an air condenser, thus preventing the loss of solvent by evaporation. 41.4 Pipet, serological type, 5-mL capacity, graduated in O.l-mL divisions. 41.5 Buchner Funnel, of a size accommodating 90-mm filter paper. .- . 41.6 Automatic Shaker, with speed regulator mechanism. 41.7 ElectricOven, maintained at 105 3C. 41.8 Oil Bath, equipped with a rack to hold several of the special reflux tubes. This bath shall be kept between 115 and 120C. -- 42. Reagents 42.1 Acetone. 42.2 Ethyl Alcohol, Formula 2B, 3A, or 30 (denatured). 42.3 Methylene Chloride-Methyl Alcohol Mixture--Mix 9 parts by weight of methylene chloride with 1 part of methyl alcohol. This mixture should have an absorbance ofless than 0.2 at 280 nm in a 1.00-cm silica cell measured against air. Pure methylene chloride has an absorbance of about 0.05, but the commercial product may have an absorbance as high as 1.00. The methylene chloride and methyl alcohol should 7 A Beckman Model DU Spectrophotometer has been found satisfactory for this purpose. 155 DUP050296676 be selected to have low absorbance; otherwise, they should be redistilled. 42.4 Phenyl Isocyanate} 42.5 Pyridine, redistilled, of low water content, preferably less than 0.05 %. 43. Procedure 43.1 In the following procedure the phenyl isocyanate reagent shall be used under anhydrous conditions. Therefore, the sample, containers, pipet, and all other equipment shall be thoroughly dried. 43.2 Place a 0.5-g sample in a special reflux tube and dry in an electric oven at 105 3C for 2 h. Remove the tube from the oven, add 5 mL of pyridine, assemble the reflux apparatus complete with glass stirring rod, and place in the 115 to 120C oil bath. Stir occasionally until the sample is completely dissolved. Add 0.5 mL of phenyl isocyanate, stir thoroughly, and reflux in the oil bath for lA h to complete the reaction. Use 0; 1 mL of phenyl isocyanate for each 1 % of estimated hydroxyl content, but never less than 0.5 mL. 43.3 At the end of the reaction time, remove the sample and dilute it with acetone to the proper viscosity for precipitation. The amount of acetone used to thin the solution is a critical factor in acquiring a good precipitate. Samples having low viscosity require little, if any, dilution. The average sample requires the addition of about an equal volume of acetone. Precipitate the carbanilate by pouring the solution into about 200 mL of ethyl alcohol, or if the ester contains more than 20 percent propionyl or butyryl, into the same volume of cold 80 % alcohol. Stir the alcohol vigor ously during the precipitation. The precipitate should be fluffy and white. Sticky precipitates indicate too little dilu tion. Filter off the precipitate using paper on a Buchner funnel, with suction applied only as long as is necessary to remove the bulk of the solvent; prolonged suction may cause undesirable clumping together of the precipitate. 43.4 Wash the precipitate with alcohol, unless the sample was precipitated in cold 80 % alcohol. In this case, wash the precipitate in cold 90 % alcohol. Washing is best accom plished by transferring the precipitate to a 4-oz screw cap bottle containing about 75 mL of alcohol and shaking for % h on an automatic shaker. Filter, pressing out as much liquid as possible with a glass stopper. Repeat the washing and filtering operations twice more. 10--Samples of high hydroxyl content and large amounts of propionyl or butyryl may give gummy precipitates when poured into cold 80 % alcohol. Samples of this type give improved precipitates when precipitated in the reverse manner. Pour the diluted reaction solution into a 600-mL beaker, taking care to distribute the solution evenly on the bottom. Chill the beaker in a brine bath for 30 to 60 s. Pour about 200 mL of cold 80 % alcohol onto the chilled liquid. Wash the resulting precipitate and filter in the usual manner using cold 90 % alcohol. 43.5 Allow the precipitate to air-dry 1 to 2 h at room temperature with good ventilation or preferably overnight to ensure complete removal of the alcohol. (Samples wet with alcohol may sinter and stick to paper or glass when dried at 8 Phenyl isocyanate available as Eastman No. 553 has been found satisfactory for this purpose. 105'C.) Dry the sample at 105C in the oven for 1 h and in a desiccator. Small manila envelopes are convenient ij| drying and cooling the samples. | 43.6 Weigh 0.1231 g of the dry precipitate into a 100-ml volumetric flask fitted with a ground-glass stopper. Add 60 to 80 mL of methylene chloride-methyl alcohol mixture, aha shake occasionally until complete solution occurs. Dilute.t| 100 mL and mix thoroughly. Using the spectrophotometer with a 1-cm silica cell, measure the absorbance of the solution at 280 nm against the solvent mixture as a reference. 44. Calculations 44.1 Calculate the percentage of carbanilate, c, for a sample weight of 0.1231 g as follows:59* * * Carbanilate, % -- A k 17.1 (21) where: A -- absorbance. 44.2 Calculate the percentage of hydroxyl as follows: Hydroxyl, % = 14.3c/(100 - c) (22) 45. Precision and Bias 45.1 No statement on bias can be made as no reference material is available as a standard. . PRIMARY HYDROXYL CONTENT 46. Summary of Test Method 46.1 The primary hydroxyl content of cellulose ester is determined by formation ofthe triphenylmethyl (trityl) ether and measurement of the trityl group by ultraviolet absorbance.9 Trityl chloride reacts preferentially with pri mary hydroxyls. Since there is also a slight reaction with secondary hydroxyls, standardized reaction conditions are important.10 11 47. Apparatus 47.1 See Section 41. __ 48. Reagents 48.1 Acetone. --, 48.2 Ethyl Alcohol, Formula 2B, 3A, or 30'(denatured). 48.3 Methylene Chloride-Methyl Alcohol Mixture--Mix 9 parts by weight of methylene chloride with 1 part of methyl alcohol. This mixture should have an absorbance of less than 0.2 at 259 mm in a 1-cm silica cell measured against air; otherwise, the solvents should be redistilled. 48.4 Pyridine, redistilled to a water content less than 0.05 %. The water content may be reduced further by storing over a suitable drying agent, such as a molecular sieve.11 48.5 Trityl Chloride (Chlorotriphenylmethane or Triphe nylmethyl Chloride). 5 Malm, C. J., Tanghe, L. J., Laird, B. G, and Smith, G. D., "Determination of Total and Primary Hydroxyl in Cellulose Esters by Ultraviolet Absorption Methods," Analytical Chemistry, ANCHA, Vol 26, 1954, p. 189. 10 Malm, C. Tanghe, L. J., and Laird, B. C., "Primary Hydroxyl Groups in Hydrolyzed Cellulose Acetate," Journal of the American Chemical Society, JACSA, Vol 72, 1950, p. 2674. 11 Molecular Sieve Type 4A as manufactured by the Unde Air Products Co., has been found satisfactory for this purpose. 156 m wmmmm DUP050296677 D 817 eedure ^The reagents must be used under anhydrous condiItis imperative that the sample and all equipment be Sghly dry. Place a 0.5-g sample in the test tube of the special jjgpparatus and dry for 2 h at 105 3C, Add 5 mL of 'p, insert the top of the reflux apparatus and the and heat with stirring in a 115 to 120C oil bath, ie sample has dissolved, add 0.5 g oftrityl chloride. If il hydroxyl content exceeds 3%, use an additional j of trityl chloride for each additional 1 % hydroxyl. |e mixture thoroughly and reflux in the oil bath for y 2 h at 115 to 120C. Remove the tube and cool. Dilute the sample with acetone to the proper visjrfbr precipitation. The amount of acetone used to thin potation is a critical factor in obtaining a good precipi'Samples having low viscosity require little, if any, ion. The average sample requires the addition of about jual volume of acetone. Precipitate the trityl derivative louring the solution into about 200 mL of ethyl alcohol vigorous stirring. The precipitate should be fluffy and lie. Sticky precipitates indicate too little dilution. Separate | precipitate by filtering through paper on a Buchner ilnel, with suction applied only as long as necessary to hove the bulk of the solvent; prolonged suction may flporate the alcohol and cause the precipitate to partially jissolve in the remaining pyridine. 19.4 Wash the precipitate by transferring it to a 4-oz screw bottle containing 75 mL <?f ethyl alcohol, capping rely, and shaking for 'h h on a shaker at medium speed. collect the precipitate on a Bflchner funnel, pressing : as much liquid as possible with a glass stopper. Repeat us washing and filtering operation twice more, or until the bsorbance of the filtrate at 259 nm is about the same as that fan alcohol blank. Allow the precipitate to air-dry on the liter paper for lh h at room temperature with good ventilaPti, or preferably overnight, to remove most of the alcohol. ' amples wet with alcohol may sinter or stick to paper or dass when dried at 105C). Transfer the sample to a manila hvelope, dry it for 1 h at 105C, and cool in a desiccator. 4 49.5 Weigh a 0.123l-g sample of the dry trityl ether privative into a 100-mb volumetric flask fitted with a aund-glass stopper, and dissolve in the methylene chlorideethyl alcohol mixture. Dilute to 100 mL and mix thorBughly. Measure the absorbance, of this solution in a 1-cm Isilica cell using a spectrophotometer at 259 nm against the fsolvent as a reference. % 50. Calculation 50.1 Calculate the trityl content, t, for this concentration |i of 0.1 g/100 g and with a correction of 0.015 for the absorbance of the cellulose acetate as follows:8 Trityl, % = 2S.25(/1 - 0.015) (23) where: A = absorbance. 50.2 Calculate the weight percentage of primary hydroxyl as follows: Primary hydroxyl, % = 7.02 t/{ 100.4 - t) (24) 50.3 Calculate the percentage primary hydroxyl of the total hydroxyl as follows: Primary hydroxyl of total hydroxyl, % = {B[C) x 100 (25) where: B = value of primary hydroxyl as determined in 50.2, and C = value of total hydroxyl as determined in 44.2. SULFUR OR SULFATE CONTENT 51. Summary of Test Method 51.1 The sulfur or sulfate content of cellulose acetate is measured by oxidizing the sample in a nitric acid-perchloric acid mixture and determined gravimetrically as barium sulfate. To determine combined sulfur the sample must first be reprecipitated into dilute acid to remove noncombined sulfur compounds. 51.2 The sulfur or sulfate content may also be determined by Test Method D 2929, The X-ray method shall be cali brated against the chemical method following in Sections 53 to 54, and the sample shall be treated in accordance with 53.1, if combined sulfur is to be determined. 52. Significance and Use 52.1 Sulfur and sulfate content indicates the amount of sulfur in the cellulose ester either as inorganic salts (usually sulfates) or as organic sulfate (usually as sulfate ester com bined to the cellulose backbone). The presence of high levels of sulfur and sulfate can be detrimental to the melt stability of the ester. 53. Apparatus 53.1 Funnel, modified by cutting the stem off at the apex of the funnel and fire polishing. 53.2 Crucibles,12 30-mL, extra-fine porosity. 53.3 Oven, controlled at 120 to 125"C. 53.4 Muffle Furnace, controlled at 800 50C. 54. Reagents 54.1 Acetone. 54.2 Acetic Acid (1+49)--Mix 1 volume of.glacial acetic acid with 49 volumes of water. . ... 54.3 Barium Chloride Solution (100 g/L)--Dissolve 100 g of barium chloride (BaCl2-2H2C>) in water and dilute to 1 L. 54.4 Hydrochloric Acid ( 1+1)--Mix 1 volume,of concen trated hydrochloric acid (sp gr 1.19) with 1 volume of water. 54.5 Nitric Add (sp gr 1.42)--Concentrated nitric acid (HN03). 54.6 Nitric Acid (2+3)--Mix 2 volumes of concentrated nitric acid (sp gr 1.42) with 3 volumes of water. 54.7 NitricAcid-Perchloric Acid Mixture--Mix 5 volumes of concentrated HN03 with 1 volume of concentrated perchloric acid (HC104, 70 %). 54.8 Phenolphtkalein Indicator Solution (l g/100 ml)-- Dissolve 1 g of phenolphthalein in 100 mL of ethyl alcohol (95 %). 54.9 Silver Nitrate Solution (50 g/L)--Dissolve 50 g of silver nitrate (AgN03) in water and dilute to 1 L. 54.10 Sodium Carbonate (Na2C03). 54.11 Sodium Hydroxide Solution (400 g/L)--Dissolve ! Selas No. 3001 crucible has been found satisfactory for this purpose. 157 DUP0502 96678 400 g of sodium hydroxide (NaOH) in water and dilute to 1 L. 55. Procedure Treatment Prior to Analysis 55.1 Remove uncombined sulfur as follows (Note 11): Dissolve 25 g ofsample in approximately 300 mL of acetone, depending on the viscosity. Ifthe sample is oftoo high acetyl content to be directly soluble in acetone, cool in a dry ice cabinet overnight; then allow to come to room temperature while tumbling or stirring. Filter the solution, if necessary, through felt or a coarse sintered-glass crucible. Precipitate with rapid stirring into a beaker or pail containing 2 to 3 L of acetic arid (1+49). Filter through a cloth bag or a Buchner funnel and give two 15-min washes with water using mechanical agitation. A little Na2C03 may be added to the last wash to stabilize samples of high sulfur content. Filter and dry overnight at 60C. 11--To analyze for total sulfur content omit this treatment. Decomposition 55.2 Weigh 10 0.1 g of cellulose acetate and transfer to a clean wide-mouth, 500-mL Erlenmeyer flask. Add 50 mL of the HN03-HC104 mixture to the flask, and swirl the flask gently to wet the sample thoroughly. Place the modified funnel in the mouth of the flask and heat the flask carefully on a hot plate in a fume hood. 12: Precaution--Use the utmost care in handling the HNO3-HCIO4 mixture. If a spill occurs, wash down with plenty of water. Wear safety glasses or a face shield. 55.3 After the mixture becomes hot and less viscous, increase the heat of the hot plate. Continue the digestion until all the sample has been oxidized and the thick reddish-brown fumes of nitric oxide have been expelled. At this point, white fumes will appear and a rather vigorous reaction will occur that is caused by the last traces of organic material being oxidized and the nitric acid fuming off. 55.4 When this reaction starts, remove the flask from the hot plate, swirl gently for a few seconds, and set it on the shelf in front ofthe hood until the reaction is complete. Place the flask back on the hot plate and continue the digestion until the HC104 refluxes about half way up the side of the Erlenmeyer flask and about 5 mL is left in the flask. The HNO3-HQO4 mixture should be clear and colorless. If it is not, set the flask off the hot plate to cool and then add 3 to 5 mL of HN03 (sp gr 1.42). Replace the flask on the hot plate and continue heating until the HC104 refluxes half way up the flask. Remove the flask from the hot plate and allow the flask and its contents to cool. Determination ofBarium Sulfate 55.5 Wash the modified funnel top thoroughly with water, collecting the rinsings in the flask. Add 50 mL of water. Swirl the flask to mix the solution thoroughly. Add 2 drops of phenolphthalein indicator solution and neutralize the acid with the NaOH solution to a faint pink. Acidify immediately with HC1 (1+1), dropwise, until the solution is just arid to phenolphthalein; then add 2 mL of HQ (1+1). 55.6 Filter through a 12.5-cm fine-porosity paper into a clean 400-mL beaker. Wash the flask thoroughly with water, filtering the washings through the paper. Finally wash the paper thoroughly with ten portions of hot water. Dilute filtrate to approximately 200 mL. Place the beaker on the hff plate and heat almost to boiling. Slowly add 10 mL of BaQj solution from a pipet, stirring the solution during tip addition. Do not add the BaCl2 solution rapidly, as from a graduate, since the rapid addition will produce an impuxg precipitate. Remove the stirring rod from the beaker and; wash it with a stream of water from the wash bottle,' collecting the washings in the beaker. Cover the beaker with a watch glass and keep the mixture near the boiling temperature for 6 h or overnight. Do not allow the liquid to evaporate to dryness. 55.7 Using suction, decant the supernatant liquid through an extra-fine porosity porcelain filter crucible that has been previously rinsed with acetone, ignited, and weighed to the nearest 0.1 mg. Transfer the precipitate with the aid of a stream of hot water. Always use a stirring rod in this transfer. Scrub the sides and bottom of the beaker with a rubber policeman to remove any adhering precipitate. The crucibles may be used to collect several precipitates one on top of the other. Close control of temperature and time of heating and cooling are necessary. Cleaning with hot water is generally sufficient; drastic attack with cleaning solution should be avoided. 55.8 Wash the precipitate on the filter until free of chlorides by the following test: To 5 mL of wash water, collected in a separate test tube or on a watch glass, add i mL of HN03 (2+3) and 1 mL of AgN03 solution. The appear ance of a milky white precipitate indicates the presence of chlorides, and the washing should therefore continue until the test is negative. Do not attempt to. get a completelynegative test for chloride. Discontinue washing when no more than a faint opalescence is produced in the test. 55.9 Finally pour a few millilitres of pure acetone through the filter and suck it dry. Place the crucible in a larger crucible or in a metal tray with perforated sides and bottom for protection and place it in an oven at 120 to 125C for 1 h. Do not handle the crucibles with the fingers between ignition and the completion of weighing; use forceps. 55.10 Remove the crucible from the oven and ignite it for 10 min in a muffle furnace at 8(Kr 50C. Cob! in a desiccator for-75 15 min and weigh to the nearest 0.0001 g. It is permissible to return the crucible to the oven for at least 15 min before transferring to the desiccator* 55.11 From time to time, and especially when using new reagents, run a blank in duplicate in the reagents. If the weight of the precipitate exceeds 0.0005 g, investigate and eliminate the cause. This is equivalent to an error of0.002 % on a 10-g sample. 56. Calculation 56.1 Calculate the percentage of sulfur and sulfate as follows: Sulfur, % = {[(C-- B) -<- D)] x 0.1374/4} x 100 (26) Sulfate, % = {[(C - B) - (E - JO)] x 0.4115/4} x 100 (27) where: A = weight of sample, g, B = weight of crucible for sample, g, C = weight of crucible and BaS04 for sample, g, C - B = weight of BaS04 for sample, g. 158 m* DUP050296679 D 817 = weight of crucible for blank, g, = weight of crucible and BaS04 for blank, g, and ?== weight of BaS04 for blank, g. E HEAT STABILITY unary of Test Method W The heat stability ofa cellulose ester is one indication ^^feuality. It is measured by heating the sample for a Hffinfiad time and temperature, observing it for amount and Igmity of color developed, and possibly also measuring ssof viscosity as a result of heating. Suggested times of j are 8 h at 160C, 8 h at 180C, or 2 h at 190C. The pEnd temperature of heating, method of grading, and jUre matters for agreement between the purchaser and IpSier, ^Significance and Use 3.1 The heat stability of a cellulose ester is one indication |ts quality. Apparatus fp9.1 Heater Block--A metal block of suitable size heated ically and maintained at the specified temperature hin rC. This is best accomplished by providing continpus heat to hold the temperature a few degrees below the ferified temperature, and providing intermittent additional at thermostatically controlled. Holes shall be drilled in the i of the block to hold test tubes, a thermoregulator, and a permometer. The block should be insulated. |59.2 Test Tubes, either 18 by 150-mm or 20 by 150-mm, l with corks. The corks shall be fitted with glass tubes the i of the cork and 4 mm in inside diameter or shall have J|:small V-shaped notch of equivalent cross-section cut in a pfertical position. f Solvent 60.1 Methylene Chloride-Methyl Alcohol Mixture--Mix 9 jjparts by weight of methylene chloride with 1 part of methyl alcohol. f 61. Heat Treatment 61.1 Place the sample, ground to pass a No. 20 (841-pm) sieve, in a clean, dry test tube and pack it firmly and K uniformly. Stopper with a cork having a notch or tube as $ described in 59.2. Heat the Tube and contents for 8 h at ^ 180C or as otherwise specified. and renewed if necessary every 6 months. 63. Solution Color Using Platinum-Cobalt Standards 63.1 Heat a 1-g sample for the specified time and temper ature and, after cooling, examine for charred or decomposed spots. Dissolve the heated sample in 15 mL of the methylene chloride-methyl alcohol mixture. Compare the color of the solution (viewing transversely) with test tubes of platinum-cobalt color standards, prepared as described in Section 80. (It may be necessary to prepare standards having as much as 2000 ppm of platinum for this purpose jor- to dilute the sample solution before grading.) 64. Solution Color by Spectrophotometer ~ 64.1 The.color of the solution prepared'as described in Section 63 may also be measured spectrophotometrically. Measure the absorbance at 400 nm against the solvent, using a suitable spectrophotometer with a 1-cm silica cell. 65. Viscosity Change || 62. Dry Color Evaluation 62.1 Examine the heated sample for uniformity of color ! and for the presence of charred or decomposed spots. 5 { Compare the color of the material at the bottom of the tube ;f with standards prepared as follows: Heat portions of a check , j batch of similar particle size, representative quality and I stability, and accepted by mutual agreement between the if purchaser and the seller. Pack portions of this check batch If firmly in each of twelve clean, dry test tubes and stopper with 1 corks as described in 59.2. Heat the tubes at 180C, or as if otherwise specified, remove one tube each 2 h, and mark the | time of heating in hours on each tube. This set of numbered tubes serves as the color standards. They should be checked 65.1 Measure the limiting viscosity number of the heated sample and of an unheated sample as described in Sections 67 to 71 of this test method. The percentage loss of viscosity as the result of heating is a measure of heat stability. 66. Precision and Bias 66.1 No statement on bias can be made as no reference material is available as a standard. 13 Wagner, R. H., and Russell, John, "Capillary Tube Viscometer for Routine Measurement of Dilute High Polymer Solutions," Analytical Ckemistry, Vol 20, 1948, pp. 151-7. & 159 DUP050296680 D 817 r TABLE 1 Solvents for Limiting Viscosity Number Determination Solvent^ Ingredients. % by weight Value of k for Cal culation (71.2) A B CorD E F 90 % acetone 10 x ethyl alcohol acetone 90 % methylene chloride 10 X ethyl alcohol 98 X acetone 4 X water 90 % methylene chloride0 10% methanol* 10 10 3 10 3 * Solvent designations conform to those used in Table 2 for viscosity determinations. B Acetone (99.4 :fc 0.1 X) containing 0.3 to 0.5 * water and under 0.3 X ethyl alcohol. Ethyl alcohol {95 % by volume). Formula 2B or 3A denatured ethyl alcohol may be used. Methylene chloride having a boiling range of 39.2 to 40.0C and less than 0.001 X acidity calculated as HCI. 'Methyl alcohol (sp gr 20/20'C = 0.785 to 0.795). LIMITING VISCOSITY NUMBER 67. Summary of Test Method 67.1 Limiting viscosity number, expressed in millilitres of solution per gram of solute, is determined by measuring the flow times of a solution of known concentration and also of the solvent used and making a calculation by means of the modified Baker-Philippoff equation. 67.2 Intrinsic viscosity, expressed in decilitres per gram of solute, is determined in the same way by expressing c in grams per 100 mL in 71.2. Limiting viscosity number is thus 100 x intrinsic viscosity. 68. Significance and Use 68.1 Limiting viscosity number can be used to estimate the molecular weight of a cellulose ester by using the Mark-Houwink equation and constants measured for the solvent, temperature, and ester of concern. 69. Apparatus 69.1 Capillary Viscometer, such as the Wagner apparatus (see Fig. 3) or an Ostwald-Fenske-Cannon pipet, that will give a flow time for the solvent of not less than 70 s. 69.2 Water Bath--A constant-temperature water bath controlled at 25.0 0.1C and with a pump for circulating the water through the viscometer jacket or tank. 69.3 Stop Clock or Watch, calibrated in Vio s. 70. Procedure 70.1 Sample Preparation--Dry about 0.26 g of sample in a weighing bottle at 105 3C for 2 h, stopper, and cool in a desiccator. Weigh the bottle containing the sample to the nearest 0.001 g, transfer the sample to a 250-mL flask, and reweigh the bottle. Pipet into the flask 100 mL of solvent at 25 0.1 "C. The solvent used should be mutually agreed upon by the purchaser and the seller. Suitable solvents are listed in Table 1. After the sample is completely dissolved, place it in the constant-temperature bath at 25C along with a portion of the solvent used, and allow sufficient time for both to come to temperature before making the viscosity measurements. During this conditioning period, water at TABLE 2 Solutions for Viscosity Determination Formula A B C- D E F Ingredients, Weight X Cellulose ester Acetone Acetone. 96 percent Water, 4 percent Ethyl alcohol Methyl alcohol Methylene chloride0 20 20 20 15 20 10 72 80 ... 80 8 8 8.5 9 72 76.5 81 Typical Solution Densities, g/mL at 25CC 0.85 0.86 1.25 1.23 0.36 1.24 Suitable for most mixed esters having less than about 40 % acetyl and more than about 8 % propionyl or butyryl. 'Suitable for most of the commercial cellulose acetate propionates and acetate butyrates. c Suitable for most of the commercial cellulose acetate propionates and acetate butyrates. Particularly good for esters containing more than 40 % acetyl. Acetone (99.4 0.1 %) containing 0.3 to 0.5 x water and under 0.3 % ethyl alcohol. e Ethyl alcohol {95 % by Vol). Formula 2B, 3A, or 30 denatured ethyl alcohol may be used. F Methyl alcohol (sp gr 20/20C = 0.785 to 0.795). 0 Methylene chloride having a boiling range of 39.2 to 40.0'C and less than 0.001 % acidity calculated as HCI. i j 25C should be circulating through the water jacket of the I viscometer to allow ample time for the pipet to reach temperature equilibrium. 10.2 Viscosity Measurements--Rinse the reservoir and | the outside of the capillary tube thoroughly with solvent, j Rinse the inside of the capillary tube twice by alternately applying pressure at points B. and A (see Fig: 3). Discard the -j wash portion of the solvent. Pour more solvent into the 1 reservoir and allow several minutes for-complete drainage and thermal equilibrium to be obtained. Adjust the outer ? meniscus to a reference point, D, that will give a flow time between 70 and 100 s. Apply air pressure at B to force, the solvent up through the capillary past the upper timing mark, C, on the measuring bulb, E. Record the time in seconds i required for the meniscus to fall between the timing marks, C and F. Take a minimum of two. readings. Repeat these operations, substituting the solution for the-solvent. | 71. Calculation j 71.1 Calculate the viscosity ratio, j j /j )0 as follows: j Viscosity ratio = tjt2 (28) 1 where: f, = efflux time of solution, and t2 = efflux time of solvent. 13--Smelly, the viscosity ratio is defined as nhta where v and no are the viscosities of the solution and solvent, respectively, and are related to the corresponding efflux times by: r\-Cl- Ep/t2 ' (29) t y0 = Cl0 - Efi0/`<i2 (30) where: C and E are constants for the particular viscometer used. The equation in 71.1 follows if the second term in these relations, a kinetic energy correction, is negligible and the respective solvent and solution densities, p0 and p, are substantially equal. 71.2 Calculate the limiting viscosity number, fa], as fol lows: 160 iv DUP050296681 D 817 Clear gkm COLOR AND HAZE 77. Summary of Test Method 77.1 Color and haze determinations on cellulose ester solutions are made by comparison with standards. Simulta neous measurement of these properties is desirable because haze reduces the amount of color observed. 78. Significance and Use 78.1 Solution color and haze of a cellulose ester is a measurement of the optical properties of cellulose esters when dissolved in a specific solvent. ebo located in <evr FIG. 4 Color and Haze Apparatus [] = (k/c)[antilog ((log nhaW - 1] (31) alere: values from Table 1 (Note 14), and concentration in g/mL. 14--Different values may be used by agreement between the iurchaser and the seller. ,71.3 Calculate intrinsic viscosity, ij, in accordance with %X but express c in grams per 100 mL. 72. Precision and Bias 72.1 No statement on bias can be made as no reference aaterial is available as a standard. VISCOSITY 173. Significance and Use . 73.1 A measurement of viscosity is of great practical futility in determining the proper processing equipment and 1 process concentrations for cellulose esters. 74. Procedure 74.1 Solution--Dry the sample for 1 to 2 h at 105 3C ; and cool in a desiccator. Prepare a solution of the dried sample in a solvent and at a concentration mutually agreed upon by the purchaser and thfe seller. Suitable solutions are listed in Table 2. 74.2 Viscosity Determination--Prepare the solution and measure the viscosity in accordance with Test Method D 1343, (see Note 16 in Section 81). 75. Report 75.1 Report the results in poises, unless otherwise speci fied. The viscosity value shall be prefixed with the letter A, B, C, etc., corresponding to the formula of the solution em ployed. 76. Precision and Bias 76.1 No statement on bias can be made as no reference material is available as a standard. 79. Apparatus 79.1 Light Box--A suitable light box (Fig. 4) is described as follows: The light source consists of a mercury vapor bulb14 1w5 hich requires an autotransformer13 for the current source. The bulb is mounted horizontally across the lower front part of a plywood box 356 mm (14 in.) wide, 430 mm (17 in.) high, and 330 mm (13 in.) deep. This box is lined with a heat resistant board and is painted black inside, except that the inside back surface toward the viewer is white. A bottle holder large enough to hold four bottles is built onto the front of the light box, and a 64 by 150-mm (2lh by 6-in) horizontal viewing hole is cut through the Front of the box. This opening is covered with clear glass, and a 6-mm (V-t-in.) strip of black tape is fastened to the glass horizontally to aid in judging haze in the solution. Holes are cut in the bottom and top of the box for cooling by air convection. For continuous use, forced circulation of air would be desirable. A black metal baffle over the bulb prevents direct light on the viewing glass.16 79.2 Sample Bottles--The bottles used for the sample solutions are French square bottles, 470-mL (16-oz), with screw caps. These same bottles may be used for the color and haze standards.17 15--These bottles may also be used for determination of viscosity, as described in 74.2. 79.3 Cap Liners--Cap liners shall be ofa composition Hot affected by the solvents used. Liners ofjfiber'board covered with cellophane or aluminum foil are usually satisfactory, but vinyl resin-or waxed liners may cause interference with viscosity, color, or haze measurements. 80. Reference Standards 80.1 Color Standards--A color standard containing 500 ppm ofplatinum may be purchased or the solution may also be prepared as follows: Dissolve 1.245 g of potassium platinum chloride (K2PtCl6), containing 0.500 g.of platinum, and 1.000 g of crystallized cobalt chloride (CoCl2-6H20), 14 A General Electric mercury vapor bulb Type H-250, A5-1, or A37/51 (differing only in the shape of the glass globe) has been found satisfactory for this purpose. 15A General Electric Autotransformer Model 9T64Y2I has been found satisfactory for this purpose. 16 A detailed drawing of the color and haze apparatus may be obtained from ASTM Headquarters. Request Adjunct No. 12-408170-00. 17 Owens-Illinois French square bottles No. A6732 with No. 48-400 caps have been found satisfactory for the sample solutions, viscosity, and for the color and haze standards, although for the color and haze standards, No. A6720 bottles with No. 28-400 caps are more convenient DUP050296682 D 817 containing 0.248 g of cobalt, in water, add 100 mL of HC1 (sp gr 1.19), and dilute to 1 L with water. Prepare standards containing 50, 60, 70, 80, 90, 100, 125, 150, 175, 200, 250, 300,350, 400 and 500 ppm of platinum by diluting suitable aliquots ofthe standard solution to 500 mL with water. Place these standards in the special bottles (see 79.2), taking care to select bottles with good clarity and free of flaws. Label and cap tightly. 80.2 Haze Standards--Prepare haze standards by diluting a stock solution having a turbidity of 1000 ppm. Prepare bottles containing 10,20, 30,40, 50,60,70,80,90,100,125, 150, 175, 200, and 400 ppm of turbidity, label, and cap tightly. 16--The previously recommended stock solution for pre paring these standards was made from fuller's earth, water, and hydrochloric acid. This solution is no longer available. A comparable stock solution can be made using diatomaceous earth,'8 To obtain haze levels equivalent to the fuller's earth standard, 1.1 parts ofdiatomaceous should be used in place of 1.0 parts of fuller's earth in preparing the aqueous suspension. No hydrochloric acid is needed'. 81. Procedure 81.1 Prepare the solution to be graded by dissolving the cellulose ester in the specified amount and kind ofsolvent, in one of the square bottles. See Table 2 for suitable solutions. At least 350 mL are required. Tumble until a uniform solution is obtained. Allow the solution to stand until it is '"Celite, available from John-Mansville Filtration and Mineral Division, Ken-Caryl Ranch, Denver, Co. 80217, has been found suitable for this purpose. free of bubbles before grading it for color and haze. 81.2 Place the bottle containing the solution to be graded' at the front of the shelf on the apparatus and place a similar bottle containing water behind it. Place the freshly shaken haze standard at the front of the shelf beside the bottle containing the soiufion*;to be festfed and place the color ^ standard behind it Determine the amount of color and h^c in the solution by, changing (he color and 'haze standards until as good a match as po&ible has beeg obtained. The haze standards settle out quickly so they must be reshaken at short intervals. Report results in parts per million for both color and haze. --When viscosity, color, and haze Setermi^Mdns, and ansj observation of general appearance are to be made on a cellulose ester'' sample, a considerable saving in time can be made by using one^solutioa in a square bottle for all three determinations.^^ thh cellulose ester as required for the viscosity determination, prepare the solution carefully, and allow the bottle to stand long enough to form a thick solution before tumbling, to avoid solvent loss. around the cap. Use a large enough sample to provide at least 350 mL of solution in the bottle. Measure the viscosity as described in Test Method D 1343. 82. Precision and Bias 82.1 No statement on bias can be made as no reference material is available as a standard. 83. Keywords 83.1 apparent acetyl; ash; cellulose acetate butyrate; cellu lose acetate propionate, cellulose esters; color, free `acidity; haze; hydroxyl; limiting; partition; sulfate content; viscosity TheAmerican 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 at this standard are expressly advised t/iaf determination of the validity of any.such patent rights, and the risk ofinfringement of siich 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 If not revised, either reapproved or withdrawn. Your comments areInvitedeither 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. If you feel diet your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standerds, 1916 Race St., Philadelphia, PA 19103. "'< 162 m DUP050296683 Designation: D 867 - 81 (Reapproved 1986)61 Standard Specification for Pumice Pigment1 This standard is issued under the fised designation D 867; the number immediately following the designation indicates the year of original adoption or, m 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 revision or reapproval. l Editorial change* were made throughout in April 1986. _____ _________________________________ _____ 11.1' This specification covers vesicular pumice suitable for Mia in the manufacture of organic coatings. jlf.2 Two types of material are described: jil.2.1 Type.A--For traffic paint EgO',2 Type B--For nonskid deck print. ^Referenced Documents jp.l ASTMStandards: I 718 Test Methods for Analysis of Aluminum Silicate I" Pigment2 D3360 Test Method for Particle Size Distribution by j Hydrometer ofthe Comihoh White Extender Pigments2 | Composition and Properties 3.1 The pigment shall be definitely vesicular and shall conform to the following requirements: ptoss os ignition, max, % ,, Moisture and other volatile matter, max, % i ***** Sieve analysis S.O 1.0 . . see Table 1 3.2 The color shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 3.3 When viewed under the microscope, or as photo graphic mounts, at a magnification ofat least 100 diameters, the sample shall exhibit no more nonvesicular particles than, ** I 1 This specification is under thejurisdiction ofASTMCoinmitteeD-1 on-Pamt and Related Coatings and Materials and isthe direct'responsibility of Subcom- rf mittee DO1.31 on figment Specification* Cunent edition approved Aug, 28, 1981. Published October 1981. Originally published as D 867 - 46 T. Last previous edition D867 - 48 (1976). tr 2 Annua! Book ofASTM Standards, Vol 06.02. a reference sample mutually agreed upon by the purchaser and the seller. 3.4 Pumice for use in paints shall be equal in mechanical analysis to a reference sample mutually agreed upon by the purchaser and the seller. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack; or other unit of: production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (3000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, or after blending in equal quantities, the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with Methods D 718, except that for sieve analysis the appropriate sieves, given in Table 1 of this specification, shall be used. 5.2 Particle Size--Test Method D 3360. TABLE 1 Sieve Analysis Requirements Sieve . . Percent Passing ... No. 60 (300 pm) No. 100(160 jun) Retained on No. 50 <300 pm) No. 100 (160 pm) -- Min 70 ... Max. 0 30 Pumice Pigment for Nonskid Deck Paint--Type B No. 40 (425 pm) ... NO. 40 (425 pm) No. 60 (250 pm) 20 No. 60 (250 pm) No. 100 (160 pm) No. 80 (180 pm) .2.6. 1 60 60 10 ' 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 entirety their own responsibility. , 5i This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and IIhotrevised, 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 A technical committee, which you may attend. If you feat that your comments have not received a fair hearing you should make your - views known to the ASTM Committee onStandarda, 1916 Race St., Philadelphia, PA 19103. } DUP050296684 # Designation: D 871 - 91 Standard Test Methods of Testing Cellulose Acetate1 This standard is issued under the fixed designation D 871; 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 These test methods cover procedures for testing cellu lose acetate. 1.2 The test procedures appear in the following sections: - Sections Ash Color and Haze Combined Acetyl or Acetic Acid Content Test Method A. Solution Method Test Method B. Heterogeneous Saponification Method Free Acidity Heat Stability Hydroxyl Content Intrinsic Viscosity Moisture Content Primary Hydroxyl Content Sulfur or Sulfate Content Viscosity 8 and 11 68 to 72 17,19 to 23 17,24 to 26 12 to 16 47 to 56 27 to 33 57 to 62 4and 7 34 to 39 40 to 45 63 and 66 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 Imitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water12 D1343 Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method3 D2929 Test Method for Sulfur Content of Cellulosic Materials by X-Ray Fluorescence3 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.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. 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.36 on Cellulose and Cellulose Derivatives. Current edition approved Feb. 22, 1991. Published April 1991. Originally published as D 871 -46. Last previous edilion D 871 -72 (1983). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 06.02. 4 "Reagent Chemicals, American Chemical Society Specifications." Am. Chem ical 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 Nostrand Co., Inc, New York, N. Y, and the "United States Pharmacopeia." 3.2 Unless otherwise indicated, references to water shall be understood to mean reagent tared, low, wide-form weighing bottle and water, conforming to Specification D1193. s MOISTURE CONTENT 4. Significance and Use 4.1 Moisture content of the cellulose ester can be used to estimate the dry weight of the cellulose ester. Since cellulose esters are desiccants, their moisture content can vary greatly depending on storage. 5. Procedure 5.1 Transfer about 5 g of the sample to a tared, low, wide-form weighing bottle and weigh to the nearest 0.001 g. Dry in an oven for 2 h at 105 3 C. Remove the bottle from the oven, cover, cool in a desiccator, and weigh. 6. Calculation 6.1 Calculate the percentage of moisture as follows:. Moisture, % = (AjB) X 100 where: A - weight loss on heating, g, and B -- sample used, g. -. 7. Precision and Bias _ 7.1 No statement on bias can'be made as no reference material is available as a standard. ASH ' ' ", __ M 1 1 I J I 1 I 8. Significance and Use 8.1 Ash content gives an estimate ofthe inorganic content of cellulose, ester .samples. The presence ofbigh levels of inorganic content (ash) can be detrimental to the melt stability and optical clarity of a cellulose ester in melt processing or act as a potential source 6f insolubles when the ester is used in solution. j j : ; 9. Procedure 9.1 Dry the sample for 2 h at 105 3G and weigh 10 to 50 g, to the nearest 0.01 to 0.1 g, depending on its ash content and the accuracy desired. An air-dried sample may be used and calculated to dry weight using the value for moisture determined as in Sections 5 and 6. Bum directly over a flame in a 100-mL tared platinum crucible that has been heated to constant weight and weighed to the nearest 0.1 mg. Add the sample in portions if more than 10 g is taken. The sample should bum gently and the portions should be added as the flame subsides. Continue heating with a burner only as long as the residue bums with a flame. 164 DUP050296685 D 871 |fer the crucible to a muffle furnace and heat at 550 to : for 3 h, or longer if required, to bum all the carbon. I the crucible to cool and then transfer it, while still Jj, to a desiccator. When the crucible has cooled to room jjerature, weigh accurately to the nearest 0.1 mg. W{Calculation '.1 Calculate the percentage of ash as follows: Ash, % = (A/B) x 100 Jte: Jpash, g, and -sample used, g. tip Precision and Bias p.l' No statement on bias can be made as no reference Snperial is available as a standard. Sf" : FREE ACIDITY Significance and Use 12.1 Free Acidity is a measure of unesterified organic acid a the ester. The presence of high levels of free acid is ptentially detrimental to the melt processing of the ester ad can impact the odor of the ester. |3o Reagents 13.1 Phenolphthalein Indicator Solution (1 g/100 mL)-- solve 1 g of phenolphthalein in 100 mL of ethyl alcohol 95 %}. Ijh 13.2 Sodium Hydroxide, Standard Solution (0.01 N)-- epare and standardize a 0.01 N solution of sodium hydroxide (NaOH). |14. Procedure 14.1 Shake 5 g of the sample, ground to pass a No. 20 1(850 pm) sieve and corrected for moisture content if jjpecessary, in a 250-mL Erlenmeyer flask with 150 mL of ifreshly boiled, cold water. Stopper the flask and allow it to istand for 3 h. Filter off the cellulose acetate and wash it with 1'water. Titrate the combined filtrate and washings with 0.01 N NaOH solution, using phenolphthalein indicator solution. 14.2 Run a blank determination on the water, using the : same volume as was used in extracting the sample. 15. Calculation 15.1 Calculate the percentage of acidity as free acetic acid as follows: Free acetic acid, % = {{A -- B)N X 0.06 x 100]/W' (1) where: A = NaOH solution used to titrate the sample, mL, B = NaOH solution used to titrate the blank, mL, N = normality of the NaOH solution, and Igi: W -- sample used, g. 16. Precision and Bias 16.1 No statement on bias can be made as no reference material is available as a standard. * COMBINED ACETYL OR ACETIC ACID CONTENT 17. Scope 17.1 Two test methods are described for determining the combined acetyl or acetic acid content. The first, described in Sections 19 to 22, is more precise, but less widely applicable, than the method described in Sections 24 to 26. 18. Significance and Use 18.1 Acetyl or acetic acid content is a measure of the amount of acetic acid esterified onto the cellulose backbone of the polymer. The amount of substitution of acetate ester has a very strong effect on the polymer's solubility and physical properties. Test MethodA--Solution Method 19. Apparatus 19.1 Weighing Bottle, glass-stoppered, 15-mL capacity, 25-mm diameter by 50-mm high, 19.2 Tray, copper or aluminum, approximately 5% in. (136.5 mm) square, containing 25 compartments 1 in. (25.4 mm) square. Each compartment shall have the correct dimensions to contain one weighing bottle. The entire tray shall fit inside a desiccator and should have a basket-type handle to facilitate the introduction and removal of the tray (convenient but not essential). 19.3 Buret, automatic zero, 35-mL, 25-mL bulb, stem graduated from 25 to 35 mL in 0.05-ml increments; or pipet, automatic zero, 30-mL, for 1.0 N NaOH solution. 19.4 Buret, automatic zero, 15-mL, 10-mL bulb, stem graduated from 10 to 15 mL in 0.05-mL increments, for ! N 2s o 19.5 Buret, 5-ml, in 0.01 or 0.1-mL divisions, for back titration with 0.1 IV NaOH solution. 19.6 Magnetic Stirrer, for single flask. 19.7 Magnetic Stirrer, capacity twelve or more flasks. 19.8 Stirring Bars, stainless steel Type 416, length 50 mm, diameter 5 to 6 mm, or equivalent, dimensions not critical. 20. Reagents 20.1 Acetone--Add one 30-mL portibn of 1.0 N NaOH solution to a mixture of 150 mL acetone and 100 mL hot water, allow to stand with frequent swirling for 30 min, and titrate with 1.0 N H2S04. Add another 30-mL-portion of 1.0 N NaOH solution to 100 mL of hot water, allow to stand for 30 min, and titrate. The difference between the two titrations shall not exceed 0.05 mL., 20.2 Dimethyl Sulfoxide. 20.3 Pyridine. 20.4 Sodium Hydroxide Solution (40 g/L)--Dissolve 40 g of sodium hydroxide (NaOH) in water and dilute to 1 L. 20.5 Sodium Hydroxide, Standard Solution (0.1 JVHPrepare and standardize a 0.1 A solution of NaOH. 20.6 Sulfuric Acid (1.0 N)--Prepare and standardize a 1.0 N solution of sulfuric acid (H2S04), 20.7 Phenolphthalein Indicator Solution (1 g/100 mL)-- Dissolve 1 g of phenolphthalein in 100 ml of ethyl alcohol (95 %). 21. Procedure 21.1 Dry 1.9 0.05 g of the ground well-mixed sample in D0 PO50296686 # D871 a weighing bottle for 2 h at 105 3C and weigh the dried sample by difference to the nearest 1 mg into a 500-mL wide-mouth Erlenmeyer flask. Prepare a blank by drying approximately 3.8 g of potassium acid phthalate and weighing it by difference into a flask as described. Carry the blank through the entire procedure. I--Potassium acid phthalate is used so that the concentration of the NaOH in contact with the solvent in the blank will be approximately the same as that in contact with the sample and so that the titration of the blank will be approximately the same as the titration of the sample, thus avoiding errors caused by using a different buret for the titration of the blank and the sample or by refilling the 15-mL buret If desired, however, the potassium acid phthalate may be omitted. 21.2 If the acetyl content is 32 to 41 % or the acetic acid content is 45 to 57 %, put the sample into solution as follows: Add 150 mL ofacetone and 5 to 10 mL ofwater and swirl to mix. Stopper the flask and allow it to stand with occasional swirling until solution is complete. Solution may be hastened by magnetic stirring or by any suitable mechan ical shaking that will provide a gentle rocking type of agitation to avoid splashing the solution on the stopper. It is essential that complete solution be effected. Proceed in accordance with 21.4. 21.3 Ifthe acetyl content is 41 to 44.8 % or the acetic acid content is 57 to 62.5 %, dissolve the sample by either of the following two methods: 21.3.1 Gently rotate the flask by hand to distribute and spread the sample in a thin layer over the bottom ofthe flask. Add 70 mL of acetone to the flask and swirl gently until the sample particles are completely wetted and evenly dispersed. Stopper the flask and allow it to stand undisturbed for 10 min. Carefully add 30 mL of dimethyl sulfoxide from a graduate to the flask, pouring the solvent down the sides of the flask to wash down any sample particles clinging to the side. Stopper the flask and allow it to stand with occasional swirling until solution is complete. Magnetic stirring or gentle mechanical agitation that will not splash the solution is recommended. When solution appears to be complete, add 50 mL of acetone and swirl or stir for 5 min. Proceed in accordance with 21.4. 21.3.2 Dimethyl sulfoxide is the preferred solvent, but if it is not available, spread the sample in a thin layer over the bottom of the flask, add 15 mL of acetone, swirl to wet the particles with acetone, stopper the flask, and allow the mixture to stand undisturbed for 20 min. Add 75 mL of pyridine without shaking or swirling, and allow to stand for 10 min. Heat the solution just to boiling and swirl or stir for 5 min. Again heat to boiling and swirl or stir for 10 min. Continue to heat and stir until the mixture is homogeneous and all large gel masses are broken down into individual highly swollen particles. When these highly swollen gel particles are well dispersed and are not fused together in large gel masses, no further heating is necessary. Cool the flask, add 30 mL ofacetone, and swirl or stir for 5 min. Proceed in accordance with 21.4. 21.4 Add 30 mL of NaOH solution (40 g/L) with constant swirling or stirring to the solution of the sample and also to the blank. Use of a magnetic stirrer is recommended (Note 2). It is absolutely necessary that a finely divided precipitate of regenerated cellulose, free from lumps, be obtained. Stopper the flask and let the mixture stand with occasional swirling, or stir on the magnetic stirring unit. Allow 30 min . for saponification of lower acetyl samples, 2 h for high acetyl,! samples when dimethyl sulfoxide is the solvent, and 3 hi when pyridine is the solvent. At the end of the saponification period, add 100 mL of hot water, washing down the sides of the flask, and stir for 1 or 2 min. Add 4 or 5 drops of phenolphthalein indicator solution and titrate the excess NaOH solution with 1.0 N H2S04 (Note 3). Titrate rapidly with constant swirling or stirring ring until the end point is reached; then add an excess of 0.2 or 0.3 mL of H2S04. Allow the mixture to stand with occasional stirring or preferably stir on the magnetic stirrer for at least 10 min. Then add 3 drops of phenolphthalein indicator solution to each flask and titrate the small excess of acid with 0.1 N NaOH solution to a persistent phenolphthalein end point. Take extreme care to locate this end point; after the sample is titrated to a faint pink end point, swirl the mixture vigor ously or place it for a moment on the magnetic stirrer. If the end point fades because of acid soaking from the cellulose, continue the addition of 0.1 TV NaOH solution until a faint persistent end point remains after vigorous swirling or stirring. Titrate die blank in the same manner as the sample. 2--While the amount of magnetic stirring is somewhat op tional, such stirring during the entire period of the determination is strongly recommended. Solution is more rapid, titrations are more rapid, and the end point can be approached directly and without a back titration. 3--It is important to correct all 1.0 N H2S04 buret readings for temperature and buret corrections. 22. Calculation 22.1 Calculate the percentage by weight of acetyl and acetic acid as follows: Acetyl or acetic acid, % = [(Z> - C)Na + (A- B)Nb + P] x (F/W) (Note 4) (2) P -- (GH x 1000)/204r2` where: A = NaOH solution required for titration of the sample, mL, .................... t B = NaOH solution required for titration of the' blank, j 3 | I 1 Nb -- normality of the NaOH solution, C = H2S04 required for titration of the sample, mL, D = H2S04 required for titration of the blank, mL, Na = normality the H2S04, F = 4.305 for acetyl and 6.005 for acetic acid, P = milliequivalents of potassium acid phthalate, G = potassium acid phthalate used, g, H = purity factor for potassium acid phthalate, and W = sample used, g. 4--When equal volumes of alkali or acid are added to samples and blank, these amounts cancel out. Thus only the amounts of each added in the titration enter into the calculations. Use of potassium acid phthalate in the blank is recommended. When it is not used, the term P drops out of the equation. | } 1 [ j j j 23. Precision and Bias 23.1 No statement on bias can be made as no reference material is available as a standard. DUP050296687 D 871 Test Method B--Heterogeneous Saponification Method ^agents Ethyl Alcohol (75 Volume %)--Mix 790 mL of jila 2B, 3A, or 30 denatured ethyl alcohol and 210 mL Hydrochloric Acid (0.5 N)--Prepare and standardize iJV solution of hydrochloric acid (HCI). fa Sodium Hydroxide, Standard Solution (0.5 ^Prepare and standardize a 0.5 N solution of sodium pxide (NaOH). procedure Jl Grind the sample in a Wiley mill or other suitable Mjfpler so that 100 % will pass a No. 20 (850-p.m). (Grinding omitted if the sample has suitable texture.) Dry about of the sample in a weighing bottle at 105 3C for 2 h, tktopper, and cool in a desiccator. (An oven with mechanical jfiilation is to be preferred over a convection-type oven). fp.2 Weigh the bottle containing the sample to the nearest g, transfer the sample to a 250-mL Erlenmeyer flask, tf^id Weigh the bottle again to the nearest 0.001 g. Handle the guttle with either tongs or a clean dry cloth during these pnipulations. Add 40 mL of ethyl alcohol (75 %) to each finple. Include a blank determination with each set of pnples and carry the blank determination through the pmplete procedure, including the back titration. |25.3 Heat the flasks, loosely stoppered, for 30 min at 50 to |`C. Add 40 mL of 0.5 N NaOH solution to each flask and at again at 50 to 60"C for 15 min. Stopper the flasks tightly Id allow to stand at room temperature for about 48 h. If the jfetyl content of the sample is over 43 %, or if the sample is f|rd and homy, allow to stand for about 72 h. At the end of > time back titrate the excess NaOH with 0.5 A HCI, using benolphthalein as the indicator. Add an excess of about 1 oL of 0.5 N HCI and allow the NaOH to diffuse from the Regenerated cellulose for several hours, or, preferably overlight. The disappearance of the pink color indicates the Complete neutralization of the NaOH. Titrate the small jfxcess of HCI with 0.5 N NaOH solution to a phenolphthalein end point. Extreme care must be taken to locate i end point. After the sample is titrated to a faint pink end point, stopper the flask and shake vigorously. The end point Jinay fade because of acid diffusing from the cellulose, fContinue the addition of 0.5 N NaOH solution and shaking until the faint pink end point persists after vigorous shaking of the flask. 26. Calculation 26.1 Calculate the percentage of combined acetyl or acetic acid as follows: acetyl or acetic acid, % = [(> - C)Na + (A - B)Nh] X (F/W) (3) j where: I A = NaOH solution required for titration of the sample, mL, : B - NaOH solution required for titration of the blank, mL, I Nh = normality of the NaOH solution, j C = HCI required for titration of the sample, mL, FIG. 1 Special Reflux Tube for Carbanilation D *= HCI required for titration of the blank,- mL, Na -- normality of the HCI solution, F = 4.305 for acetyl or 6.005 for acetic acid, and W = sample used, g. HYDROXYL CONTENT 27. Scope 27.1 This test method is applicable to pyridine-soluble cellulose esters and is especially useful when the hydroxyl content is low. Samples containing plasticizer' may be analyzed directly'by this test method because the plasticizer is removed during washing of the carbanilate. 28. Summary of Test Method 29.1 Hydroxyl in cellulose acetate is determined by reac tion with phenyl isocyanate in pyridine solution under anhydrous conditions to form the carbanilate derivative. The derivative is then analyzed for its carbanilate. content by ultraviolet absorption. 29.2 The acetyl content of cellulose acetates may be calculated provided that the degree of polymerization is not excessively low. 29. Significance and Use 29.1 Hydroxyl content is a measure of the free hydroxyl on the cellulose backbone of the polymer. Hydroxyl content has a strong effect on the polymer's solubility and physical properties. Hydroxyl content also impacts the propensity for this polymer to crosslink with various crosslinking agents. DUP050296688 D871 30. Apparatus 30.1 Spectrophotometer,351complete with hydrogen light source and a set of four 1.00-cm quartz cells, or an equally suitable apparatus. The wavelength calibration, as checked against a mercury lamp, shall be within the-manufacturer's tolerances. As a further check, measure the absorbance of a potassium chromate (K2Cr04) solution prepared as follows: Dissolve 0.0400 g of K2Cr04 or 0.0303 g of potassium dichromate K2Cr207 in 0.05 N potassium hydroxide (KOH) solution and dilute to 1 litre in a volumetric flask with 0.05 IV KOH solution. Using the hydrogen lamp, measure the absorbance at 280 nm of a silica cell filled with the K2CrQ4 solution and also of the same cell filled with water. The absorbance of the solution minus that of the blank shall be 0.723 0.023. 30.2 Bottles, 4-oz, with screw caps, for washing the samples. 30.3 Special Reflux Tubes for the carbanilation, con structed as follows (see Fig. 1): Make a test tube approxi mately 20 by 150 mm from the outer part of a 24/40 standard-taper ground glass joint by closing the open end in a blast lamp. Draw the tubing on the inner joint to a constriction just above the joint. Cut the glass at that point and seal on a short length of 8-mm tubing to provide a bearing for a glass stirrer. Make a stirrer of 4-mm glass rod with a semicircle at right angles to the shaft at the bottom and small enough to fit into the test tube. When properly constructed this unit acts as an air condenser, thus pre venting the loss of solvent by evaporation. 30.4 Pipet, serological-type, 5-mL capacity, graduated in 0.1-mL divisions. 30.5 Bitchner Funnel, of a size accommodating 90-mm filter paper. 30.6 Automatic Shaker, with speed regulator mechanism. 30.7 Electric Oven, maintained at 105 3C. 30.8 Oil Bath, equipped with a rack to hold several of the special reflux tubes. This bath shall be kept between 115 and 120C. 31. Reagents 31.1 Acetone. . 31.2 Ethyl Alcohol, denatured, Formula 2B, 3A, or 30. 31.3 Methylene Chloride-Methyl Alcohol Mixture--Mix 9 parts by weight of methylene-chloride with 1 part of methyl alcohol. This mixture should have an absorbance of less than 0.2 at 280 nm in a 1,00-cm silica cell measured against air. Pure methylene chloride has an absorbance of about 0.05, but the commercial product may have an absorbance as high as 1.00. The methylene chloride and methanol should be selected to have low absorbance; otherwise, they should be redistilled. 31.4 Phenyl Isocyanate.6 31.5 Pyridine, redistilled, low water content, preferably less than 0.05 %. 32. Procedure 32.1 In the following procedure the phenyl isocyanate reagent shall be used under anhydrous conditions. Therefore, the sample, containers, pipet, and all other equipment shall be thoroughly dried. 32.2 Place a 0.5-g sample in a special reflux tube and dry' in an electric oven at 105"C for 2 h. Remove the tube from the oven, add 5 mL of pyridine, assemble the reflux apparatus complete with glass stirring rod, and place in the 115 to 120C oil bath. Stir occasionally until the sample is completely dissolved. Add 0.5 mL of phenyl isocyanate, stir thoroughly, and reflux in the oil bath for1ft h to complete the reaction. Use 0.1 mL of phenyl isocyanate for each percent of estimated hydroxyl content, but never less than 0.5 mL. 32.3 At the end of the reaction time, remove the sample and dilute it with acetone to the proper viscosity for precipitation. The amount of acetone used to thin the solution is a critical factor in acquiring a good precipitate, Samples having low viscosity require little, if any, dilution. The average sample requires the addition of about an equal volume ofacetone. Precipitate the carbanilate by pouring the solution into about 200 mL of ethyl alcohol. The precipitate should be fluffy and white. Sticky precipitates indicate too little dilution. Stir the alcohol vigorously during precipita tion. Filter off the precipitate, using paper on a Buchner funnel, with suction applied only as long as is necessary to remove the bulk of the solvent; prolonged suction may cause undesirable clumping together of the precipitate. 32.4 Wash by transferring the precipitate to a 4-oz screw cap bottle containing 75 mL of ethyl alcohol, capping securely, and shaking for xh h on an automatic shaker at medium speed. Filter the precipitate on the Buchner funnel, pressing out as much liquid as possible with a glass stopper. Repeat the washing and filtering operations twice more. Allow the precipitate to air-dry 1 to 2 h at room temperature with good ventilation or preferably overnight to ensure complete removal of the alcohol, (Samples wet with alcohol may sinter and stick to paper or glass when dried at 105C.) Dry the sample at 105C in the oven for 1 h and cool in a desiccator. Small manila envelopes are convenient for drying and cooling the samples. 32.5 Weigh-Q. 1231 g of the dry precipitate into a 100-mL volumetric flask fitted with a ground-glass stopper. Add 60 to 80 mL of the methylene chloride-methyl alcohol mixture, and shake occasionally until complete solution occurs. Dilute to 100 mL and mix thoroughly. Using the spectropho tometer with a 1-cm silica cell measure the absorbance of the solution at 280 nm against the solvent mixture as a reference. 33. Calculation 33.1 Calculate the percentage of carbanilate, c, for a sample weight of 0.1231 g as follows:7 Carbanilate, % =A x 17.1 (4) where: A = absorbance. 33.2 Calculate the percentage of hydroxyl as follows: 5 A Beckman Model DU Spectrophotometer has been found satisfactory for this purpose. 6 Phenyl isocyanate available as Eastman No. 553 has been found satisfactory for this purpose. 7 Malm, C. J.. Tanghe, L. J., Laird, B. C., and Smith, G. C\, "Determination of Total and Primary Hydroxyl in Cellulose Esters by Ultraviolet Absorption Methods," Analytical Chemistry, ANCHA, Voi 25, 1954, p. 189, DUP050296689 D 871 Hydroxyl, % = 14.3c/(l00 - c) Calculate the percentage of acetyl as follows: Acetyl, % - (4480 - 65.1c)/(l00 - c) 5--The calculation for acetyl content assumes exactly three s per anhydroglucose unit and applies to cellulose acetates only. PRIMARY HYDROXYL CONTENT summary of Test Method ' i The primary hydroxyl content of cellulose acetate is ermined by formation ofthe triphenylmethyl (trityl) ether 1 measurement of the trityl group by ultraviolet s'ance.7 Trityl chloride reacts preferentially with prihydroxyls. Since there is also a slight reaction with dary hydroxyls, standardized reaction conditions are rtant.8 Apparatus See Section 30. jail Acetone. <2 Ethyl Alcohol, denatured. Formula 2B, 3A, or 30. 6.3 Methylene Chloride-Methyl Alcohol Mixture--Mix 9 i by weight of methylene chloride with 1 part of methyl obol. This mixture should have an absorbance ofless than at 259 nm in a 1-cm silica cell measured against air, 4rwise the solvents should be redistilled. 36.4 Pyridine, redistilled to. a water content less than 5 %. The water content may be reduced further by storing er a suitable drying agent, such as a molecular sieve.9 36.5 Trityl Chloride (Chlorotriphenylmethane or triphenylmethyl Chloride), reagent grade. I.Procedure . 37.1 The reagents shaft be used under anhydrous condivons. It is imperative that the sample and all equipment be droughty dry. 37.2 Place a 0.5-g sample in the test tube of the special Mux apparatus and dry for 2 h at 105 3C. Add 5 tnL of yridine, insert the top ofthe reflux apparatus and the stirrer nd heat with stirring in a 115 to 320C oil bath. After the iple has dissolved, add 0.5 g of trityl chloride. If the total ydroxyl content exceeds 3 %, use an additional 0.075 g of trity! chloride for each additional 1 % hydroxyl. Stir the mixture thoroughly and reflux in the oil bath for exactly 2 h at 115 to 12(TC. Remove the tube and cool. 37.3 Dilute the sample with acetone to the proper vis cosity for precipitation. The amount of acetone used to thin the solution is a critical factor in obtaining a good precipi tate. Samples having low viscosity require little, if any, dilution. The average sample requires the addition of about an equal volume of acetone. Precipitate the trityl derivative by pouring the solution into about 200 mL of ethyl alcohol with vigorous stirring. The precipitate should be fluffy and* * 8 Malm. C. J., Tanghe, L. J., and Laird, B. C., "Primary Hydroxyl Groups in Hydrolyzed Cellulose Acetate," Journal of ihe American Chemical Society, JACSA, Vol 72, 1950, p. 2674. * Molecular Sieve Type 4A as manufactured by the Unde Air Products Co., has been found satisfactory for this purpose. white. Sticky precipitates indicate too little dilution. Separate the precipitate by filtering through paper on a Buchner funnel, with suction applied only as long as necessary to remove the bulk of the solvent; prolonged suction may evaporate the alcohol and cause the precipitate to partially redissolve in the remaining pyridine. 37.4 Wash the precipitate by transferring it to a 4-oz screw cap bottle containing 75 mL of ethyl alcohol, capping securely, and shaking for 'h h on a shaker at medium speed. Again collect the precipitate on a Buchner funnel, pressing out as much liquid as possible with a glass stopper. Repeat this washing and filtering operation twice more, or until the absorbance of the filtrate at 259 nm is about the same as that of an alcohol blank. Allow the precipitate to air-dry on the filter paper for 'A h at room temperature with good ventila tion, or preferably overnight, to remove most of the alcohol. (Samples wet with alcohol may sinter or stick to paper or glass when dried at 105C.) Transfer the sample to a manila envelope, dry it for 1 h at 105C, and cool in a desiccator. 37.5 Weigh 0.1231 g of the dry trityl ether derivative into a 100-mL volumetric flask fitted with a ground-glass stopper, and dissolve in the methylene chloride-methyl alcohol mix ture. Dilute to 100 mL and mix thoroughly. Measure the absorbance of this solution in a 1-cm silica cell using a spectrophotometer at 259 nm against the solvent as a reference. 38. Calculation 38.1 Calculate the trityl content, t, for this concentration of 0.1 g/100 g and with a correction of 0.015 for the absorbance of the cellulose acetate as follows:7 Trityl, % = 25.25 (A - 0.015) (5) where: A = absorbance. 38.2 Calculate the weight percentage of primary hydroxyl in cellulose acetate as follows: Primary hydroxyl, % = 7.021/(100,4 - /) ""(6) 38.3 Calculate the percentage primary hydroxyl of the total hydroxyl as follows: ... . Primary hydroxyl of total hydroxyl, (B[C) x-100- (7) where: B = value of primary hydroxyl as determined in 38.2, and C = value of total hydroxyl as determined in '33.2. 39. Precision and Bias 39.1 No statement on bias can be made as no reference material is available as a standard. SULFUR OR SULFATE CONTENT 40. Summary of Test Method 40.1 The sulfur or sulfate content of cellulose acetate is measured by oxidizing the sample in a nitric acid-perchloric acid mixture and determining gravimetrically as barium sulfate. To determine combined sulfur the sample must first be reprecipitated into dilute acid to remove noncombined sulfur compounds. 40.2 The sulfur or sulfate content may also be determined by Test Method D 2929. In this case the X-ray method shall be calibrated against the chemical method following in 169  D 871 Sections 42 to 45, and the sample shall be treated in accordance with Section 44 if combined sulfur is to be determined. 41. Significance and Use 41.1 Sulfur and sulfate content indicates the amount of sulfur in the cellulose ester either as inorganic salts (usually sulfates) or as organic sulfate (usually as sulfate ester com bined to the cellulose backbone). The presence of high levels of sulfur and sulfate can be detrimental to the melt stability of the ester. 42. Apparatus 42.1 Funnel, modified by cutting the stem off at the apex of the funnel and fire polishing. 42.2 Crucibles,10 30-mL, extra-fine porosity. 42.3 Oven, controlled at 120 to 125C. 42.4 Muffle Furnace, controlled at 800 50C. 43. Reagents 43.1 Acetone. 43.2 Acedc Acid (1+49)--Mix 1 volume of glacial acetic acid with 49 volumes of water. 43.3 Barium Chloride Solution (100 g/L)--Dissolve 100 g of barium chloride (BaCl-2H20) in water and dilute to 1 L. 43.4 Hydrochloric Acid (l+l)--Mix 1 volume of concen trated hydrochloric acid (HC1, sp gr 1.19) with 1 volume of water. 43.5 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HNOs). 43.6 Nitric Acid (2+3)--Mix 2 volumes of concentrated HN03 (sp gr 1.42) with 3 volumes of water. 43.7 Nitric Acid-Perchloric Acid Mixture--Mix. 5 volumes of concentrated HN03 with l volume of concentrated perchloric acid (HC104, 70 %). 43.8 Phenolphthalein Indicator Solution (1 g/100 mL)-- Dissolve 1 g of phenolphthalein in 100 mL of ethyl alcohol (95 %). 43.9 Silver Nitrate Solution (50 g/L)---Dissolve 50 g of silver nitrate (AgN03) ip water and dilute to 1 L. 43.10 Sodium Carbonate (Na2C03). 43.11 Sodium Hydroxide Solution (400 g/L)--Dissolve 400 g of sodium hydroxide (NaOH) in water and dilute to 1 L. 44. Procedure 44.1 Treatment Prior to Analysis--Remove uncombined sulfur as follows (Note 6): Dissolve 25 g of sample in approximately 300 mL of acetone, depending on the vis cosity. If the sample is of too high acetyl content to be directly soluble in acetone, cool in a dry ice cabinet overnight; then allow to come to room temperature while tumbling or stirring. Filter the solution, if necessary, through felt or a coarse sintered-glass crucible. Precipitate with rapid stirring into a beaker or pail containing 2 to 3 L of acetic acid (1+49). Filter through a cloth bag or a Buchner funnel and give two 15-min washes with water using mechanical agita- 10 Selas No. 3001 crucible has been found satisfactory for this purpose. tion. A little Na2C03 may be added to the last wash to '.m stabilize samples of high sulfur content. Filter and dry 'fljj overnight at 60C. ' 6--To analyze for total sulfur content omit this treatment. II 44.2 Decomposition: ill .944.2.1 Weigh 10 Q.1 g of cellulose acetate and transfer to a clean, wide-mouth, 500-mL Erlenmeyer' flask. Add 50 9 mL of the HN03-HC104 mixture to the flask, and swirl the fj flask gently to wet the sample thoroughly. Place the modified f| funnel in the mouth ofthe flask and heat the flask carefully 31 on a hot plate in a fume hood. fl 7: Precaution--Use the utmost care in handling the HNOr m HCt04 mixture. If a spill occurs, wash down with pleijty of vrater. Wear 9 safety glasses or. a face shield. ' 44.2.2 After the mixture becomes hot and less viscous, 9 increase the heat of the hot plate. Continue the digestion until all the sample has been oxidized and the thick m reddish-brown fumes of nitrogen dioxide. (N02) have been expelled. At this point, white fumes will appear and a rather 1 vigorous reaction will occur that is caused by the last traces 1 of organic material being oxidized and the HN03 fuming off. ; 44-.2.3 When this reaction starts,, remove the flask from 1 the hot plate, swirl gently for a few seconds, and set.it on the l shelfin front ofthe hood until the reaction is complete. Place 1 the flask back on the hot plate and continue the digestion 1 until the HC104 refluxes about half way up the side of the Erlenmeyer flask and about 5 mL is left in the flask. The jj HN03-HC104 mixture should be clear and colorless. If it is Jj not, set the flask off the hot plate to cool and then add 3 to 5 jjj mL of HN03 (sp gr 1.42). Replace the flask on the hot plate -JJ and continue heating until the HQ04 refluxes half way up fj the flask. Remove the flask from the hot plate and allow the jj flask and its contents to cool. I 44.3 Determination ofBarium Sulfate: I 44.3.1 Wash: the modified funnel top thoroughly with 1 water, collecting the rinsings in the flask. Add 50 ml ofwater. I Swirl the flask to mix the solution thoroughly. Add 2 drops of phenolphthalein indicator solution and neutralize the acid with the NaOH solution to a faint pink. Acidify immediately with HC1 (1+1), dropwise, .until the solution is just afcid to phenolphthalein-; then add 2 mL of HQ (1+1), .... 44.3.2 Filter through a 12.5-cm fine-porosity paper into a clean 400-mL beaker. Wash the flask thoroughly with water, filtering the washings through the paper. Finally wash the paper thoroughly with ten portions of hot water. Dilute the filtrate to approximately 200 mL. Place the beaker on the hot plate and heat almost to boiling. Slowly add 10mL of BaCl2 solution, from a pipet, stirring the solution during the addition. Do not add the BaCl2 solution rapidly, as from a graduate, since the rapid addition will , produce an impure precipitate. Remove the stirring rod from the beaker and wash it with a stream of water from the wash "bottle, collecting the washings.in the beaker. Cover the beaker with a watch glass and keep the -mixture near the boiling temperature of 6 h or overnight. Do not allow the liquid to evaporate to dryness. 44.3.3 Using suction, decant the supernatant liquid through an extra-fine porosity porcelain filter crucible that has been previously rinsed with acetone, ignited, and weighed to the nearest 0.1 mg. Transfer the precipitate with DUP050296691 `d of a stream of hot water. Always use a stirring rod in Jtransfer. Scrub the sides and bottom of the beaker with a er policeman to remove any adhering precipitate. The ibles may be used to collect' several precipitates one on of the other. Close control of temperature and time of !ng and cooling are necessary. Cleaning with hot water is erally sufficient; drastic attack with cleaning solution uld be avoided. *.3.4 Wash the precipitate on the filter until free of brides by the following test: To 5 mL of wash water, ected in a separate test tube or on a watch glass, add 1 mL IN03 (2+3) and 1 mL of AgN03 solution. The appeare of a milky white precipitate indicates the presence of brides, and the washing should therefore continue until - test is negative. Do not attempt to get a completely Iftative1 test for chloride.- Discontinue washing when no ire than a faint opalescence is produced in the test. Ws 44.3.5 Finally pour a few millilitres of pure acetone through the filter and suck.it dry. Place the crucible in a *"Vger crucible or in a metal tray with perforated sides and 'c'pttom for protection and place it in an oven at 120 to 125Cf fo 1 h. Do not handle the crucibles with the fingers between hition and the completion of weighing; use forceps, i 44.3.6 Remove the crucible from the oven and ignite it for 0 min in a muffle furhafoe at 800 50CC. Cool in a esiccator for 75 15 min and weighs to the nearest 0.0001 g. is permissible to return the crucible to the oven for at least 5 min before transferring totjie desiccator. 44.3.7 From time to time,fo|M( especially when using new gents, run a blank in duplicate in the-reagents. If the eight of the prp&pitate exceeds 0.0005 g,^investigate and Jiminate the cause. This is equivalent to ajfcgrror of0.002 % h a 10-g sample. 1`5. Calculation , -IS' 45.1 Calculate the percentage of sulfur ([follows: : sulfate as Sulfur, % = ({(C -B)-(E -2]X 0.1374 x 100)/^ (8) Sulfate, % - {[(C-B)-(E- D)] X 0.4115 X 100/A <9) vhere: A = weight of sample, g, . .. B - weight of crucible for sample, g, C = weight of crucible and BaS04 for sample, g, C - B = weight of BaSQ4 for sample, D -- weight of crucible for blank, g, . E = weight of crucible and Ba$04 for blank, g, and E - D weight of BaS04 for blank, g. 46. Precision and Bias 46.1 No statement on bias can be made as no reference material is available as a standard. HEAT STABILITY 47. Summary of Test Method 47.1 The heat stability of cellulose acetate is one indica tion of its quality. It is measured by heating the sample for a specified time and temperature, observing it for amount and uniformity of color developed, and possibly also measuring the loss of viscosity as a result of heating. Suggested times of heating are 8 h at 180C or 2 h at 190C, The time and temperature of beating, method of grading, and limits are matters for agreement between purchaser and the supplier. 48. Significance and Use \ 48.1 The heat stability of a cellulose e$terjs one indication of its quality, 49. Apparatus ` 49.1 Heater Block--A qjetal block of*suitable Size is heated electrically and maintained at the specified tempera ture within i`C. This is best accomplished by providing continuous .heat to hold the temperature a few degrees below the specified temperature, and providing intermittent addi tional heat thermostatically controlled. Holes are drilled in the top of the block tfo hold test tubes, a thermoregtilatb'r, and a thermometer. The blobk should be4nsplated. . . 49.2 Test tubes, either. 18 by 150 mm or "20 by. 150 mm, fitted with corks; The cofks shall be fitted with glass tubes the length of the cork and 4 jjihn in inridq diametetot Sllail .have a small V-shaped notch of equivalent cross-section cut'in a vertical position. ., 50. Solvent 50,1 Methylene Chlorlde-Methgnol Mixture--Mix 9 parts by weight of methylene chloride with 1 part of methyl alcohol. " 51. Heat Treatment 51.1 Place the sample, ground to pass a No. 20 (850-jrm) sieve, in a clean dry test tube and pack it firmly and uniformly. Stopper with a cork having a notch for tube as described in 49.2. Heat the tube and contents for, 8 h at '1 Wagner, R. H., and Russell, John, "Capillary X"he Viscometer for Routine Measurement of Dilute High Polymer Solutions," Analytical Chemistry, ANCHA, Vol 20, 1948, pp; 151-157. DUP050296692 D 871 TABLE 1 Solvents for Intrinsic Viscosity Determination Solvent'' Ingredients, weight 56 Value of k for Calculation (see 61.2) A B CorD E F 90 56 acetone 10 56 ethyl alcohol acetone 90 56 methylene chloride 1056 ethyl alcohol 96 56 acetone 4 96 water 90 56 methylene chloride 1056 methanol 10 10 3 10 3 `'Solvent designations conform to those used In Table 2 for viscosity determinations. Acetone (99.4 0.1 56) containing 0.3 to 0.5 56 water and under 0.3 56 ethyl alcohol. Ethyl alcohol (95 volume 56). Formula 2B or 3A denatured ethyl alcohol may be used. Methylene chloride having a boiling range of 39.2 to 40.0 C and less than 0.001 56 acidity calculated as HQ. ' Methyl alcohol (sp gr 20/20'>C = 0.785 to 0.795). 180"C or as otherwise specified. 52. Dry Color Evaluation 52.1 Examine the heated sample for uniformity of color and for the presence of charred or decomposed spots. Compare the color of the material at the bottom of the tube with standards prepared as follows: Heat portions of a check batch of similar particle size, representative quality and stability, and accepted by mutual agreement between the purchaser and the seller. Pack portions of this check batch firmly in each oftwelve clean, dry test tubes and stopper with corks as described in 49.2. Heat the tubes at 180C, or as otherwise specified, remove one tube each 2 h, and mark the time of heating in hours on each tube. This set of numbered tubes serves as the color standards. They should be checked and renewed if necessary every 6 months. 53. Solution Color Using Platinum - Cobalt Standards 53.1 Heat a 1-g sample for the specified time and temper ature and, after cooling, examine for charred or decomposed spots. Dissolve the heated sample in 15 mL of the methylene chloride-methanol mixture. Compare the color of the solu tion (viewing transversely) with test tubes of platinum-cobalt color standards, prepared as described in Section 70. (It may be necessary to prepare standards having as much as 2000 ppm of platinum for this purpose or to dilute the sample solution before grading.) 54. Solution Color by Spectrophotometer 54.1 The color of the solution prepared as described in Section 53 may also be measured spectrophotometrically. Measure the absorbance at 400 nm against the solvent, using a suitable spectrophotometer with a 1-cm silica cell. 55. Viscosity Change 55.1 Measure the intrinsic viscosity of the heated sample and of an unheated sample as described in Sections 57 to 61 of this test method. The percentage loss of viscosity as the result of heating is a measure of heat stability. 56. Precision and Bias 56.1 No statement on bias can be made as no reference TABLE 2 Solutions for Viscosity Determination Formula A B C" D E F Ingredients, weight % Cellulose aoetate Acetone ' Acetone, 86% Water, 4 56 Ethyl alcohol Methyl alcohol Methylene chloride 20* 20* 20 15 20* 10c 72 80 8 8 8.5 9' 72 76.5 81 Typical Solution Densities, g/mL at 25 C 0.84 0.86 1.25 1.23 0.86 1.24 * Acetyl content 40.5 56, max. Acetyl content 40.5 to 42.7 56. Acetyl content 42.7 to 44.8 55. Acetone (99.4 0.1 %) containing 0.3 to 0.5 56 water and under 0.3 56 ethyl alcohol. e Ethyl alcohol (95 volume 56). Formula 2B or 3A denatured ethyl alcohol may be used. * Methyl alcohol (sp gr 20/20 C 0.785 to 0.795). Methylene chloride having a boiling range of 39.2 to 40.0"C and less than 0.001 56 acidity calculated as HCI. FIG. 3 Color and Haze Apparatus material is available as a standard. INTRINSIC VISCOSITY 'a- 57. Summary of Test Method 57.1 Intrinsic viscosity, expressed in decilitres of solution per gram of solute, is determined by. measuring the flow times of a solution of known concentration and also of the solvent used and making a calculation by means of the modified Baker-Philippoff equation. 8--By expressing concentration in grams per millilitre rather than grams per decilitre, the result will he limiting viscosity number instead of intrinsic viscosity, and will be 100 times greater. 58. Significance and Use 58.1 Intrinisic viscosity number can be used to estimate the molecular weight of a cellulose ester by using the Mark-Houwink- equation and constants measured for the solvent, temperature, and ester of concern. 172 'TO5 DUP050296693 D 871 ri 44.4 3% 95.2 614 63.5 4% 120.6 714 76.2 5 127.0 514 82.6 6 152.4 FIG. 4 Color and Haze Apparatus (Details) 158.8 190.5 209.6 212.7 8Va 13 17V4 2014 215.9 330.2 444.5 520.7 Apparatus 59. i Capillary Viscometer, such as the Wagner apparatus jFig. 2) or an Ostwald-Fenske-Cannon pipet, that will give a |flow time for the solvent of not less than 70 s. 59.2 Water Bath--A constant-temperature water bath Ibntrolled at 25.0 0.1C and with a pump for circulating ,|he water through the viscometer jacket or tank. 59.3 Stop Clock or Watch, calibrated in tenths of a second. 60. Procedure 60.1 Sample Preparation--Dry about 0.26 g of sample in a weighing bottle at 105 3"C for 2 h, stopper, and cool in a desiccator. Weigh the bottle containing the sample to the nearest 0.001 g, transfer the sample to a 250-mL flask, and reweigh the bottle. Pipet into the flask 100 mL of solvent at 25 0.1*C. The solvent used should be mutually agreed upon by the purchaser and the supplier. Suitable solvents are listed in Table 1. After the sample is completely dissolved, place it in the constant-temperature bath at 25C along with a portion of the solvent used, and allow sufficient time for both to come to temperature before making the viscosity measurements. During this conditioning period, water at 25C should be circulating through the water jacket of the viscometer to allow ample time for the pipet to reach temperature equilibrium. 60.2 Viscosity Measurements--Rinse the reservoir and the outside of the capillary tube thoroughly with solvent. Rinse the inside of the capillary tube twice by alternately applying pressure at points B and A (Fig. 2). Discard the wash portion of the solvent. Pour more solvent into the reservoir and allow several minutes for'complete drainage and thermal equilibrium to be obtained. Adjust the outer meniscus to a reference point, D, that will give a flow time between 70 and 100 s. Apply air pressure at 2Mo force the solvent up through the capillary past the upper timing mark, C, on the measuring bulb, E. Record the time in seconds required for the meniscus to fall between the timing marks, C and F. Take a minimum of two readings. Repeat these operations, substituting the solution for the solvent. 61. Calculation 61.1 Calculate the relative viscosity, vKh as follows: . (10) where: t, = flow time of solution, and t2 = flow time of solvent. 61.6 Calculate the intrinsic viscosity, [17], as follows: [7] = (k/c) lantilogflog v,Jk) - 1] (11) where: 173 DUP050296694 D871 k = values from Table 1, and c = concentration in grams per decilitre (Note 8 in Section 57). 62. Precision and Bias 62.1 No statement on bias can be made as no reference material is available as a standard. VISCOSITY 63. Significance and Use 63.1 A measurement of viscosity is of great practical utility in determining the proper processing equipment and process concentrations for cellulose esters. 64. Procedure 64.1 Solution--Dry the sample for 1 to 2 h at 105 3C and cool in a desiccator. Prepare a solution of the dried sample in a solvent and at a concentration mutually agreed upon by the purchaser and the seller. Suitable solutions are listed in Table 2. 64.2 Viscosity Determination--Prepare the solution and measure the viscosity in accordance with Test Method D 1343, (Note 10 in Section 71 of these methods). 65. Report 65.1 Report the results in poises, unless otherwise speci fied. The viscosity values shall be prefixed with the letter A, B, C, etc., corresponding to the formula of the solution employed. 66. Precision and Bias 66.1 No statement on bias can be made as no reference material is available as a standard. COLOR AND HAZE 67. Summary of Test Method 67.1 Color and haze determinations on cellulose ester solutions are made by comparison with standards. Simulta neous measurement of these, properties is desirable because haze reduces the amount of color observed. 68. Significance and Use 68.1 Solution color and haze of a cellulose ester is a measurement of the optical properties of cellulose esters when dissolved in a specific solvent. 69. Apparatus 69.1 Light Box--A suitable light box (Figs. 3 and 4) is described as follows. The light source consists of a mercury vapor bulb,12 which requires an auto transformer13 *fo*r**the current source. The bulb is mounted horizontally across the lower front part of a plywood box 14 in. (350 mm) wide, 17 in. (430 mm) high, and 13 in. (330 mm) deep. This box is lined with a heat resistant board and is painted black inside. 12 A General Electric mercury vapor bulb Type H-250, A5-1, or A37-5 (differing only in the shape of the glass globe) has been found satisfactory for this purpose. 13 A General Electric Autotransformer Model 9T64Y21 has been found satisfactory for this purpose. except that the inside back surface toward the viewer is J white. A bottle holder large enough to hold four bottles is I built onto the front of the light box, and a 2'h by 6-in. (63.5 , by 152.4-mm) horizontal viewing hole is cut through the i front ofthe box. This opening is covered with clear glass, and I a l/4-in. (6.4-mm) strip of black tape is fastened to the glass j horizontally to aid in judging haze in the solution. Holes are cut in the bottom and top of the box for cooling by air '! convection. For continuous use, forced circulation of air ) would be desirable. A black metal baffle over the bulb j prevents direct light on the viewing glass. 69.2 Sample Bottles--The bottles used for the sample j solutions are French square bottles, 16-oz, with screw caps.14 j These same bottles may be used for the color and haze \ standards.14 9--These bottles may also be used for determination of f viscosity, as described in 64.2. 1 69.3 Cap Liners--Cap liners shall be ofa composition not ; affected by the solvents used. Liners of fiber board covered with ceEophane or aluminum foil are usually satisfactory, but vinyl resin or waxed liners may cause interference with j viscosity, color, or haze measurements. ] 70. Reference Standards 70.1 Color Standards--A color standard containing 500 ppm of platinum may be purchased15 or the solution may also be prepared as follows: Dissolve 1.245 g of potassium platinum chloride (K2PtCl<;), containing 0.500 g ofplatinum, and 1.000 g of crystallized cobalt chloride o 2-6H20), containing 0.248 g of cobalt, in water, add 100 mL of HC1 (sp gr 1.19), and dilute to I L with water. Repare standards containing 50, 60, 70, 80, 90, 100, 125, 150, 175, 200, 250, 300, 350, 400 and 500 ppm ofplatinum by diluting suitable aliquots of the standard solution to 500 mL with water. Place these standards in the special bottles (see 69.2), taking care to select bottles with good clarity and free of flaws. Label and cap tightly. 70.2 Haze Standards--Prepare haze- standards by diluting a stock solution having a turbidity of 1000 ppm. Prepare bottles containing 10,20, 30,40, 50, 60^70, 80,90, 100,125, 150, 175, 200^ and 400 ppm of turbidity," label, and cap tightly. ' " . 10--The previously recommended stock -6011111011 for pre- paring these standards was made from fuller's earth, water, and hydrochloric acid. This solution is no longer available. A comparable stock solution can be made using a diatomaceous earth.16 To obtain haze levels equivalent to the fuller's earth standard, 1.1 parts diatomaceous should be used in place of 1.0 parts of fuller's earth in preparing the aqueous suspension. No hydrochloric add is needed. j j j M || I I m j j jj j I 1 1 1 I 1 I J 31 71. Procedure 71.1 Prepare the solution to be graded by dissolving the cellulose ester in the specified amount and kind of solvent, in 14 Owens-Illinois French square bottles No. A6732 with No. 48-400 caps have been found satisfactory for the sample solutions, viscosity, and for the color and haze standards, although for the color and haze standards, No. A6720 bottles with No. 28-400 caps are more convenient ** This color standard may be purchased as platinic cobalt chloride (APHA color standard) from the Hariman-Leddon Co., Philadelphia, Pa. >6Celite9 available from Johns-Manville Filtration and Mineral Division, K.en-Caryl Ranch, Denver, CO. 80217 has been found suitable for this purpose. DUP050296695 1 D 871 is 'the square bottles. See Table 2 for suitable solutions. sample, a considerable saving in time can be made by using one solution k 350 mL are required. Tumble until a uniform in a square bottle for all three determinations. Dry the cellulose ester as 5 gn is obtained. Allow the solution to stand until it is required for the viscosity determination, prepare the solution carefully, and allow the bottle to stand long enough to form a thick solution before 10 : bubbles before grading it for color and haze: tumbling, to avoid solvent loss around the cap. Use a large enough d Place the bottle containing the solution to be graded sample to provide at least 350 mL ofsolution in the bottle. Measure the i front of the shelf on the apparatus and place a similar viscosity as described in Test Method D 1343, and then rate the color r I containing water behind it. Place the freshly shaken and haze. a standard at the front of the shelf beside the bottle i bI lining the solution to be tested and place the color lard behind it. Determine the amount of color and haze solution by changing the color and haze standards f as good a match as possible has been obtained. The 72. Precision and Bias 72.1 No statement on bias can be made as no reference material is available as a standard. ptandards settle out quickly so they must be reshaken at intervals. Report results in parts per million for both 73. Keywords j- and haze. 73.1 apparent acetyl; ash; cellulose acetate; cellulose ester, ||pTE 11--When viscosity, color, and haze determinations, and an of general appearance arc to be made on a cellulose ester color; free acidity; haze; hydroxyl; intrinsic viscosity; sulfate content 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 thia 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 mid If notrevised, either reapproved or withdrawn. Your comments are invitedeither torrevision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments wW 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 DUP050296696 <1 Designation: D 911 - 87 Standard Specification for Mercuric Oxide for Use in Antifouling Paints1 This standard is issued under the fixed designation D 91-1; 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 (i) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers mercuric oxide for use in antifouling paints. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints21 D284 Test Methods for Chemical Analysis of Mercuric Oxide Pigment3 3. Composition 3.1 The pigment shall consist of finely divided red or yellow mercuric oxide and shall conform to the following 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.3L on Pigment Specifications. Current edition approved Aug. 19, 1987. Published October 1987. Originally published as D 911 -47 T. Last previous edition D 911 -86. 1 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTMStandards, Vol 06.0Z requirements: Chemically combined mercury, calculated as metallic mercury, min, % Free mercury Coarse particles (total residue retained ou a No. 325 (45-pm) sieve, max, % 91 0.0 10 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods: 5.2 Chemically Combined and Free"Mercury--Test Methods D 284. 5.3 Coarse Particles--Test Methods D185. The American Society lor Testing and Materials takas 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 pedant 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 end ifnotrevised, eitherreapproved or withdrawn. Your comments are invitedeither forrevision of this 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 shoutd'make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 176 DUP050296697 Designation: D 912 - 81 (Reapproved 1986) Standard Specification for Cuprous Oxide for Use in Antifouiing Paints1 This standard is issued under the fixed designation D 912; 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 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: fScope 1.1 This specification covers cuprous oxide for use in jiifouling paints. [ Referenced Documents ASTM Standards: il85 Test Methods for Coarse Particles in Pigments, f? Pastes, and Paints12 H>283 Test Methods for Chemical Analysis of Cuprous In Oxide and Copper Pigments3 Composition j|'3.1 The pigment shall consist essentially of finely divided feprous oxide and shall conform to the following requireTients: |iprous oxide, min, % pal copper, calculated as Cu, min, % pal reducing power as Cu20, min, % petals other than copper, max, % ombined chlorides, calculated as G, and sulfates, calcu lated as SO* max, % 97 86 97 0. 0.5 1 This specification is under the jurisdiction of ASTM Committee D-1 on Paint Knd Related Coatings and Materials and is the direct responsibility of Subcompnittee DO 1.31 on Pigment Specifications. fi Current edition approved Oct 30, 1981. Published December 1981. Originally |ubiished as D 912 -47 T. Last previous edition D 912-'65 (1975). 2 Annual Book ofASTM Standards, Vois 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. Acetohe-soluble matter, max, % Stability: decrease in total reducing power after stability test, max, % Coarse particles (total residue retained on a No. 325 (45-pm) sieve), max, % Total nitric acid insoluble residue oh a No. 200 (75-pm) sieve, max, % 0.5 2.0 0.5 0.1 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for bach 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested Separately or after blending in equal quantities the samples' from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.2 Coarse Panicles--Test Methods D 185. 5.3 Cuprous Oxide Content, Total Copper, Reducing Power, Other Metals, Chlorides, Sulfates, Acetone, Soluble Matter, and Stability--Methods D 283. ' -- 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 ol this standard are expressly advised that determination of the validity of any such patent rights, and She risk of Infringement of such rights, are entirely their own responsibility. This standards subject & revision at any time by the responsible technical committed and must be reviewed every five years and It not revised, either reapproved orwithdrawn. Tour comments are invitedeither forrevision ofthis standard or for additionsI standards 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. 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. ! 177 DUP050296698 Designation: D 914 - 72 (Reapproved 1989)'ei Standard Test Methods for Ethylcellulose1 This standard is issued under the fixed designation D.914; the number immediately fallowing the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parenthesesindicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision,or reapproval. This test method has been approvedJor 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.. --Editorial changes were made throughout, including the title, in October 1989. 1. Scope ;, 1.1 These test methods cover the testing of ethylcellulose. 1.2 The test procedures appear in the following order. Sections Moisture Suliated Ash Chlorides (as Sodium Chloride) Alkalinity (as free Sodium Hydroxide) Ethoxy! Content Viscosity 4 to $ 7 to 11 12 to 16 17 to 19 201 to 24 25 to 39 1.3' This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthesafety problems associated with its use. it is the responsibility qf 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 362 Specification for Industrial Grade Toluene12 D446 Specifications and Operating Instructions for.Glass Capillary Kinematic Viscometers3 > D 841 Specification for Nitration Grade Toluene2 E 1 Specification for ASTM Thermometers4 3. Purity of Reagents and Materials 3.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, all of the reagents used shall conform to the specifications of the Committee on Analyt ical Reagents of the American Chemical Society, where Such specifications are available.* Where such specifications have not been established, reagents ofthe best grade available shall be used. References to water shall be understood to mean distilled water. 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 1.36 on Celiulosics. Current edition approved May 1, 1972. Published July 1972. Originally published as D 914 - 47 T. Last previous edition D 914 - 69. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.01. 4 Annual Book ofASTM Standards, Vol 14.03. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Cbem. 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." MOISTURE 4. Procedure 4.1 Weigh accurately 2 to 5 g of the sample to the nearest 1 0.001 g into a tared dish (fitted with a fid) and dry for 2 h in an oven at 100 to 105C. Remove the (fish from, the oven, cover with a lid, .cool in a desiccator, and weigh. 5. Calculation 5.1 Calculate the percent moisture, M as follows: Mr* (A/)x 100 : (1) where: A = mass loss on heating, g, and B - sample used, g. 6. Precision .' 'f 6.1 Replicates, within a given labojatory should, agree within 5 % at the 95 % confidence level f3 SULFATED ASH 7. Apparatus '.. ; 7.1 Muffle Furnace, maintained at' 575 ,25"C.. l',,.., 7.2 Crucibles, either porcelain, Coors No. l, or piatinum. 8. Reagent 8.1 Sulfuric Acid (sp gr 1.84)- -Concentrated sulfuric acid <2s o 9. Procedure 9.1 Ignite a Crucible for 10 to 15 mid at 575 25C, cool in a desiccator, and weigh to the nearest 0.001 g. 9.2 Weigh about 5 g of sample to the nearest 0.001 g (previously dried for 3 h at 105C) into the crucible. Bum off the bulk of the carbonaceous material directly over a flame. After cooling, add 1 mL of H2S04 in such a way as to moisten the entire ash; then cautiously heat with the burner to dense white fumes. Ignite in a muffle furnace at 575 25<>C until all signs of carbon are gone. Cool in a desiccator and reweigh to the nearest 0.001 g. 10. Calculation 10.1 Calculate the percent ash (as sulfate), C, as follows: C = (A/B) x 100 (2) DUP050296699 # D 914 kg, and gpample used, g. ;j precision Jp'l Data obtained from the above procedure indicate laboratory results should agree within 10 % at the ^confidence level. 1 CHLORIDES (AS SODIUM CHLORIDE) ^Apparatus l2J Titration pH Meter* 12.2 Mercury-Mercurous. Sulfate Reference Electrode1-- electrode uses a potassium sulfate electrolyte to avoid flloride contamination from a chloride electrolyte. >12.3 Silver-Silver Chloride Electrode*--The electrode is jjfed with silver chloride periodically. Prepare the electrode polishing with fine steel wool, briefly soaking it in 5 % I* sium cyanide solution, and rinsing it with water. Coat lectrode with silver chloride by electrodeposition from r potassium chloride solution using a 3-V dry cell and a turn wire electrode. Connect the silver electrode to the ,ve pole of the battery,and electrolyze for 20 s; then se the-connections for 5 s. Repeat these operations , and finally, chloridize the silver electrode for 20 s at lositive terminal. Store the silver electrode in 0.1 N sium chloride solution. .Rinse the electrode with water ripe it with a soft tissue before each titration. 4 Salt Bridgefor Reference Electrode--Figure 1 shows Ills. Roenafgigenutrsation in use. Exact dimensions are not impor(lliee1nm3a.t1T5puaEhlrluAeetgRdhirgsea-ciaDvnnolegotrnnilbvfwuore(ei9ridntm.5hgSietnvhtgioiersrlteuoeurmts.h.Feeydo, lcn%teonl)ul,uklleauoens2ped'Betshnoleuafrttrruheyref.eedrUe.nSocr.eBseuplreeeccatiaruolldyoef 1*13.2 Ethamf-Distilled Witter Solvent Mixture (80 + 20)-- Mix 800 g of 2B ethanol with 200 g of water. Add 7.5 g of fterosol OT69'71*00 % surface-active agent per 3000 g of |thanol-water mixture. ( 13.3 Potassium Nitrate (KN03) Solution (saturated) for lalt bridge {Fig. 1). * f-13.4 Silver Nitrate, StandardSolution (0.02 N)--Dissolve 3.4 g of silver nitrate (AgN03) in water, dilute to 1 L with ii water in a volumetric flask, and mix. Weigh exactly 0.5845 g of dry, primary standard sddium chloride (NaCl), dissolve in 25 mL of water, and dilute to 1 L with water in a volumetric flask. Add 10 mL of H2S04 (1 + 16) to each aliquot before titrating. Titrate aliquots of this solution potentiometrically 6 MacBeth Model T or Leeds and Northmp pH meters have been found satisfactory for this purpose. 7 Beckman No. 40453 electrode, manufactured by Beckman Instruments, Inc., 2500 Harbour Blvd., Mail Station E 3 ID, Fullerton, CA 92634, has been found satisfactory for this purpose. s Beckman No. 39261 electrode, manufactured by Beckman Instruments, Inc., uas been found satisfactoiy for this purpose. * Aerosol OT is available from the American Cyanamid Co., Linden, NJ. FIG. 1 Sail Bridge and Reference Electrode for Chloride Determination, with the AgN03 solution, Calculate the normality, N, of the AgN03 solution as follows: 7V=* (A/B) X 0.01 (3) where: A = 0.01 ANaQ solution added, mL, and B = AgN03 solution required for the titration, mL., 13.5 Sulfuric Acid (1 + 16)--Add 1 volume of concen trated sulfuric acid (H2S04, sp gr 1.84) slowiy with stirring into 16 volumes of water. 13.6 Toluene, meeting the requirements of Specification D362. 13.7 Toluene-Ethanol Solvent Mixture (90 + 10)--Mix 900 g of toluene with 100 g of ethanol. 14. Procedure -- 14.1 Weigh accurately 10 g ofsample to the nearest 0.001 . g (previously dried for 2 h at 100 to 105C) and transfer to a 600-mJL beaker containing 200 mL of the toluene-ethanol solvent mixture. Stir with an air-driven stirrer until solution is complete. ' 14.2 Add 200 mL of the ethanol-water mixture and agitate for 5 min to form a uniform emulsion. Immerse the electrodes in the emulsion using an air-driven stirrer for mixing. Add 10 mL of H2S04 (1 + 16) and agitate for 3 to 4 min to allow the system to reach equilibrium. 14.3 Titrate slowly with the 0.02 N AgNOj solution. Make intermittent additions of 0.1 mL. It is advisable to allow longer periods of time between additions of titrant as the end point is approached to avoid passing the equivalence point. Run a blank by the same procedure. 15. Calculation 1,5.1 Calculate parts per million of chlorides as NaCI, C, as Hollows: DUP050296700 C= [(W x 0.05845)/W7] X 1 000 000 where: V = AgN03 solution, mL, N = normality of AgN03 solution, W = sample used, g, and 0.05845 = milliequivalent mass of NaCl. (4) 16. Precision 16.1 Data obtained from the above procedure indicate interlaboratory results should agree within 5.0 % at the 95 % confidence level. ALKALINITY (AS FREE SODIUM HYDROXIDE) 17. Reagents 17.1 Hydrochloric Add, Standard (0.1 N)--Prepare and standardize a 0.1 N solution of hydrochloric acid (HQ), 17.2 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in 100 mL of ethanol (95 %). 17.3 Strontium Chloride Solution (100 g/L)--Dissolve 100 g of strontium chloride (SrCl2) in water and dilute to 1 L. 18. Procedure 18.1 Weigh about 10 g of the sample to the nearest 0.001 g (previously dried for 2 h at 100 to 105C) into a 500-mL Erlenmeyer flask. Add 150 mL of water and heat at the boiling point for 5 min. Add, while stirring, 5 mL of SrCI2 solution and allow the solution to cool. 18.2 Add 2 drops of phenolphthalein indicator solution and titrate to the first faint pink color with 0.1 AC HC1. 19. Calculation f 19.1 Calculate the percent of alkalinity, D, as NaOH as follows: D = {{AB x 0.040)/C] x 100 (5) where: A = HC1 required for titration of the sample, mL, B = normality of the HQ; and C = sample used, g. ETHOXYL CONTENT 20. Apparatus 20.1 Distillation Apparatus, as illustrated in Fig. 2, con sisting of a boiling flask with a side arm for admission of carbon dioxide (C02) or nitrogen, an air condenser with a trap, and a receiver. 20.2 Oil Bath, equipped with a heating device, preferably electrical, so that the bath can be maintained at 145 to 150'C. 21. Reagents 21.1 Bromine Solution--Dissolve 5 mL of bromine in 145 mL of the potassium acetate (KC^OJ solution. Prepare the bromine solution fresh daily in a hood to remove bromine vapors. 21.2 Carbon Dioxide--Pass the C02 through a bubble counter and a dry trap, and then through a pressure regulator consisting of a glass tee whose vertical arm extends almost to the bottom of a 10-in. (254-mm) column of water. A screw clamp shall be attached to the thin-walled rubber tubing connecting the horizontal arm of the tee with the boiling flask. This arrangement permits regulation of the flow of gas and allows any excess gas to escape. Nitrogen may be used in place of C02. 21.3 Formic Acid (90 %). .......... 21.4 Gelatin Capsules--Gelatin capsules of a .suitable size10 1to1 hold from 50 to 60 mg of the dried sample will be required. 21.5 Hydriodic Add (sp gr 1.70)11'12--Hydriodic acid (HI) forms with water a constant-boiling mixture (boiling point 126 to 127Q that contains 57 % HI. The concentra tion of HI in the reagent used should be not less than 56.5 %. The blank determination, which is affected primarily by free iodine in the reagent, should require no more than 0.5 mL of 0.1 N sodium thiosulfate (Na2S203) standard solution. If necessary, the add may be purified by adding to it a small amount of red phosphorus and boiling for 20 to 30 miq in a hood while passing a stream of C02 into the liquid. Distillation is then carried out behind a safety-glass shield in 10 Size 0 gelatin capsules available from Parke, Davis aod Co. are satisfactory for this purpose. 11 Hydriodic add, available from Merck and Co., WBC 220, P.O. Box 2000, Rahway, NJ 07065, under the designation "For Methoxyl Determination" has been found satisfactory for ethoxyl determination. 12 Hydriodic acid suitable for ethoxyl determination may also be prepared by the method of Samsel, . P., and McHard, J. A., Industrial and Engineering Chemistry, Analytical Edition, Vol 14, 1942, 180 DU P0502 96701 D 914 j|tood, using an all-glass apparatus with a slow stream of IWHlhinning through the receiver. Under some conditions, poisonous gas phosphine (PH3) is formed during distillaij-and this may unite with molecular iodine to form phorus triiodide (PI3) which may explode on contact |air. It is, therefore, advisable to keep the current of C02 ^ after the distillation is ended and until the apparatus pooled; this will prevent air from being sucked into the sratus. Put the purified HI in small, brown, glasspered bottles, previously swept out with 0O2, and seal fstoppers with molten paraffin. Store in a dark place. To. size decomposition of HI due to contact with air, run m into the bottle while withdrawing portions of the acid pse. 1.6 Phosphorus Slurry (0.06 g/100 mL)--Add about g of red phosphorus to 100 mL of water. Shake well re using. 21.7 Potassium Acetate Solution (100 g/L)--Dissolve 100 of anhydrous potassium acetate (KC2H302) crystal in 1 L |a solution containing 900 mL of glacial acetic acid and ) mL of acetic anhydride. 1.8 Potassium Iodide (KI). 21.9 Sodium Acetate Solution (220 g/L)--Dissolve 220 g hydrous sodium acetate in water and dilute to 1 L. 1,10 Sodium Thiosulfate, Standard Solution (0.1 )--Dissolve 25 g ofsodium thiosulfate (Na2S203- 5H20) in Q0 mL of water and dilute to 1 L, Use freshly boiled and |roled water. It is preferable to allow the solution to stand a few days before standardization. Standardize the jhition against 0.1000 N potassium dichromate (K2Cr2Q7) plution prepared by dissolving exactly 4.9037 g of K2Cr207 jfational Institute of Standards and Technology Standard j&mple No. 136) in water and dilutingto 1 L in a volumetric k. By means of a buret, measure accurately 35 to 45 mL ' the K2Cr207 solution into a 250-mL Erlenmeyer flask. 12 g of KI and 50 mL ofsulfuric acid (H2S04,1 + 9) and 'Blow to stand for about 5 min. Titrate die liberated iodine B^vith the Na2S203 solution, using starch indicator solution . jear the end point. At the end-point, the blue color of the p starch indicator will be destroyed, leaving the pale green |\ colop of the chromate ion. The normality of the Na2S203, L solution should be checked at least once a week. Calculate s|ihe normality, N, of the Na2S203 solution as follows: if' N = (A/B) x 0.1 (6) where: fA = 0.1000 iVK2Cr207 solution'added, mL.and ( B = Na2S203 solution required for the titration, mL. |i As an alternative procedure, the Na2S203 solution may be gstandardized against 0.1 N iodine that has been standardized fin turn against arsenic trioxide (AS203) (National Institute of `Standards and Technology Standard Sample No. 83) or potassium iodate (KI03). 21.11 Starch Indicator Solution. 21.12 Sulfuric Acid (1 + 9)--slowly add with stirring 1 volume of concentrated H2S04 (sp gr 1.84) to 9 volumes of | water.22 22. Procedure 22.1 Dry the sample at 105"C for at least 30 min. Through the condenser, add to the trap in the distillation apparatus (Fig. 2) enough of the phosphorus slurry to make the trap about half full. Add 19 to 20 mL of the bromine solution to the receiver. Accurately weigh from 50 to 60 mg of the dry sample into a gelatin capsule and drop ft into the boiling flask. (The weighing should be done as rapidly as possible without sacrificing accuracy because dry ethyl-cellulose picks up moisture rapidly.) 22.2 Add a few small glass beads or chips ofclay plate and then 6 mL of HI. Attach the boiling flask at once to the condenser, using a few drops of HI to moisten the groundglass joint, and then connect the side arm of the flask to the source of C02. Pass a current of COz into the apparatus at the rate of about 2 bubbles per second. Immerse the flask in the oil bath, maintained at 150C, and heat for 40 min. 22.3 Add 10 mL of sodium acetate solution to a 500-mL Erlenmeyer flask and wash into it the contents of the receiver; dilute to 125 mL with water. Add formic acid dropwise, with swirling, until the brown color of bromine is discharged, and then add about 6 drops more. A total of 12 to 15 drops is usually required. After about 3 min, add 3 g of KI and 15 mL of H2S04 (1 + 9) and titrate immediately with 0.1 N Na2S203 solution to a light straw color. Add a little starch solution and continue the titration to the disappear ance of the blue color. 22.4 Blank--Make a blank determination, using the same amounts of reagents and the same procedures as for the specimen. (Usually, about 0.1 mL of 0.1 N Na2S203 solution is required.) 23. Calculation. 23.1 Calculate the percent ethoxyl, E, as follows: E = ([<A - B)N x 0.00751]/W) x 100 (7) where: A ms NajSjC^ solution required for titration of the sample, mL, B = Na2S203 solution required for titration of the blank,- mL, , N = normality of the Na2S203 solution, and W = sample used, g. ... 24. Precision 24.1 Replicates within a given laboratory should agree within 1.0 % at the 95 % confidence level. VISCOSITY 25. Scope 25.1 Ethylcellulose viscosity is arbitrarily measured on a 5 % solution in a specific solvent system. The viscosity normally ranges from 7 to 200 cP at 25C. 25.2 Two test methods for measuring ethylcellulose vis cosity are given below. One test method specifies use of the Hercules Horizontal Capillary Viscometer and a solvent system of 80 + 20 toluene-ethanol while the other specifies the Dow Modified Ubbelohde viscometer and solvent sys tems of 80 + 20 toluene-ethanol for product with an ethoxyl content above 47 % and 60 + 40 toluene-ethanol for ethoxyl content below 47 %. 25.3 The two test methods given below do not give the same resultant viscosity. Therefore, they should be used only in a relative sense and not interchangeably. I DUP050296702 D 914 25.4 Neither test method is intended to be a referee method. HERCULE HORIZONTAL CAPILLARY VISCOSITY 26. Apparatus 26.1 Hercules Horizontal Capillary Viscometer13 (Fig. 3)--The tube is surrounded by a glass tube that acts as a water jacket and is connected with it by rubber stoppers at both ends which have proper holes to provide for water inlet and outlet and for insertion of a thermometer. For conven ient use, it is desirable to cut the openings in the stopper at the end next to the reservoir bulb. One of the thermostated water lines should extend inside the jacket, nearly to the opposite end, to provide good circulation. The tube and its jacket are attached to a wood or metal baseboard large enough to support its entire length. The board is in turn hinged at one end to a larger board and is provided with a movable-support arm to hold it at a 45' angle with the base. The bottom board should have adjustable legs so that it can be leveled. The board that supports the capillary tube is equipped with a spirit level. Care must be taken in mounting the tube to see that the capillary is exactly parallel to the board holding the spirit level. The water running through the jacket should come from a constant-temperature bath main tained at 25.0 O.I'C. 26.2 Shaker, Bottle.1* 26.3 Timer, calculated in 0.1-s units. 27. Reagents 27.1 Standard Calibrating Liquid}5 100 cP and 25 C. 27.2 Ethanol (95 volume %)--Undenatured or specially denatured conforming to Formula 2B of the U.S. Bureau of Internal Revenue. 27.3 Mixed Solvent (80 + 20 toluene ethanol by mass)-- Prepare by weighing proportional amounts of toluene and ethanol described in 27.1 and 27.2. Mix thoroughly. 27.4 Toluene, meeting the requirements of Specification D 362.* 14 15 28. Calibration J 28.1 Make a mark on the capillary tube about lOcmfroml the point where the capillary is attached to the reservoir,] | Mount the tube in a water jacket, adjust the temperature, | elevate the board holding the tube to the 45 position, and fill j the reservoir to the etched mark with the standard liquid, j Lower the board holding the tube to the baseboard and level | the instrument while holding one finger over the end of the ` capillary tube. Remove the finger when ready and the liquid will start to flow through the capillary. Start the timer when ( the liquid reaches the etched mark. Determine the place f where the second mark is. to be placed by noting the distance j the liquid has traveled when the elapsed time, in seconds, is; j equal to the viscosity of the oil in centipoises. It is advisable to use a movable mark, such as a small-rubber band, until the exact position of the mark has been recheeked quite carefully; then an etched line can be made. 29. Procedure 29.1 Dry a portion of the sample at 100 to 105C for 1 h. Weigh 5 g of the sample to the nearest 0.01 g into an 8-oz (250-mL) widemouth bottle. Add -95.00 g of the'.mixed solvent, cover the neck of the bottle with a sheet of cellophane, and screw on the cap. -- .- 29.2 Agitate on a bottle shaker until the solution is complete by visual inspection. After the solution is complete, place the bottle of the solution in a copstant-tempefature bath maintained at 25 0.1'C for 1 h. 29.3 Remove the bottle of solution from the bath and check to be sure it is free of air bubbles. Fill the viscometer reservoir to the etched mark, while vertical, with the solution to be tested. Place a finger over the end of the capillary, release the brace, lower the tube, and level; 29.4 Release the finger and determine the time for the liquid to flow from the first mark to the second. 30. Calculation 30.1 Calculate the viscosity as follows: N m eet/D (8) sIf 23 Detailed drawings ofthe complete installation can be obtained from Hercules where: N = viscosity, cP, incorporated, Wilmington, DE as Drawings No. 2173U and 2174U. t = time of flow for the sample, s, y 14 Size No. 2, International Equipment Co., Boston, MA or equivalent. 15 Viscometer calibrating oil S-60, available from Cannon Instrument Co., P. 0. Box 16, State College, PA 16801, has been found satisfactory for this method. d = density of the sample solution at 25C (0.859), and D -- density of the oil used for calibration of the viscometer. 182 DUP050296703 D 914 TABLE 1 Solutions for Viscosity Determination . Dow 'Viscometer If'Designation Pr Pir p |'!n Q R S |T f: U Capillary Bore Diameter, mm 1.10 1.49 1.77 2.51 3.15 4.40 Approximate Viscosity, CP at 25 C . 10 20 60 160 Approximate D 446 Design Ubbeiohde Viscometers 2 2C 2B 3C 3B 4C Cannon Standard Viscometer Calibrating Liquid S-60 S-200 S-200 M00 S-600 S-0000 Report ' 31.1 Report the viscosity in centipoises, the solution ocentration, and the test method (Hercules Horizontal apillary). - 32. Precision 32.1 Duplicate determinations should agree within 5 % of 'pie value obtained. Jfi DOW MODIFIED UBBELOHDE VISCOSITY 33. Apparatus 33.1 Constant-Temperature Bath, capable of maintaining a temperature of 25 0. PC. 33.2 Shaker, Bottle.1* 33.3 Timer, calibrated in 0.1-s units. 33.4 Viscometers, modified Ubbeiohde (Fig. 4). 33.5 Thermometer--ASTM Kinematic Viscosity Ther mometer, having a range from 74.5,to 79.5 F and con forming to the requirements for Thermometer 45F as prescribed in Specification E 1. 34. Reagents 34.1 Ethanol (95 volume %), undenatured or specially denatured conforming to Formula 2B of the U.S. Bureau of Internal Revenue. 34.2 Toluene, meeting the requirements of Specification D841. 34.3 Standard Calibrating Liquids15 (see 35.2). 34.4 Mixed Solvents (80 4- 20 and 60 + 40 tolueneethanol by mass)--Mix proportional amounts of toluene and ethyl alcohol described in 34.1 and 34.2. Mix thor oughly. 35. Calibration 35.1 Select viscosity-calibrating liquids that will yield a minimum efflux time of 200 s in the viscometers to be standardized at 25 0.1C. See Specification D 476. 35.2 Calibrate one viscometer of each capillary size to be used in the viscosity test work using the calibrating liquid that is indicated in Table 1. 35.3 Charge the Ubbeiohde viscometer selected with the appropriate viscometer calibrating liquid by pouring the liquid into the large tube to a level in line with the bottom of Heavy wall nrlrttis-opprox. ronje SlZS OS follows : I5cps viscosity 1.5 mm X.D. 25cps viscosity 1.8 mm 1.0. lOOcps viscosity 2.4mm X.D. 400 cps viscosity 5,2 mm l.D. FH3. 4 Dow Modified Ubbeiohde Viscometer m DU P050296704 D 914 the vent-tube entrance. Charge the viscometer in such a manner so that the U-tube at the bottom fills completely without trapping air. 35.4 Place the viscometer in a constant-temperature water bath at 25 0.1 C, immersing the viscometer to cover the functioning areas. Allow the liquid to reach the required temperature. Determine the temperature by placing the thermometer into the liquid. Remove the thermometer. Place a suction bulb over the end ofthe calibrated flow tube and your finger over the end of the vent tube; then apply suction on the calibrated tube until the liquid level is drawn half way up into the upper bulb of the calibrated tube. Release the suction and finger from the viscometer. 35.5 Time the flow in seconds between the upper and lower calibration lines to the nearest 0.10 s with a timer. If the time in seconds is less than 200, select a viscometer with a smaller capillary and repeat the operation. 35.6 Without recharging the viscometer, make check determinations by repeating the procedures five times. De termine the efflux time by averaging the five values. The range of the individual values should not exceed 0.5 s. 35.7 Calculate the standard viscometer constant, F, for ethylcellulose solutions as follows: F^(VxdM/`) (9) where: V = absolute viscosity of the calibrating liquid at 25^3, dQ = density ctfthe calibrating liquid at 25C, de = density ofthe sample solution at 25C (use 0.861 for 80 + 20 and 0.845 for 60 + 40 toluene-ethanol), and l = flow time, s. 36. Procedure 36.1 Weigh 57 0.02 g of the solvent solution into an 8-oz (250-mL) jar. Weigh 3.0 0.01 g ofdry sample and add to the solvent in the jar. Close the jar with a lined screw cap and shake to wet and disperse the sample. Continue to shake for about 15 min on the shaker, or until the sample is completely dissolved. 36.2 Select a Ubbelohde viscometer based on the approx- imate viscosity range (see 35.2). Add'sample solution to the large tube to a level in line with the bottom of the vent tube entrance. 36.3 Place the viscometer in the 25 0.IC constant- I temperature bath. (Immerse the viscometer to cover the functioning areas.) 36.4 Place a thermometer in the viscometer (see 35.4). After the liquid has reached the required temperature, remove the thermometer. Charge the viscometer by placing a ; suction bulb over the end of the calibrated flow tube and then, with a finger over the opening of the vent tube, apply ; suction on the calibrated tube until the liquid level is drawn j half-way up into the upper half of the calibrated tube. : Release suction and finger from the tubes. ! 36.5 Time the flow between the upper and lower calibra- j tion lines to the nearest 0.1 s. 36.6 Repeat the above procedure and average the two { efflux times. If the time range exceeds 1 s, repeat the ; operation a third time and average the two values that deviate the least. 37. Calculation 37.1 Calculate viscosity, F, in centipoises as follows: I F,=FxT (10) where: F = viscometer constant (see 35.7); and T = efflux time, s, from 36.6. 38. Report 38.1 Report viscosity in centipoises, solution concentra- i tion, and the test method (Dow Modified Ubbelohde). 39. Precision 39.1 Data obtained by this procedure indicate a precision of 5 %. '} The American Society for Testing and Materials takes no position respecting the validity ol anypatent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity oTany 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 additionalstandards and should be addressed to ASTM Headquarters.' Your comments will receive careful consideration at a meeting of the responsible technical commltteerwhlch you may attend. If you feel that your comments have net received a fair hearing you should make your v/aivs known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. I | i 184 DU P050296705 Designation: D 962 - 81 (Reapproved 1986)41 istant,! er tht1 Standard Specification for Aluminum Powder and Paste Pigments for Paints1 This standard is issued under the fixed designation D 962; 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 reappzoval. A superscript epsilon {) indicates an editorial change since the last revision or reapproval. > Note--The title of this specification was editorially changed in April 1986. {Scope |5i,l This specification covers four types and three classes bf aluminum pigments for use in paints. (ibra- i. Referenced Documents '2.1 ASTM Standards: two 'D480 Test Methods for Sampling and Testing of Flaked the Aluminum Powders and Pastes5 that ?>;E 34 Test Methods for Chemical Analysis of Aluminum i! and Aluminum Base Alloys3 3.Classification 3.1 Type I--Leafing Aluminum Pigment Powder: 00) j 3.1.1 Class A, Fine--Maximum of 0.1 % retained on a [jo. 325 (45-jim) sieve. 3.1.2 Class B, Medium--Maximum of 1.5 % retained on . ajNo. 325 (45-pm) sieve. | ; 3.1.3 Class C, Coarse--Maximum of 20 % retained on a iijo. 325 (45-pm) sieve. ra- if 32 Type II--Leafing Aluminum Pigment Paste: || 3.2.1 Class A, Fine--Maximum of 0.1 % retained on a |lo. 325 (45-p.m) sieve. 3.2.2 Class B, Medium--Maximum of 1.0 % retained on ya 1 No. 325 (45-pm) sieve. I 3.2.3 Class C, Coarse--Maximum of 15 % retained on a po. 325 (45-pm) sieve. I 3.3 Type III--Nonleafing Aluminum Pigment Powder iplote): y 3.3.1 Class A, Fine--Maximum of 1.5 % retained bn a pTo. 325 (45-pm) sieve. 3.3.2 Class B, Medium--Maximum of 6.0 % retained on a No. 325 (45-pm) sieve. * 3.3.3 Class C, Coarse--Maximum of 20 % retained on a |[!f>Jo. 325 (45-pm) sieve. 3.4 Type IV--Nonleafing Aluminum Pigment Paste ^(Note):* i |i 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint ^"and Related Coatings and Materials and is the direct responsibility of Subcom? ndttee DO 1.31 on Pigment Specifications. ' Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 962 - 48 T. Last previous edition D 962 - 66 (1973). 2 Annual Book ofASTM Standards, Vot 06.02. i 3 Annual Book ofASTM Standards, Vol 03.05. 3.4.1 Class A, Fine--Maximum of 0.1 % retained on a No. 325 (45-p.m) sieve. 3.4.2 Class B, Medium--Maximum of 1.0 % retained on a No. 325 (45-pm) sieve. 3.4.3 Class C, Coarse--Maximum of 11.0 % retained on a No. 325 (45-pm) sieve. --The particle size characteristics of the Type 3 and Type 4 pigments of the same class do not correspond with each other; in the case of Types 1 and 2 they do. 4. Composition and Properties 4.1 Aluminum Pigment Powder (Type 1, Leafing and Type 3, Nonleafing)--The aluminum pigment powder shall consist of commercially pure aluminum in the form of fine, polished flakes, and a suitable fatty lubricant. It shall contain no filler or extender pigments. 4.2 Aluminum Pigment Paste (Type 2, Leafing and Type 4. Nonleafing)--The aluminum pigment paste shall consist ofcommercially pure aluminum in the form offline, polished flakes, and a suitable fatty lubricant combined with a volatile thinner. It shall contain no filler or extender pigments. 4.3 The aluminum pigments, powder, and paste of both leafing and nonleafmg types shall conform to the require ments given in Table 1. __ 4.4 The paint made from the powder or paste shall be free-flowing and shall give a continuous coating at least equal in smoothness, luster, and general appearance to that of a reference sample mutually agreed upon bythe purchaser mid the seller. 4.5 The aluminum pigments, powder and paste of both leafing and nonleafing types, stored in unopened original - packages within 6 months after shipment shalfpass all tests applicable to the respective type and class as described in Test Methods D 480. 5. Test Methods and Sampling 5.1 Sampling and tests shall be conducted in accordance with Test Methods D 480. Since several of the methods are empirical and the results are affected by the method, the specified procedures should be closely followed. 6. Packaging 6.1 Aluminum paste should be packaged in a polyvent container that can be safely vented in case of pressure build-up. 185 DUP050296706 # D 962 TABLE 1 Requirements for Aluminum Pigments Leafing Nonleafing Typel (Powder) Type 2 (Paste) Typc3' (Powder) Type 4 (Paste) Nonvolatile matter at 105 to 110C, min, % Easily extracted fatty and oily matter {polishing lubricant), max, %A Total impurities other than fatty and oily matter, max, %A Coarse particles, max, 56: Class A (total residue retained on a No. 325 (45-pm) sieve) Class B (total residue retained on a No. 325 (45-pm) sieve) Class C (total residue retained on: No. 100 (150-pm) sieve No. 325 (45-pm) sieve) Leafing, min, Class A Class B Class C ; > 99 4.0 1.0 0.1 1.5 0.5 20.0 50 50 50 85 3.0 0.7 . 0.1 " 1.0 0.5. 15.0 55 50 -. 50 . 99' 4.0 1.0 1.5 6.0 0.5 20.0 absent absent absent 65 3.0 1.25 0.1 1.0 0.5 11.0 absent absent absent A Nonleafing pigments may contain metal compounds as dispersants; If required, a complete analysis may be made In accordance rwith Test Method E 34. The American Society for Testing and Materials fates 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'suchrights, 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 reapproved or withdrawn, your comments are Invitedeitherfor 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 fee/ that 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. v. , HS DUP050296707 Designation: D 963 - 81 {Reapproved 1986)et Standard Specification for. I Gdpp# Phthato^Srtirife Blue Pigment1 Ws;standard is issued imdr the fix*# designation D 9$3; .the number immediately following the designation indicates the year of . otighalihdoptioh or, in the Of revion, the year of last jrevision. A number in parentheses indicates the year of last rcapproval. A v superscript epsDon (e) indicates an editorial change since the last revision or reapproval. Jtr ' iTjfr., Editorial changes were made throughout in April 1986. v:T: .. vmi.l This specification covers copper phthalocyanine blue tobepurchased in dry powder form for use in nis; printing inki and related products. Several types are ^^faMe, intended for different encf uses. The specific end MaJ|B6iise,, will .determine which of the tests in Section 5 are '.able. t,Ti - oper- ySions and equipment- this standard Hoes not purport to JfithMess all ofthe safetfproblems associated with its use. It is IK Responsibility of the user of this standard to establish ""yjpfiropHdte safety and health practices and determine the tiipplicbbility ofregulatory limitations prior to use. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods f6r Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments12 D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out2 ID 362 Specification for Industrial Grade Toluene3 = D 387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D476 Specification for Titanium Dioxide Pigments2 D 600 Specification for Liquid Paint Driers3 D1135 Test Methods for Chemical Analysis of Blue Pigments2 D1208 Test Methods for Common Properties of Certain Pigments2 -; 1;3.; Composition and Properties; * 3. lr Pigment--The pigment shall consist of the product j known commercially as copper phthalocyanine blue, with or J1 without other ingredients incorporated during manufacture to improve or alter the working properties of the pigment, |p but free of any other coloring matter, either organic or inorganic. The pigment shall conform to the following requirements: 1 This specification 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 1.31 on Pigment Specifications. Current edition approved Oct 30, 1981. Published December 1981. Originally published as D 963 - 48 T. Last previous edition D 963 - 65 (1975). 2 Annual Book ofASTM Standards. Vo] 06.02. 3 Annual Book ofASTM Standards, Vol 06.03. ____________________________________ Moisture and pther volatile matter, max, % 3.0 Other coloring matter none 3.2 Mass Color and Character of Tint--The mass color and character of the tint formed by mixture with a white pigment shall be the same as, and the strength not less than, that of a reference sample mutually agreed upon by the purchaser and the seller. 3.3 Oil Absorption--The oil absorption shall be between 90 and 110 % of that of a reference sample mutually agreed upon by the purchaser and the seller. 3.4 Reaction in Identification Tests--The pigment shall show the same reaction in identification tests (see 5.5 through 5.9) as a reference sample mutually agreed upon by the purchaser and the seller. 3.5 End Product Dispersion Stability--When specified, end product dispersion stability, determined as described in 5.10 or by Using a mutually agreed upon test, shall be the same as or better than that of a reference , pigment sample mutually agreed upon by the purchaser and the seller. --End product dispersion stability of a phthalocyanine pig ment is frequently referred to as flocculation-resistance. It is judged as the difference in depth of tint between a sprayed and a poured or brushed coating. The behavior ofthe pigment can be markedly .affected by the formulation used, the type of vehicle, thinner, etc. It is important that the purchaser and seller define the type ofcomposition to be used in carrying out the test if the one described in 5.10 is not acceptable. 3.6 End Product Storage Stability--When specified, end product storage stability, determined as described in 5,11, shall be the same as or better than that ofa reference pigment sample mutually agreed upon by the purchaser and the seller. Norn 2--Storage stability ofa phthalocyanine pigment is frequently referred to as crystal stability, since it may be a measure ofthe tendency of the phthalocyanine to grow in particle size, that is, to grow crystals and thus lose strength. It is also related'to a change in dispersion stability as defined in Note 1. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other .unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 1000 lb (500 kg), except that for shipments of less than 1000 lb, two samples shall be taken. At the option of the purchaser, each sample may be tested or samples from the same production may be blended in equal quantities to form a composite sample. DUP050296708 # D 963 TABLE 1 Ingredients for Dispersion Stability Test Ingredient Amount Specification Porcelain bate, Va-in. (12.7-mm) dia Toluene (industrial grade) Titanium dioxide (rutile type) Soya-modified phthalic aikyd solution.4 50 S solids 1360 g 380 mL 750 g 275 g D 362* D476B A Specification D 362. B Specification D 476. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon by the purchaser and the seller. 5.2 Moisture and Other Volatile Matter--Method A of Test Methods D 280 or D 1208.. 5.3 Mass Color and Tinting Strength--Test Method D 387. 5.4 Oil Absorption--Test Method D 281. 5.5 Identification--Procedure section (of Identification) of Test Methods D 1135. 5.6 Basic Dye Derivatives--Test Methods D 1135. 5.7 Other Organic Coloring Matter--Test Methods D1135. . 5.8 Ultramarine Blue--Test Methods D 1135. 5.9 Iron Blue--Test Methods D 1135. 5.10 End Product Dispersion Stability--The dispersion stability Shall be determined with a paint, enamel, or lacquer agreed upon, using the pigment sample under test and a reference pigment sample. Unless the purchaser and seller agree otherwise, the following procedure shall be used. It has the advantage of combining the. dispersion stability and storage stability (see 5.11) tests. " 5.10.1 Tinting White--Charge a 1-gal' (3.8-L) porcelain ball mill with the ingredients given in Table 1. Rotate the mill at 70 to 75 r/min for 24 h; then add 1900 g of alkyd resin solution,4 90 mL of toluene, and 15 g of liquid drier containing lead and cobalt and conforming to Specification D 600. Rotate the mill for 1 h and pour the mixture through a paint strainer and store in tightly closed containers. 5.10.2 Mill Base--In an 8-oz flat, cream jar,5 charge 315 g of `/8-in. (3.2-mm) diameter steel shot? 63 mL of toluene, 31 g of alkyl resin solution,4 and 12.5 g of copper phthalocyanine blue. Rotate for 24 h, at 60 to 80 r/min. Add 100 g of alkyd resiri and 10 mL of toluene, and rotate for 30 min. Pour the mixture through a paint strainer and store in a tightly closed container until used. 5.10.3 Tint--Mix 32 g of mill base (see 5.10.2), 93 g of tinting white (see 5.10.1) and 40 mL of toluene. Shake vigorously for 30 min. Spray at once to good covering on 4 AROPLAZ 7310-X-50, available from Spencer Kellog Div. of Cargill Inc., P.O. Box 807, Buffalo, NY 14240, a short oil alkyd soya type, is suitable for this purpose. 5 Cream jars available from Zuckerman Honickman, Inc., 36th and Reed Sts., Philadelphia, PA, have been found satisfactory for this purpose. FIG. 1 Illustration of Relative Flocculation Tendency glazed cardboard or primed metal panels. 5.10.4 Procedure--Allow the freshly sprayed panel to dry until the film becomes tacky (15 to 30 min)? then vyith the ' finger gently rub a portion ofthe panel. This area will usually show an increase in tint depth over the sprayed portion (Fig. 1). Allow the remaining portion of tint to stand for 30 min, then hand-mix or shake it briefly and pour over a part ofthe previously sprayed panel. Air dry the panels for 2 h at-room temperature and force-dry for 1 h at 105"C. The poured portion ofthe film is generally equal to or lighter in tintThan the sprayed portion. The. difference between the strength of the sprayed portion and that of the rubbed and pouredareas shali be no .more than that of a previously agreed upon standard sample. 5.11 End Product Storage Stability--Unless the purchaser and the seller have agreed otherwise, the following procedure shall be used. Tint a portion of the mill base prepared as described in 5.10.2 and spray the panel at once. Store the remainder at 50 to 60C for a period ofsix weeks in a tightly closed container (Note 3). Then cool to room temperature, shake well, and prepare a tint as before. Any tendency toward crystallization, or. flocculation will result in a loss of tinting strength. The behavior of a given sample shall be compared to that of a previously agreed upon, standard sample. 3--Prolonged storage at elevated temperatures will cause some alkyds to gel. DUP050296709 # D 963 The Amerloan 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 euoh 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 trie responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved orwithdrawn. Your comments are Invitedeither for revision ofthis standard or for additionalstandards and sAoutd 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. 189 DUP050296710 # Designation: D 964 - 65 <Reapproved 1989) Standard Specification for Copper Powder for Use in Antifouling Paints1 This standard is issued under the fixed designation D 964; 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 reapprovai. 1. Scope 1.1 This specification covers copper powder for use in antifouling paints. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D283 Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments3 3. Composition 3.1 The pigment shall consist essentially of finely divided 1 This specification is under the jurisdiction ofASTM Committee D* l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Aug. 31, 1965. Published October 1965. Originally published as D 964 - 48. Last previous edition D 964 - 55. 2 Annual Book ofASTM Standards, Vols 06.0 i and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. copper metal and shall conform to the following require ments: Copper, min, % Coarse particles, max, 99 1.0 4. Sampling ,4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods: 5.1.1 Copper--Methods D 283. 5.1.2 Coarse Particles--Test Methods' D 185. 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. Uaers 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 reapprovad or withdrawn. Your comments areInvited either forrevision ofthis standard orfar 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. DUP050296711 Designation: D 970 - 86 (Reapproved 1991)' Standard Test Methods for Para Red and Toluidine Red Pigments1 This standard is issued under the fixed designation D 970; 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. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 7191 ofFederal Test Method Standard No. 14IA. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. 11 Keywords were added editorially in January 1991. fgcope 111 These test methods cover para red and toluidine red jffftients (toners) in the dry form commercially known as Bee." jjta This standard does not purport to address all of the fhfety problems, if any, associated with its use. It is the H&rhjponsibility of the user of this standard to establish approwyriate safety.and health practices and determine the applica~~~~Mlity of regulatory limitations prior to use. % Referenced Documents he i 2.1 ASTM Standards: |D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 1 1 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 D 387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller3 D1193 Specification for Reagent Water4 D3335 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy5 D 3624 Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy5 p3. Significance and Use 3.1 These test methods are used to determine the purity j and some physical properties of para red and toluidine red pigments. This information ft significant to pigment pro ducers and to coatings manufacturers. I 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 1 These tesl methods ate under the jurisdiction of ASTM Committee CM on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.2I on Chemical Analysis of Paints and Paint Materials. Current edition approved Sept. 26.1986. Published November 1986. Originally published as D 970 - 48. Last previous edition D 970 - 73 (I979){1. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards. Voi 06.02. 4 Annual Book ofASTM Standards, Vols06.03and 11.01. 3 Annual Book ofASTM Standards, Vol 06.01. 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. 4.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean water con forming to Type II of Specification D 1193. 4.3 Chloroform. 4.4 Hydrochloric Acid (1+1)--Mix equal volumes of con centrated hydrochloric acid (HC1, sp gr 1.19) and water. 4.5 Nitric Acid (3+5)---Mix 3 volumes of concentrated nitric acid (HNOj, sp gr 1.42) with 5 volumes of water. 4.6 Potassium Hydroxide, Alcoholic Solution--Dissolve 10 g of potassium hydroxide (KOH) in 90 mL of ethyl alcohol (95 %). 4.7 Sodium Hydroxide (WO g/L)--Dissolve 100 g of sodium hydroxide (NaOH) in water and dilute to 1 L. 5. Solubility in Chloroform 5.1 Place about 0.05 g of the dry pigment in a 50-mL Nessler tube, add 40 mL of chloroform, and warm slightly, stirring with a glass rod. Compare this solution with, a similarly prepared solution of a standard sample of known purity. Complete solubility of the pigment in chloroform is indicated if a .dear orange red solution is obtained. 1--Any turbidity indicating an impurity may be separated- conveniently by extracting 5 g of the pigment in a Sbxhlet extractor, using chloroform as the solvent The residue may then be examined and estimated. 6. Qualitative Test for Identity and Purity 6.1 To 10 mL of the chloroform solution (5,1) add 2 mL of alcoholic potassium hydroxide (KOH) solution. An in tense violet coloration indicates the presence of para red toner, (l-(p-nitro-phenylazo)-2-naphthol). A wine red coloration indicates the presence of toluidine red toner (l-(2-nitro-p-tolyI-azo)-2-naphthol). It is well to make sideby-side comparisons, using a standard pigment as control. 6 "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." 191 iiifr DUP050296712 D 970 2--Infrared spectrophotometry may also be employed for this purpose if equipment is available and suitable reference spectra have been agreed upon by purchaser and seller. 7. Ash 7.1 Transfer about 2 g of the sample (weighed to 0.1 mg) to a tared porcelain or platinum crucible and heat at red heat until all organic matter is destroyed. Cool and weigh. 3--For examination for low concentrations of lead and mercury, refer to Test Methods D 3335 and D 3624. 7.2 Calculate the percent of ash present as follows: Ash, % - (R/S) x 100 where: R = residue, g, and S = sample used, g. 8. Resistance to Adds and Alkalis 8.1 Place about 0.5 g of the dry pigment in a 50-mL beaker and add about 40 mL of HN03 (3+5). Stir well and allow the pigment to settle. Decant the liquid and filter it. The filtrate should show no more color than a reference pigment mutually agreed upon by the purchaser and the seller. Repeat using HQ (1+1). Repeat using NaOH solution (100 g/L), omitting the filtration. 9. Moisture and Other Volatile Matter 9.1 Determine the percent moisture and other volatile matter in accordance with Test Methods D 280. 10. Coarse Particles 10.1 Determine the percent of coarse particles in accord ance with Test Methods D 185. 11. Mass Color and Character of Tint 11.1 Determine the mass color and character of tint in accordance with Test Method D 387. 12. Precision and Bias 12.1 Data are not available to determine the prerision and bias of these test methods. There are no plans at present to obtain such data. The methods have been in use for several years and are considered acceptable. 13. Keywords 13.1 para red pigment, analysis of; pigment; toluidine red pigment, analysis of; toner, para red and toluidine red The American Society for Testing and Materials takes no position respecting the velidity ofany patent rights assertedin connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ofany such potent 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 arid must be reviewed every five years and il 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 wll receive careful consideration at a meeting of the reaponelble 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 theASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296713 Designation: D 1013 - 88 Standard Test Method for Determining Total Nitrogen in Resins and Plastics1 This standard is issued under the fixed designation D 1013; 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 supetscript 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 of Specifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. ffScope 1.1 This test method covers the determination of total 'f'nitrogen in nitrogen-containing plastics, resins, and resin ijjjblutions. This test method is not applicable for use on frnaterials containing nitro-groups. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to ddress ail ofthe safety problems associated with its me. It is responsibility of the user of this standard to establish ppropriate safety and health, practices and determine the pplicability ofregulatory limitations prior to me. Referenced Document 11*2.1 ASTM Standard: D1193 Specification for Reagent Water12 Significance and Use - If 3.1 Total nitrogen content gives an indication of the level l or purity of a nitrogen-containing material such as an amine Ifesin. It is important for the quality control of amine resins | tod is often used to determine whether the proper amounts ofmany types of nitrogen-containing materials are present in formulated products. 4. Apparatus 4.1 KjeldahlFlasks, for digestion and distillation, 800-mL capacity, moderately heavy wall, and made of hard glass. 4.2 Connecting Bulbs, of the Davisson type, or a bulb equally effective in preventing mechanical carry-over of the contents of the distillation flask to the condenser. 4.3 Digestion and Distillation Equipment--A suitable Kjeldahl digestion and distillation apparatus, such as any of the well-known commercial units for multiple work. The units may be heated either electrically or by gas burner. 4.4 Connecting Tubes made of moderately heavy-wall glass tubing, 6 to 8 in. (150 to 200 mm) in length, for conducting the distillate from the condenser to the receiver. 4.5 Weighing Tube (for Liquid Resins)--Any convenient device for weighing a few grams of sample in a matter such that no loss of volatile constituents will be sustained during the weighing operation. 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.3 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 ence to w^ter shall be understood to mean reagent water conforming to Type II of Specification D 1193. 5.3 Hydrochloric or Sulfuric Acid, (standard 0.5 N)-- Dilute 43 mL of HC1 (sp gr 1.19) or 14 mL of H2S04 (sp gr 1.84) to 1 L with water. Standardize against the 0.5 ;VNaOH solution (3.7), using the same indicator as will be used in titration of the specimen (4.4). . 5.4 Metallic Mercury or Mercuric Oxide: 5.5 Methyl Purple Indicator Solution. . 1--Methyl purple has recently met with considerable favor, and is to be recommended because ofthe abruptness of its color change in the. presence of ammonium salts. This indicator may be purchased.in solution form ready for use. 5.6 Methyl Red Indicator Solution--Dissolve 0.2 ,g -of methyl red in, 1Q0 mL of methanol, ethanol, or isopropanol. 5.7 Potassium Sulfate. 5.8 Sodium Hydroxide Solution (760 g/L)--Dissolve' 1000 g of technical grade NaOH in 1 L of water. 5.9 Sodium Hydroxide, Standard Solution (0.5 N)--Pre pare a 0.5 N NaOH solution free ofcarbonates, using reagent grade NaOH, and standardize against the National Bureau of Standards standard reference material No. 84 of potassium acid phthalate, using phenolphthalein indicator. Protect the solution against C02 absorption. 5.10 Sulfide or Thiosulfate Solution--Dissolve 40 g of K2S or Na2S, or 80 g of Na2S203 5H20, in water and dilute to 1 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 D01.33 on Polymers and Resins. Current edition approved Oct. 31, 1988. Published December 1988. Originally published as D 1013 - 49. Last previous edition D 1013 - 81 (1987)'1. 2 Annual Bock 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." 193 DUP050296714. # D 1013 5.11 Sulfuric Acid (sp gr 1.84). 6. Procedure 6.1 Transfer a portion of the sample, weighed to 1 mg, to a Kjeldahl flask, using a weighing tube if the material is a liquid. The quantity of sample taken should be an amount that will contain from 150 to 250 mg ofnitrogen. Add from 0.5 to 0.75 g of metallic mercury or the equivalent weight of HgO, 10 g ofK2S04, and 25 to 35 mL of H2S04 (sp gr 1.84). If the material under test is a urethane resin or polymer the amount of H2S04 (sp gr 1.84) should be increased to 60 mL. If preferred, H2S04 (1+1) may be used for digestion in place of H2S04 (sp gr 1.84) in which case the number of millilitres used should be doubled. 6.2 Mix the contents of the flask thoroughly, place on the digestion rack, and heat slowly at first until frothing subsides. Increase the heat until the acid boils briskly then continue the digestion for 2 h after the solution becomes colorless or nearly so. 6.3 After allowing the flask to cool, add about 500 mL of water and a little granular zinc or a few boiling aids to prevent bumping. Add an excess (25 to 30 mL) of K2S, Na2S, or Na2S203 solution. If Na2$203 solution is used, it should be mixed with die NaOH solution (760 g/L) so that both are added together. Add an excess (80 to 90 mL) of NaOH solution (760 g/L), pouring it slowly down the side of the flask so that it does not mix at once with the acid solution. Immediately connect the flask to the connecting bulb and condenser, .and mix the contents of the flask thoroughly. 6.4 Distill the solution into 50 mL of 0.5 N HC1 or H2S04, making certain that the connecting tube from the condenser extends below the surface of the acid in the receiver. Continue the distillation until the ammonia has been collected in the receiver (about 3Q0 mL.ofdistillate). 6.5 Add 5 to 7 drops of methyl red or methyl purple indicator solution and titrate the excess acid with 0.5 N NaOH solution. 6.6 Blank--Make a blank determination, following the same procedure and using the same amounts of all reagents. 7. Calculation 7.1 Calculate the percent nitrogen A as follows: A = [((B -- V) N x 0.014)/5] X 100 where: . : B = NaOH solution required for titration of the blank, mL, V. = NaOH solution required for titration of the specimen, mL, N = normality of the NaOH solution, and S -- specimen weight used, g. 8. Precision 8.1 On the basis of an interlaboratory test of this test method in which operators in five laboratories analyzed six materials, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 8.1.1 Repeatability--Two results, each the mean ofdupli cate determinations, obtained by the same analyst should be considered suspect if they differ by more than- 0.25 % absolute. ., 8.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by analysts in different laboratories, should be considered suspect iTthey differ by. more than 0.5%, absolute. . The American Society lor Testing and Materials takes no position respecting the validity ofanypatent 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 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 eitherforrevision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ol 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 S(., Philadelphia, PA 19103. 194 DUP050296715 Designation: D 1135 - 86 {Reapproved 1991)ei Standard Test Methods for ."t Chemical Analysis of Blue Pigments1 This standard is issued under the fixed designation D 1135; 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 reapprovai. A superscript epsilon (r) indicates an editorial change since the last revision or reapprovai. This standard has been approved for use by agencies of the Department ofDefense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. <> Keywords were added editorially in January 1991. _______________________ _________________________________ fpScope j|ui These test methods cover procedures for the chemical JSnalysis of blue pigments known commercially as iron blue, ^copper phthalocyanine blue, and ultramarine blue. . fj.2 The analytical: procedures appear in the following tier: . ( B0 !Et s Sections Identification bisture by the Brabender Moisture Tester 6 7 and 8 Sioisture by Toluene Distillation BVater-Soluble Matter by Extraction 9 10 fiVater-Soluble Salts by Electrical Conductivity 11 election of Acid-Insoluble Extenders detection of Add-Soluble Extenders ^tection of Organic Colors and Lakes 12 and 13 14 to 17 18 & 3375D766 B "#$%')t s lentification pStoisture and Other Volatile Matter pbetection of Basic Dye Derivatives if Detection of Other Organic Coloring Matter | Detection of Ultramarine Blue f Detection of Iron Blue U124777489@ BABC 19 20 21 22 23 24 I Identification : Moisture and Other Volatile Matter Water-Soluble Matter Detection of Basic Dye Derivatives . Detection of Other Organic Coloring Matter 25 26 ; 27 28 29 1.3 This standard does not purport to address thesafety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate sctfety arid health practices and determinejhe applicability ofregulatory limitations prior to use. t! 2. Referenced Documents 2.1 ASTM Standards: ,, D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 1 These test methods are under the jurisdiction of ASTM Committee D-J oo Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved March 27, 1986. Published May 1986. Originally published as D1135 - SO T. Last previous edition D 1135 - 81. 2 Annual Book ofASTM Standards, Vol 06.02. D1193 Specification for Reagent Water3 D1208 Test Methods for Common Properties of Certain Pigments2 D2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment2 E 11 Specification for Wire-Cloth Sieves for Testing Purposes4 3. Significance and Use 3.1 These test methods are suitable for determining if impurities are present and establishing that the required pigments are present. These test methods may be used for manufacturing quality control. 4. Purity of Reagents and Water 4.1 Purity ofReagents--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.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 conformihg to Type II of Specification D 1193. 5. Preparation of Sample 5.1 Mix the sample thoroughly and take a representative portion for analysis. Reduce any lumps or coarse particles to a fine powder by grinding. 5.2 Grind extracted pigments to pass a No. 80 (180-pm) sieve.6 Discard any skins that do not pass through the sieve. Mix the finely ground pigment thoroughly. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ifASTM Standards, Vol 14.02. 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. Sac., 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." 6 Detailed requirements for this sieve are given in Specification Eli. DUP050296716 IRON BLUE (Prussian Blue, Chinese Blue, Milori Blue) IDENTIFICATION MOISTURE BY THE BRABENDER MOISTURE TESTER 6. Procedure 6.1 To approximately 0.1 g ofpigment in a 50-mL beaker, add 15 mL of NaOH solution (50 g/L). Heat to boiling. In a few minutes the blue color should be completely destroyed, giving in its place the characteristic reddish brown precipitate of ferric hydroxide. Add HCI (1-4-1) until faintly acid to litmus. The iron blue should be reformed, yielding again the characteristic blue color. ./01 2--If the NaOH treatment does not completely destroy the blue color, the evidence is strong that a foreign pigment is present. Ifthis occurs, it is best to filter the alkaline solution, weakly acidify the filtrate with HCI (1+1), and add approximately 2 mL of a ferric salt-solution (ferric sulfate or ferric alum (20 g/L, The formation of a blue precipitate established the pigment as consisting, at least in.part, of iron blue. .` 7. Apparatus 7.1 Brabender Moisture Tester--The Brabender moisture tester (Fig. 1) consists of a constant-temperature oven with weighing apparatus attached. Specimens placed in the oven may be weighed without opening the oven door or removing the specimen from the oven, as the balance scale is calibrated to read directly in percent of moisture. 8. Procedure 8:1 Set the temperature controj at 160"C and allow the oven to reach this temperature before checking or makingany weighing. Check the scale by'placing a sample dish containing 9.200 g standard analytical balance weights in the oven. The apparatus should read 8.0 % moisture. If it does FIG. 1 Brabender Moisture Tester 196 DUP050296717 D 1135 adjust to a reading of 8.0 % by turning either the right d or left hand foot screw, .2 Weight 10.000 g of the sample in the aluminum dish place in the oven. For a series ofspecimens, all should be d in the oven at as nearly the same time as possible. No cimen should occupy the position directly in front of the Weigh the specimen at the end of each hour for 5 h. :er each weighing, return the specimen to its original place oven. 3456 2--The dried pigment is very hygroscopic. In order to obtain nsistent results, the specimen position must not be changed and the len door must not be opened. 4 *8.3 Calculation and Report--Plot time against percent s in weight on rectilinear cross-section paper. Extrapolate e linear portion of the curve to zero time. That portion yond about 2 h will be essentially linear. Report the loss in weight at the extrapolated zero time as the rcent moisture in the pigment 789: 3--The pigment undergoes a slight loss in weight due to omposition during the heating. The method of plotting and extrapot corrects for this loss. An approximate value for moisture content be obtained by taking the reading at the end of the first hour's iting. An occasional pigment may decompose rapidly at the oven emperature. In such cases, determine moisture by the toluene distilla tion method (Section 91. MOISTURE BY TOLUENE DISTILLATION 9. Procedure 9.1 Determine the moisture content in accordance with Sections 7 and 8 of Method. D 1208, but using 25 g of pigment and 200 mL of toluene and adjusting the calcula tion accordingly. WATER-SOLUBLE MATTER BY EXTRACTION 10. Procedure u 10.1 Determine whether or not the pigment is easily wet | by water at room temperature by adding a little to some ! iwater in a beaker. If it tends to float on top of the water with very little, if any, tendency to sink to the bottom or disperse throughout the solution, even after agitation, it contains a hydrophobic treating agent. 10.2 Weigh to 1 mg about 2.5 g of the pigment into a 250-mL volumetric flask. If the pigment is hydrophobic as tested above, moisten thoroughly with a few mL of ethyl alcohol (Note 4). If the pigment is easily wet with water, no alcohol is necessary. Fill the flask about half full with water and shake to disperse the pigment thoroughly. Fill to the mark and again shake. Allow to remain at room temperature for not less than 15 h, shaking from time to time, preferably with an automatic shaking device. ;<=> A--Ethyl alcohol denatured with acetone (Formula No. 23A) or denatured with methyl alcohol (Formula No. 3A) has been found suitable. 10.3 Let settle, filter through a dry filter paper, and discard the first 20 mL of the filtrate. Transfer 100 mL of the clear filtrate to a weighed dish, and evaporate to dryness on a steam bath. Dry for 1 h in an oven at 105 2C, cool, and weigh. 10.4 Calculation--Calculate the percent of water-soluble matter as follows: Water-soluble matter, % * grams of residue x 100 WATER-SOLUBLE SALTS BY ELECTRICAL CONDUCTIVITY 11. Procedure 11.1 Determine water soluble salt content in accordance with Test Method D 2448. DETECTION OF ACID-INSOLUBLE EXTENDERS 12. Scope 12.1 Acid-insoluble extenders include barium sulfate, silica, and silicates. Alumina may also be found, in part, with this group. 13. Procedure 13.1 Ignite about 1 g (weighed to 0.1 mg) ofthe sample at a low temperature, just enough to decompose the last trace of pigment but not high enough to render the iron difficultly soluble in HC1 (Note 5). Cool, and add 15 mL of HQ (sp gr 1.19) and a few drops of bromine. Cover with a watch glass and evaporate to a sirup. Add about 15 mL of water, and boil. It may be necessary to add a drop or two of HQ to effect complete solution of the ferric iron residue. Filter and wash with hot water. Save the filtrate for the determination of alumina hydrate (Section 16). ?@AB 5--The ignition can conveniently be carried out in a 250-mL beaker or a porcelain (fish over a free flame. Oxidation of the specimen is evidenced by a dull glowing. While being heated, it is advisable to roll the specimen around in the beaker or dish exposing all of the surface to the oxygen of the air. A moderately low flame should be used and the ignition is complete when the specimen ceases to glow and acquires a uniform brown color. 13.2 A residue of less than 3 mg that-appears as small black specks can be neglected, since quite frequently a small amount of iron is rendered insoluble or a small amount of blue pigment escapes destruction. Ignite the residue and weigh. If appreciably more than 3 mg are present, extenders should be suspected, and if it is required to know which extenders are present, analyze the residue for silica, barium sulfate, and alumina. ?CDE 6--If alumina is present, it may appear both with the acid-insoluble and add-soluble extenders. As a rule, most of it will appear with the add-soluble extenders. DETECTION OF ACID-SOLUBLE EXTENDERS 14. Scope 14.1 Acid-soluble extenders include the alkaline earth carbonates or sulfates, magnesium carbonate, and alumina hydrate. 15. Reagents 15.1 Ammonium Oxalate Solution--Dissolve 40 g of ammonium oxalate monohydrate in warm water and dilute to 1 L. 15.2 Ammonium Phosphate Solution--Dissolve 100 g of (NH4)2HP04 in water and dilute to 1 L. 16. Procedure for Alumina Hydrate 16.1 To the filtrate from 13.1, add NaOH solution (50 g/L) until just alkaline; then add 5 mL excess. Boil for about 2 min and let stand in a warm place until the hydrous iron 197 DUP050296718 # D 1135 oxide is coagulated. Filter through a rapid filter paper, wash a few times with hot water, and discard the precipitate. 16.2 To the filtrate add 7 mL of HC1 (1+1). Add NH4OH (1+4) until just ammoniacaL Boil about 2 min. If no precipitate is apparent, allow to stand about l/z h. If the solution is still clear, no alumina hydrate is present. A white gelatinous precipitate indicates alumina hydrate. Filter and save the filtrate for the detection of alkaline earth and magnesium salts (Section 17). 16.3 Ifa rough estimate ofthe amount ofalumina hydrate is desired, the residue may be washed, dried, ignited, and weighed as A1203. 17. Procedure for Alkaline Earth and Magnesium Salts 17.1 To the filtrate from Section 16, add HC1 (1+1) until faintly acid. Divide the filtrate into two portions. 17.2 To one portion of the filtrate, add 15 mL of (NH4)j NF04 solution and neutralize with NH4OH (sp' gr 0.90). Add 10 mL excess NH4OH. If no precipitate forms immediately, let stand for a short time in a cool place with occasional vigorous stirring. Rub the inside of the beaker from time to time with a glass rod to initiate crystallization. A white microcrystalline precipitate indicates the presence of magnesium salts and possibly some alkaline earth salts as well. 17.3 To the other portion of the filtrate, add 5 mL of ammonium oxalate solution. Make slightly alkaline with NH4OH (sp gr 0.90). If no precipitate forms immediately, : warm on a hot plate and let stand for a short time. A white ; microcrystalline precipitate indicates the presence of alkaline i earth salts. If it is required to know specifically which acid 1 soluble extenders are present, any of the established tests for 9 these metal salts may be employed. 1 DETECTION OF ORGANIC COLORS AND LAKES 18. Procedure 18.1 Boil 2 g of the sample for 2 min with 25 mL ofwater. Let settle and decant the supernatant liquid. Similarly, boil the residue with 25 mL of denatured ethyl alcohol (95 %) and decant as before. Likewise boil with 25 mL of chloroform and again decant. If any one of the above solutions is colored, organic colors are present If all solutions remain colorless, disregarding a slight yellowish cast, organic colon are presumably absent. The presence of organic colors resistant to the above reagents is unlikely, but may be tested by reference to procedures given in standard reference works.7 I J i s j I j j :! 1 Reference may be made to the following: Payne, H. F., "Organic Coatings Technology," Vol II, John Wiley & Sons, Inc., New York, NY, 1961. COPPER PHTHALOCYANINE BLUE IDENTIFICATION 19. Procedure 19.1 To about 0.05 g of the sample in a 50-mL beaker, add 30 mL of H2S04 (sp gr 1.84). Stir occasionally for 15 min; the sample should dissolve, forming a dark greenish yellow solution (color best seen on the side of the beaker). Pour the solution into 250 mL of water and stir. The copper phthalocyanine should immediately precipitate as a brilliant blue flocculent mass. 19.2 Filter off the precipitate, washing once or twice with water. Scrape a small amount of the precipitate offthe filter, place on a clean platinum wire moistened with HC1, and subject it to the low flame of a bunsen burner. As the precipitate bums, a light blue-green flame should be clearly evident. This indicates organically combined copper. GHIJ 7--Characteristic spectrophotometric absorption spectra in the near infrared range (700 to 900 nm) are exhibited by dilute solutions of copper phthalocyanine blue pigments in H2S04 (sp gr 1.84) (2 to 50 mg/L). The absorption maxima are so sharp and well defined that they may be used for positive qualitative identification of the various phthalocyanine pigments. MOISTURE AND OTHER VOLATILE MATTER 20. Procedure 20.1 Determine moisture in accordance with Method A of Test Methods D 280. DETECTION OF BASIC DYE DERIVATIVES 21. Procedure 21.1 Add to 1 g of the sample, 50 mL of a mixture of equal parts of NH4OH (sp gr 0.90) and . denatured ethyl alcohol (95 %). Warm gently and filter. Neutralize the filtrate with tartaric acid solution (200 g/L) until slightly acid to litmus. If the solution is colorless, discounting a slight yellow tinge, no basic dye is present. 21.2 Ifthe solution is colored beyond a slight yellow tinge, add about 5 mL of 0.1 N TiCl3 solution (Note 8). If a-basic dye is present, the color will lighten significantly. If no basic dye is present, no significant color change will occur. KLMO 8--Titanium trichloride is marketed as a 16 % solution in HO. Mix 7 mL of this solution with 90 mL of HQ (1+2) to obtain a reagent approximately 0.1 N. Protea from oxidation. j j : ! .j j i j DETECTION OF OTHER ORGANIC COLORING MATTER j 22. Procedure 22.1 Weigh about 0.05 g of the sample into each of two 50-mL beakers. Add 25 mL (at room temperature) of denatured ethyl alcohol (95 %) to one beaker and about 25 mL of acetone to the other. Stir each well for a few minutes, and let stand for about 2 h. Filter through two thicknesses of medium-texture, qualitative filter paper. If neither filtrate possesses more than an extremely slight pink, yellow, or blue cast, organic colors are presumably absent, but may be tested for by procedures given in standard reference works.7 j DETECTION OF ULTRAMARINE BLUE 23. Procedure 23.1 Warm gently about 1 g of the sample with HC1 (1+1). Decomposition of the ultramarine blue takes place with evolution of H2S. This may be detected by either its 198 'T~' ' DUP050296719 D 1135 i coloration appearing on a strip ofmoistened aper. PQRQSRTUV o f WXYZ [\]^ _j ofthe sample in a 100-mL beaker, add 25 mL ation (50 g/L). Boil for about 1 min. Dilute to approximately 40 mL and filter. 24.2 Add HC1 (1+1) to the filtrate until faintly acid to litmus. Add 2 mL of a ferric iron solution (ferric sulfate or ferric alum (20 g/L)). The development of a blue color reveals the presence of ferrocyanide, and hence iron blue in the original pigment. For amounts around 0.05 % iron blue, the color may take 2 to 3 h to develop. ULTRAMARINE BLUE IDENTIFICATION gently approximately 0.1 g pigment with HC1 . pigment is ultramarine blue, the color will be Sjestroyed with the liberation of sulfur and H2S, I be detected by its characteristic odor or by a iration appearing on a strip of moistened lead j^-JaJbr when held above the beaker. Quite frequently not necessary, the destruction taking place at prature. jg-filf any color remains after this treatment, it can be Wraievidence that a foreign pigment is present alcohol is not necessary. Add 250 mL ofwater and boil for 5 min with good agitation. 27.3 Cool and transfer to a 250-mL volumetric flask. Dilute to the mark with wash water from the beaker; com plete transfer of the pigment to the flask is not necessary. After thorough shaking, allow to settle somewhat and filter the supernatant liquid through a dry paper, discarding the first 20 mL. Evaporate 100 mL ofthe clear filtrate to dryness in a weighed dish. Heat for 1 hat 105 2C, cool, and weigh. 27.4 Calculation--Calculate the percent of water-soluble matter as follows: Water-soluble matter, % = grams of residue x 100 DETECTION OF BASIC DYE DERIVATIVES IVSlOISTURE AND OTHER VOLATILE MATTER yb*E^ure ermine moisture in accordance with Method A of hods D 280. WATER-SOLUBLE MATTER gedure Establish whether or not the pigment is easily wet by dding a little to some water in a beaker. If it tends : top with little tendency to sink to the bottom or through the solution it contains a hydrophobic Jagent. ansfer 2.5 g (weighed to 1 mg) of the sample to a beaker. If the pigment is hydrophobic as tested |moisten thoroughly with a few millilitres of ethyl If'(Note 4). If the pigment is easily wet with water, the 28. Procedure 28.1 Determine basic dye derivatives in accordance with Section 21. DETECTION OF OTHER ORGANIC COLORING MATTER 29. Procedure 29.1 Determine other organic coloring matter in accord ance with Section 22. 30. Precision and Bias 30.1 Precision and Bias have not been determined. 31. Keywords ' 31.1 blue pigment, chemical analysis of; Brabender mois ture tester, copper phthalocyanine blue, identification of; moisture, Brabender tester; moisture, -tqluene distillation; pigment, acid soluble extenders; ultramarine blue pigment, identification of * The American Society for Testing ami 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 lights, 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 notrevised, eitherreapproved or withdrawn. Yourcomments areinvited either {or revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive oareful consideration at a meeting of the responsible .. technical commlttea, 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. 199 DUP050296720 Designation: D 1155 - 89 Standard Test Method for Roundness of Glass Spheres1 This standard is issued under the fixed designation D 1155; 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. 1. Scope 1.1 This test method12 covers the determination of the percent of true spheres in glass spheres used for retroreflective marking purposes and industrial uses. 1.2 This'test method includes two procedures as follows: 1.2.1 Procedute A, in which the selected specimen is split into two size ranges or groups prior to separation into true spheres and irregular particles, and 1.2.2 Procedure B, in which the selected specimen is split into five size ranges or groups prior to separation. 1.2.3 In determining compliance with specification re quirements, either Procedure A or Procedure B may be used. Where tests indicate failure to meet the specified percent of true spheres and irregular particles, the referee test shall be made in accordance with Procedure B. 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: E 11 Specification for Wire-Cloth Sieves for Testing Purposes3 3. Summary of Test Method 3.1 The glass particles are mechanically separated into true spheres and irregular particles by controlled vibration on a glass plate fixed at a predetermined slope. 4. Significance and Use 4.1 The roundness of glass spheres is one measureable aspect relating to their performance as a retroreflective media. The function of this test method is to measure the percent of true spheres as related to compliance with applicable specifications. _`ab 1 --This method has been used in other industrial areas outside the intended scope of this test method. 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 May 26, 1989. Published July 1989. Originally published as D 1155- 51 T. Last previous edition D 1155 - 53(1983)el. 2 For information on the development of this test method, reference may be made to the paper by Keeley, A. E., "Roundness Testing ofGlass Spheres," ASTM Bulletin, No. 174, May, 1951, p. 72. 3 Annual Book ofASTM Standards, Vol 14.02. 5. Apparatus (Fig. 1) 5.1 Electrical Feeder-Vibrator, upon which is mounted a smooth glass panel, 6 in. (152.4 mm) wide and 15 in. (381 mm) long. 5.2 Hinged Base, supporting the vibrator and panel in such a manner that the angle of slope of the glass panel with the horizontal may be varied and fixed in any predetermined position. 5.3 Vibrator--Means of varying the amplitude or strength of the vibrations transmitted to the glass panel, at a fixed frequency of 60 impulses per second. 5.4 Feeding Device or Pan, affixed to the glass panel in such a manner that the selected sample of glass may be evenly dropped at a uniform rate upon the glass panel, from various heights above the panel and at various points on the slope. 5.5 Collecting Pans or Containers, at either end of the sloping panel, in which to collect the spheres and irregular particles. 6. Selection of Specimen 6.1 Select a 50-g specimen of the glass spheres to be tested for roundness in one of the following ways: 6.1.1 By mechanically splitting a bag or other container of glass spheres, selected at random from the shipment to be tested, or 6.1.2 By grain or seed-rod selection from the container. 7. Procedure A 7.1 Sieve the selected , specimen through' a 300-pm (No. 50) sieve (Note 2). Run the spheres retaTned-on the sieve as one group, and-run the spheres passing the sieve as a second group. cdef 2--Detailed requirements for ASTM sieves are given in Specification E 11. 7.2 Level the glass panel; then raise one end from the horizontal by the distance in inches indicated on the calibra tion curve in Fig. 2 for the average diameter of spheres in the group. Affix the feed hopper to the side of the. panel at the upper one-third point ofthe slope, so that the spheres may be dropped in a uniform monolayer onto the glass panel from a height of approximately V2 in. (13 mm). 7.3 Place the size group to be tested in the feed pan, and start the vibrator. Set the vibrator amplitude control at such a position that irregular particles on the upper half of the panel will move slowly up the slope, while the true spheres roll down. Feed slowly, at such a rate that no "bunching up" or flooding of spheres on the panel occurs. 7.4 When the glass panel is well covered with spheres, stop feeding until separation of true spheres has occurred. Stop the vibrator and, after all true spheres have rolled down the 200 DUP050296721 # D 1155 i sHr.. PIG. 1 Apparatus for Roundness Test of Glass Spheres 00-55 -- -- \^ 0025 l CO T-W -- 0.020 Coel 5 O 0.015 Vs \x -1 00`0 $! s 0005 / JO. Horizontal v<y 6 ------------2 rO C3 o: 0.0232 us I * t c T3 c e *aEC. 00H6 *5 M *n 020 040 *060 oeo 100 120 Stole Reading, H, in. FIG. 2 Calibration Curve for Roundness Tester slope into the sphere pan, brush or scrape all particles remaining on the panel into the upper pan containing the irregular particles. For purpose of test, all particles not rolling freely down the slope are considered as irregular. 7.5 Repeat the procedure described in 7.3 and 7.4 until the selected size group has been completely separated, removing the true spheres and irregular particles from the collecting pans into appropriate containers. 7.6 Fill the feed pan with the true spheres collected in the primary separation, and repeat the procedure described in 7.3 and 7.4. Next, fill the feed pan with the irregular particles collected in the primary separation, and again repeat the procedure described in 7.3 and 7.4. Examine the separated spheres and irregular particles under a 20-diameter magni fying glass and repeat the reruns until satisfactory separation is obtained. 7.7 Determine the total weights of the true.spheres and of the irregular particles obtained by the above separations, and record.' - 7.8 Using the second size group obtained in accordance with 7.1, repeat the procedure described in 7.2 to 7.7. 7.9 From the total weight of true spheres obtained from both size groups, calculate the percent of true spheres iirthe total specimen, using as 100 % the total weight of true spheres plus irregular particles collected in the test--thereby eliminating from the calculation any loss ofspheres that may have occurred during handling and testing. - - 8. Procedure B 8.1 Divide the specimen into five size ranggs or groups, as follows: Passing Sieve Retained on Sieve 600-ftm (No. 30) 425-fim (No. 40) 300-nm (No. 50) 212-jim(No. 70) 425-jim 300-iun 212-fim 8.2 Level the glass panel; then raise one end from the horizontal by the distance in inches indicated on the calibration curve in Fig. 2 for the minimum diameter of spheres in the group. Affix the feed hopper over the center line of the panel, at the upper one-third point of the slope, with the feed end up-slope and approximately Vs in. (10 mm) from the glass panel. 8.3 Place the size group to be tested in the feed pan, and start the vibrator. Set the vibrator amplitude control at such a position that irregular particles on the upper half of the panel will move slowly up the slope, while the true spheres DUP050296722 D 1155 roll down. Feed slowly, at such a rate that no "bunching up" or flooding of spheres oh the panel occurs. 8.4 When the glass panel is well covered with spheres, stop feeding until separation of true spheres has occurred. Stop the vibrator and, after all true spheres have rolled down the slope into the sphere pan, brush or scrape all particles remaining on the panel into the upper pan containing the irregular particles. For purposes of this test, all particles not rolling freely down the'slope are considered as irregular. 8.5 Repeat the procedure described in 8.3 and 8.4 until the selected size group has been completely separated, removing the true spheres and irregular particles from the collecting pans into appropriate containers. 8.6 Fill the feed pan with the true spheres collected in the primary separation, and repeat the procedure described in 8.3 and 8.4. Next, fill the feed pan with the irregular particles collected in the primary separation and again- repeat the procedure described in 8.3 and 8.4. Examine the separated spheres and irregular particles under a 20-diameter magni fying glass and repeat the reruns until satisfactory separation is obtained. 8.7 The procedure described in 8.3, 8.4, and 8.5 com prises the primary separation and that in 8.6 is one complete rerun. Make a primary separation for each of the five size groups listed in 8.1 and then make the appropriate number of reruns for each size group, as follows: Spheres Retained on Sieve Reruns 425-yim (No. 40) 300-p.m (No. 50) 212-fJ.m (No. 70) Spheres Passing Sieve 212-pm (No. 70) 5 8.8 From the total weight of true spheres obtained from separations from all five size groups, calculate the percent of true spheres in the total specimen, using as 100 % the total weight Of true spheres plus irregular particles collected in the complete test--thereby eliminating from the calculation any loss of spheres that may pave'occurred during handling and testing. 9. Report , 9.1 Report the following information: 9.1.1 The weight percent of true spheres in the total specimen and 9.1.2 Whether Procedure A'or Procedure B was used. 10. Precision and Bias 10.1 A round-robin study is currently underway in order to generate a precision statement,. 11. Keywords 11.2 roundness; glass spheres The American 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 of Infringement'of such rights, are entirely their own responsibility. This standsrd is subjeel to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapprovedorwithdrawn. Your comments are invitedeitherfor revision ofthis 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 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. DUP050296723 Designation: D 1198 - 88 Standard Test Method for Solvent Tolerance of Amine Resins1 This standard is issued under the fixed-designation D 1198; 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 supersaipt epsilbn () indicates an editorial change since the last revision or reapproval: SKj^cope . ' TX.1 This test method covers, the determination of the. 'ntity of hydrocarbon solvent that ah amine resin will erate at 770F.(250C). %2. This standard may involve hazardous materials, oper- ! and equipment. This standard does not purport to fdress all ofthe safety problems associated with its use. it is responsibility of the user of this standard to. establish ppropriate safety arid health practices and determine the plicabiliiy ofregulatory limitations prior to use. Referenced Documents 2.1 ASTM Standards: ... ..... D 362 Specification for Industrial Grade Toluene12 D891 Test Methods for Specific Gravity of Liquid Industrial Chemicals3 . Summary of Test Method 3.1 A standard solvent prepared from three, relatively pure hydrocarbons is employed to titrate a specimen of the resin . a defined degree of turbidity and the solvent tolerance is ilculated from the volume of solvent added. Significance and Use 4.1 This test method gives an indication of the solubility bf an amine resin. This property is important in determining he utility of the resin in new paint formulations and in isuring its compatibility with existing paint formulations, test method is thus useful for evaluation and quality control of amine resins. S5. Apparatus ghi j Erlenmeyer Flask, wide-mouth, 250-mL capacity. : 5.2 Buret, 50-mL capacity, graduated in 0.1-mL divisions. 5.3 Print Specimen--A sheet of paper having on it printing in a black ink from 10-point, No. 31 old style type, including a double quotation mark (lower case letters ap proximately */i6 in. (1.5 mm) high) with normal spacing, [upper and lower case with no italicized or bold letters. 6. Reagents 6.1 Decahydronaphthalene, having a boiling range be tween 188 and 195C and a density, at 25C, between 0.885 and 0.890 g/mL.4 ' 6.2 Isooctane (2,2,4-trimethylpentane), having a pqfity of at least'99 mol %. 6.3 Toluene, conforming to Specification D 362. 6.4 Solvent Mixture. 6.4.1 Blend the above three-hydrocarbons in the propor tions indicated below and determine the density at 25C in accordance with Test Methods D 891. isooctane Decahydronaphthalene Toluene Parts by Weight 84 8 8 6.4,2 Standardize the solvent by titration against 20 0.1 g of mineral-spirits-standardized kauri-butanol solution.5 The volume of solvent necessary to reach the end point described in 7.3 should be between;31 and 32 mL. If the . volume of solvent is not between 31 and 32 mL make an adjustment by . varying the concentration, of decahydro naphthalene. Ifthe titrant volume is low add more decahydro naphthalene, if high add 84 + 8 isooctane-toluene mixture. Determine the density of the final mixture at 25C. jklm 1--Although similar in certain respects to commercial prod ucts identified as mineral spirits, the solvent possesses an advantage for this determination in that it is a mixture of known constant composi tion. 7. Procedure 7.1 Adjust the temperature of the solvent_and the sample , to 77 1F (25 0.5C), and conduct the determination at this temperature. ~ 7.2 Weigh the Erlenmeyer flask on a suitable balance to 10 mg. Transfer approximately 10 g of resin to the flask and again weigh to 10 mg to obtain the weight of the specimen. 7.3 Fill the buret with the solvent, and titrate the spec imen while swirling the flask constantly. Add the solvent rapidly, but at a rate such that precipitation caused by local excess of solvent is kept to a minimum, until about 90 % of the required amount has been added. As the end point is approached, add the solvent in small increments. The end point is reached when the 10-point print placed beneath the flask becomes illegible. Alternatively the end point may be taken as the point where a double quotation mark can no 1 This test method is under the jurisdiction ofASTM Committee D-l on Paint land Related Coatings and Materials and is the direct responsibility of Subcom- ; mittce D 01.33 on Polymers and Resins. Current edition approved Oct. 31, 1988. Published December 1988. Originally [' published as D 1198 - 52. Last previous edition D 1198 - 73 (1987)*'. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 15.0J. 4 The product commercially available as "Decalin" has been found satisfactory for this purpose. 3 Mineral-spirits-standardized kauri-butanol solution (Catalog No. 1846), avail able from Harieco Co.. 60th and Woodland Ave., Philadelphia, PA 19143, have been found suitable for this purpose. 203 IjfSPPiggg DUP050296724 longer be resolved. Record the volume of solvent added. 8. Calculation 8.1 Calculate the solvent tolerance T, expressed as grams of solvent tolerated by 100 g of resin, as follows: T = (VD/S)xm where: V = solvent used in the titration, mL, D = density of solvent, and S = specimen weight used, g. nopq 2--If preferred, instead of determining the density of the solvent the flask may be weighed again after completing the titration, thus obtaining directly the weight of solvent required. 9. Report 9.1 Report the grams of solvent tolerated by 100 g of sample to 1 g. Duplicate runs that agree within 2.7 % relative are acceptable for averaging (95 % confidence level). 10. Precision 10.1 The precision estimates are based on an interlabora tory study of this test method on one sample each of a modified urea-formaldehyde resin and a butylated melamine-formaldehyde resin. Six -laboratories analyzed each sample in duplicate and repeated the analysis on another day for a total of 48 determinations. The results do s not include the component of variation due to difference in solvent since the same solvent was used by all participants. The within-laboratory coefficient of variation was found to be 0.65 % with 11 degrees of freedom and the betweenIaboratory coefficient of variation was found to be 1.67 % with 5 degrees of freedom. Based on these coefficients the following criteria should be used forjudging the acceptability of results at the 95 % confidence limit: 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 2.9 % 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 6.1 % relative. 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 ofsuch rights, are entirely 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 if not revised, eitherreapproved or withdrawn. Yourcomments are invited either forrevision ofthis standard orfor additionalstandards andshould be addressed (o ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technics! committee, 'which you may attend. II you teel 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. ! DUP050296725 Designation: D 1199 - 86 (Reapproved 1991)' Standard Specification for Calcium Carbonate Pigments1 This standard is issued under the fixed designation D 1199; 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 rstuvKeywords were added editorially in July 1991. |cppe .1 This specification covers two types of high-content jum carbonate pigments, as follows: ,1,1 Type PC--Calcium carbonate precipitate, prepared jlr by complete solution or by carbonation of lime. |l.2 Type GC--Ground mineral product. j',2 Six grades of pigments, based on particle size (see 3.3) Covered. Referenced Documents |.l ASTM Standards: : 25 Test Methods for Chemical Analysis of Limestone, lb* Quicklime, and Hydrated Lime12 M* ii|. .D280 Test Methods for Hygroscopic Moisture (and Other t Matter Volatile Under the Test Conditions) in Pig- I ments3 D281 Test Method for Oil Absorption of Pigments by j 5fv, t Spatula Rub-Out3 I tV- ;D 718 Test Methods for Analysis of Aluminum Silicate nflfc Pigment3 , D1366 Practice for Reporting Particle Size Characteristics of Pigments3 D3360 Test Method for Particle Size Distribution by Hydrometer ofthe Common White Extender Pigments3 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry4 3. Composition and Properties 3.1 The pigment may be prepared by chemical precipita- Ijtion or by the fine grinding of natural calcium carbonate (containing minerals. If additional agents are used or any surface treatment is given, theif purpose shall be indicated; ; acceptance shall be as agreed upon by the purchaser and the s seller. 3.2 Composition--The pigment shall conform to the requirements for composition prescribed in Table 1. 3.3 Fineness--The pigment shall conform to the fol lowing general requirements for fineness for the grade specified: 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved June 27, 1986. Published August 1986. Originally published as D 1199 - 52 T. Last previous edition D 1199 - 80. 2 Annual Book ofASTM Standards, Vol 04.01. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 3.3.1 Grade I (Fine Paint Grade)--This grade possesses substantial amounts of material in the fine sizes, and is in general essentially below 15 to 20 pm maximum size. Coarse particles retained on the No. 325 (45-pm) sieve shall be less than 0.05 %. The maximum Specific Surface Diameter (SSD) shall be 2.5 pm. 3.3.2 Grade II (Coarse Paint Grade)--This grade is char acterized by substantial amounts in the 5- to 45-pm range, and is lower in pigment value than Grade I, Coarse particles retained on the No. 325 (45-pm) sieve shall be less than 0.5 %. The maximum SSD shall be 6 pm. 3.3.3 Grade III (Filler Grade)--This grade is character ized by substantial amounts in the 10- to 45-pm range but with the coarse particles retained on No. 325 (45-pm) sieve less than 25 % and a maximum SSD of 9 pm. 3.3.4 Grade IV {Putty Powder Grade)--This grade pos sesses less fines, and have substantial amounts of coarse particles. The coarse particles, however, shall, not exceed 30 % retained on the No. 200 (75-pm) sieve. The maximum SSD shall be 12 pm. 3.3.5 Grade V {Superfine Grade)--This grade is a super fine ground natural limestone and is characterized by major amounts less than 5 pm and a weight median particle size in the range of 1 pm. The SSD is finer than 1 pm. 3.3.5.1 Particle size methods for Grade V that are appli cable include transmission electron microscopy, scanning electron microscopy, and the Sedigraph.f_ Specific Surface Diameter can be determined by BET nitrogen absorption. The method ofTneasurement produces different values, therefore, the method of measurement shall be agreed upon by the purchaser and the seller. 3.3.6 Grade VI (Ultrafme Grade)--This grade is an ultrafme precipitated calcium carbonate and is characterized by major amounts less than 2 pm and a median particle diameter determined by electron microscopy in the range of 0.05 pm. 3.3.6.1 Particle size methods for Grade VI that are appli cable include transmission electron microscopy and scan ning electron microscopy. The Sedigraph will give weight' median particle size values aproximately 10 times greater (~0.5 pm) than by microscopy. Since the method of mea surement produces different values, the method of measure ment shall be agreed upon by the purchaser and the seller. 3.3.7 When closer control within a grade is required, the 5 Sedigraph, manufactured by Micromeritics, 5680 Goshen Springs Rd., Norcross, GA 30093, has been found suitable for this purpose. 205 ma DUP050296726 D 1199 fineness requirements shall be as agreed upon by the purchaser and the seller. 3.4 Dry Brightness or Dispersed Color--The dry bright ness or dispersed color shall be equal, within agreed upon tolerances, to that of a reference sample agreed upon by the purchaser and the seller. 3.5 Oil Absorption--Oil absorption values shall be as agreed upon by the purchaser and the seller. 4. Sampling 4.1 Two samples, each more than 1 lb (0.45 kg) shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of produc tion appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, or after blending, in equal quanti ties, the samples from the same production unit forming a composite sample. Before testing, each of the samples shall be split, and one half of each may be sealed for referee testing. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be agreed upon by the pur chaser and the seller. 5.2 Calcium and Magnesium Reported as Carbonate-- Methods C 25. TABLE 1 Composition of Calcium Carbonate Pigments Type PC Type GC~ Moisture and other vofatila matter, max, % Calcium reported as carbonate, moisture-free, min, % Total calcium and magnesium reported as carbonates, moisture-free, min, % Magnesium as carbonate, max, % 0.7 96.5* 0.2 94 * Does not apply to specialty calcium carbonate. 5.3 Moisture and Other Volatile Matter--Method A of Test Methods D 280. 5.4 Oil Absorption--Test Method D 281. 5.5 Coarse Particles--Method D 718. 5.6 Dispersed Color--Method D718, substituting the reference and test samples of calcium carbonate pigment for the standard extender pigment and sample respectively. 5.7 Specific Surface Diameter--Practice D 1366.6 I 5.8 Dry Brightness--The test sample and reference sample shall be prepared into suitable smooth, dry, packed surfaces in accordance with accepted practice and tested for reflectance using the green filter in accordance with Test Method E 97. 5.9 Particle Size--Test Method D 3360 is applicable only to Grades I, II, III, and IV. wxyz 2--See 3.3.5 for other acceptable methods. 6. Keywords 6.1 calcium carbonate 6 The Fisher Sub-Sieve Sizer has been round satisfactory fbr use with thb practice. | l I: I * 1 The American Society for Testing and Materials takesno position respecting the validity ofany patent 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 of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the tesponsible technical committee and must be reviewed every five years and II not revised, eitherreapproved 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 of the responsible technical committee, which you may attend. If you leeI 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. . ___ s I1 ii( f DUP050296727 Designation: D 1208 - 84 (Reapproved 1989)e1 Standard Test Methods for Common Properties of Certain Pigments1 This standard is issued under the fixed designation D 1208; 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 (c) indicates an editorial change snce the last revision or reapproval. This standard has been approvedfor use by agencies of the Department ofDefense to replace Methods 4462, bill, 524J, 6261 of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsforthe specificyear ofissue which has been adopted by the Department ofDefense. 41 {|}~--Editorial changes were made throughout in March 1989. Scope y, 1 These test methods cover procedures for determining cja trin properties of pigments. The procedures appear in the pdwing order: D s Sections in Ignition and Ash Sutter Soluble in Water . igen Ion Concentration (pH Value) pinity or Acidity by Titration r Content (Distillation Method) 7s O 4 5 6 7 and 8 9 and 10 r Content (Distillation Method) jient Content of Paste in Oil fiVolatile Matter in Paste in Oil 9 and 10 11 12 T3t This standard may involve hazardous materials, operqns, and equipment. This standard does not purport to ess all ofthe safety problems associated with its use. It is ' responsibility of the user of this standard to establish fropriate safety and health practices and determine the Ilicability ofregulatory limitations prior to use. Referenced Documents %.l ASTM Standards: 95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation*2 1 ID 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments1 f D1135 Test Methods for Chemical Analysis of Blue : Pigments3 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 Significance and Use | 3.1 This collection of test methods is used by pigment producers and paint manufacturers for process control, for product acceptance, and for research and development. tIt p 1 These test methods are under the jurisdiction of ASTM Committee D-i on pot and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.31 on Figment Specifications. ISCurrent edition approved Oct. 26, 1984, Published January 1985. Originally taished as D 1208 - 52 T. Last previous edition D 1208 - 78. 1 Annual Book <fASTM Standards, Vols 05.01, 06.01, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.02. ' 4Annual Book ofASTM Standards, Vol 15.05. LOSS ON IGNITION AND ASH 4. Procedure 4.1 Dry about 5 g of the sample at 105 2"C for 2 h. Transfer about 1 g of the dried pigment, weighed to 0.1 mg, to a previously ignited, weighed porcelain crucible, and ignite at 900 to 1000C for 20 min. Cool in a desiccator and weigh. Heat again for 10 min at 900 to 1000C to check the loss in weight 4.2 Calculation--Calculate the percent of loss on ignition, L, and of ash. A, as follows: L = -- x 100 (7 x100) where: Lw = loss in weight on ignition, g, A = ash, %, WB = weight of ash, g, and Ss -- specimen weight, g. MATTER SOLUBLE IN WATER 5. Procedure (Note 1} 5.1 Weigh about 10 g of the sample to 1 mg, and place in a 400-mL beaker. Add 100 mL of water (Note 2), boil for 5 min cool, and transfer quantitatively to a 250-mL volumetric flask. Dilute with water to 250 mL, mix, and allow to settle. Filter the supernatant liquid through a dry paper (Note 3) and discard the first 25 mL. Evaporate 100 mL of the clear filtrate to dryness in a weighed flatbottom dish, preferably in an oven at 105 2C. Cool and weigh. 1--This test method is not suitable for use with iron blue pigment. Use the conductivity method given in Test Methods D 1135. 2--If the pigment is found to be strongly water-repellent, wet the sample with a small amount of alcohol or carry out a preliminary washing with chloroform. 3--Water-dispereible pigments must be filtered by suitable means or the method may not be appiicable. An asbestos-fiber filter paper pad is useful. 5.2 Calculation--Calculate the percent of matter soluble in water, M, as follows: M = Rt x 2.5 x 100 S2 207 m DUP050296728 D 1208 where: R, - residue weight, g, and S2 = specimen weight, g. HYDROGEN ION CONCENTRATION (pH VALUE) 6. Procedure 6.1 Determine hydrogen ion concentration in accordance with either of the following methods: 6.1.1 Electrometric Method (Preferred Procedure)--Weigh about 5 g of the sample to 10 mg, place in a 150-mL beaker, and add 50 g of warm distilled water, freshly boiled to remove carbon dioxide. Mix well by means ofa glass rod and cool to 25C. Measure the pH of the mixture in accordance with Test Method E 70. 6.1.2 Colorimetric Method--Weigh about 10 g of the sample to the nearest 10 dig, place in a 250-mL glassstoppered Erlenmeyer flask, and add 150 g of warm distilled water, freshly boiled to remove carbon dioxide. Stopper the flask and shake vigorously for about 1 min. Cool to 25C. Let stand 1 h to allow the pigment to settle. Decant the clear liquid and determine its pH at once by means of a suitable indicator, using a block comparator or similar colorimetric method. 4--A block comparator or equivalent device is necessary in order to compensate for the color of the extract. 6.2 Report--In reporting test results, state the particular method used. ALKALINITY OR ACIDITY BY TITRATION 7. Reagents 7.1 Methyl Orange Indicator Solution--Dissolve 1 g of methyl orange in 1 L of reagent water. 7.2 Sodium Hydroxide, Standard Solution (0.02 N). 7.3 Sulfuric Acid, Standard Solution (0.02 N).8 9 8. Procedure 8.1 Shake 20 g ofthe dry pigment with 200 mL ofdistilled water for 5 min, let settle, and filter through a dry filter paper into a dry beaker, discarding the first 10 mL of the filtrate. Transfer 100 mL ofthe clear filtrate to a flask, add 3 drops of methyl orange indicator solution', and titrate to the end point with 0.02 N sulfuric acid (H2S04), if alkaline, or 0.02 N sodium hydroxide (NaOH)-solution, if acid: 8.2 Calculation--Calculate the acidity or alkalinity, ex pressed as milligrams of NaOH equivalent to 1 g of the sample, as follows (1 mL of 0.020 N NaOH solution is equivalent to 0.8 mg of NaOH): ' Alkalinity or acidity = mL of NaOH or H2S04 x 0.8 WATER CONTENT 9. Apparatus 9.1 Distillation Apparatus--A water distillation apparatus consisting of a 250-mL roundbottom flask, a straight-tube reflux condenser, and a graduated receiving trap similar to Fig. 1 of Test Method D95. 9.2 Heat Source consisting of a gas burner and oil bath, or an electric heater of the enclosed element type. 10. Procedure (Notes 5 and 6) 10.1 Place 50 g of the sample in the flask and add 100 mL of toluene or of petroleum solvent having a boiling point between 110 and 120C. Mix well. Add more solvent, if necessary, to cover the pigment. 10.2 Rinse the inner tube of the condenser with a little toluene or petroleum solvent just before starting the distilla tion, so as to wet the inner surface completely. Distill at a moderate rate until the volume ofcondensed water no longer increases (about 3 h). If any water is lodged in the condenser tube at the end of the test, wash it down with solvent or with a brush wetted with solvent 10.3 Calculation--Calculate the weight percent of water, W, as follows (assuming that 1 mL of water weighs 1 g): W-- Wj. 50 x 100 where Wc = water collected, mL. 5--This test method is not suitable for pigments that release combined water under the conditions of the test. 6--Test methods especially adapted for the determination of moisture in iron blue pigments are given in Test Methods D 1135. 7--Test Methods designed for the determination of free water (as opposed to water of crystallization) in dry pigments are given in Test Method D 280. PIGMENT CONTENT OF PASTE IN OIL procedure 11.1 Select a portion of the well-mixed sample that is free of skins. Weigh to 10 mg, about 15 g of the sample in a weighed 60-mL centrifuge tube. Add about 30 mL of., petroleum ether, mix thoroughly with a glass rod, and wash the rod with more petroleum ether (Note 8). Centrifuge at a moderate speed until well settled. Decant the clear superna tant liquid, and repeat the extraction twice with 40 mL of petroleum ether and once with 40 mL of ethyl ether. After decanting the ether, set the tube on top of a warm oven for 10 min and then in an oven at 105 2C for 2 h. Cool and weigh. 8--Other solvents or solvent mixtures may be used, provided that they leave no residue on evaporation. ~ - 11.2 Calculation--Calculate the percent pigment content, P, as follows: . P^xioo Oj where: R2 = residue weight in centrifuge tube, g, and = specimen weight, g. TOTAL VOLATILE MATTER IN PASTE IN OIL 12. Procedure N 12.1 Weigh to 1 mg a flatbottom dish about 80 mm in diameter containing a piece of stiff wire 100 mm long. Leave the wire in the dish throughout the test. Place about 4 g of the sample, weighed to 1 mg in the dish. Spread the specimen over the bottom by means of the wire and heat for 2 Vi h in an oven at 105 2C. If a skin forms, break it up at intervals during the heating by means of the wire. Cool the dish and contents in a desiccator and weigh. Heat again for 30 min to check the loss in weight. DUP050296729 # D 1208 2 Calculation--Calculate the percent volatile matter in tple, V, as follows: V = -x 100 loss in weight on heating, g, and specimen weight, g. PRECISION AND BIAS 13. Precision and Bias 13.1 Precision data are not available at this time. When they are available the appropriate statements will be added. 13.2 Bias--No bias has been determined for this test method. The American Society for Testing and Materials takes no position respecting the validity of any pedant 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 thetr own responsibility. ^--,.. .. f to nvj3i0n at any time by the responsible technicalcommittee end must be reviewed every five yetis and mved or withdrawn. Yourcomments are Invitedeitherfor revision ofthisstandard or for additional standards to ASTM Headquarters. Your comments will receive carefulponslderatign at a meeting of the responsible h you may attend. If you feel that your comments have not received a fair hearing you should make your Committed on Standards, .1916 Raise St., Philadelphia. PA 19103. 209 mm DUP050296730 Designation: D 1214 - 89 Standard Test Method for mU Sieve Analysis of Glass Spheres1 This standard Is issued under the fixed designation D 1214; 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 chaoge since the last revision or reapproval. 1. Scope 1.1 This test method covers the sieve analysis of glass spheres used for retroreflective. pavements markings and industrial uses. 1.2 This standard may involve Hazardous materials ', oper ations, and equipment. This standard does pot purport to address dll 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: D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis21 D2013 Method for Preparing Coal Samples for Analysis2 E 11 Specification for Wire-Cloth Sieves for Testing Purposes3 3. Summary of Test Method 3.1 The spheres are hand-sieved through standard sieves, starting with the sieve with the largest opening specified and progressing successively through the specified sieves in the order of decreasing size of opening, and computing the weight of glass spheres and the percent passing each of the sieves. 4. Significance and Use 4.1 The size or gradation of glass spheres is one meas urable aspect of performance as a retroreflective media. The function ofthis test is to measure the size ofglass spheres and to determine compliance with applicable specifications. 1--This method has been used in other industrial areas outside the intended scope of this test method. 5. Apparatus 5.1 Balance, sensitive to 50 mg. 5.2 Sieves, 8 in. (200 mm) in diameter, conforming to Specification Ell, and including such sieves as may be required by the specifications for the glass spheres. 5.3 Oven. 1 Hus 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 1.44 on Traffic Coatings. Current edition approved May 26, 1989. Published July 1989. Originally published as D 1214 - 52T. Last previous edition D 1214- 58(1983)**. 2 Annual Book ofASTM Standards, Vol 05.05. 3 Annual Book ofASTM Standards, Vols 05.05 and 14.02. 6.SampIes 6.1 By quartering or riffle sampling (Note 2), select a representative sample from the material to be tested. Take at least two representative samples of approximately 500 g each from separate packages from each shipment in the ratio of two samples for each' 10 000 lb (50.00 kg) or fraction thereof. Approximately 50 g of dry glass spheres are required for each test. This specimen is also selected by quartering or riffling. 2--The quartering procedure for reducing bulk samples, to obtain representative test samples of suitable size, is described and illustrated in Methods D346. Various types of riffle samplers are illustrated in Method D 2013. 7. Procedure 7.1 Hand Sieving: 7.1.1 Dry the specimen to substantially constant weight at a temperature of 105 to 110 C. 7.1.2 Weigh 50 g of the dried glass spheres to the nearest 0.1 g and place on the sieve with the largest opening in the series specified for the test, which shall be thoroughly dry. Hold the sieve, with pan and cover attached, in one hand in' a slighty inclined position so that the specimen will be well distributed over the sieve, at the same time gently striking the side about 150 times per minute against the palm of the other hand on the upstroke. Turn the sieve every 25 strokes about one sixth of a revolution in the same direction. Continue the operation until not more than 0.05 g passes, through the sieve in 1 min of continuous sieving. Each.time, before weighing the material passing through the sieve, tap the side ofthe sieve with the brush handle in order to remove any material_adhermg to the wire cloth. 7.1.3 When the sieving has been finished, remove the cover of the sieve and carefully remove, the residue re maining- on the sieve to a tared container. Invert the sieve over a piece of glazed white paper and clean the wire cloth by brushing the underside. Add the material thus removed from the wire cloth to the residue removed from the sieve. 7.1.4 Weigh the portion of the specimen retained on the sieve to the nearest 0.1 g. Place the material passing through the largest sieve on the sieve with the next smaller opening for the series selected for the sieve analysis. Continue sieving in a similar manner, using successively each of the selected series of sieves in the order ofdecreasing size of opening, and recording the weight of that portion ofthe specimen retained on each sieve. 7.1.5 Washers, slugs, or shot shall not be used on the sieves. 7.2 Machine Sieving: 7.2.1 Mechanical sieving devices may be used but the glass spheres shall not be rejected if they meet the specifica tion requirements when tested by the hand-sieving method 210 DUP050296731 # D 1214 glribed in 7.1. When mechanical sieving devices are used, thoroughness of sieving shall be tested by using the ad method for comparison. {Calculation .1 Calculate the weight of material and the percent of t specimen passing each of the sieves. Report 9.1 Report the following information: 9.1.1 Results ofthe sieve analysis reported as the total per cent passing each sieve, expressed to the nearest 0.5 %, and 9.1.2 The method of sieving used. 10. Precision 10.1 A round robin is currently underway in order to generate a precision statement 11; Keywords 11.1 sieve; glass spheres i *5 $ 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 ol 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 reqpproved or withdrawn. Your comments are Invitedeitherfor 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 yoa leel that your comments have not received a fair; hearing you should make your views known to the ASTM Committee on Standards, 1910 Race St., Philadelphia, PA 19103. DUP050296732 Designation: D 1259 - 85 {Reapproved 1990)1 Standard Test Methods for Nonvolatile Content of Resin Solutions1 This standard is issued unddr the fixed designation D1259; 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 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. Section 12 was added editorially in May 1990. 1. Scope coatings producers and users for the determination of the If 1.1 These test methods cover, the determination of non volatile content of solutions of resins in volatile organic total solids available for film formation and for the estima- 1 tion of the volatile organic content. 1 solvents. TEST METHOD A--NON-HEAT-REACTIVE RESIN I 1.2 Two test methods are included as follows: 1.2.1 Test Method A--For solutions of non-heat-reactive SOLUTIONS M resins. These solutions contain resins that remain stable and 4. Apparatus 1 release the solvent under conditions ofthe test. Examples are 4.1 Ovens: jj ester gums and alkyds. 4.1.1 Gravity-convection type, maintained at 105 2C, 1 1.2.2 Test Method B--For two types of solutions: with vents open. i 1.2.2.1 Solutions of heat-reactive resins. These solutions 4.1.2 Forced-ventilation type, maintained at 105 2C. ;l contain resins that undergo condensation or other reactions For ovens with adjustable air flow rate, set the control a under the influence of heat. Examples include the formalde damper at 50 %. m hyde reaction products of urea, melamine, and phenols. 4.2 Aluminum or Tin Foil,2 from 0.0015 to 0.0020 in. (38 1 1.2.2.2 Solutions that release solvent slowly. Examples to 50 pm) in thickness. Either one piece 6 by 12 in. (150 by 1 include epoxy resin solutions. 300 mm), or two 6 by 6-in. (150 by 150-mm) pieces may be'ij | 1.3 Test Methods A and B differ primarily in the drying used. The foil must be perfectly smooth; if it becomes 1 times and types of oven used. wrinkled during the initial handling, roll smooth as directed I 1.4 This standard does not purport to address the safety in 5.2. 1 problems associated with its use. It is the responsibility ofthe 4.3 Plate Glass--Two pieces about Vi6 in. (5 mm) thick; I user of this standard to establish appropriate safety and one piece 5`/2by 5l/2in. (140by 140 mm) and one piece 7 by | health practices and determine the applicability ofregulatory 7 in. (180 by 180 mm). j limitations prior to use. 4.4 Devicefor Weighing Specimens3--Apparatus that will j 2. Summary of Test Methods 2.1 In both test methods, a weighed specimen of resin solution is spread under pressure between two weighed sheets of aluminum or tin foil. The coated foil sheets are separated and then dried. The weight of residue is determined and the nonvolatile content is calculated. The test method is unique in that it provides for drying'of a very thin film of resin, thus minimizing chances for volatiles to be trapped and held during the heating operation. 2.2 Either a gravity-convection or a forced-ventilation oven and a 30-min heating period at 105C are used in Test Method A. 2.3 A forced-ventilation oven and a 2-h heating period at 105C are used in Test Method B. prevent loss of volatile matter during the weighing operation j such as any of the following, or equivalent: ,, j 4.4.1 Syringe, Luer, 2 or 5-mL capacity; ! 4.4.2 Weighing Buret, Smith, 10-mL capacity, or 4.4.3 Bulb Pipet, dropping, with 50-mL lylenmeyer flask, i 4.5 Roller, for Smoothing Foil--Use a ground and pol- ` ished cylinder, preferably stainless steel, approximately 7 in. (180 mm) long and 2 in. (50 mm) in diameter. 4.6 Foil Trays, two types as follows: [ 4.6.1 Trays measuring 6V2 by 12 in. (165 by 300 mm), for 1 use with 6 by 12-in. foil, constructed from No. 22-gage f (0.6-mm) aluminum sheet in accordance withdimensions f shown in Fig. 1. Several trays may be stacked in the oven to J permit running several specimens simultaneously. _ 3 4.6.2 Trays measuring 6l/2 by 6V2 in. (165 by 165 mm), 3. Significance and Use 3.1 The nonvolatile content of resin solutions is useful to 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 Paints and Paint Materials. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 1259 - 52. Last previous edition D 1259 - 61 <1980)CI. 2 Aluminum foil available from Thomas Scientific Co., P.O. Box 99, Swedesboro, NJ 08085; or from Sargent and Welch Scientific Co., 7300 North Under Ave., Skokie, IL 60077 has been found satisfactory for this purpose. Tin foil available from J. T. Baker Co., North Broad St., North Philipsburg, NJ 0886S has been found satisfactory for this purpose. 3 A Smith weighing buret is available from Ace Glass Co., 1430 Northwest B3vd., Vineland, NJ 08360. The bulb pipet is available from Thomas Scientific Co. or from Fisher Scientific Co. DUP050296733 -Millimetre dimensions appear in section on Apparatus. FIG. 1 Tray for 6 by 12-in. (150 by 300-mm) Foil FIG. 2 Trays and Holder lor 6 by 6-in. (150 by 150-mm) Foil for use with 6 by 6-in. foil, with holder, shall be constructed ifrom No. 22-gage aluminum sheet, as shown in Fig. 2.5 5. Procedure 5.1 Use the following procedure with the 6 by 12-in. (150 by 300-mm) foil sheets and the 6Vi by 12-in. (165 by 300-mm) trays. Alternatively two 6 by 6-in. (150 by 150. mm) foil sheets may be used in a similar manner with the :: 61/2 by 6`/2-in. (165 by 165-mm) trays. In handling the foil, 11 avoid wrinkling or creasing the sheets until after the spec;,s imen has been dried. Sheets may be rolled for convenience of | handling and making the initial weighing, but must be kept | smooth throughout the pressing and drying operations. 5.2 Weigh the foil to 0.1 mg. Open and place half the foil, with the shiny side up, on the 7 by 7-in. (180 by 180-mm) glass plate. If necessary, roll smooth with the metal roller. By means of the weighing device, weigh by difference a 0.9 to 1.1-g specimen of the resin solution, to 0.1 mg. Place the specimen on the center of that area of the foil covering the glass plate. Place the other half of the foil on top. Cover the foil with the second glass plate, centering the glass on the foilr and press down sufficiently to cause the specimen to spread uniformly into a thin film, about 3 in. (75 mm) in diameter. The pressure that must be exerted depends on the viscosity of the sample. In case a specimen of low viscosity should extend beyond the edge of the foil, repeat the determination, allow ing a few minutes for a portion of the solvent to evaporate from the weighed specimen before covering and pressing it. 5.3 After pressing, open the foil to its full length and place it in the foil tray. Place the tray in either a gravity-convection DUP050296734 # D 1259 or a forced-ventilation oven at 105 2C for 30 min. 5.4 Remove the tray from the oven and then carefully remove the foil sheet from the tray. Return the dried film surfaces to the face-to-face position. While the foil is still warm, fold the edges together to enclose completely the dried film. Without undue delay, weigh to 0.1 mg. 6. Calculation 6.1 Calculate the percent nonvolatile content, C, as fol lows: C~[(A-B)x 100J/S where: A ~ weight of foil plus dried solids, g, B -- weight of foil, g, and S = weight of sample taken, g. 7. Precision and Bias 7.1 The following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 7.1.1 Repeatability--The difference between two results, each the mean of duplicate determinations obtained by the same analyst, is normally about 0.2 %, absolute. Two such results should be considered suspect if they differ by more than 0.5 %, absolute. 7.1.2 Reproducibility--The difference between two re sults, each the mean of duplicate determinations. Obtained by analysts in different laboratories is normally about 0.4 %,absolute. Two such results should be considered suspect if they differ by more than 1.0 %, absolute. 7.1.3 No bias has been determined for this test method. TEST METHOD B--HEAT-REACTIVE RESIN SOLUTIONS AND SOLUTIONS THAT RELEASE SOLVENT SLOWLY8 9 8. Apparatus 8.1 Oven--Forced-ventilation type, maintained at 105 2C. For ovens with adjustable air flow rate, set the control damper at 50 %. 8.2 The remainder of the apparatus is identical with that given in 4.2 to 4.6. 9. Procedure 9.1 Weigh the specimen of resin solution and press it between two sheets of foil as described in 5.1 and 5.2. il 9.2 After pressing, open the foil to its full length and place 1 it in the foil tray. Then place the tray in a forced-ventilation I oven at 105 2C for 2 h. When using 6V2 by 6>/2-in. trays and holder, place the assembly in the oven with the open 1 ends perpendicular to the direction of air flow. fl 9.3 Complete the determination as described in 5.4. J 10. Calculation 1 10.1 Calculate the nonvolatile content as described in I Section 6. I 11. Precision and Bias j 11.1 The following criteria should be used for judging the 1 acceptability of results at the 95 % confidence level. I 11.1.1 For Heat-Reactive Resin Solutions: I 11.1.1.1 Repeatability--The difference between two re- f suits, each the mean of duplicate determinations obtained by I the same analyst, is normally about 0.3 %, absolute. Two j such results should be considered suspect if they differ by I more than 0.7 %, absolute. j 11.1.1.2 Reproducibility--The difference between two re- suits, each the mean ofduplicate determinations obtained by I analysts in different laboratories, is normally about 0.7 %, I absolute. Two such results should be considered suspect if I they differ by more than 1.7 %, absolute. I 11.1.1.3 No bias has been determined for this test I method. I 11.1.2 For Solutions that Release Solvent Slowly: j 11.12.1 Repeatability--The average difference between 1 two results each the average of duplicate determinations, 1 obtained by the same analyst is normally about 0.1 absolute. Two such results should be considered suspect if | they differ by more than 0.3 %, absolute. I 11.1.2.2 Reproducibility--The average difference between 1 two results obtained by analysts in different laboratories will 5 approximate 0.2 %. Two such results should be considered ' suspect if they differ by more than 0.5 %, absolute. 11.1.2.3 No bias has been determined for this test I method. ... 1 12. Keywords 12.1 foil'method; heat-reactive; non-heat-reactive; non- volatile; resin solution j The American Society lor Testing and Materials takes 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 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 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. 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 Pace St., Philadelphia, PA 19103. DUP050296735 Designation: D 1301 - 91 Standard Test Methods for Chemical Analysis of White Lead Pigments1 This standard is issued under the fixed designation D 1301; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year af last revirion. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the fast revision or reappraval. These test methods have been approvedfor use byagencies oftheDepartment ofDefense to replace Methods 7041, 7051 ofFederal Test Standard No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. ijScope l.l These test methods cover procedures for the chemical tlysis of basic carbonate white lead and basic sulfate white ad. | 1--If it is necessary to separate these pigments from others, efer to Methods D 215. 1.2 The analytical procedures appear in the following brder: Section * Preparation of Sample......................................................... phasic Carbonate White Lead: . . Small Amounts of Iron.................................. ............. t,, Total Lead...................................................................... Moisture and Other Volatile Matter................................ > Carbon Dioxide (Evolution Method)............................... ^ Carbon Dioxide and Combined Water (Combustion . Method)...................................................................... i,- Lead Carbonate.............................................................. |' Total Matter Insoluble in Acetic Acid............................ - Total Matter Insoluble in Acid Ammonium Acetate....... Total Impurities Other Than Moisture............... Coarse Particles............... Sasic Sulfate White Lead: Small Amounts of Iron.......................... Total Lead............................ Moisture and Other Volatile Matter................................ Total Sulfate..................................................................... Zinc Oxide..................................... Basic Lead Oxide............................................................. Total Impurities............................................;................ Coarse Particles............................ 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 1.3 This standard does not purport to address the safety lproblems associated with its use. It is the responsibility ofthe fuser 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 25 Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime2 D 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D 28G Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments4 D1193 Specification for Reagent Water5 D2371 Test Method for Pigment Content of Solvent- Reducible Paints6 D2372 Practice for Separation of Vehicle from Solvent- Reducible Paints6 D3280 Test Methods for Analysis of White Zinc Pigments4 E 11 Specification for Wire-Cloth Sieves for Testing Purposes7 * 3. Significance and Use 3.1 These test methods are suitable for determining the level of purity and for determining the levels of various impurities. They may be used to establish compliance with specification requirements. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that ail reagents shall conform to 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.- 4.2 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. 4.3 Concentration ofReagents: 4.3.1 Concentrated Acids and Ammonium Hydroxide-- When acids and ammonium hydroxide are specified by name or chemical formula only, it shall be understood that concentrated reagents of the following specific gravities or concentrations are intended: Acetic acid, CHjCOOH Hydrochloric add, HC1 Hydrofluoric acid, HF Nitric acid, HNO3 Sulfuric acid, H2S04 Ammonium hydroxide, NH<OH 99.5 % ~ spgr 1.19 48% spgr 1.42 sp gr 1.84 sp gr 0.90 1 These test methods are under the jurisdiction of ASTM Committee D-l on Faint and Related Coatings and Materials and are the direct responsibility of * Annual Book ofASTM Standards, Vol 06.02. 5 Annua! Book ofASTM Standards, Vols 06.03 and 11.01. Subcommittee DO1.21 on Chemical Analysis of Paints and Paint Materials. 6 Annual Book ofASTM Standards, Vol 06.01. Cunrent edition approved Feb. 22, 1991. Published April 1991. Originally 7 Annual Book ofASTM Standards, Vol 14.02. published as D1301 - 53 T. Last previous edition D 1301 - 86. s Reagent Chemicals, American Chemical Society Specifications," Am. Chem 2 Annual Book ofASTM Standards, Vol 04.01. ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 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." 215 DUP050296736 The desired specific gravities or concentrations of all other concentrated acids are stated whenever they are specified. Warning--See Section 5. 4.3.2 Diluted Acids and Ammonium Hydroxide---Con centrations of diluted acids and ammonium hydroxide, except when standardized, are specified as a ratio stating the number of volumes of concentrated reagent to be diluted with a given number of volumes of water, as in the following example: HC1 (1+99) means 1 volume of concentrated HC1 (sp gr 1.19) diluted with 99 volumes of water. 5. Hazards .5.1 The concentrated acids bases and other reagents used in these test methods can be dangerous. Check their Material Safety Data Sheets, (MSDS) before use. 6. Preparation of Sample 6.1 Grind dry pigments, if lumpy or not finely ground, to a fine powder for analysis. Large samples may be thoroughly mixed and a representative portion taken and powdered if lumpy or not finely ground. Mix the sample in all cases thoroughly and comminute before taking specimens for analysis. 6.2 In cases of pastes in oil, extract the oil from the pigment as described in Test Methods D 2371 or D 2372, but without straining. 6.3 Dry pigments separated from paints or pastes in oil in an oven at 203 to 210T (95 to 98C) for 2 h, grind to a fine powder, pass through a No, 80 (180-jj.m) sieve (Note 2) to remove skins, and mix thoroughly. Such pigments, after weighing, should be moistened with a little ethyl alcohol (95 %) before adding reagents for analysis. 2--Detailed requirements for this sieve are given in Specifica tion Ell. 6.4 Preserve all samples in stoppered bottles or containers. BASIC CARBONATE WHITE LEAD 7. Small Amounts of Iron 7.1 Reagents: 7.1.1 Ammonium Hydroxide (sp gr 0.90). Warning--See 5.1. 7.1.2 Hydrofluoric Acid (48 %). Warning--See 5.1. 7.1.3 Nitric Acid (sp gr L42). Warning--See 5.1. 7.1.4. Sulfuric Acid (sp gr 1.84). Warning--See 5.1. 7.2 Procedure: 7.2.1 Weigh to 10 mg about 1 g of specimen into a 400-mL beaker. Treat the sample with 10 mL of HN03 (1 + 1) and dilute to about 200 mL with water. Ifinsoluble matter remains following treatment with HN03 and dilution, filter and wash the residue with hot water until lead free. Evapo rate the filtrate and washings to about 200 mL. Add 20 mL of H2S04 (1 + 1) to precipitate the bulk of the lead (it is unnecessary to evaporate down). Cool, filter, and wash with diluted H2SQ4 (1 + 99). Save the precipitate for determina tion of total lead (Section 8). 7.2.2 Ignite the HN03-insoluble matter and treat with HF and H2S04. Bring into solution, filter (any precipitate is probably BaS04), and add to the PbS04 filtrate. 7.2.3 Colorimetrically determine iron in the combined filtrates by the thiocyanate method,9 using the same amounts J of reagents in preparing the reference standards. If copper i$, J Jpresent in the filtrate, as shown by the characteristic blue- 3 green or yellow color, remove it by precipitating the iron with NH4OH, filtering, washing redissolving the Fe(OH)3 in t 10 mL of HN03 (1 + 1), and diluting to about 200 mL 1 before proceeding with the thiocyanate method. i! i 8. Total Lead 8.1 Apparatus: j 8.1.1 Gooch Crucible, prepared prior to use. j 8.2 Reagents: } 8.2.1 Acetic Acid (glacial)--Warning--See 5.1. j 8.2.2 Ammonium Hydroxide (sp gr 0.90)--Warning--See m 5.L I 8.2.3 Ethyl Alcohol (95 volume %)--Warning--See 5.1. IS 8.2.4 Potassium Dichromate Solution (100 g K2Cr20,/ m L)--Warning--See 5.1. 1 8.3 Procedure: 1 8.3.1 Ignite the PbS04 precipitate and filter paper from 1 7.2.1 at or below 1020F (550C), and transfer.the residue to 1 a 400-mL beaker. (If preferred, a new 1-g specimen of jj pigment may be weighed to 10 mg into a 400-mL beaker. 1 Proceed to 8.3.2.) if 8.3.2 Moisten with water and add 5 mL of glacial acetic 1 acid. Warm to dissolve the material and dilute to about 200 I mL with water. Neutralize the solution with NH4OH and m then make slightly acid with acetic acid, adding bout 3 mL ii excess. Filter off any insoluble residue and wash thoroughly if with hot water. jl 8.3.3 Unite the filtrate and washings, heat to boiling, andj add 15 mL of K2Cr207 solution. Stir and heat until the ]j yellow precipitate assumes an orange tplor. Let settle and | filter on a weighed Gooch crucible. Wash by decantation 1 with hot water until the washings are colorless. Finally | transfer all the precipitate from the beaker to the crucible j and wash with ethyl alcohol (95 %). Dry at 220 4F-fl05 j 2C) for 1 h. Cool in a desiccator and weigh as PbCr04. 8.4 Calculation: PbO, % =(P x 0.691/Syx ioo ' where: ___ P = PbCr04 precipitate, g, S = specimen, g, and 0.691 =PbO/PbCr04 = 223.19/323.18. 9. Moisture and Other Volatile Matter ] j 9.1 Procedure--Determine moisture and other volatile j matter in accordance with Method A of Test Methods i D 280. 10. Carbon Dioxide (Evolution Method) 10.1 Apparatus--Knorr type of C02 evolution apparatus with dropping funnel, condenser, and suitable 'purifying train. 3--A description of a suitable purifying train, is found in the Carbon Dioxide Standard Method section of Methods C 25. 10.2 Reagent: 9 Described in Scott, Standard Methods ofChemical Analysis, Fifth Edition, D. Van Nostrand Co., New York, NY, 1939, p. 486. ms m DU P050296737 D 1301 i.2.1 Nitric Acid (l + 19). ;3 Procedure--Transfer about 2 g of the sample, ied to 10 mg, to a clean, dry evolution flask. Connect evolution flask to the absorption train, which previously been flushed free ofany C02, and add 100 mL of HN03, 19) through a separatory funnel. When all of the HN03 been introduced into the flask, close the stopcock from separatory funnel. Heat the solution in the flask to gentle g and boil for 5 min. Turn off the heat and aspirate 2 free air through the system for 20 min. Remove the (sorbing tube from the system, seal, cool in a desiccator, *nd weigh. The increase in weight is CO2. jO.4 Calculation--Calculate the percent of carbon di vide as follows: CO2,%-(Cj/Si)x 100 Inhere: = C02, g, and = specimen, g. Carbon Dioxide and Combined Water (Combustion Sf Method) ? 11.1 Apparatus--Combustion Train, consisting of the ^following parts connected in the order specified; tank of spurified compressed nitrogen, purifying jars including a C02 'sorption jar, drying tube, combustion tube, tube furnace provided with suitable controls to maintain the teihperature pom 840 to 1Q20F (450 to 550C), absorption bulb for vater, and an absorption bulb for C02. 11..2 Procedure: 11.2.1 Heat the furnace, without the combustion tube, rom 840 to 1022F (450 to 550C). Connect the combustion abe beside the furnace, connect the absorption tubes to the iaitrogen supply, and pass a slow stream of nitrogen (about 30 pnL/min) through them, to clear out any residual moisture land C02. Accurately weigh the absorption bulbs and Sfeconnect them in the train. Transfer 1 g of the specimen, fiweighed to 10 mg, to a combustion boat that has been previously ignited and cooled. p- 11.2.2 With the nitrogen still flowing, disconnect the train land place the boat containing the speciinen in the middle of he tube with the aid of a hooked wire. Flush the combustion Itube thoroughly with nitrogen and reconnect with the train. 1 Place the tube in tire furnace. ' 11.2.3Continue the combustion for 30 min, or until the U water that condenses in the inlet arm of the first absorption I bulb has been completely swept into the bulb. Disconnect I the absorption bulbs from the combustion tube, after closing I all stopcocks, place in a desiccator to cool, and then weigh. I 11.3 Calculation: Carbon dioxide, % 100 x C, Combined water, % = Combined water as Pb(OH)2, % ' (100 Wl~M)X 13.39 where: C, = C02, g, Wt = total water, g, M = free moisture, %, and 13.39 = Pb(OH)2/H20 =241.20/18.015. 12. Lead Carbonate 12.1 Calculation--Calculate the percent of PbC03 from the C02 content, as follows: PbC03, % = C, x 6.071/^, x 100 whcrci C, =CO2(10.4or 11.3), g, 52 = specimen weight used in the C02 determination, g, and 6.071 = PbC03/C02 = 267.20/44.01. 13. Total Matter Insoluble in Acetic Acid 13.1 Apparatus--Gooch Crucible, prepared and weighed prior to use. 13.2 Reagent--Acetic Acid (3 + 2). 13.3 Procedure--Transfer 10 g of the sample, weighed to 10 mg, to a 250-mL beaker and add 40 mL of acetic acid (2 + 3). Heat until solution is cbmplete and filter through a previously prepared and weighed Gooch crucible. Wash thoroughly with hot water, dry at 220 4T (105 2'C) for 1 h, cool, and weigh. 13.4 Calculation--Calculate the percent of total matter insoluble in acetic add as: (7?/y3) x 100 where: R -- residue, g, and 53 = spedmen, g. 14. Total Matter Insoluble in Acid Ammonium Acetate 14.1 Apparatus--Gooch Crucible, prepared and weighed prior to use. 14.2 Reagent--Acid Ammonium Acetate Solution--Mix. 150 mL ofacetic add (3 + 2) with 100 mL ofwater and then with 95 mL of NH4OH (sp gr 0.90). 14.3 Procedure--Transfer about 10 g of the sample, weighed to 10 mg, to a 250-mL beaker. Add 40 mL of add ammonium acetate solution and heat until solution is complete. Filter through a previously prepared and wdghed Gooch crudble and wash thoroughly with hot water. Dry pt 105 to 1KTC for 1 h, cool, and weigh. -- _ , ._ 14.4 Calculation--Calculate the percent of total matter insoluble in add ammonium acetate as: {R/SJ x 100 . ' where: i?j = residue, g, and 54 = specimen, g. 15. Total Impurities Other Than Moisture 15.1 Calculations: 15.1.1 Calculate the percent oftotal impurities other than moisture as: 100 -- (Z, + C + H + M) where: L = PbO % (8.4), C =C02% (10.4 or 11.3), H = combined water, % (11.3), and M= free moisture, % (9.1). 15.1.2 In the case of extracted pigments where direct determination of combined water cannot be made conve niently, calculate the impurities other than moisture as: 100 217 9SS k. DUP050296738 D 1301 (L + 1.205 D 4- M) where L, D, are as defined in 15.1.. 1 and J .025 = 2 COa + H20/2 COa = 106.035/88.02. 16. Coarse Particles 16.1 Procedure--Determine coarse particles in accord ance with Test Methods D 185. BASIC SULFATE WHITE LEAD 17. Small Amounts of Iron 17.1 Procedure--Determine small amounts of iron in accordance with Section 7. > > 18. Total Lead 18.1 Procedure--Determine, total lead in accordance with Section 8. .. . 19. Moisture and Other Volatile Matter .19.1 Procedure--Determine moisture and other volatile matter- in ^accordance with Method A of Test Methods D280. 20. Total Sulfate " . 20.1 Apparatus--Gooch Crucible, ignited and weighed prior to use. 20.2 Reagents: 20.2.1 Barium Chloride Solution (100 g BaClj/L)--Dis solve 117 g of BaCl2 2 H20 in water and dilute td I L). 2Q.2.|Bromine tyatpr (saturated).., , ,,, 2Q.$3 HydrochloricAcii'(l+\$. 20.2.4 SodBm Chloride. 1 , 20.2.5 Sodium Carbonate Solution (saturated): : < 20.3 Procedure: 20:3.1 Ttansfer 0.'625 g dfthe sampld td a 400-riiL bfeaker. Add 2 g of NaCl, 3 to 4 mL of brbtainewdter, and'25 ml: of HQ (f+1), and 'he'Ut over a loW flame until solution is complete. Dilute to 75 fnL with water and bring to boiling-to expel the bromine. Cbol somewhat,' but not enough for the PbGi to separate,-and then -cautiously add, by means of a pipet; Na2C03 solhtton' until'decidedly alkaline.- Bring to boiling and transfer to a 250-mL vbluinetric flisk. Cool to room 'temperature, dilute to- the'mark, and niix. Filter through a dry paper, discarding the first 15 io 20 iriL of filtrate. Measure exactly 200t mL in a volumetric flask and transfer to a 600-mL beaker. The test solution will now. be equivalent to 0.5 g of the original specimen. . 20.3.2 Carefully add HC1 (sp gr 1.19) front.a pipet to the alkaline solution until the solution is neutral^ and add 0.4 mL excess for each-100 mL of solution.. Bring to boiling to expel the C02 and then add to the boiling solution, drop by drop, -20 to 25 mL of a BaCl2 solution. Allow to stand in a warm place for at least 2 h. Filter on a previously ignited and j weighed Gooch crucible or a fine-textured filter paper and 1 wash with hot water. Dry and ignite. Cool, and weigh as BaSQ4. 20.4 Calculations: Total sulfate as S03i % = 68.6 X P total sulfate as PbS04, % - 259.8 xP , where: P = BaSQ4-precipitate, g. 68.6 = SOs/BaS04 x 100/0.5 = 80.06/233.40 x 200 259.8 = PbS04/BaSO4 x 100/0.5 = 303.25/233.40 5 21. Zinc Oxide v21.1 Procedure--Determine zinc oxide in accordance 3 with Methods D 3280. 22. Basic Lead Oxide 22.1 Calculation--Calculate the percent of basic lead f oxide as follows: ;} Basic PbO, % = L~ S,(0.736) | where:.. .. : i~. L = total lead as PbO, % (Section 18), . Sui = total sulfate as PbS04, % (20.4), and 0.736 = Pb0/PbS04 = 233.19/303.25. ' ." j ! 23. .Total Impurities..... j , 23.1 Calculation--Calculate the percent of total impuri- 3 ties as follows:;. > ... I 1 - Total impurities, % =' 100 - (L + Su;, + Z) t where: ' '.-4''-4 L = total lead as PbO, % (Section 18), 1 j iSti2 total sulfate as S03, % (20.4), and ' { Z ; =''zihc oxide, % (Section 21). I 24. Coarse Particles `1 , 24.1 Procedure--rDeterjmine coarse partiples in accord- J aijce with Test Methods D 185. J " > 25. Precision . r \-- ;- - I 25. Id Data-are nOLavailable- to determine the precision of I these test methods..There are no plans at present to obtain i such data. The test methods have been in use for many years | and are considered acceptable. | 26. Keywords .. * 26.1 ammonium , acetate soluble, pigment; basic car- | bonate, white lead; basic lead oxide, pigment; basic sulfate j white lead; carbon dioxide, pigment; chemical analysis,'white lead pigment; lead carbonate pigment The American Society for Testing end Materials takes noposition 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 arty time by the responsible technical committee and must.be reviewed every five years and ffnot ravised, eitherreapproved or withdrawn. Yourcomments are Invited eithertor 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 fee) 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 19103. DUP050296739 Designation: D 1306 - 88 Standard Test Method for Phthaiic Anhydride Content of Alkyd Resins and Esters Containing Other Dibasic Acids (Gravimetric)1 This standard is issued Under the fixed designation D 1306; 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 reappjpval.. So P" ..This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 7022 ofFederal Test Method Standard No. J41 ConsuU'ilie DqD Index ofSpecifications and Standardsforthe specific year ofissue which has been adopiedby the Department ofDefense. ' '1 ' : " ' : $f& Scope,.', ' ' , , .. * 1.1,1 Thisjlest method covers the gravimetric ^termination. "Siphthalic anhydride in alkyd resins and qtq-s.that contain "jibasic acids such as maleic, .ftnparie, adipic, and sebacic, ^hick woidd interfere if Test Nlethod D 563 wijs used, 1-.2 This standard may involve hazardous materials, oper- i, tdons, and equipment.. This standard dops not purport to it'address all, ofthe safety prqblemsdss'ociated.yvith itspse. It is r- fa. 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 563 Test Method for Phthaiic Anhydride Content: of Alkyd Resins and Resin Solutions12 D1193 Specification for Reagent Water3 ; 3. Summary of Test Method 3.1 The specimen is saponified with alcoholic potassium hydroxide and benzene to precipitate quantitatively the : potassium salt of phthaiic acid as C6H4 (COOH)2 C2H5OH. Interfering substances are eliminated by dissolving the pre cipitate in water, adjusting the pH ofthe solution to 2.5 with nitric acid, and filtering. Phthaiic acid is then precipitated as if- nonstoichiometric lead phthalate and calculated to phthaiic anhydride, using a factor obtained when compositions of known purity'were analyzed similarly,, t 4. Significance and Use . 5.3 Guard Tube, filled with soda lime. 5.4 Fritted-Glass Filter .Crucible, medium porosity, of 30-ruL capacity. , 5.5 Filter Flasks, suction-type. 5.6 Crucible Holder. 5.7 Oven, of gravity convection type. 5.8 Desiccator, containing concentrated H2S04 (sp. gr U84) as the desiccant. .; 5.9 Flash Filtrator. 5AQ pH Test Assembly. 5.11 Volumetric Flask, 100-mL. ?;, 5.12 Erlenmeyer Flask, 250-mL, wide-mouth, with glass stopper not smaller than a No. 27. ,< 5.13 Delivery Pipet, 2-mL. 6. Reagents J / 6.1 Purity ofReagent--Reagent grade chemicals shall be used in all tests. Unless Otherwise indicated, it is intended that all reagents shall bcdfiuin 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 as defined by Type II of Specification D 1,19fT ' 6.3 Acetfc AddrGlacial. - ; .- 6.4 Alcohol-Benzene Wash Solution--Mix i volume of .absolute ethyl alcohol (Note i).with 3 volumes of benzene. 4.1 The phthaiic anhydride cgntent of alkyd fesins con trols the properties of the final film. 1--The alcohol may be denatured Formula 2-B, but must be anhydrous. 5. Apparatus ' 6.5 Benzene (anhydrous). ; 5.1 Flask and Condenser--A 500-mL Erlenmeyer flask fitted with an air-cooled glass reflux condenser 30 in. (760 ' 6.6 Ether (athydrqus). 6.7 Lead Acetate Solution--Dissolve 25 g of lead acetate mm) in length. The connection between the flask and trihydrate in glacial acetic add and dilute to 100-mL volume condenser shall be a standard-taper 24/40 ground-glassjoint. 5.2 Water Bath. with acetic acid. 6.8 Methanol (anhydrous). 6.9 Nitric Acid (1+3)--Mix 1 volume of concentrated nitric add (HN03) (sp gr 1.42) with 3 volumes of water. 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 DO 1.33 on Varnish and Resins, Including Shellac. Current edition approved May 27, 1988. Published October 1988. Originally published as D 1306 -54 T. Last previous edition D 1306 - 80. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book of ASTM Standards, Vols 06.03 and 11.01. 4 "Reagent Chemicals, American Chemical Society Specifications,'' Ant. Chcm. 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." 219 DUP050296740 # D 1306 6.10 Potassium Hydroxide Alcoholic, Solution (66 g/ L)--Dissolve 66 g of potassium hydroxide (KOH) in 1 L of absolute ethyl alcohol (Note 1). Allow the solution to stand overnight protected against carbon dioxide (C02) absorption. Filter just before use. 7. Procedure 7.1 Weigh by difference, from a closed container into the 500-mL Erlenmeyer flask, a sample of resin or resin solution sufficient to yield from 0.8 to 1.2 g of potassium alcohol phthalate. Add 150 mL of benzene, warming slightly on the steam bath if necessary, to effect solution. Add 60 mL of alcoholic KOH solution, and attach the condenser. Place the flask in a water bath to a depth approximately equal to that of the contents of the flask. Warm the bath, maintaining a temperature of 40C for 1 h, then gradually raise the temperature until the alcoholic solution boils gently. Reflux for 11/2 h. 7.2 Remove the flask from the bath and wash down the inside of the condenser with a few millilitres of alcoholbenzene wash solution. Remove the condenser, cap the flask with the soda-lime guard tube, and cool by means ofrunning water or an ice bath. 7.3 When cool, filter immediately and as rapidly as possible, through a fritted-glass crucible that previously has been tared, using the alcohol-benzene wash solution for transferring the precipitate and washing the reaction flask. Wash the precipitate with successive portions of alcoholbenzene wash solution until a few millilitres of washings collected in a second suction flask are no longer alkaline to phenolphthatein. (Normally about 75 mL of wash solution are sufficient.) Do not allow air to be drawn through the crystals as they are hygroscopic. Finally, pour 25 mL of ether into the crucible and draw through the precipitate with the aid of suction. 7.4 Wipe the outer surface of the crucible with a clean cloth and place in a gravity convection oven at 60C for 1 h. Cool to room temperature in a desiccator, and weigh. 2--The crucible weighings are for determining aliquot size and need be weighed to the nearest 10 mg only. 7.5 Dissolve the contents of the crucible in 70 mL of water, using a filtrator so as to collect the washings in a 250-mL beaker. Adjust the pH of the specimen to 2.5, using HN03( 1+3) and a pH test assembly. After the specimen has stood 30 min or longer, filter through double thicknesses of the finest paper directly into a 100-mL volumetric flask (Note 3). Dilute to volume with water, simultaneously using the water to wash the beaker and filter paper; mix thoroughly. 3--If the solution does not cloud when acidified, it may be diluted to volume at once and the filtering omitted. j j 1 1 1 1 I j ! 7.6 Withdraw an aliquot containing not less than 60 nor more than 90 mg of the dissolved salts. Transfer this aliquot into the 250-mL Erlenmeyer flask. Dry the contents of the flask in the oven at 60C. Add 5 mL of glacial acetic acid, vent the stopper by inserting a paper strip under one side, and heat in the oven at 60C for 1 h. Add 100 mL of anhydrous methanol and continue heating in the oven with occasional agitation until the material is completely dis- solved. To the hot solution, add slowly, by pipet, 2.0 mL of lead acetate solution. Agitate the solution during the addition of this reagent. Return the flask to the 60C oven for 1 h. Remove and stopper tightly after 30 min. Allow to stand 12 h or longer. Filter the solution through a dry tared fritted- glass crucible of medium porosity, to which additional mats of coarse and fine asbestos have been added. Agitate the solution just before filtering. Wash the flask thoroughly, using anhydrousmethanol. Examine the filtrate carefully before discarding and, if cloudy, filter again through the same crucible. Dry the crucible for 1 h at lOS'C, cool iii a desiccator, and weigh. - . jS !j I 1 f 1 jj I j | 1 j ;| f j | 8. Calculation -- 8.1 Calculate the percent of phthalic anhydride A in the specimen as follows: " A =[(P x 0,323)/SJ x 100 | | j | where: P -- lead precipitate, g, and S = specimen represented in the aliquot used, g. ' | 9. Precision _ 9.1 Two results obtained by operators should be consid ered suspect IFfiey differ by more than 1 % absolute. j 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 arty 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, eitherreapproved or withdrawn. Your comments are Invitedeither (or revision of tfiis standard orlor additional standards and should be addressed to ASTM Headquarters. Your comments mil 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, 1$is Race St., Philadelphia, PA 19103. DUP050296741 I Designation: D 1312 - 56 {Reapproved 1987),61 Standard Test Methods for Apparent Free Phenols in Synthetic Phenolic Resins or Solutions Used for Coating Purposes1 This standard is issued under the fixed designation D 1312; 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 revision or reapproval. Editorial changes were made throughout, includingrenumbering Sections 4 through 18 in November 1987. |Scope These test'methods cover die determination of the (bunt of apparent free phenol in synthetic phenolic resins solutions used for coating purposes. The test method for ation of the free phenolapplies to all the commonly used ghs except those containirig p-phenyl-pheiiol. Test Method Implies to the simpler phenols up to and including the enols; Test Method B applies to the common alkylated enols. |l.2 This standard may involve hazardous materials, operjjrohs, and equipment. This standard does not purport to ddress all ofthe safety problems associated with its use. It is ? responsibility of the user of this standard to establish safety and health practices arid determine the '^applicability of regulatory limitations prior to use. Specific ' forwards are given in Sections 11 and 15. t. ' ! M Referenced Document , it #?* 2.1 ASTM Standard: D1193 Specification for Reagent Water12 i Purity of Reagents 3.1 Reagent grade chemicals shall be used in all tests, ipnless otherwise indicated, it is intended that all reagents pfiall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, Jwhere such specifications are available.3 Other grades may be fused, provided' it is first ascertained that the reagent is of ^sufficiently high purity to permit its use without lessening the Jaccuracy of the determination. |, 3.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type III | of Specification D 1193. 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 D01.33 on Varnish and Resins, Including Shellacs. . Current edition approved Sept, 10,19561 Published November 1956. Originally oublished as D 1312 - 54. Last previous edition D 1312 - 54 T. 2 Annual Book ofASTM Standards, Vols 06.03 and i 1.01. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chetn. 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." ISOLATION OF FREE PHENOLS 4. Apparatus 4.1 Steam Generator. 4.2 Distillation Flask- -A 500-mL Kjeldahl flask. 4.3 Condenser. 5. Reagents 5.1 Sodium Hydroxide Solution (100 g NaOH/Lh-Dis solve 100 g of NaOH [Caution] in water and dilute to 1 L. 6. Procedure 6.1 Transfer 1 to 2 g of the sample, weighed to the nearest 0.01 g, to a 500-mL Kjeldahl flask. Add 50 mL ,,of water. Lead steam from a steam generator through a T-trap and then through a tube extending to the bottom of the flask. Take; off the distillate through a second bent tube that extends just through the stopper of the flask and is attached to the top of an inclined long condenser. Using a 1000-mL volumetric flask as a receiver, collect 900 mL ofthe distillate. A small flame may be applied to the bottom- of the Kjeldahl flask during distillation to maintain the volume of water constant. If the distillate is clear, dilute to 1000 mL; if not, add several millilitres of NaOH solution to dissolve the insoluble phenols. Determine the apparent free phenol in accordance with Method A or B, as required.'' 1--p-Phenylphenol is not completely isolated by this proce dure. TEST METHOD A--SIMPLER PHENOLS 7. Summary of Test Method 7.1 Free phenols are isolated by steam distillation, reacted with a measured excess of bromine, and the excess backtitrated with standard sodium thiosulfate solution. 8. Apparatus 8.1 Iodine Flasks, 500-mL, glass-stoppered. 9. Reagents 9.1 Bromide-Bromate Solution--Dissolve 2.784 g of KB1O3 [Caution] and 10 g of KBr [Caution] in 1 L of water. 9.2 Potassium Iodide Solution (100 g KI/L)--Dissolve 100 g of Ki.[Caution] in water and dilute to 1 L. 9.3 Sodium Thiosulfate, Standard Solution (0.1 N)--Dissolve 25 g of Na2S203 5H20 [Caution] in 1 L of water. Standardize against iodine. DUP050296742 # D 1312 9.4 Starch Indicator Solution--Dissolve 1 g of soluble starch in 100 mL of boiling water and cool. 10. Procedure 10.1 Pipet a 25-mL (or larger) aliquot of the distillate into a 500-mL iodine flask. Add 25 mL of KBr - KBr03 solution, shake, and add 10 mL of HC1 (sp gr 1.19). Stopper quickly, shake to mix thoroughly, and fill the gutter with water. Let stand 15 min. (If the bromine color disappears during the shaking, take a fresh aliquot, add double the amount of bromate solution, and proceed as described.) Raise the stopper carefully and add 10 mL of the KI solution. Shake, and wash down the stopper and walls of the flask. Titrate with 0.1 ANa2S203, solution using 1 mL of starch indicator at the end. 10.2 Blank--Run a blank in exactly the same manner, except to omit the test material. 11. Calculation 11.1 Calculate the percentage of apparent free phenols (Note 2), as follows: Phenols, % = [(7) - T)Nx 1.567}/W where: T, = Na2S203 solution required for titration of the blank, mL, T = Na2S203 solution required for titration of the sample, mL, N = normality of the Na2S203 solution, and W -- sample represented in'the aliquot used, g. 2--The cresols (CH3C6H4OH) and xylenols (CH3)2C6H3OH have one or two reactive positions on the ring, depending on the isomer, but their tendency to add more bromine as an addition product that is not later removed by KI renders the exact extent of reaction uncertain. Since those materials are ordinarily used as mixtures in a resin-forming reaction, it is convenient and sufficiently informative to express the amount found as primary phenol. 12. Precision 12.1 The individual test results should not differ from the mean by more than 0.5 %. . TEST METHOD B--COMMON ALKYLATED PHENOLS 13. Summary of Test Method 13.1 Free phenols are isolated by steam distillation, re acted with a measured excess of iodine, and the excess back-titrated with standard sodium thiosulfate solution. 14. Apparatus 14.1 Iodine Flasks, 500-mL, glass stoppered. 15. Reagents 15.1 Iodine Solution--Dissolve 4.2 g of iodine [Caution)!? in 15 g of a saturated aqueous KI solution and dilute to 1 L,s 15.2 Sodium Bicarbonate Solution (84 g NaHC03/L) Dissolve 84 g of NaHC03 in water and dilute to 1 L. 15.3 Sodium Hydroxide Solution (100 g NaOH/L)-- Dissolve 100 g of NaOH [Caution] in water and dilute to 1L, 15.4 Sodium Thiosulfate, Standard Solution (0. i N)--See 7.3. 15.5 Starch Indicator Solution--See 7.4. 15.6 Sulfuric Acid (1+19)--Add slowly, while stirring, l volume of concentrated H2S04 [Caution] (sp gr 1.84) to 19 volumes of water. 16. Procedure 16.1 Add 15 mL of NaOH solution to the steam distillate and dilute to 1 L. Add 100 mL of water to a 500-mL iodine flask. Pipet a 10-mL (or larger) aliquot of distillate into the flask (Note 3) and add 30 mL ofthe iodine solution. Stopper and shake continuously for 5 min. Add 50 mL of H2S04 (1+19) to the flask and titrate with 0.1 N Na2S203 solution to a colorless end point, using 1 mL of starch solution as the indicator. 3--If the sample is pure p-phenylphenol, add 50 mL of the NaHC03 solution to the flask before the sample is added to prevent the formation of color that interferes with the titration end point. 16.2 Blank--Run a blank in exactly the same manner, except omit the sample. 17. Calculation if 17.1 Calculate the percentage of apparent free alkylphenols (Note 4) as follows: Phenols, % = [(B - V)N x F]/S where: B = Na2S203 solution required for titration of thejblank, mL, V = Na2S203 solution required for titration of the sample, mL, N -- normality of the Na2S203 solution, . F - conversion factor = 3.755'for p-tertiary-butyl phenol = 4.106 for p-tertiary-amyl phenol ^. = 4.255 for p-phenyl phenol, and S = sample represented in the aliquot used, g; 4--The alkyl phenols form normal di-iodo compounds. 18. Precision 18.1 The individual test results should not differ from the mean by more than 0.5 %. 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 ifnot revised, either reapproved 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 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. 222 HR -4BH5 T'V. "'V31 DUP050296743 Designation: D 1343 - 86 (Fteapprdtfici 1&01)161 Standard Test Method for Viscosity of Cellulose Derivatives by Bail-Drop Method1 This standard is issued under the fixed designation D 1343; 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. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4272-1 ofFederal Test Method Standard No. 14U. Consult the DoDIndex ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 11 Keywords were added editorially in March 1991. iScope 1.1 This test method describes the apparatus and'general jrpcedure'for making ball-drop viscosity measurements on Blutions of various cellulose derivatives. Instructions for sample preparation, solution concentration, and other details jJJjare discussed in the ASTM methods for the respective t%celluiose derivatives. K 1.2 This test method is applicable to solutions of various Icellulose derivatives having viscosities greater than 10 P, by raising balls of various diameters and densities. Viscosity Ifesults are expressed preferably in poises. 1.3 In commercial practice, viscosities are often expressed i, m seconds using %2-in. (2.38-mm) stainless steel balls.? f.When the viscosity is outside the practical range for these balls (75 to 300 P), the measurement can be made using a j,calibrated pipet viscometer or a different ball and calculating If flie observed viscosity to the corresponding time for a 13/3121-in*, ball, even though it is a small fraction of a second, j 1.4 This standard does not purport to address, all of the J safety problems, if any, associated with its use. It is the | responsibility of the user ofthis standard to establish approj priate safety and health practices and determine the applica nt bility ofregulatory, limitations prior to use. 2. Referenced Documents 12.1 ASTM Standards: D301 Test Methods for Soluble Cellulose Nitrate3 D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)4 D817 Test Methods of Testing Cellulose Acetate #:i Propionate and Cellulose Acetate Butyrate3 If D 871 Test Methods of Testing Cellulose Acetate3 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 D01.36 on Cellulose and Cellulose Derivatives. Current edition approved July 25* 1986. Published September 1986. Originally published as D 1343 - 54. Last previous edition D 1343 - 69 (85). 3 When a Vn-in. stainless seed ball is used, the viscosities in seconds should be practically the same as those obtained using the apparatus described in Section 11 of Methods D 371 - 48. and in Section 10 of Specifications D 301 - 50, which last appeared in the J9S2 Annual Book ofASTM Standards, Part 4. 3 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vol 05.01. 3. Summary of Test Method . 3.1 A solution of the cellulose derivative is made in a suitable solvent and allowed to equilibrate at a chosen temperature. A stainless steel or aluminum ball is dropped into the solution, and the time, required for it to cover a measured distance in its fall is recorded. The viscosity ofthe solution can then be calculated in poise or recorded in seconds. 4. Significance and Use 4.1 This test provides an easy method of determining the viscosity of cellulose derivatives in a given solvent. The answers are in units commonly used in industrial practice. Such information is needed for cellulose derivatives that are to be extruded, molded, sprayed, or brushed as is or in solution. 5. Apparatus 5.1 Constant-Temperature Water Bath, glass-walled. 5.2 Bottles and Caps: 5.2.1 Bottles, round or square, conforming to the dimen sional requirements shown in Table 1, shall be used. Screw caps of metal or phenolic plastic in sizes to fit the bottles aid having aluminum foil or cardboard and cellophane liners may be used to close the bottles. Alternatively, rubber, stoppers coveredwith aluminum or tin foil, may alsb be used as closures. In this latter case, solvent loss during measure ment ofviscosity can be minimized by removing the stopper,' leaving the foil in place, and making a small hole in the center of the foil through which the tells may be dropped. 5.2.2 Timing marks shall be provided around each bottle or on the front and back of the glass-walled constanttemperature water bath, to avoid parallax errors. The lower timing mark shall be approximately 1.25 in. (32 mm) above the base of the bottle, and the upper mark shall be 2.00 0.02 in. (50.8 0.5 mm) above the lower mark. A practical means of marking consists of wrapping a 2-in. strip of transparent sheeting around the water bath at the proper location. The edges of the sheeting may be darkened with crayon. A light located back of the water bath aids in observing the ball during its fall. 5.3 Balls--Unless specifically directed otherwise, balls of varying size and density shall be used, depending on the viscosity of the solution. Table 2 gives the useful ranges, approximate apparatus constants, and dimensions of several DUP050296744 # D 1343 1I Sfo/qfssi Steot i 965, o* zest k Is Stoinles ' Stett i QIKK'C 560tc* zest - '//ff-ii i SfeeJ t 236, a* test he-In Alumina m ,1 BalliK* 0.25$, 0*2.3.V ' * 1 1' - 7 08 0.9 1.1 1.2 Solution Donsity* , p*r cu cm FIG. 1 Factors for Converting Viscosities in Seconds to Poises t( = Fxt TABLE 1 Bottles'* Bottle Round Square Capacity, oz Weight, 02 Height, in. Inside diameter, cm Side to side, cm Corner to corner, cm 16 12 6.7 6.4 . ... 16 12 ' 7 6.0 7.2 A Approximate sizes. Bottles satisfactory for this purpose may be obtained from the Owens Illinois Glass Co., Ohio Illinois Bldg., Toledo, Ohio, 43601, as follows: round bottle No. Q-3145 with cap 63-400, French square bottle A-6732 with cap 48-400. such, balls, the exact diameter, weight, and density shall be determined accurately.for each lot of balls used. 5.4 Graduate--A 50 or 100-ml graduated cylinder, having a round top opening that can be tightly stoppered, shall be used for determining the density of the solution in grams per millilitre. 5.5 Stop Watch--A stop watch reading to 0.2 s.6 6.Calibration 6.1 Calculate the apparatus constant, K, using the follow ing equation and exact dimensions of the bottle and balls used: K = 2gr2H - 2.(04[d/D) + 2.09(d/D)3]/9L where: g = acceleration of gravity in cgs units r = ball radius, cm, d = ball diameter, cm, D = bottle diameter, cm (in the case of square bottles the average of the side to side and comer to comer diameters shall be used), and L = distance of ball drop, cm. 7. Procedure 7.1 Preparation ofSolution--Dry the sample and prepare a solution as specified for the particular material. Such instructions are given in the viscosity sections of Methods E) 301, D 871, and Methods D 817. Weigh into the bottle an appropriate amount of dry sample and specified solvent, accurate to 0.1 g, to make about 350 ml of solution. Close the bottle tightly. Allow to stand a short time for the solvent to penetrate the sample. Then tumble or shake until a uniform solution is obtained. Transfer to the water bath at 25 0.1 C, and allow the solution to coine to temperature, 7.2 Viscosity Determination--Drop a %2-in. (2.38-mm) stainless steel ball through the center of the column of solu tion and time its fall through the marked 2-in. (50.8-mm) distance, using a stop watch and taking precautions to avoid parallax errors. If the observed time is less than \20 s or greater than 100 s repeat the measurement^ unless directed otherwise, using a different ball (see Table.2) which has U time of fall within these limits. If the solution is known to be thixotropic in nature or ifthe times of falLfor successive-balls vary significantly,' use freshly prepared solutions for dupli cate measurements or measurements with balls of other sizes. 7.3 Determination of Lower Viscosities---Ifthe viscosity of the solution is too low to measure satisfactorily using One of the balls, use a calibrated pipet as described in Test Method D445, or other instrument of suitable range. Calculate the result in poises. Convert poises to equivalent ball-drop seconds as shown in 8.2. . 7.4 Density-Determination--Determine the density ofthe solution in grams per cubic centimetre by measuring the volume at 25 0,1 C of a known weight *of the solution contained in a suitable tightly stoppered graduated cylinder. 8. Calculation 8.1 Ball-Drop Viscosities--Calculate the viscosity in poises as follows: = K(a - b)t Ball Vto-in. (1.59-mm) (aluminum) Via-in. (1.59-mm) (stainless steel) sfoa-in. (2.36-mm) Ve-in. (3.18-mm) %2-in. (5.56-mm) TABLE 2 Balls Viscosity Range. P 10 to 50 35 to 150 76 to 300 125 to 600 350 to 1800 Apparatus Constant. K 0.256 0.256 0.560 0.965 2.70 Typical Data Diameter, cm Weight, g 0.1588 0.00691 0.1588 0.2380 0.3170 0.5656 0.01605 0.0542 0.1277 0.6897 Density, g/cm3, a 2.82 7.86 7.68 7.68 7.68 DUP050296745 # D 1343 -re: viscosity at the specified temperature, P, i apparatus constant,5 bali density5, in g/cm3, >solution density, g/cm3, and ' time of tall, s. jthe case of a ball of stated diameter and density, this ' ulation can be simplified to:5 Fxt, ere: L K(a -b). factor varies with solution density, b. Approximate ois for the various balls can be read from Fig. 1. Exact ors can be calculated from the exact measurements ofthe cometer and balls. 2 Poises to Seconds--Poises may be converted to equivnt ball-drop seconds, t, as follows: J(for V32-'m. ball) = v/K(a -b) ere: ... = observed viscosity, P, -- apparatus constant for the %2 in. stainless steel ball, = ball density for the 3/32-in. stainless steel ball, and 5 See Table 2 for approximate values. b = solution density for the solution being tested. 9. Report 9.1 Results shall be reported in poises,or in seconds, for a V32-in. stainless steel ball. 10. Precision and Bias 10.1 The within-laboratory precision of the test was determined by submitting 25 pairs of replicate samples to be run by any one of several operators. Each sample in a specific pair was submitted within 3 to 5 days. Each pair consisted of one sample at the 20-second viscosity level and one at the 60-second viscosity level. The data below shows the 95 % confidence limits (two sigma) for the two levels. Viscosity Level 95 % Confidence Limits 60 sec 20 sec 3.83 sec . 1.00 sec Data are not available at this time to show interlaboratory precision. 10.2 Since there is no accepted reference material suitable for determining the bias for the procedure in this test method for measuring ball-drop viscosity, no statement on bias can be made. 11. Keywords 11.1 ball drop; cellulose esters; viscosity 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 ofsuch.rights, are entirely their cmn responsibility. This standard Is subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years arid ifnot revised, eitherreapprovador withdrawn. Your comments are Invited either for revision ofthis standard or foradditional 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 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. DUP050296746 Designation: D 1347 - 72 (Reapproved 1989)2 Standard Test Methods for Methytcellulose1 : This standard is issued under the fixed designation D 1347; the numberjmriiedftitely following the designation indicates the year of original adoption or, iit the base.'ofrevision, the year oflast revision. A number in parentheses indicates the year oflast reapproyal. A superscript epsilon (e) indicates' aD editorial change'since the last revision or reapproval. --KejnvordJ were added editorially-in April 1991'. 1. Scope ;- . .' 1.1 These test methods cover the testing of methylcellulose. 1.2 The test methods appear in the following order: Sections Moisture............. ...................... .................................. . 4 and 5 Ash--as Sulfate...................................................................... 6trf8 '' Chlorides--as Sodium Chloride............. ....... .. 9 to 11; Alkalinity--^as,Na2tp03 ................. ; 12,tq l4 Iron..,............ .......................................... ......................... 15 to 19 j Heavy Metals...... ......... ... ......... ........... ............................20to22 Methoxyl Content.................................................................. 23-to 26 Viscosity: Water-Soluble Methylcellulose.......................................... 27 to 29. Alkali-Soluble Methylcellulose.................................... ,... 30 to 31 pH.............................................;................................... '.. 32 Solids................. ........................... .................... ................. 33 to 34 Density................... .-........... ........................ ...................... r3S to 39 - ... 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 ike-applicability of regulatory limitations prior to use. For ^"specific hazard statement, see Note 1. 2. Referenced Document 2.1 ASTM Standard: D 96 Test Methods for Water and Sediment in Crude Oil by Centrifuge Method (Field Procedure)12 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.3 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. . 3.3 Unless .otherwise indeed, references to, water .sij^fl be understood tp tpean distjlle^ water.. ' ", MOISTURE : i: " 4, Procedure t 4.1 Transfer 2 to 5 g ofthe sample, weighed to the nearest 0.01 g, to a tared dish (fitted with a lid) and dry it for 3 h in an oven at 105 3"C. Remove the,dish from the oven, cover it with a lid, coal in a desiccator, and weigh. 5. Calculafioh' ' 5.1 Calculate the percent moisture, M, as follows: M=(A/B)x 100 .where: . A mass,loss .on heating, g, andB = sample used, g,, 1 - (i) .... . ... .. ASH--AS SULFATE 6. Reagent >< 6.1 Sulfuric 'Acid'<sp gr ,1.84)-r-Coricentrated sulfuric acid (II2S04).' 7. Procedure 7.1 Weigh, to the nearest 0.01 g, about 2 g of the sample (previously dried for lh h at 105C) and transfer it to a tared platinum crucible. Place it in a muffle-furnace at 575 25C for approximately % h, to char the organic material. 7.2 Cool the crucible and add 1 mL of H2S04 so that it completely wets the charred residue. Then cautiously heat it over a small flame to dense white fumes. Place the crucible in a muffle furnace at 575 25C and leave it there until all signs of carbon are gone (approximately 1 h). Transfer the specimen to a desiccator until cool, then weigh. 8. Calculation 8.1 Calculate the percent of ash, C, as follows: C = {A/B) x 100 (2) 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 D01.36 on Celluiosics. Current edition approved Feb. 9, 1972. Published March 1972. Originally published as D 1347 - 54 T. Last previous edition D 1347 - 64. 2 Annual Book ofASTM Standards. Vol 05.01. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soe., 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 Noslrand Co., Inc., New York, NY, and the "United States Pharmacopeia." where: A = ash, g, and B = sample used, g. CHLORIDES--AS SODIUM CHLORIDE 9. Reagents 9.1 Ferric Alum Indicator Solution--Add 100 g of ferric aluminum sulfate (Fe2SO4)3-(NH4)2SO4-24H20) to 250 mL DUP050296747 1347 vater, Heat it to boiling and add HN03 (sp gr 1.42) slowly 1 the red color is removed. This will usually require about ;15 mL of HN03. Filter the solution and store it in a glass Me. 9.2 Potassium Thiocyanate,. Solution, Standard (0.1 N)-- psolve 10 g of potassium thioagonate (KCNS) in 1 L of iter. By means of a pipet, measure 25 mL of 0.1000 N SN03 solution into a 400-mL beaker. Add 100' mL of per, 10 mL of nitric acid (NH03, sp gr 1.42) and,.5 mL of .... lie alum indicator solution. Titrate with the KCNS jution, while stirring, until a faint persistent red color is J bduced. Calculate the normality ofthe KCNS solution, N, I follows: ,. . 13.2 Add 4 drops .of methyl purple indicator to the flask solution and titrate to a blue-gray end point with 0.01 N 14. Calculation 14.1 Calculate the percent of alkalinity, D, as anhydrous sodium carbonate (Na2C03) as follows: b = ((AB * QXSSSifC] X 100 . (5) where: -.3 . 4- = H2SO^required for.titration pf the sample, mL, B , = nonnality of the H2S04, and C = sample used, g.. . , , A" = (A/S) x 0.1 : , (3) IRON here: V|i = 0.100 N AgN03 solution added, mL, and jp = KCNS solution required for the tittation, mL. B Silver Nitrate, Solution, Standard (0.1 N)--Grind ' 'silver nitrate (AgNOj) crystals fine enough to pass through a ^50-p.m (No. 20) sieve,, and then dry for 2 h at 110C. gjflepare a 0.1000 N solution by dissolving 16.989 g of dry )3 in chloride-free water and diluting it to 1 L in a Volumetric flask. ||0. Procedure 10,1 Weigh, to . the nearest 0.01 g, about 1.0 g of the fjample (previously dried for Vi h at 100 to 105C) and Itransfer to a 500-mL wide-mouth Erlenmeyer flask, Add 250 pnL of hot water to the flask and swirl it for a few minutes, then cool to dissolve. - , .. 10.2 Add 5 mL of0.1000 N AgN03 solution and 5 mL of |ferric,alum,inchcator solution,;and tbep.back-jitrate with. (XJl Jj sgk 6KS- solution to the Jirst appearance of a faint pink color. _ , . .... . \ .., ; 11. Calculation i 11.1 Calculate the percent of chlorides, C, as sodium chloride (NaCl) as follows: f C = (HAS - CX>) X 0.0585J/C) x 100 (4) ivyheife; . _ : : " `. |M-= AgN03 solution added, mL, , ` . I B = ndniiality tip thd'AgN03 solurion, , C = KCNS. solution required to back-titrate the excess Aghto3, mt, D = normality of the KCNS solution, and E = sample used, g. ALKALINITY--AS SODIUM CARBONATE, ANHYDROUS 15. Apparatus 15.1 Photometer--Any photoelectric filter photometer or spectrophotometer suitable for measurements at 430' nm. 15.2 Kjeldahl Flasks, calibrated to contain 30 mL, and made of heat- and chemical-resistant glass. 16. Reagents 16.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OHJ, 16.2 Buffer Solution--Dissolve 20 g of sodium bicar bonate (NaHC03) and 10 g of sodium carbonate (Na2C03) in water and dilute to 1 L. 16i3 bisodium-1,2->ihydroxybenzene-3,5-Disulfonate Solution4--Prepare an aqueous solution containing 25 g/L. 16.4 Hydrogen Peroxide (30 %)--Concentrated hydrogen peroxide (H202). 16.5 Iron, Solution, Standard (0.0001 g Fe/mL)--Dis solve 0:01 g of iron powder containing riot less than 99:9 % Fe in Hydrochloric acid (HC1, sp gr 1.19). Oxidize the solution with bromine water and expel the excess by-boiling. Dilute to 1 L' in a vtiiumetric flask; __ 16.6 Phenolphthalein Indicator Solution,' 16.7 Sulfuric Acid (sp gr 1.84)--`Concentrated sulfuric_ acid(H2S04). ... 16.8 Sulfuric Acid (1 + 4)--Carefully-mix 1 volume of H2S04 (sj> gr 1..84) with 4 volumes of watfcfr adding the H2S04 gradually while mixing. 17; Preparation of Calibration Curve ' - 17.1. Following the procedure given in Section 1.8, and using varied ainounts of the standard iron solutfon prepared in accordance with 16.1, prepare a calibration curve showing iron content in parts per million and the corresponding photometer readings. ' i;L Reagents. 12.1 Methyl Purple Indicator Solution. 12.2 Sulfuric Acid, Standard (0.01IV)--Prepare and stan dardize a 0.01 N solution of sulfuric acid (H2S04). 13. Procedure 13.1 Weigh, to the nearest 04)1 g, .about hO g of the sample (previously dried for Vi h at5100 to 105C) and transfer it to a 500-mL wide-mouth Erlenmeyer flask. Add 250 mL of hot water to the flask and swirl it for a few minutes, then cool to dissolve. 18. Procedure 18.1 Weigh approximately 2 g of the satriple of methyl- cellulose to the nearest 0.01 g, arid transfer by means of a funnel to a Kjeldahl flask. Place'the flask at a 20 angle in a furnace at 600C, or on a microdigestion rack equipped with electric heating elements, and heat until some chairing ofthe methylcellulose has taken-place. (Care must be taken not to 4 A suitable prepared solution of this reagent, known as Tiron, is available from the La Motte Chemical Products Co., Chestertown, MD. I. t 227 DUP050296748 char too much.) Remove and allow to cool. 18.2 Add 3 mL of concentrated H2S04 to the flask. Place the flask on the digestion rack and digest Cool, and add H202 dropwise until the solution is clear. Heat over a Meker burner to a volume of 2 mL. Cool, and wash the sides of the flask with water. Add 3 drops of phenolphthalein indicator solution. Add NH4OH to a red end point. Wash the neck of the flask. The solution should be clear and not greater than 20 mL in volume. 18.3 Add 2 mL ofthe color-forming solution described in 16.3 and mix. Dilute to near the mark with buffer solution and mix thoroughly. Adjust the solution to a pH of 7 by adding NH4OH or H2S04 (1 + 4), and then dilute to the mark. Transfer a small portion to an absorption cell and determine the photometer reading at 430 nm. 19. Calculation 19.1 Read the iron content, in parts per million, directly from the calibration curve (Section 17). HEAVY METALS 20. Apparatus 20.1 Nessler Tubes, 50-mL. 20.2 Volumetric Flasks, 50-mL. 21. Reagents 21.1 Acetic Acid (6 + 94)--Mix 6 volumes ofglacial acetic' acid with 94 volumes of water. 21.2 Ammonium Hydroxide (1 + 5)--Mix 1 volume of concentrated ammonium hydroxide (NH4OH, sp gr 0.90) with 5 volumes of water. 21.3 Hydrochloric Acid (l + 3)--Mix 1 volume of con centrated hydrochloric add (HQ, sp gr 1.19) with 3 volumes of water. 21.4 Hydrogen Sulfide Solution (Saturated)--Saturate cold water with hydrogen sulfide (H2S). 21.5 Lead, Solution, Standard (1 mL = 0.1 mg Pb)-- Dissolve 0.1598 g of lead nitrate (Pb(N03)2) in 100 mL of water to which has been added 1 mL of concentrated nitric add (HN03, sp gr 1.42). Dilute to 1000 mL with water. 21.6 Lead, Solution, Standard (1 njL = 0.01 mg Pb)-- Dilute 10.0 mL of Pb(N03)2 solution (1 mL = 0.1 mg Pb) to 100 mL with water. This solution must be freshly prepared. When 0.1 mL of this standard lead solution is employed to prepare the standard to be compared with a solution of 1 g of the substance being tested, the comparison solution thus prepared contains the equivalent of one part of lead per million parts of the substance tested. 21.7 Phenolphthalein Indicator Solution. 22. Procedure 22.1 Add 5 mL of HC1 (1 + 3) to the residue in the platinum crucible that was used in the sulfate ash determina tion (Sections 6 and 7). Digest the residue by slowly boiling for a few minutes over a small flame. Transfer the contents of the crucible to a 50-mL volumetric flask, using about 25 mL ofwater to rinse the crudble. Neutralize with NH4OH (1 + 5) to a phenolphthalein end point and dilute to 50 mL. 22.2 Transfer a 25-mL aliquot of the solution to a 50-mL Nessler tube, and add 2 mL of acetic add (6 + 94) and 10 FIG. 1 Distillation Apparatus for MethoxytDeterminaHon mL ofa saturated solution of H2S.,Mix, allow to stand for 10 min, and compare with a standard lead solution to which H2S has been added. 22.3 Report the lead content in parts per million. METHOXYL CONTENT 23. Apparatus .__ 23.1 Distillation Apparatus (Fig. 1), consisting ofa boiling flask with a side arm for admission of carbon dioxide (C02) or nitrogen, an air condenser with a trap, and a receiver. 23.2 Oil Bath, equipped with a heating device, preferably electrical, so that the bath can be maintained at 145 to 150C. 24. Reagents and Materials 24.1 Bromine Solution--Dissolve 5 mL of bromine in 145 mL of the potassium acetate solution. Prepare the bromine solution fresh daily in a hood to remove bromine vapors. - 24.2 Carbon Dioxide--This may be obtained by the interaction ofmarble and HC1 (1 + 1) in a Kipp generator or, preferably, from a cylinder of the gas equipped with a suitable needle valve. The C02 shall be passed through a bubble counter and a dry trap, and then through a pressure regulator consisting of a glass tee whose vertical arm extends almost to the bottom of a 10-in. (254-mm) column of water. A screw clamp is attached to the thin-walled rubber tubing connecting the horizontal arm of the tee with the boiling DUP050296749 # B 1347 _ , This arrangement permits regulation of the flow of gas |allows any excess gas to escape. Nitrogen may be used in : of C02. 13 Formic Acid (HCOOH, 90 %). 4.4 Gelatin Capsules--Gelatin capsules of a suitable size jtold 50 to 60 mg of the dried specimen will be required. 4.5 Hydriodic Acid (57 %, sp gr 1.70)--Hydriodic acid Informs with water a constant-boiling mixture (boiling gpt 126 to 127C) which contains 57 % HI. The concention of HI in the reagent used should be not less than i %. The blank determination, which is affected primarily ffiree iodine in the reagent, should require not more than [mL of 0.1 N sodium thiosulfate (Na2S203) solution.5 If essary, the acid may be purified by adding to it a small iount of red phosphorus and boiling for 20 to 30 min in a |od, while passing a stream of C02 into the liquid, stillation shall then be carried out behind a safety glass fpeld in a hood, using an all-glass apparatus with a slow ream of C02 running through the receiver. --Warning--Under some conditions, the poisonous gas (iosphine (PH3) is formed during distillation and this may unite with polecular iodine to form phosphorus triiodide (PI3), which may explode t contact with air. it is, therefore, advisable to keep the current ofC02 going after the distillation is ended and until the apparatus has cooled; |his will prevent air from being sucked into the apparatus. Put the |purified HI in small, brown, glass-stoppered bottles, previously swept }>ut with C02 and seal the stoppers with molten paraffin. Store in a dark jpiace, To minimize decomposition of HI due to contact with air, run C02 into the bottle while withdrawing portions of the acid for use. 24.6 Potassium Acetate Solution--Dissolve 100 g of anhy- Jdrous potassium acetate crystals in I L of a solution Econtaining 900 mL of glacial acetic acid and 100 mL of acetic anhydride. 24.7 Potassium Iodide (KI). 24.8 Sodium Acetate Solution (220 g/L)--Dissolve 220 g of anhydrous sodium acetate in water and dilute to 1 L. 24.9 Sodium Thiosulfate Solution, Standard (0.1 N)-- rDissolve 25 g of sodium thiosulfate (Na2S203'5H2O) in 200 mL of water and dilute to 1 L. Use freshly boiled and cooled water. It is preferable to allow the solution to stand for a few days before standardization. Standardize the solution against 0.1000 N potassium dichromate (K2Cr207) solution pre pared by dissolving exactly 4.9037 g of K2Cr20T (National Institute of Standards and Technology Standard Sample No. 136) .in water and diluting tq_ 1 L in a volumetric flask. By means of a buret, measure accurately 35 to 45 mL of the K2Cr207 solution into a 250-mL Erlentneyer flask. Add 2 g of KI and 50' mL of H2S04 (1+9) and allow to stand for about 5 min. The flask should be stoppered during the standing period to avoid loss of iodine. Titrate the liberated iodine with the Na2S203 solution, using starch indicator solution near the end point. At the end point, the blue color of the starch indicator will be destroyed, leaving the pale ' f; green color of the chromate ion. The normality of the Na2S2Q3 solution should be checked at least once a week. $ 5 Hydriodic acid suitable for methoxyl determination may be prepared by the method of Samsel, E. P., and McHard, J. AM Industrial and Engineering Chemistry, Analytical Edition, Vol 14,1942, p. 750. Hydriodic acid available from Merck & Co., WBC 220, P.O. Box 2000, Rahway, NJ 07065 under the designation "For Methoxyl Determination1' has been found satisfactory for this purpose. Calculate the normality of the Na2S2Q3 solution, N, as follows; N={A/B)x0.l (6) where; A = 0.1000 N K2Cr207 solution added, mL, and B = Na2S203 solution required for the titration, mL. As an alternative procedure, the Na2S203 solution may be standardized against 0.1 N iodine solution that has been standardized in turn against arsenic trioxide (As^, Na tional Institute of Standards and Technology Standard Sample No. 83) or potassium iodate (KI03). 24.10 Starch Indicator Solution. 24.11 Sulfuric Acid (l + 9)--Carefully mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84) with 9 volumes of water, adding the H2S04 gradually while mixing. 25. Procedure 25.1 Dry the sample at 105DC for at least 30 min. Through the condenser, add to the trap in the distillation apparatus (Fig. 1) enough distilled water to make the trap about half full. Add 8 to 9 mL of bromine solution to the receiver. Weigh 50 to 60 mg of the dry sample, to the nearest 0.1 mg, into a gelatin capsule and drop it into the boiling flask. (The weighing should be done as rapidly as possible without sacrificing accuracy, since dry methylcellulose picks up moisture rapidly.) 25.2 Add a few small glass beads or chips ofclay plate and then 6 mL of HI. Attach the boiling flask at once to the condenser, using a few drops of HI to moisten the groundglass joint, and then connect the side arm ofthe flask to the .. source of C02. Pass a current of C02 into the apparatus at the rate of about 2 bubbles/s. Immerse the flask in the oil bath, maintained at 150C, and heat for 50 min. 25.3 Add 10 mL of sodium acetate solution to a 500-mL Erlenmeyer flask and wash into it the contents of the receiver; dilute to 125 mL with water. Add HCOOH dropwise,' with swirling, until the brown color of bromine is discharged, and then add about 6 drops more. A total of-J 2 to 15 drops is usually required. After about'3 min add 3 g of KI and 15 mL of H2S04 (1 + 9) and titrate immediately with 0.1 N Na2S2Of solution to a light straw color. Add a little starch solution and continue the titration to the disappear ance of the blue color. 25.4 Blank--Make a blank determination, using the same amounts of reagents and the same procedure as for the sample. (Usually, about 0.1 mL of0.1 ArNa2S203 solution is required.) 26. Calculation 26.1. Calculate the percent of methoxyl, M, as follows: M = [((ri - B)C x 0.00517)/>] x 100 ' (7) where: A = Na2S203 solution required for titration of the sample, mL, B -- Na2S2Q3 solution required for titration of the blank, mL, C = normality of the Na2S203 solution, and D = sample used, g. 229 DUP050296750 # t> 1347 ! k FIG. 2 Methylcellulose Viscometers } 9 o f 17 $i !" '#%&()0#))2)34# bottle containing the 2-g specimen of methylcellulose. 28.5 Agitate with a mechanical stirrer for 10 min, then 27. Apparatus place the bottle in an ice bath (0 to 5Q until solution is 27.1 Viscometer, Fig. 2(a) or (b). 5678 2--If a viscometer has been repaired, it should be recalibrated before it is used again. Even minor repairs can cause significant changes in the K value. 27.2 Mechanical Stirrer. complete. Equip the stirrer assembly with a one-hole stepper or bottle cap so that no water vapor is lost during agitation. For precision, it is preferable to deair the.solution by some means such as centrifuging. 28.6 When solution is complete; as evidenced 'by-the absence of partially swollen or undispersed particles, deter 28. Procedure mine the viscosity in a methylcellulose viscometer at 20 O.rc. Observe two precautions at this point: {!) the solution 28.1 Determine the moisture content of a portion of the shall be essentially free of air bubbles, and (2) the tempera sample. Since cellulose and its water-soluble derivatives are ture of the material in the tribe shall be checked to make hygroscopic, exposure of the sample to the atmosphere certain that it is actually at the bath temperature. should be kept to a minimum. Changes in moisture content 28.7 The methylcellulose viscosity tube (Fig. 2) consists of can introduce large errors into the accuracy of the determi three parts: (/) a large filling tube with a reservoir at its lower nation and this step should never be omitted ifprecise results extremity, A; (2) the orifice tube, 3; and (3) an air vent to the are desired. reservoir, C. When B is filled, close Cto prevent the sucking 28.2 Correcting for the moisture content, weigh out of air bubbles into the orifice tube. enough of the sample of undried methylcellulose to give 28.8 Before the specimen is allowed to flow through the 2.000 g of solids, calculated as follows: orifice for the viscosity determination, open the vent, C, so Weight of specimen, g = [100/(100 -- moisture content, %)] x 2 (8) 28.3 Place the sample in an 8-oz (250-cm3) wide-mouth bottle. This weighing step is critical in obtaining good checks and should be done on a good balance sensitive to 1 mg. Weights to the nearest 0.01 g will be sufficiently accurate. that the column of solution in B will flow into the reservoir against atmospheric pressure. Failure to open C before running will cause false values in the viscosity results. 29. Calculation 29.1 Calculate the viscosity as follows: j 28.4 Add 98.0 g of hot water (85 to 90"C) to the 8-oz V = Kdt (9) 230 wm -T7? DUP050296751 D 1347 ^jiere: S= viscosity, cP, |l= viscometer constant (Note 2), Ip density of the methylcellulose solution at 20/20"C (Note 3), and |== time for the solution to pass from the upper to the lower mark of the viscometer, s. \foTE 3--The viscometer constant is determined by passing a lard oil of known viscosity through the tube and determining the of flow. The above equation can then be solved for K. ( 4--For routine work, the density of solutions of methyllose may be assumed to be 1.00; 3SITY OF ALKALI-SOLUBLE METHYLCELLULOSE I. Reagents 10.1 Sodium Hydroxide Solution (40 g NaOH/L>--Disjjve 40 g of sodium hydroxide (NaOH) in carbon dioxide >2)-frep water and dilute, to 1 L. |r Procedure II.1 Proceed as directed ip Sections 2.8 and 29, except add f.O g ofthe NaOH solution to the sample, instead ofadding 3t water in accordance with 28.3. IP'' pH 2. Procedure |p: 32.1 Determine the pH of the viscosity solution from lection 28, using any suitable pH meter. SOLIDS 3. Apparatus 33.1 Oil Tubes, graduated, 100-mL, tapered, conforming the requirements prescribed in 3.2 and Fig. 1 of Test lethods D 96. 33-2 Centrifuge, capable of whirling filled centrifuge tubes H$jfa speed that will produce a centrifugal force of725 times avity. 34. Procedure 34.1 Add 1.50 g of bone-dry methylcellulose to 148.5 g of |90C water in a 2Vi by 6-in. (32 by 152-mm) bottle and jitate vigorously for about 15 min, or until the material has become finely divided. Place an ice bath around the bottle land agitate the mixture until the solution is effected. (This usually requires about 15 min.) 34.2 Place 100 mL ofthis 1 % solution in an oil tube, cool to 10C, and centrifuge at 725 times gravity for 5 min. The solution temperature shall be below 20C when finished. Read the volume percent of solids from the graduations on the tube. DENSITY 35. Scope 35.1 This test method covers the determination of the bulk density of methylcellulose. 36. Summary of Test Method 36.1 A weighed amount of methylcellulose is transferred to a 250-mL graduated cylinder and the graduate vibrated to settle the powder. 37. Apparatus 37.1 Vibrator--A magnetic-type electric vibrator attached to the vertical support rod of a ring stand approximately 1 ft (0.3 m) above the base. A condenser clamp of sufficient size to hold a 250-mL graduated cylinder also shall be attached to the above rod. The base of the stand should be weighted. 38. Procedure 38.1 Place 50.0 g of methylcellulose in a 250-mL gradu ated cylinder and place the cylinder in the condenser clamp. Turn on the Vibrator and allow the cylinder to vibrate for 3 min. Record the level (in millilitres) to which the specimen has compacted. 38.2 Alternatively, the specimen may be cqjnpacted man ually. Tap it on a hard surface by dropping the cylinder repeatedly from a height of about 1 in. (2$ min), until the volume of the specimen remains constant. In order to prevent cylinder breakage, cover the tapping surface with a Hi to `A-in. (3 to 6-mm) thick rubber sheet, or use a plastic graduated cylinder. -- 39. Calculation 39.1 Calculate the density, D, in grams per-millilitre as follows: - JT= 50/observed reading, mL (10) 40. Keywords 40.1 ball drop; cellulose esters; viscosity 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 ofthis standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement ol such rights, are entirely their own responsibility. This standerd is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapprovedor withdrawn. Your comments are invited either for revision ofthis 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. DUP050296752 Designation: D 1348 - 89 iI I Standard Test Methods for Moisture in Cellulose1 | This standard is issued under the fixed designation D 1348; 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 1. Scope - 1.1 These test methods cover the determination of mois ture in cellulose using two oven-drying procedures nd one Karl Fischer procedure. 1.2 The test procedures appear in the foEowing order:' Sections Test Method A--Specimen Weighed in Oven.................................... 4 to 10 Test Method B--Specimen Weighed Outside of Oven........................ 11 to 17 Test Method C--Karl Fischer Method............................................... 18 to 25 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 tfie 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 These test methods determine the amount of moisture contained in a cellulose sample which determines the amount ofbone dry cellulose present in a sample. The actual amount of cellulose in a sample is an essential entity when using cellulose as a starting material for the production of cellulose derivatives. . 3. Sampling 3.1 Cellulose in a variety of forms is sampled for mois ture, and no single set of directions can be given that is applicable to all types of cellulose material. The following general considerations should be borne in mind. 3.1.1 Cellulose, either in compact form, such as wood, sheeted pulp or paper, bided cotton or baled staple rayon, or in loose form such as sawdust or chips, may have an appreciably different moisture content in sections lying relatively dose together. In order to secure representative samples, therefore, a bulk sample should be . made up of small portions taken from various parts of the lot and having the proper proportion of edge and center material. 3.1.2 Except for those samples taken in an atmosphere with which the sample is in equilibrium, the moisture content of the sample will begin to change immediately after it is removed from its original surroundings. This change can be reduced by taking extra layers of sheeted material and discarding a few layers from the top and bottom before weighing, folding, or rolling the sample to reduce the exposed area, and by placing small samples in cans or bottles and 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 1.36 on CeUulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 1348 - 54. Last previous edition D 1348 - 61 (1985). protecting larger samples by wrapping in rubber sheets, moistureproof cellophane, or other protective wrappings, These means do not provide continuous protection, and the test samples should be weighed as soon as possible. 3.1.3 When possible, bulk samples should be taken. These samples should, weigh from 100 to 300 g, the larger samples being taken When the moisture content is low or variable, Following the initial weighing, the bulk samples should be cut up or tom into small pieces and then mixed and aU'owed to stand overnight or longer in a sealed container to obtain moisture equilibrium before weighing out test specimens; or the sample may be allowed to come to approximate equilibrium with the laboratory air and reweighed to determine moisture change before weighing test specimens. The latter f i jj \ j j -I | | I procedure is recommended singe it permits routine weighing j of samples without the use of special weighing bottles or boxes, and a series of accumulated samples can be weighed j simultaneously. Predrying is very desirable on samples with a ] high moisture content (more than 5 % aboveequilibrium j| value). When samples have been predried,calculate the j moisture lost, as follows: ; R= [M-A/A]x 100 "" (1)- | where:. - R = moisture, air-dry sample basis, %, ,1 1 M= original mass of the sample, g, and 1 A = air-dry mass of sample, g. 1 3.1.4 The apparent moisture subsequently observed When j testing a predried sample must be calculated on the basis of '1 the original sample mass in order to get the original moisture 1 content. Calculate the original mass of the air-dried sample 1 as follows: '. ' " j Origmafsaniple mass, g = [A x (100 + R)]/100 (2) j )*+, -. Exaniple--If 1000 g ofbulk (wet) sample on exposure to air lose 200 g of water, the apparent 'moisture content is 20% and equivalent regain is 25 %. If an 8:g specimen of the .air-dry material is taken for drying in the oven, the original mass is 8 x 1.25 -- 10 g. ! | TEST METHOD A--SPECIMEN WEIGHED IN OVEN 4. Scope 4.1 This test method for moisture determination is appli cable to a variety of cellulose types and can be used in most cases where a sample does hot contain noiiaqueous material volatile at 105C. The test method can be used for samples having either high or low moisture content. 5. Summary of Test Method 5.1 The specimen is heated to constant mass at 105C in a ventilated gravity-convection oven, in a current of dry air, for a period of 2 h. If no dry air is used, the specimen is heated for 4 h. j DUP050296753 # D 1348 Apparatus fkl Oven with Built-In Weighing Equipment--Such an jjjfcn employs a system of tared containers mounted on a |le or track that can be rotated to bring specimens to a spe- gc point in the oven, where the specimen and container , be placed on a hook or a tray connected to an outside lance. The oven must be capable of maintaining a constant perature of 105 3*C, with an average temperature of |5C; continuous operation below 105C is not satisfactory. /012f 2--In ovens having heating elements at the bottom only, and i: cross circulation, the temperature of the lower shelves should be lecked before they aie used. |T6.2 Dry Air Stream--Adi, dried by passing through silica aluminum oxide, concentrated sulfuric acid, or other jtttable drying agent, should be passed through the oven at a |ite sufficient to effect a complete change once every 2 min. f the air is dried by means of concentrated sulfuric add, Jequate traps must be provided. The use of sulfuric acid followed by perchloric drying agents should be avoided. 6.3 Shallow Glass Weighing Bottles---Bottles with groundjlass stoppers, measuring 30 mm high, and having a capacity pf 30 mL.2 6.4 Seamless Metal Weighing Boxes, having a wall height, , when open, preferably not over 1 in. (25.4 mm). ' 7. Procedure 7.1 Remove the basket, shallow pan, or other container ^supplied for use with the oven (Note 3). Weigh the container and place in it a specimen of 10 to` 50 g weighed to the , nearest 0.005 g. Designate this mass as M. Place the ' specimen in a tared container in the oven in such a manner : that it can be reweighed without removal from the oven. 3456 3--Experience has shown that when yarn and fiber specimens are left in comparatively deep weighing bottles in the oven, relatively discordant results are obtained and the drying period is unnecessarily long. To avoid,these difficulties specimens should be dried in containers that give the' cellulose free access to the air. For fibrous or bulky materials to be weighed in an oven, use containers such as open wire grills or baskets. For small specimens to be weighed out ofthe oven, use wire screen baskets that will fit in Weighing bottles, but ifthe specimen is ; powdery or tends to shed lint or fine short fibers, use a rinall weighing bottle or metal boxes. 7.2 Dry the specimen for 2 h at 105 3C, passing a cur rent of dry air into the bottom of the oven during the drying period. (Ifdry air is not forced through the oven, dry for 4 h.) 7.3 At the end of the specified period, cut off the flow of air and weigh the- specimen without removing it from the oven. Continue drying for Vi h longer, with the normal air flow, and reweigh the specimen. Repeat the drying and weighing until the mass loss between successive weighings is not more than 0.005 g, or until the specimen shows a gain in mass. Designate this mass as D. 7.4 Additional specimens should not be placed in die oven until the first specimens have attained constant mass. | 8. Calculation ! 8.1 Calculate moisture, as measured in the oven, as follows: 2 Weighing bottles similar to Nos. J-555, J-560, or J-574, available from Scientific Glass Apparatus Co., 2007 Kramer Lane, Suite 100, Austin, TX 78759, have been found satisfactory for this purpose. Moisture content, % [{M - D)/M] x 100 Moisture, dry basis (regain), % = [{M -- D)/D\ X 100 where: M = original mass of specimen, and D = mass of oven-dry specimen. (3) (4) 9. Report 9.1 Report the moisture in the cellulose on either or both of the following bases: 9.1.1 On the basis of the original sample, when it is termed "moisture content," "moisture as received," or "moisture as is" basis. 9.1.2 On the basis of the oven-dry cellulose, when it is termed "moisture, dry basis" or "moisture regain." 9.2 In order to avoid confusion always use the appropriate term. 10. Precision and Bias 10.1 Samples having a moisture content in the range of 5 to 15 % should show a standard deviation of 0.07 or less on replicates in a specific laboratory, and a standard deviation of 0.1 or less on replicates between laboratories. 10.2 Reproducible but less accurate values (under unfa vorable conditions the absolute error may be as high as 1 %) will be obtained' if the current of predxied air is omitted. Since the enror will be identical for all similar samples in the oven at one time, the results obtained in these cases will be comparable. The magnitude of error will vary directly with the relative humidity of the air entering the oven and with the equilibrium moisture content of samples at low relative humidity. Thus, the error will be higher on regenerated cellulose than on wood pulp or cotton, but it still would not usually be greater than 0.2 %, absolute. TEST METHOD B--SPECIMEN WEIGHED OUTSIDE OF OVEN 11. Scope 11.1 The scope and application of this test method are the same as those of Test Method A (see Section 4). .- 12. Summary ofTest Method 12.1 See Test Method A (Section 5). 13. Apparatus 13.1 Oven Without Built-In Weighing Equipment--Any ventilated oven capable of maintaining a constant tempera ture of 105 3C, with an average temperature of 105*C; continuous operation below 105C is not satisfactory. 3012 4--In ovens having heating elements at the bottom only, and no cross circulation, the temperature of the lower shelves should be checked before they are used. . 13.2 Dry Air Stream--See 6.2. 13.3 Shallow Glass Weighing Bottles--See 6.3. 13.4 Seamless Metal Weighing Boxes--See 6.4. 13.5 Weighing Bottles, glass with ground-glass stoppers, approximately 40 mm wide and 80 mm high. 13.6 Wire Baskets--Fitted baskets for weighing bottles made from approximately 15-mesh stainless steel. Monel, or other suitable screen. The height and depth of the basket will be determined by the weighing bottle used; the basket must 233 DUP050296754 # D 1348 slide into and out of the bottle without binding. The basket should have a solid bottom, but no top is required. 14. Procedure 14.1 If the sample is free oflint, dust, or short fibers, place approximately 10 g of the sample into a previously dried and desiccated wire basket (Note 2) contained in a dry weighing bottle. Stopper the weighing bottle, and weigh to the nearest 0.001 g. Designate this mass as M. Remove the basket, containing the specimen from the weighing bottle and place the basket, weighing bottles, and stopper in the oven. If the specimen includes powder-like material, transfer the spec imen directly into a small weighing bottle or can. Stopper the bottle and weigh to the nearest 0.001 g (Ad). Remove the stopper from the, bottle and place the bottle containing the specimen and the stopper in the oven. 14.2 Dry for 2 h at 105 3`C, passing a current of dry air into the bottom of the oven during the drying period. (If dry air is not forced through the oven, dry for 4 h.) 14.3. At file end of.the specified period, quickly, place the basket and specimen in the weighing.bottle again and stopper it (or stopper directly). Remove the weighing bottle from the oven and place it in a desiccator .containing an efficient desiccant, such as anhydrous calcium sulfate.3 .Allow it to cool for 1; h, momentarily open the weighing, bottle to equalize the pressure, and weigh to the nearest 0.001 g. 14.4 Return the specimen to the oven, exposing it as directed above, and dry for at least .1 h more., Place it in. a desiccator to cool and weigh in accordance with 14.3. Repeat the drying and weighing until , the mass loss between two successive weighings Js not more than 0.005 g,(or until the specimen shows a gain, in mass). Designate the lowest observed mass as D. 14.5 When constant mass has been obtained, discard the specimen and weigh the weighing bottle (plus basket) or can. Designate this mass as T, 14.6 Do not place additional specimens in the oven until the first specimens have attained constant mass. 15. Calculation ~ 15.1 Calculate moisture, as measured outside of the oven, as follows: Moisture content, % [(M -- D)/(M -- 7)] x *00 (5) Moisture, dry basis, (regain), % = [(M -- D)/(D - 7)]' X 100 (6) where: M = original mass of the specimen (plus basket) and weigh ing bottle, D = oven-dry mass of the specimen (plus basket), and T = mass of the empty weighing bottle (plus basket). 16. Report 16.1 Report the moisture in the cellulose as directed in Section 9. 17. Precision and Bias 17.1, See Section 10. TEST METHOD C--KARL FISCHER METHOD IS. Scope .. . 18.1 This test method covers the determination of mois ture in celltilose by titration with Karl Fischer reagent. The test method is applicable to all types and forms of cellulose. It is especially useful with samples containing tionaqueous material volatile at 110C, since such substances interfere in the oven-drying methods. Anhydrides, alkalies, and large amounts of aldehydes and ketones interfere.. 18.2 The Karl Fischer titration method is especially valu able where only small amounts of samples are available. The procedure lends itself-to multiple.determinations. 18.3 It is essential that the Karl Fischer reagent, standard water solution, and anhydrous methanol be protected from atmospheric, moisture at all times. During the titration ,a stream .of dry air or nitrogen will protect the contents of the titration flask from atmospheric moisture pick-up. . 19. Summary of Test Method 19.1 An excess of Karl Fischer reagent is added to the specimen suspended in anhydrous methanol. After shaking for 15 to 20 min to extract the moisture, the excess is back-titrated with standard water solution. It is also permis sible to titrate directly to the end point with Karl Fischer reagent. The end point is best detected electrometrically, but, with practice, it may be satisfactorily determined visually. 789: 5--To determine the moisture content of certain plastic materials the following solvents or solvent combinations may be used: chloroform, m-cresol, pyridine, o-dichlorobenzene-ihethanol, dioxane- methanol; dioxane-pyridiney methylene ' chloride-methanol (1+1), pyridine-methanol, and toluene-methanoL : 20. Apparatus 20.1 Buret, automatic,' 25 or 50 mL, attached to an amber glass reservoir so that any air entering the system must pass through an efficient absorber containing anhydrous calcium sulfate (Drierite) apd ^soda-asbestos (Asparite). 20.2 Pipets, automatic or transfer, 50- and' IOO-rriiL, 20.3 Flasks, or bottles, glasst-stopperedT 125-mL or 250- mL, for visual end point, or suitable enclosed reaction vessel for electrometrically determined erjd point. . ", 20.4 Bottle, dropping, or equivalent, for weighing water for standardization of reagent. 20.5 Electrode and. Meter System, with provision for ade quate stirring, and flasks-or containers adapted to the assem bly if the end point is to be determined electrometrically. 20.6 Filter, sintered glass,4 coarse porosity, 30-mL. 20.7 Bottle, weighing, low-form, 45 by 65 mm for drying wet pulp! 21. Reagents 21.1 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- 3 Indicating Dn'erite, available as No. 07-578-3 from Ftsher Scientific Co., 50 Faden Rd, Springfield, NJ 07081, has been found satisfactory for this purpose. ' 4Pyrex No. 36060-30C. manufactured by Corning Glass Works, Houghton Park, Corning, NY 14830, or equivalent has been found satisfactory for this purpose. 234 DUP050296755 ety, where such .specifications are available.5 Other may be used, provided it is first ascertained that the t is of sufficiently high.purity to permit its use without j the accuracy of the determination,, :2 Air.or Nitrogen, under a pressure of 6 to 12 in. of j;fl,5;to. 3.0 kPa) and dried by passing through concen' sulfuric acid (H2S0.4, sp gr 1.84) followed by indig grade anhydrous calcium sulfate or Other, suitable ting desiccant. If the titration assembly provides ades protection from atmospheric moisture, this will not be 'red. . ....... *.3 Karl Fischer Reagent--Suitable, reagent may be pur ged from laboratory supply houses or prepared as follows: 1.3.1 Place 530 5 mL of dry methanol (CH3OH) in a a, dry, 9-L chemical-resistant glass carboy; Add 2025 ;L of pyridine. Add 1270 1 g of iodine crystals . and the carboy until the iodine is completely dissolved, ce the carboy in a cracked ice bath and allow to stand hit 1 h. 1.3.2 Weigh on a platform scale to 25 g (0.05 lb) a 'nder of sulfur dioxide (S02) with chemical-resistant glass ng attached to the outlet with polyethylene tubing. Tilt cylinder with the outlet down. 1.3.3 Open the cylinder valve and allow the sulfur dde to run into the' solution in tlie carboy. Use the emical-resistant glass tubing, through which the S02 flows, stir the solution. When 955 5 g (2.1 ,0.05 ib), as termined by- difference in scale mass reading, have run in, pper the bottle tightly. 21.3.4 Add about 4300 mL of methylene chloride :H2C12) and mix well. If desired, the methylene chloride ay be omitted and a total of 6375 mL of pyridine used. ,'ow the solution to stand 24 h before, use. Protect from ntamination by atmospheric moisture by storing in an -glass apparatus. Standardize daily as described in Section ' 21.4 Methanol, anhydrous, water content lessthan 0.05 %. 21.5 Watfr Solution, for use if back-titration is desired, irepare by adding 1.0 m.L of water to 1 litre of anhydrous ethanol. Mix well and store in an all-glass assembly otected from contamination by, atmospheric moisture. ^Standardize as described in Section 22. 22. Standardization of Reagents 22.1 Back-Titration--Standardize the Karl Fischer' re agent and water solution daily. It is important that the same technique and end point be used both in the standardization and in subsequent analyses. The following directions apply to the visual detection of the end point, but with obvious modification, depending upon the particular apparatus used, they may be followed for instrumental end point detection. 22.1.1 Pass a stream of dry air or nitrogen through the flasks during all additions and titrations unless the titration assembly provides protection from atmospheric moisture. s "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." 22.1.2 Add Karl Fischer reagent to 50 mL of anhydrous methanol contained in a dry 25G-mL Erlenmeyer flask until a dark brown color has been reached (AF). Back-titrate with water solution until the end point described in Section 23 has been reached (A^). Reserve this solution, refill burets, and accurately measure approximately 15 mL of Karl Fischer reagent into this same flask (WF). Back-titrate with water solution as described above (' 22.1.3 Weigh to the nearest' 0.0001 g, by difference (conveniently from a Sattler weighing pipet), from 0.15 to 0.20 g of water (G) (Note 6) into a dry 250-mL Erlenmeyer flask containing 50 mL of anhydrous methanol. .Titrate with Fischer reagent to a dark brown color (S'/,),, indicating, an excess of 2 to 5. mL of the reagent. Back-titrate with water solution to the end point (S^). If the end point should .be passed, more Fischer reagent may be added and the titration with water solution continued until the exact .end point has been reached. <=>? 6--If desired, standard Rochelle salts or other material with known water <jf hydration, may be used instead of weighing the water directly. `, 22.1.4 Calculate the water .equivalent, T,, of the Karl Pischer reagent as follows: a - WF!WW (7) where: - '" '' A = millilitres of Karl Fischer reagent equivalent to 1 mL of water roliition, WF = millilitres of Karl Fischer reagent measured into the titrated nfethanof, and Ww = millilitres of water solution required to titrate the excess Karl Fischer reagent. ' B = AF-(Ax Aw) __ (8) where: .4; B = millilitres of Karl Fischer reagent required by 50 mL of methanol, AF -- millilitres of Karl Fischer reagent added to 50 mirof methanol, and Aw -- millilitres of. water solution required to titrate the excess Karl Fischer reagent in 50 mL' Ofmethanol. jr=G/{SF-(SwxA)-~B1 - ' >) where: ' ,. T = water equivalent of the Karl Fischer reagent, g/mL, " G =? grams of water added (21.1.3), SF - miUiiitres of Karl Fischer reagent added to the Weighed water, and ` Sw = millilitres of water solution required to titrate the excess Karl Fischer reagent. 22.2 Direct Titration: 22.2.1 Alternatively, add from an automatic pipet or from an oven-dried pipet, 50 mL of methanol to each of four oven-dried titrating flasks or bottles. Weigh by difference to the nearest 0.1 mg, 0.10 to 0.25 g of distilled water from a weighing bottle fitted with a dropper, into each of two of the flasks. Titrate the solvent-water standards directly to the end point with Karl Fischer reagent (Tj). Titrate the solvent blanks to the same end point as for the standards (T2). 22.2.2. Calculate the water equivalent of the Karl Fischer reagent as follows: T^A/iT-TJ (10) II DUP050296756 D 1348 where: T -- water equivalent of the Karl Fischer reagent, g/mL, A * grains of water added (22.2.1), T2 = millilitres of Karl Fischer reagent required for titration of solvent blank, and 7, = millilitres of Kari Fischer reagent required for titration of solvent and water. 22.2.3 Average the duplicate results and round off the average to three significant figures. Duplicate values of T should agree within 0.0001. 23. Procedure 23.1 Weigh to the nearest 0.0001 g an amount of sample estimated to contain from 0.10 to 0.15 g ofwater. For samples containing from 4 to 6 % water, a test specimen weighing from 2.5 to 3.0 g is satisfactory. Transfer the weighed specimen to a dry, 250-mL Erlenmeyer flask with minimum exposure to the atmosphere and add 100 mL of anhydrous methanol. Stopper the flask and shake slowly for 15 to 20 min, or allow the stoppered flask to stand for 1 h with occasional shaking. 23.2 With an oven-dried pipet, transfer 50 mL of the supernatant liquid to a 125-mL oven-dried, glass-stoppered bottle. Exposure to the atmosphere may be minimized by covering all flask openings with rubber sheeting during transfer and titration operations. Pipets and buret tips may be inserted through a small slit in the rubber sheeting. . 23.3 Titrate with Karl Fischer reagent to the same end point as in the standardization. Ifback-titration is to be used, rapidly titrate with Karl Fischer reagent until the solution has a dark brown color. Stopper the flask and allow to stand for 15 min. If the brown color should fade during the standing period, add more Karl Fischer reagent. Record the amount of reagent added. 23.4 Pass a stream of dry air or nitrogen through the flask and titrate with water solution until the end point has been reached, as shown by an instrument or indicated visually. In the latter case, the titrated solution will have a yellow color with just a trace of brown at this point. If the end point should be overtitrated, add more Karl Fischer reagent dropwise to the first appearance of the brown color. 23.5 Alternatively, titrate directly to the end point with Karl Fischer reagent. The visual end point is a color change from light brown to dark reddish-brown. @ABD 7--An excellent visual standard of comparison is an 0.016 N iodine solution (prepared by mixing IS mL of0.1 Niodine solution and 75 mL of water). The end point is best observed by examining the solu tion by transmitted light from a 15-W fluorescent tube.6 It is essential to titrate to the same end point in the standardization and the same titration. 6 General Electric Gold 15-W fluorescent tube, or its equivalent, has been found satisfactory for this method. 23.6 Run a blank on 50 mL of the methanol by titrating as described in 23.3 and 23.4 or 23.5. The titrated alcohol may be stoppered and used as an end point color standard ! when the end point is detected visually. j 23.7 If calculation on the dry mass basis is desired, trans- j fer the cellulose specimen to a coarse, fritted-glass crucible previously washed with methanol or with alcohol conform ing to Formula 30 of the U. S. Bureau of Internal Revenue, j dried at 120C, and weighed to the nearest 1 mg. Wash, using j suction, with about 15 mL of methanol or Formula 30 \ alcohol. Suck as dry as possible to remove all alcohol vapors, 23.8 Place the crucible on a hot plate or steam bath (be j sure the surface is clean) for 3 to 5 min to flash off any remaining alcohol, and then place it in an oven at 120C to j dry for 30 min. Cool the crucible containing the cellulose in a desiccator and weigh to the nearest 1 mg. Determine the I mass of the dry pulp by difference. 24. Calculation j 24.1 Calculate the percent moisture as follows: 24.1.1 For Back-Titration Method j P~{{C-DA-E)xTxR\lW)y.m (11) 24.1.2 For Direct Titration Method: p=([C-B)xTxRyw)x\m (12) | and. Moisture, dry basis, (regain), % = [f>/(100 - P) X 100 i = [(W - Z)/Z] X 100 ^ vj where: P - moisture content, %, . j C = millilitres of Karl Fischer reagent required for titration | of the sample, ^ 1 D = millilitres of water solution added ^23.4), j A = millilitres of Karl Fischer reagent equivalent to 1 mL I of the water solution, 1 B = millilitres of Karl Fischer reagent required for titration 1 of 50 mL of methanol (23.6),- 1 T -- grams of water equivalent to 1 mL of the Karl Fischer j reagent, '1 W = grams of sample used, -- _ | R = aliquot factor (Note 8), and Z = grams of dried cellulose. FABD 8--The aliquot factor is 2 when 100 mL of-methanol is taken to extract the water from the cellulose and SO mL is titrated. j 25. Precision and Bias 25.1 Moisture in cellulose determined by Fischer titration is approximately 0.6 % (absolute) higher than by oven drying, and the higher value is believed to represent the true moisture content of the sample with greater accuracy. The standard deviation assignable to a single test by a single operator is 0.41. j s 1 77ia American Socieity for resting and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this stendsrd. 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 riot revised, either reapproved or withdrawn. Yourcomments are Invitedeither forrevision ofthis stsndard 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. ;J 3 I j ;) J i 236 mffiRtm- DUP050296757 A Designation: D 1366 - 86 (Reapproved 1991)61 Standard Practice for ans* Reporting Particle Size Characteristics of Pigments1 This standard is issued under the fixed designation D 1366; 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 of last reapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. GHIJKLKeywords were added editorially in July 1991. j Scope 1.1 This practice for reporting the fineness characteristics f pigments is designed to apply in most cases where ell-known methods for determining these particle size characteristics in, the subsieve range are employed, such as Pmicroscopic, sedimentation, and turbidimetric methods; and -'partially to absorption and permeability methods. 1.2 Laminar, plate-like pigments and composite pigments iving a definite bimodai distribution are not considered rithin the scope of this practice.' 1.3 Parameters--The fineness characteristics are reported |n the following three parameters; 1.3.1 Particle Size Parameter. 1.3.2 Coarseness Parameter--A parameter descriptive of jj|he coarseness character of the pigment, making use of a limiting value in the subsieve range similar to that used in pHe sieve ranges. || * 1.3.3 Dispersion Parameter--A parameter descriptive of lihe uniformity of the particle size distribution. J-! K4 This standard does not purport to'address the safety mprobiems, if any, associated with its use. It is the responsiWhility of the user of this standard to establish appropriate i safety and health practices and determine the applicability of I regulatory limitations prior to use, 2. Referenced Document 1 2.1 ASTM Standard: E 20 Practice for Particle-Size Analysis of Particulate Substances in the Range of 0.2 to 75 pm by Optical Microscopy12 . Terminology * 3.1 Definitions: 3.1.1 particle size parameter (specific surface diameter, SSD)--diameter d3 used elsewhere in ASTM test methods. This parameter is the same as that frequently reported as "Average Particle Size by Surface Mean," and "Specific Particle Size," and is defined as follows: SSD=Zdf/Zd2f where: 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 1.31 on Pigment Specifications. Current edition approved June 27, 1986. Published August 1986. Originally published as D 1366-55T. Last previous edition D 1366-65{198l)tl. 2 Annual Book ofASTM Standards, Vol 14.02. SSD -- specific surface diameter, pm, d = mean class size, pm, and / = frequency. Therefore the SSD is the diameter of a sphere having the specific surface characteristic of the pigment. The true specific surface of all pigments involves a shape factor. Report SSD whether or not the effect of shape has been considered in the calculations. Presumably, as the effect of shape is better understood, it will figure more and more in calculations involving particle size, -but in the meantime it wifi of necessity be ignored in many cases. 3.1.2 coarseness parameter (CP)--that diameter, ex pressed in micrometres, below which 99.5 % of the pigment falls. 3.1.3 dispersion parameter (DP)--the ratio of the micrometre size within which 50 % of the pigment lies, to the specific surface diameter, SSD. The larger the DP number, the greater the dispersion parameter and the lower the uniformity. Report the dispersion parameter in all cases when a distribution curve' can be prepared from the original data. The dispersion parameter cannot be calculated from data obtained by absorption or permeability methods. Deter mine as follows: 3.1.3.1 Prepare a cumulative-size distribution curve, on 3-phase log paper, using the vertical axis for the percent failing below the size indicated, and the horizontal axis (log scale) for diameter in micrometres. Use the.upperjclass limit corresponding to the cumulative weightpsrcentage. Subtract the micrometre size at 25 % cumulative weight from the micrometre size at 75 %, and multiply the difference by 100 -* SSD, as follows: ^- DP = (pm at 75 % - pm at 25 %)((SSD) x 100 4. Significance and Use 4.1 This practice is of value (7) to the producer of fine particles as a means of reporting particle characteristics with respect to quality control and (2) to the buyer to assure that the particle size and particle size distribution meet his requirements. 5. Procedure 5.1 Particle Size by Microscopical Methods--Procedures for determining particle size by microscopical methods are described in Practice E 20. Whenmicroscopical methods are employed, report the data in tabular form similar to that shown in Table 1. 5.2 Particle Size by Sedimentation Methods--Sedimenta tion methods provide data from which may be calculated the DUP050296758 Class Limits, pm Lower Upper 0.25 0.75 1.25 1.75 2.25 2.75 3.25 3.75 4.25 4.75 5.25 5.75 6.25 6.75 7.25 7.75 3.25 Totals 0.75 1.26 1.75 2.25 2.7S 3.215 3.715 4.215 4.75 5.215 5.75 6.25 6.75 7.25 7.75 8.25 8.75 # D -1366 TABLE 1 Example of Data Sheet for Microscopic Method Mean Class Size, d 0.5 1.0 14 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 Frequency, f 71.4 50.9 57.9 36.9 41.1 34.5 34.5 21.0 42.0 81.2 283.8 155.9 71.0 73 5.1 4.2 0.5 999.6 d`f 17.8 50.9 130.2 1474 256.8 310.9 423.2 336.1 850.8 2 030.8 8 586.3 5 613.4 2 998.1 388.9 288.8 268.9 33.7 22 733.1 dsf 8.9 50.9 195.4 295.0 641.9 932.7 1 4812 1 344.5 3 828.8 10 154.0 47 225.0 33 680.0 19 487.9 2 722.4 2 166.3 2 161.4 286.8 126 653.1 d*f,% 0.007 0.040 0.164 0233 0.506 0.738 1.17 1.06 3.02 6.02 3725 28.60 1528 2.15 1.71 1.71 023 Cumulative Weight, % 0.007 0.047 0.191 0.424 0.93 1.69 2.86 3.92 8.94 14.96 5221 78.81 94.19 96.34 98.05 99.76 99.99 mean class size and percentage by weight for each of these class sizes. Table 2 presents in the second and third columns data normally obtained by sedimentation methods. Column 3 of Table 2, which gives the distribution by weight of the class sizes, is identical with the function d3f Therefore, the d2f function in Column 4 equals d3f/d. The fifth column, cumulative weight, percent, is obtained from the values in Column 3. 5.3 Particle Size by Turbidimetric Methods--Like the sedimentation method, the turbidimetric methods provide class sizes and a percentage by weight for each class size, and the calculation is the same as that in Table 2. However, frequently a weight distribution curve is obtained from data not directly convertible into the class-size distribution table. In such cases, reconstruct the size-weight distribution table from the distribution by weight curve. 5.4 Particle Size by Absorption and Permeability Meth ods--The absorption and permeability methods, and a few others, provide no means of making a distribution curve. Therefore, obtain specific surface either as square metres per cubic centimetre, or as square metres per grant of material. In the first case, where s equals square metres per cubic centimetre, the equation is as follows: TABLE 2 Example of Data Sheet for Sedimentation Method Diameter Class Size Limits Lower Upper Class Size Diameter, d, pm Weight 56, cf9f daf Cumulative Weight, * 0.0 0.5 1.0 1.5 2.0 3.0 4.0 5.0 7.5 10.0 15.0 20.0 Totals 0.5 1.0 1.5 2.0 3.0 4.0 5.0 72 10.0 15.0 20.0 30.0 0.25 0.75 125 1.76 2.50 3.50 4.50 6.25 8.75 12.50 17.50 25.00 11.0 10.0 10.0 9.0 15.0 9.5 8.5 12.5 8.0 S.3 1.2 0.0 100.0 44.00 13.33 8.00 6.14 6.00 2.71 1.89 2.00 0.91 0.42 0.07 0.00 84.47 11.0 21.0 31.0 40.0 55.0 64.5 73.0 85.5 93.5 98.8 100.0 SSD=6/s In the second case, where S equals square metres per gram (Note), the equation is as follows: SSD = 6/(sp gr X s) MNOP Q Example--Channel black has a specific gravity of 2.0. If the specific surface in square metres per gram is reported as 94.0, then: SSD = 6/(2 x 94) = 0.032 6. Calculation and Report 6.1 To determine the coarseness and dispersion parame ters from the microscopical data of Table 1, draw Curve I of Fig. 1, using the cumulative weight percentage and the upper class size units of Table 1. From this curve, read the CP at the point where the curve crosses the 9$.5 % line, that is, 8.7, and obtain the DP from the sizes where the curve.crosses the 25 and 75 % lines; then calculate as follows: SSD = 126 653.1 /22 733.1 = 5.57 pm -- px -- d1%%o -- d2S % = 0.70 pm DP = 100 pJSSD = (100 x 0.70)/5.57 = 12.6 . ... CP = 8.7 pm 6.2 To determine the coarseness "End dispersion parame ters from the sedimentation data of Table 2, draw Curve II of Fig. 1, using the cumulative weight percentage and upper class size units of Table 2. From this curve, determine the coarseness and dispersion parameters as described in 5.1, as follows: SSD = Sd3f/Xd2f= 100.0/84.47 = 1.183 pm DP = 17.0 pm p2 = 5.30 - 1.18 = 4.12 pm . DP*= 100 p2/SSD = 348,0 ' CP = 17.0 pm 6.3 While theoretically the size of pigment particles is independent of the method of determination "used, it is recognized that various methods of determining subsieve particle size distribution give somewhat different results, depending on the assumption made in the particle method. It is recommended, therefore, that the method of determina tion always be made a part of the report of the size distribution determined under this practice. DUP050296759 D 1366 ywords microscopic; pigments; sedimentation; turbidimetric permeability absorption 0.2 0.5 5.0 . Diameter, micrometres 10.0 FIG. 1 Curves for Obtaining Coarseness and Dispersion Parameters 20.0 The American Society tor Testing anti-Materials takes noposition respecting the validity atanypatent rights assertedIn contraction with any Item mentioned In this standard. Users cl this standard are expressly advised that determination of the validity of any suchpatent rights, mid the risk of infringement ofsuch rights, are entirely their own responslbilltyr- Thls standard Is sublet to revision at any time bythe responsible technical committee end must be reviewed every five years and ' Ifnot revised, either reapproved or withdrawn. Your comments areinvitedeitherfor revision ofthis standard orfor additional standards 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 teeI that your comments hare not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 9 T.O'Q: DUP050296760 4 Designation: D 1394 - 76 (Reapproved 1991)1 Standard Test Methods for Chemical Analysis of White Titanium Pigments1 This standard is issued under the fixed designation D 1394; the number immediately-following the designation indicates the year of original adoptlon'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. These lest methods have been approved/or 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. e> RSTUWKeywords were added editorially in June 1991. 1. Scope 1.1 These test methods cover procedures-for the chemical analysis of white titanium dioxide pigments. 1.2 The analytical procedures appear in the. following order: ^ Preparation of Sample Qualitative Analysis Moisture Total Titanium: Jones Reductor Method Aluminum Reduction Method Aluminum Oxide Silica Sections 4 S and 6 7 8 to 12 13 to 17 18 to 22 23 to 29 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 ofregulatory limitations prior to use. A specific hazard statement is given in Sdction 19. 2. Referenced Documents i- 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments12 D1193 Specification for Reagent Water3 4 E 50 Practices for Apparatus; Reagents., and Safety Pre cautions for Chemical Analysis of Metals'! 3. Reagents ^ 3.1 Purity ofReagent--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 1 These test methods arc under the jurisdiction of ASTM Committee D-l on Paints and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved June 25, 1976. Published August 1976. Originally published as D 1394 - 56 T. Last previous edition D1394 - 75. 2 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 03.05. 5 "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 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. 3.2Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193.. 4. Preparation of Sample 4.1 The sample shall, in all cases, be thoroughly mixed and comminuted before taking portions for analysis. QUALITATIVE ANALYSIS 5. Reagents 5.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 5.2 Ammonium Sulfate ((NH4)2S04). ' 5.3 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric add (HC1). 5.4 Hydrogen Peroxide (30 %)--Concentrated hydrogen peroxide (H202). 5.5 Hydrogen Sulfide (H2S). 5.6 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04). 5.7 Sulfuric Acid (1+19)--Carefully mix. 1, volume of H2SG4 (sp gr L84) with 19 volumes oflwater. ' 5.i'Tartaric'Acid. 1 5.9 fin oFZinc Metal. 6. Procedure ." 6.1 Plte about 0.5 g of the sample in a 250-mL glass beaker,6 and add 20 mL of H2S04 (sp gr 1.84) and 7 to 8 g of (NH4)2S04. Mix well and boil for a few minutes. The sample should go completely into solution; a residue denotes the presence of silicon dioxide (SiOj) or siliceous matter. Cool the solution, dilute with 100 mL ofwater, heat to boiling, let settle, filter, wash with hot H2S04 (1+19) until free of titanium, and test the residue for lead, etc. 6.2 Test the filtrate for calcium, zinc, iron, chromium, etc., by the regular methods of qualitative analysis.7 For the iron determination add to a portion of the filtrate 5 g of tartaric add, render slightly ammoniacal, pass in H2S in 6 Borosilicate glass has been found satisfactory for this purpose. 7 Treadwell, F. P., and Hall, William T, Qualitative Analysis, John Wiley & Sons. Inc., New York, NY, Vol. 1, Ninth English Ed., 1937. m DUP050296761 OUTSIDE DIAMETER ,40 mm H.5mm /FIRE POLISHED 100+ 2 mm 100 2 mm OUTSIDE DIAMETER -- 8 0.8 mm TIRE POLISHED FIG. 1 Jones Reduction gxcess, and digest on a steam bath. No precipitate after 30 pin indicates the absence of iron, nickel, cobalt, lead, popper, etc. A black precipitate readily soluble in dilute HCl denotes iron. For titanium, test a small portion of the original filtrate with H202. (a clear yellow-orange color hould result) and another portion with metallic tin or zinc (a pale blue to violet coloration should result). Negative Rsults should be shown for sulfide, carbonate, or appreciable Water-soluble matter. I; MOISTURE mjiz X 7. Procedure iLf 7.1 Determine moisture and other volatile matter in 'accordance with Test Method A of Test Methods D 280. ?! TOTAL TITANIUM BY THE JONES REDUCTOR METHOD i.8. Scope 8.1 This method gives results similar to those obtained with the Aluminum Reduction Method, Sections 13 to 17. Apparatus 9.1 Jones Reductor8 having a zinc column at least 450 Dm in length, and 19 mm in diameter (Figs, i and 2). The 8 Directions for preparing a Jones Reductor may be found in Hillebrand, W. F., f|f al., Applied Inorganic Analysis, John Wiley & Sons, Inc., New York, NY, ond Ed., 1953, p. 108. filtering pad must be tight enough to hold all the particles of amalgamated zinc resting on it, and may be made of asbestos or, preferably, glass-wool supported by platinum gauze or a perforated porcelain plate. Use the least amount (Q.l to 1.0 %) of mercury that will enable satisfactory control of hydrogen evolution;, since heavy amalgamation tends to reduce the rate of reaction. Prepare the amalgam by washing 20-mesh zinc for 1 min in enough 1 N HC1 tQ cover it, adding the proper amount of 0.25 M mercuric nitrate or chloride solution, and stirring rapidly for 3 min. Decant the solution and wash the amalgam with water and stone under water to which a few drops of HCl have been added. After using, keep the reductor filled with water when not in use, in order that basic salts will not be formed and clog it. 10. Reagents 10.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 10.2 Ammonium Sulfate ((NH^SO^. 10.3 Carbon Steel or Iron--Pure iron or plain carbon steel. 10.4 Ferric Sulfate Solution (1 mL=0.02 g Fe)--Dissolve 20 g of iron or carbon steel in a slight excess of HCl, oxidize with approximately 12 mL of HN03, add about 80 mL of H2SO4, and beat to dense white fumes. Cool, dilute with water to 1 L, digest on a steam bath until sulfates are DUP050296762 dissolved, and filter if necessary.-To oxidize any ferrous iron that may be present, add 0.1 N fcMi^04 solution until a faint pink color persists for 3 min. Ferric ammonium sulfate (FeNH4(S04)2- 12H20) may also be used'to prepare this solution (See 15.4). 10.5 Hydrochloric Acid (sp gr-1.19)--Concentrated hy drochloric acid (HQ). 10.6 Iron or Carbon Steel--Pure iron or plain carbon steel. , . : 10.7 Nitric Acid (sp gr 1,42)-+Concentrated nitric acid (HNQ3). -v j, 10.8 Sodium' Oxalate---National Institute of Standards and Technology standard reference material No. 40 of sodium oxalate (Na2C204). ( 10.9 Potassium Permanganate, Standard Reference Mate rial (0.1 N, 1 mL = 0.008 g fi02)--Dissolve 3.16 g of KMn04 in water and dilute to 1L. let stand 8 to 14 days, siphon off th.e ele^1solutiQn"(c)f fiitfcr through sintered glass, medium porosity), and standardize against the National Bureau of Standards standard sample Nd: 40 of sodium oxalate (Na2C204) as follows: In a, 400-mL beaker dissolve 250 to 300 mg Na2C204 in 2$) mL ofhot water (80 to 90C) and add 15 mL of H2S04 (1+1). Titrate at once with the KMn04 solution, stirring the liquid, vigorously and continu ously. The KMn04 solution 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 caire to allow each drop to be fully decolorized before th(e next is introduced. The solution shall not be below 60C by the tihae the end; point has been reached. (More rapid cooling may be prevented by allowing the beaker to stand on a small hot plate during the titration. The use of a small type thermometerasa:stming rod is most convenient.) Keep the KMri04 solution in a glass-stoppered bottle painted black f'o keep out light or in a brown glass bottle stored in a dark place. Calculate the Ti02 equivalent in grains , of T1O2 per millilitre of, the KMriP* solution as fpUQWS: a . .! - : ; > : Ti02 equivalent ^ (IFx- l.l9Z)fV b ' where:','. ''V'* W = Na2C2b4 used, g, add J1' [' V'i -,4 KMn04 sqlutfon required for the titration, mL: . la 16 Sulfitrib'Acid (sp gr 1.84)--Concentrated sulfiiric acid (H2S04). ' f ', 10.11 Sulfurit Acid (l.+l)---Carefully mix 1 volume of H,Sp4 (sp gr 1.84) into 1. vdliihfe 'ofwater with' rapid stirring. 16.12 Sulfuric Acid (1+19)~Carefully mix 1`vbluiiie'bf H2SQ4 intd`19 volumes of water with rapid stirring. ''11 11. Procedure 11.1 Determine the dry weight of a weighing bottle and' cap to 0:1 mg. Weight to 0.1 mg 300 to 350 mg of the sample to be analyzed into the weighing bottle. - v 11.2 Dry the specimen in the opened weighing bottle for 2 h at 105 to 110C. Cool in a desiccator, cap the bottle, and weigh as rapidly as possible. Calculate the dry weight of'the specimen and use in the actual calculation. 11.3 Transfer the dried specimen to a dry 250 mL chemical- and heat-resistant glass beaker,6 add. 20 mL of K2S04.(sp gr 1.84) and 7 to 8 g of (NH4)2S04. ,Mix well and heat on a hot plate until dense white fumes are evolved, and then continue the heating over a strong flame until solution is complete (usually requires not over 5 min of boiling) or it is apparent that the residue is composed of Si02 or siliceous matter. Caution should be observed in visually examining this hot solution. Cool the solutioh, dilute with 100 mL of water, stir, heat carefully to boiling while stirring, let settle, filter through paper, and transfer the precipitate completely to the paper. 11.4 Wash the insoluble residue with cold H2S04 (1+19) until titanium is removed. Dilute the filtrate to 200 mL and add about 5 mL of NH4OH to lower the acidity to approximately 10 to 15 % H2S04i (by volume). Wash out the Jones reductor with B2S04 (1+19) and water, leaving sufficient water in the reductor to-fill to the upper level of the zinc. (These washings should require not more than one or two drops of 0.1 N KMn04 solution to obtain a pink color.) Empty the receiver, and put in tit 25 mL of ferric sulfate solution. Reduce the prepared titanium solution as follows: 11.4.1 Run 50 mL of H2SQ4 (1+19) through the reductor at such a uniform rate as to require 5 to 10 min for passage. 11.4.2 Follow this with thb titanium solution at such a uniform rate as to require 10 min to pass through the reductor. 11.4.3 Wash out with 100 mL of H2S04 (1+19). 11.4.4 Finally run through atyout 100 mL of water. Take care that the reductor,- is always filled with solution or water to the upper level of the zinc. 11.5 Gradually release the suction, wash thoroughly the glass tube that was immersed m.the ferric sulfate solution, remove the receiver, and titrate immediately with 0.1 N KMn04 solution. Run a blank determination, using the same reagents and' washing the reductor as in the above determination. 12, Calculation < , 12. r Calculate the percent. Of Tf02aS fcilbws: ! (K,. - B)xT x 100 S: : ., where: ;+"d Ki = KMn04 solution required for titration1 ofspecimen, mL v -. .1' "! B = KMn04 solution required for titration of the blank, mL ! T = Ti02 equivalent of the KMn04 solution, g/piL, and S = dried specimen, g. 12.2 The results calculated in accordance with: 12.1 will include iron, chromium, arsenic, and any other substa'nce that.ps. reduced by zipc arid, acid. Howevei*, appreciable quantities of interfering materials are not likely to be encountered in normal, white titanium pigments. : TOTAL TITANIUM BiY THE XtliMINUM. REDUCTION METHOD 13. Scope 13.1'This method gives results similar to those obtained With the Jones Reductor Method (Sections`8 to 12). 14. Apparatus 14.1 Delivery Tube, made.of about 4-mm inside diameter glass tubing bent so that there is a horizontal run of about .6 242 mum m <r DUP050296763 if # D 1394 |jj. (152 mm) and a vertical drop of about 3 in. (76 mm) at band, and a vertical drop of about 6 in. at the other end. |&2 Weighing Bottle, wide-mouth, with ah extemal- ng cap, and no larger than necessary for the required jpbunt ofsaihple; :- L-ReagentS:. -.. , fbSA `Aluminum-Metal Foil, electrolytic grade. ft5,2 Ammonium Sulfate ((NH^SOJ. 5.3 Ammonium Thiocyanate Indicator Solution--Dis- ve-24.5 g of ammoniurii thiocyanate (NH4CNS) in 80 mL Ihot water, fiRer, bring to room temperature, and dilute to So mL. Keep in a well-stoppered, dark-colored bottle.1 Jp5.4; Ferric AmmoniumSulfale Solution (1 mL = 0.005 g p02)--Dissolve 30.16 g of fresh ferric ammonium sulfate eNH4(S04)2- 12H20) in 800 mL of water containing 15 |L of H2S04 (spgr-1.84). Add 5 mL of 3 % H2G2 and boil |f at least 15 min then cool to room temperature. Dilute to actly 1 L and mix well. FiRer if cloudy. Standardize using i to 210 mg of NBS-standard reference material No, 154 Jfptitanium dioxide and proceeding as directed, in Section 16; HSlculate the.Ti02 equivalent of the solution in grams, of BEiD2 per. millilitre, of solutionj as follows:, *" TiQ2.equivalent (W, x P)/{V2 X 100) '" ' Bpiere: \ i . ' . ,, " National Bureau of Standards standard sample of Kf T. -/. , V. Ill t .= percent TiOz in National Bureau of Standards Jklj standard sample,.^.pd Pta ^ ferric ammonium sulfate solution required for the ' titration, nit, ... . 15.5 Hydrochloric Acid (sp gr 1.19)--Concentrated, by- ^drochloric. acid (HC1), , ' ' " 15.6 Hydrogen Peroxide--3 %, , ... ' ; 15'.7. Sodiiap Bicarbonate Solution-r-Hlake up a saturated solution at tihe time of analysis! About 10 g of sodium mcarbonate (NairiCOa) to 90 g of water is required. IL, \5.B'^Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric irfi(f(H2sp4),.r , ", Titanium Dioxide (Ti02)--TSatipnal Bureau . of I ^Itandards.staiidard sample .No. 154 of titanium dioxide. i6.'Procedure ' " f.. ; f 6.1 EJeterniine the djy.wgightdfthe weighing bottle ft,n^ cap. Weigh to the nearest 0.1 mg, 190 to 210 nig of the Sample to be analyzed into the weighing bottle." 16.2 Dry the specimen in the open weighing bottle.for 2 h at; 105 to . 110C , Cool.in a desiccator, cap the bottle, and Weigh as rapidly as possible. Calculate the ory weight of the specimen and use in the actual calculation. 16.3 Transfer the dry specimen to a 500-mL dry, widemouth Erlenmeyer flask. Add 7 to 9 g of (NH4)2S04 and 20 mL of H2S04. Mix well, heat on a hot plate until dense white femes are evolved, and-continue the heating over a strong flame until solution is complete (usually requires fiot over 5 min of boiling) or it is apparent that the residue is-composed of Si02 or siliceous matter. Cool and, with caution, add 120 mL of water and 20 mL of HCL Bring to a boil and remove from heat. 16.4 Insert the short end ofthe delivery tube into one hole of a two-hole rubber stopper suitable for the Erlenmeyer flask. Insert a glass rod with a slight hook or collar at the bottom;end into the other hole of the stopper in such a way that the .bottom end will be near the bottom 'of1 the flask when the stopper is inserted into the; flask. Attach approxi mately .1- g ofalurnimun foil to-the bottom end offfte rod by crumpling or coiling the foil around the rod. It may be possible to use a thermometer instead of a collared.glass rod and, tfone ranging from.0 tod 50G is used, it can be usedfor determining temperature later. Insert the stoppetr, carrying the rod with the foil and the delivery tube, into the flask'in such a way that the foilwill be near the bottom of the flask at the same time that the.long end of the delivery tube will be near the bottom of a 250-mL beaker containing about'150 mL of NaHCOjsolution. . *'.;- ' 16.5 As soon as dissolution of the aluminum is complete, heat the flask to gentle boiling: for 3 to 5 min Without removingthe delivery tube froth the NaHC03 solution. Cool to about 60C, preferably by partial immersion ofthe flask in a vessel of water. The NaHC03 solution should siphon into the flask during this .coolingp giving an atmosphere of C02 Over the reduced- titanium solution; Withdraw the stopper, but, rinse the glass rod attachedcto it with a little water, catching the rinse water in the flask before(removing the stopper, rod; arid delivery tube completely. . : 16.6 Add-2 mLof NH4CN-S indicator solution and titrate immediately with ferric ammonium-sulfate solution (15.4) to a straw-eoldred end point. It is best to-add the bulk of the ferricammonium stilfate solution, at once,;,shake well, and .finish the titration drop by drop.-.. - 1 > ` r 17, Calculations 17.1 Calculate the-percent of TiOz as follows: - ` Ti2, % = (r3 x r,' k ioo)/5 ' r1 whefe: ^', , s h ' . ' ,, _ ; r V' V3 = ferric ammonium sulfate solution required for' titration of specimen, mL Tt = Ti02 equivalent of the'ferric ammonium sulfate solu tion, g/raL, and .... ...... - S' = dried specimen,: g.: 1 17f2 The results-ealculated, in accordance with 17.1 will include chromium, arsenic, andany other substance which is reduced by aluminum and subsequently oxidized' by ferric ion. However,, appreciable quantities of interfering materials are not likely to be encountered in normal, white titanium pigments. ALUMINUM OXIDE J 18/Scope,, ' " \ ./' : 18.1 This method covers the determination ofaluminum oxide in titanium dioxide pigments. 19- Reagents YZ[\] Precaution--Absolutions should .be stored in polyethylene pottles. ., ... 19; 1 Acetic Acid, glacial., - 19.2 Ammonium Acetate Solution (Buffer Solution)-- Dissolve 77 g ofammonium acetate in water, add 10 mLof glacial acetic aGid1 and dilute with,water to 1 L. 243 DUP0502 96764 D 1394 19.3 Ammonium Hydroxide (1+4)--Dilute 1 volume of concentrated ammonium hydroxide (sp gr 0.90) with 4 volumes of water. 19.4 Ammonium Phosphate, Dibasic Solution--Dissolve 150 g of (NH4)2HP04 in 700 mL of water. Adjust pH to 5.5 with HQ (1+1). Dilute with water to 1 L. 19.5 EDTA Solution (0.02 M)--Dissolve 7.45 g of disodium ethylenediamine tetraacetate dihydrate in water and dilute to 1 L. 19.6 Hydrochloric Acid (1+1)--Dilute 1 volume of con centrated hydrochloric acid (sp gr 1.19) with 1 volume of water. 19.7 Methyl Orange Indicator Solution--Dissolve 0.1 g of methyl orange in 100 mL of water, in accordance with Practices E 50. 19.8 Sodium Bisulfate Monohydrate (NaHS04 H20). 19.9 Sodium Fluoride (NaF). 19.10 Sodium Hydroxide Solution (6.25 M)--Dissolve 500 g of sodium hydroxide (NaOH) in water and dilute to 2 L. 19.11 Sulfuric Acid (1+1)--To 1 volume of water add slowly with stirring 1 volume of concentrated H2S04. 19.12 Xylenol Orange Indicator Solution--Dissolve 0.2 g of xylenol orange tetrasodium salt in 100 mL of water. Renew solutions weekly. 19.13 Zinc Sulfate, Standard Solution (0.01 M)--Dis solve 2.90 g of zinc sulfate (ZnS04- 7H20) in water and dilute to 1 L. Standardize as follows: 19.13.1 Dissolve with the aid ofheat 0.50 g of high-purity (99.8 %) aluminum wire, weighed to (hi mg, in 20 mL of concentrated HC1. Transfer to a 1-L volumetric flask and dilute to volume with water. 19.13.2 Place a lG-mL aliquot of this solution into a 500-mL Erlenmeyer flask containing approximately 90 mL of water and 3 mL of HC1. Add 1 drop of methyl orange indicator solution. Continue with step 20.4. 19.13.3 Calculate the titre of the ZnS04 solution as follows: A = (18.8955 X Wt)/V4 where A = A1203 per millilitre of ZnS04 solution, mL W, - weight of aluminum wire dissolved in 19.13.2, g, V4 = ZnS04 solution consumed in the second titration, mL, and 18.8955 - m01 TMeight f X -. 2 x mol weight of A1 20. Procedure 20.1 Fuse about 1 g of pigment weighed to 0.1 mg with 10 g of NaHS04-H20 in a 250-mL Erlenmeyer flask until the melt is clear. Use a 250-mL high-silica glass Erlenmeyer flask to prevent cracking. Do not use more sodium bisulfate than specified since excess concentrations of salt will interfere with the EDTA titration. Heat on a hot plate starting at low heat, then gradually raise the heat until full heat is reached. When the spattering has stopped and light fumes of S03 appear, heat the flask in the full flame of a Meker burner, with the flask tilted so that the fusion is concentrated at one end of the flask. Swirl constantly until the melt is clear. Avoid prolonged heating to prevent precipitation of titanium dioxide. Cool and add 25 mL of H2S04 (1+1). Heat until the ,! mass has dissolved, and a clear solution results. (If silica is 1 present, a little insoluble silica may remain.) Cool and add | 120 mL of water. j 20.2 Measure out 200 mL of 6.25 Af NaOH solution. Add j 65 mL of this NaOH solution to the sample solution while stirring constantly with a magnetic stirrer. Pour the re- ! maining NaOH solution into a 500-mL volumetric flask, j Slowly, and with constant stirring, add the sample solution to ; the NaOH solution. Police with water, cool, and dilute to " volume. (If the procedure is delayed at this point for more S than 2 h, transfer the contents of the volumetric flask to a | polyethylene bottle.) Either centrifuge for 5 min, or allow I most of the precipitate to settle out, then filter the supema- t tant liquid through a very fine filter paper until a little more | than 100 mL have been collected. 20.3 Place a 100-mL aliquot of the above solution in a I 500-mL Erlenmeyer flask; add 1 drop of methyl orange indicator solution and acidify with HQ (1+1) until the color i changes to red; add approximately 3 mL in excess. 1 20.4 Add 25 mL of EDTA solution. (If the approximate alumina level is known, use the following mathematical formula for determining the amount of EDTA to add for ; best results: 4 x % A1203 + 5 = mL of 0.02 M EDTA.) Add, " dropwise, NH4OH (1+4) until the solution color is just * completely changed from red to orange-yellow. Add 10 mL | of buffer solution and 10 mL of (NHUVHPO,, solution, boil 1 for 5 min, and cool quickly to room temperature in running 1 water. Add 3 drops of xylenol orange indicator solution. If the solution is purple, yellow-brown, or pink, bring the pH to j 5.3 to 5.7 with acetic acid. If the pH is correct, a pink color % indicates insufficient EDTA; repeat with a new aliquot, I starting with 20.3 and using 50 mL of EDTA solution in 20.4. ` -' 1 20.5 Titrate with ZnS04 solution to a yellow-brown or 1 pink end point. This titration should be performed quickly I near the end point by rapidly adding 0.2-mL increments S until the first color change occurs. This color will fade in 5 or jj 10 s, but is the true end point. This step is critical, and failure j to observe the first color change will result.in an incorrect j value. The fading end point does, not occur in the second j titration. This first titration must be greater than 8 mL of J ZnS04 solution. For most accurate work this first titration ! should require 10 to 15 mL of ZnS04 solution. j 20.6 Add 2 g of NaF, boil for 2 to 5 min, and cool in j running water. Titrate the EDTA, released from its alu- j minum complex by the fluoride, with ZnS04 solution to the 5 same end point as in 20.5. 21. Calculation 21.1 Calculate the aluminum oxide content of the pig ment sample as follows: A = (Zx DK2 x 5) where: A = percent A1203, Z = ZnS04 solution consumed in the second titration, mL T = A1203 per millilitre of ZnS04 solution, g, and S = specimen used, g. 22. Precision 22.1 Based on interlaboratory studies the following cri- 244 i DUP050296765 # D 1394 ie i should be used forjudging the acceptability of results at is r 95 % confidence level: 1)22.1.2 Repeatability--Two results obtained by the same gerator on the same sample should be considered suspect if ' differ by more than 0.22 % relative. 22.1.3 Reproducibility--Two results, each the mean of Iplicates obtained by operators in different laboratories ' iould be considered suspect if they differ by more than 162 % relative. SILICA Scope S!?3.1 This method covers the determination of silica in lium dioxide (Ti02) pigments. , S. Summary of Method 24.1 The , fusion of TiOz pigment with sodium bisulfate aves only the silica insoluble when the melt.is dissolved in Jfuric acid. To assure no loss ofthe silica the sulfuric acid is en to fuming to dehydrate the silica. The silica content is jtetermined by volatilizing the silica in the weighed filtration jjesidue with hydrofluoric acid. 5. Apparatus 25.1 Erlenmeyer Flask, 250-mL,:high silica. 25:2 Filter Paper, very fine, ashless, acid washed. 25.3 Platinum Crucible and Cover. t 254 Oven, controlled at 12CfC. 25.5 Muffle Furnace, controlled at1000 25C. ft. Reagents ; ,. 26.1 Hydrofluoric Acid (sp gr 1115)--Concentrated hydrofluoric acid (HF). - ;26.2 Sodium Bisulfate1 (NaHS04 H20). . iff ' 26.3: Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric If acid (H2S04). "ft 26.4 Sulfuric Acid (1+1)--To 1 volume ofwater add ,slowly with stiningT volume of concentrated H2S04. ' " 4 26.5 Sulfuric Acid (1+9)--To 9 volumes of water add jj! slowly with stirring 1 volume of concentrated H2S04. : p|27. Procedure 27.1 Transfer 1 g of pigment weighed to 0.1 mg to a f 250-mL high silica Erlenmeyer flask containing 10 g of NaHS04"H20. If an SiOz content in excess of 5% is expected a 0.5-g specimen of pigment may .be used to facilitate complete fusion with 10 g of NaHS04*H20. 27.2 Heat over a Meter burner, frequently swirling the flask until decomposition and fusion is complete and clear (except for SiOz). Be careful of overheating at start and of spattering ofthefusion. 27.3 Allow to cool and to the cold melt, add 25 mL of H2S04 (1+1), and heat very carefully and very slowly until the fusion is dissolved. Carefully evaporate to fumes of ^2s o _` ` a' 27.4 Cool and carefully add 150 mL of water. Pour very small amounts of water down the sides of the flask with frequent swirling of the contents to avoid overheating and spattering. Let cOol and Filter through fine ashless filter paper, using a 60 gravity fiinneL 27.5 Wash out all silica from the flask onto the filter paper with H2S04 (1+9). Police the flask carefully. 27.6 Place the filter paper in a platinum crucible and dry in a 120C oven. Heat the partly covered crucible over a bunsen burner. Avoid flaming the filter paper by heating first the cover from above and then' the. cfuOiblc from below. When the filter paper is consumed, heat at 1000C for 30 min in a muffle furnace. Copl in a desiccator arid weigh the crucible: 27.7 Add 2 drops of H2S04 (1+1) and 5 mL of HF (sp gr 1.15). Carefully evaporate to dryness, first on. a low heat hot plate to remove the HF and then over a bunsen burner to remove the H2S04. Avoid spattering, especially after re moval of the HF. 27.8 Ignite at 1000C for lO min. Cool in a desiccator and weigh the crucible'again. The difference in weight is silica: 28. Calculation 28.1 Calculate the silica content as follows: Si02, % (IT2/53) x 100. where: W2 = Si02 found, %, and; , S3 = specimen used, g. ': ,,>< 29. Precision 29.1 On the basis of an interlaboratory-test of this test method iii which six laboratories tested, in duplicate, five samples1 of titanium dioxide ranging in silica content froth 1.5 to 8,2 %, within-Iaboratory standard deviation was fourid to be 1:79 % and between-laboratories standard deviation was found tp Be 3.44'%'. Based on this! the followirig criteria: should be used forjudging the precision Sfresultsatfhe 95 ~% confidence level-- - ' 29.1. T Repeatability--Two results obtained by the same , operator should be considered suspect if they differ by mote than 5.1 % relative. 29.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by mote than 9.7 % relative. . 30. Keywords 30.1 aluminum oxide; aluminum reduction; Reductor; titanium pigment, chemical analysis Jones. 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 expreesly 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 lor revision oI 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. DUP050296766 Designation: D 1396 - 73 (Reapproved 1987)1 Standard Test Methods for Chemical Analysis of Poiy(Vinyl Butyral)1 This standard is issued under the fixed designation D 1396; 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. fl bcde--Editorial changes were made throughout, including renumbering of Sections 4 through 6 in November 1987. 1. Scope 1.1 These method!; cover procedures for the determina tion of poly(vinyl alcohol), poly(vinyl acetate), and buiyraldehyde in poly(vinyl butyral). 1.2 The procedures appear in the following order Sections . Polyvinyl alcohol) 4 Poly(vinyl acetate) 5 Butyraldehyde 6 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 Document 2.1 ASTM Standard: D1193 Specification for Reagent Water12 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 tine specifications of the Committee on Analytical Reagents, of the American Chemical Society, where such, specifications are available.3 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 file determination. 3.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specifi cation D 1193. 4. Poly(Vinyl Alcohol) 4.1 Reagents: 4.1.1 Ethylene Dichloride, technical grade. 1 These lest methods are under the'jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and arc the direct responsibility of Subcommittee EX)1.33 on Varnish and Resins, Including Shellac. Current edition approved April 27, 1973. Published July 1973. Originally published as D 1396 - 56 T. Last previous edition D ! 396 - 58. 2 Annual Book ofASTM Standards, Vols 06.03 and U.01. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. Soc., Washington, DC. For suggestions on the testing of reagents not Hsted 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.'* 4.1.2 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol, or isopropanol. 4.1.3 Potassium Hydroxide, Standard Alcoholic Solution (0.5 N)--Dissolve 33 g of KOH in methanol and dilute to 1 L. Standardize against potassium acid phthalate using phe nolphthalein indicator solution. 4.1.4 Pyridine Acetic Anhydride Reagent--Mix slowly 1000 mL of pyridine and 87 mL of acetic anhydride. Make only about a week's supply, and keep it in a brown bottle. 4.2 Procedure: 4.2.1 Transfer 2.2 g of the dry sample to a clean, dry, 500-mL glass-stoppered flask. Add 25,0 mL of pyridineacetic anhydride reagent. Insert the stopper, and heat the flask on a sand or steam bath below the boiling point for 5 `A h. Swirl gently until the sample is completely dissolved. Vent the flask occasionally during the first part of the heating period to prevent the stopper from blowing out. 4.2.2 At the end of the 5`/2-h period, add 25 mL of ethylene dichloride and shake well. Add 100 mL of water, and shake vigorously immediately aftef adding the water. Let the flask stand for */2 h. 4.2.3 Add a few drops of phenolphthalein solution and titrate with 0.5 N alcoholic KOH solution. Shake vigorously during the titration. 4.2.4 Blank--Run a blank determination on the reagents, following the same procedure as for the. sample. 4.3 Calculation--Calculate the-percentage of poly(vinyi alcohol) asfollows: Poly(vinyl alcohol), % = ([B -- V) N X 4.4]/5 where: B = KOH solution required for titration of the blank; mL, V -- KOH solution required for titration ofthe sample, mL, N -- normality of the KOH solution, and S - specimen weight, g. 5. Poly(Vinyl Acetate) 5.1 Apparatus: 5.1.1 Flask, Wide-Mouth; 500-mL capacity, equipped with a metal reflux condenser. 5.2 Reagents: 5.2.1 Hydrochloric Acid Standard Alcoholic Solution (0.5 N).. 5.2.2 Methanol: 5.2.3 Phenolphthalein Solution (10 g/L)--See 4.1.2. 5.2.4 Potassium Hydroxide Alcoholic Solution (28 g KOH/L)--Dissolve 33 g of potassium hydroxide (85 % KOH in ethyl alcohol and dilute to 1 L with methanol. This 246 DUP050296767 D 1396 feutioD is approximately 0.5 iV so standardized solution ]|l.3) may be used if desired, ft5.3 Procedure: f:5.3.l Transfer 2.15 g of the dry sample to the 500-mL Sk. Add 200 mL of methanol, measured in a graduate, ieasure from a buret 25.6 mL of KOH solution (4.2.4). influx on a sand or water bath for 2 h. 5.3.2 Rinse down the condenser and flask with a small nount of water, add a few drops of phenolphthalein lolution, and backtitrate, using 0.5 N alcoholic HC1. |* 5.3.3 Blank--Run a blank determination on the reagents, jhllowing the same procedure as for the sample, f[5.4 Calculation--^Calculate the percentage of poly(vinyl etate) as follows: HR Poly(vinyl acetate), % =[(B -- V)N x 8.6]/S' Jlsere:. K = HC1 required for back-titration of the blank, mL, HC1 required for back-titration of the sample, mL, = normality of the HQ, and = sample used, g. |. Total Butyxaldehyde 6.1 Reagents: 6.1.1 BromphenolBlue Indicator Solution--Dissolve 0.2 g of bromphenol blue indicator solution in 100-mL of meth anol, ethanol, or isopropanol. ; 6.1.2 n-Butanol. ! fghi j--The same lot of n-butanol should be used for all determi nations that are to be compared. A- ; % 6.1.3 Hydroxylamine Hydrochloride Solution (0.5 N). 6.1.4 Methanol 6.1.5 Sodium Hydroxide Standard Solution (0.5 N)-- dissolve 20 g of NaOH in water and dilute to 1 L. (Standardize against potassium add phthalate. ! 6.2 Blank Determination: 1 6.2.1 Place 50 mL of w-butanol and 50 mL of the hydroxylamine hydrochloride solution in a 500-mL ^JErlenmeyer flask, and fit by means ofthe ground-glass joint *to a 12-in. (305-mm) reflux condenser. Be sure the ground' ss joint is dry. Add a porous plate boiling chip, and reflux Iffor 2 h on a hot plate. Cool to 24 2C. 1 6.2.2 Add exactly 5 drops of bromphenol blue indicator (solution and 50 mL of methanol to the solution and titrate (with 0.5 N NaOH solution to* a green end point (Note 2). 'Run at least two blank determinations checking to within 0.5 mL of each other, titrating to the same end point at 24 2<>C (Note 3). klmn 2--The pH value of the blank and sample vary with tempera ture; ifthe temperature is raised the green end point will turn yellow and if the temperature is lowered the green end point will mm blue. The pH value of die blank changes more quickly than the pH of the sample solution for a given change in temperature. Therefore, the blank is titrated and kept at 24 2"C and the sample is titrated at the same temperature. klmn 3--The color change of the indicator will be a gradual one from yellow to green to blue. No sharp transition point will be found. Choose a point of yellow green to green coloration. A buffer solution containing 2.05 g of potassium acid phthalate 24 mL of 0.1 N H2S04, and 50 mL ofmethanol gives a color matching a blank titrated with 6.85 mL of 0.0938 N NaOH solution. The color in the buffer solution will fade out but the regular blank may be kept as a standard for the determination. 6.3 Procedurefor Analysis ofSample: 6.3.1 Transfer 2 g of the dry sample, weighed to the nearest 0.1 mg, to the 500-mL Erlenmeyer flask. Add 50 mL of n-butanol and 50 mL of hydroxylamine hydrochloride solution, and attach the 12-in. (305-mm) reflux condenser. Be sure the ground-glass joint is dry. Add a boiling chip, and reflux for 2 h. olmn 4--The resin gradually forms a milky emulsion. At this point, the reaction tends to bump and must be watched. After approximately 1.5 h the bumping lessens considerably and the mixture clears. 6.3.2 Cool, add 5 drops of bromphenol blue solution and titrate with 0.5 N NaOH solution until at least two-thirds of the expected requirement has been run in. Add 50 mL of methanol. At the first appearance of a green tinge, bring the flask to 24 2C (Note 5). Titrate to the same color as the blank (Note 6). klmn 5--The heat of neutralization changes the temperature during the titration. plmn 6--The blank may be diluted to give the same intensity of color as in the analysis ofthe sample if the percentage of butyraldehyde in all determinations is fairly constant. Otherwise, adjust tee intensity of color by tee amount of indicator present. 6.5 Calculation--Calculate the percent of total butyralde hyde as follows: .......... Butyraldehyde,% = [(V- B)N-x 1.2}/S - . where: -- V = NaOH solution required for titration of the specimen,. mL, w B = NaOH solution required for titration of the blank, mL, N = normality of the NaOH solution, and S = specimen weight, g. The American Society tor Tasting and Materials takes no position respecting We 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 We 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 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 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. ^ " j t V jSsf- W tf DUP050296768 Designation: D 1397 - 88 Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions1 This standard is issued under the fixed designation D 1397; 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. This standard has been approvedfor use by Agencies ofthe Department ofDefense to replace Method 7012.1 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. . 1. Scope 1.1 This test method covers the determination of unsaponifiable matter in alkyd resins and resin solutions. This test method is not applicable to alkyd resins containing modifying agents such as urea, melamine, phenols, roan, and styrene. 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 of regulatory limitations prior to use. For a specific hazard statement, see Note 4. 2. Referenced Document 2.1 ASTM Standard: D 1193 Specification for Reagent Water12 3. Significance and Use 3.1 The unsaponifiable matter in alkyd resins controls the properties of the final film. 4. Apparatus 4.1 Aluminum Beaker, havinga capacity of 125 mL.3 4.2 Flask and Condenser--A 200-mL Erlehmeiyer flask fitted with a water-cooled glass reflux condenser. The con nection between the flask and condenser shall be a standard 24/40 taper ground-glass joint. 4.3 Separatory Funnels--Three 500-mL capacity fitted with standard-taper, ground-glass stoppers and stopcocks. Stopcocks should be lubricated sparingly with ether-in soluble stopcock grease. Alternatively, funnels fitted with tetrafluoroethylene (TFE-fluorocarbon) stopcocks may be used. 4.4 Steam Bath. 4.5 Vacuum Drying Oven--A small, laboratory-size vacuum oven, thermostatically controlled to operate at 80 5C. A water aspirator vacuum source is satisfactory. 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 D01.33 on Varnish and Resins, Including Shellac. Current edition approved May 21, 1988. Published October 1988. Originally published as D 1397 - 56 T. Last previous edition D 1397 - 80. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Aluminum beakers. Catalog No. 2100, manufactured by the A. H. Thomas Co., W. Washington Square, Philadelphia, PA 19105, have been found satisfactory for this purpose. 5. Reagents and Materials 5.1 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.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. 5.2 Unless otherwise indicated references to water shall he understood to mean reagent water as defined by Type II of Specification D 1193. 5.3 Benzene. 5.4 Benzene-Alcohol Mixture--Mix. equal volumes of benzene and ethyl alcohol, add 2 drops of phenolphthalein indicator solution, and neutralize with 0.02. N sodium hydroxide (NaOH) solution to a persistent faint pink color. 5.5 Ethyl Alcohol (95 volume %)--Pure ethyl alcohol' or denatured alcohol conforming to Formula No. 2B of the U. S. Bureau of Internal Revenue. ' 5.6 Ethyl Ether. 5.7 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in ethyl alcohol (95.%) and dilute to 100 mL with ethyl alcohol. 5.8 pH Indicator Paper, universal type. 5.9 Sodium HydroxideSolution (50 %)--Dissolve sodium hydroxide (NaOH) in an equal weight of water. , ^ 5.10 Sodium Hydroxide, Standard Solution (0.02 N)--Prepare and accurately standardize a 0.02 N aqueous NaOH solution. 6. Procedure 6.1 Weigh by difference, from a closed container into the 200-mL Erlenmeyer flask, a portion ofresin or resin solution containing from 0.05 to 0.2 g of unsaponifiable matter (Note 1) (8 to 10 g of resin solution usually is sufficient). qrst I--The maximum specimen size is limited to 10 g of nonvolatile matter; otherwise saponification or separation difficulties may arise. The specimen should be weighed to the nearest milligram. 6.2 Add 10 mL of benzene, and warm to dissolve the sample. Add 50 mL ofalcohol, swirl gently to mix, and then add slowly 5 mL of the NaOH solution (50 %), while 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." 248 DU P050296769 # D 1397 png gently. Add 5 mL of water, attach to the condenser, allow to reflux gently on the steam bath for 2 h. 3 Remove from the heat source, cool to room temperaand wash down the condenser and joint with a few tres of water from a wash bottle. Transfer the contents ie flask to a 500-mL separatory funnel with the aid of ir from the wash bottle. Finally, rinse the flask with three inL portions of ether, adding the ether washes to the pie in the separatory funnel. Add sufficient water to ig the volume of the lower aqueous layer to 300 mL, and 10 mL of alcohol. 14 Stopper the separatory funnel, shake gently, and allow llayers to separate. Draw off the lower aqueous layer into Jll^econd separatory funnel (Note 2). Continue the- extrac' Wm.:of the aqueous layer with successive 20-mL portions ||p less than three) until a colorless ether extract is obtained, Jmbining the ether extracts in the first funnel, and using the jj|^ond and third funnels for the successive extractions. ijjjj ,, uvwx 2--If the layers do not separate easily, carefully draw off the "jdpiver, dear, aqueous layer and add 2 to 3 mL ofalcohol, by means ofa g||kt, to the ether-emulsion phases in the separatory funnel. Swirl gently ' the emulsion, and continue to draw off the lower layer. This ipdiire for breaking the emulsion may be repeated on subsequent 'jj||actions, if necessary. *6.5 Wash the final combined ether extracts with 25-mL dftions of water until the washings are neutral when tested the indicator paper or solution. Transfer the final ether portion-rwise into the 125-mL beaker containing a . boiling stone and previously weighed to the nearest 1 evaporating the ether from each portion on the steam (Note 3). (Precaution--See Note 4.) Finally, rinse the iparatory funnel with a few successive millilitres of ether, " ` ! these washes to the extract in the beaker. uyz{ 3--The metal top of the steam bath should be covered with ISclcan aluminum foil to prevent corrosion of the aluminum beaker jiipting the evaporation. |} ~ 4: Precaution--In addition to other precautions, be sure to use fjrbood. f 6.6 Evaporate the final portion of ether, then transfer the ker and its contents to the vacuum oven, previously ^heated to 80C. Heat to constant weight, allowing to cool to fom temperature in a desiccator before weighing. 6.7 After weighing, take up the residue in 50 mL of warm (approximately 50C) benzene-alcohol mixture. Titrate with 0.02 IVNaOH solution to the same persistent feint pink color as in the neutralization of the benzene-alcohol mixture (see 5.3). 7. Calculation and Report 7.1 Calculate the unsaponifiable matter as follows, and report the results to the nearest 0.1 %: F = VN x 0.280 where: F = fatty acids in extract, g, V -- NaOH solution required for titration of the res idue, mL, N = normality of the NaOH solution, and 0.280 = the factor used'for normal 18-carbon atom fatty acids. If cocoanut, lauric, pelargonic, or other short chain fatty acids are suspected or known to be present, use the arbitrary factor 0.216 in the above equation. u = [(R - Rys] x where: U = unsaponifiable matter, %, R = residue, g, and S = specimen, g. 8. Precision and Bias 8.1 On the basis of an interlaboratory study of this test method in which the within-laboratory standard deviation was found to be 0.08 % absolute and the between-laboratory standard deviation was found to be 0.11 % absolute the following criteria should be used forjudging 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, should be considered suspect if-they differ by more than 0.25 % 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 0.33 %"absolute. 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 at this standard are expressly advised that determination of the validity of any such patent rights, and the risk ef 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 orwithdrawn. Yourcomments are Invitedeither forrevision ofthisstandard 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. 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. mm DUP050296770 Designation: D 1398 - 84 1 Standard Test Method for ! Fatty Acid Content of Alkyd Resins and Aikyd Resin Solutions1 This standard is issued under the fixed designation D 1398; 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 lastVeapprovaj. A superscript epsilon (e) 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; r 1. Scope 1.1 This test method covers the gravimetric determination of the total fatty acids in alkyd resins and .alkyd resin solutions. The test method is not applicable to alkyd resins containing*, modifying agents such as urea, melamine, phenols, rosin,;and styrene. 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 arid deter mine the applicability of regulatory limitations prior to use. Specific precaution statements are given in 5.4.1 and'6.1. 2. Referenced Documents .2,1 ASTMStandards: D563 Test Method for Phthalic Anhydride Content of Alkyd Resins and Resin Solutions;12 D1193 Specification for -Reagent Water3 ... D1615 Test Methods for Glycerol, Ethylene Glycol, and , Pentaerytbritol in Alkyd Resins2,. v D2245 Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints4 3. Significance V 3.1 This test method is used to determine total fatty acid content of alkyl resins and this solution, in the absence of interfering compounds, as a means whereby the relative applicability of the alkyd resin to the particular end use may be estimated by buyer and seller. 4. Apparatus 4.1 Beakers, having capacities of 150 and 400 mL. 4.2 Desiccatorcontaining, concentrated H2S04 as. the desiccant. 4.3 Filter Paper, rapid, low-ash filter paper, to fit the filtering funnel. 4.4 Filtering Funnel, 75-mm diameter, long-stem. 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 1.33 on Varnish and Resins, Including Shellac. Current edition approved Aug. 31, 1984. Published January 1985. Originally published as D 1398 - 56. Last previous edition D 1398 - 77. 2 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vols 06.01 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.03. '<1.5 Flask, 250-mL, flat-bottom, with standard taefj| bpening. .' " .4.6 Nitroget} Gas Supply.' ' ` `, 4.7- Separatdry Funnels, three 500-mL capacity. glass^l stoppered, fitted with standard-taper`ground-glass stoppers | and stopcocks. ............................... 4.8 Steam Bath. ; 4.9 Water-Bath. 1 4. iO Vacuum Drying Oven, small, laboratory-size, flier- mostatidally controlled to operate at 60 2C. A water- aspirator vacuum source is satisfactory. 4.11 Cotton, absorbent, 'USP: .' 5* Reagents and Materials 5.1 Purity ofReagents^--Reagentgradechemicals shalibel used in'all tests. Unless otherwise indicated,'' it is intended I that all reagents', shall conforih to the specifications of die j Committee dri-Analytical Reagents of the American Cheih-1 ical Society, where such specifications are'available!5 OtKerlj grades may be used,'provided it is first asceftained thaf the I reagent is of sufficiently high purity to permit its use without 1 lessening the accuracy of the determination. I 5.2 Purity of Water--Unless otherwise indicated, refer-1 ences to Water shall be understood to mean reagent water | conforming to Type IV of Specification D 1193. .J 53-Ether, anhydrous,. j 5.4Hydrochloric Acid (sp gr 1.19)--Concentrated hydro- j chloric acid (HC1). . . .. . .---. ; :s -r . If 5.4.1 Caution--Concentrated hydrochloric acid is corrov f sive and may cause burns to the skin and eyes; the vapor is j irritating to mucous .membranes;1 Use care in handling this j acidic substance. In case of contact, flush skin or eyes with j plenty'of water while removing contaminated clothing. Call a physician. Wash clothing before reuse. See supplier's j Material Safety Data Sheet for further information. 5.5 Indicator Paper, universal-type. 5.6 Sodium Sulfate (Na2S04), anhydrous; 6. Procedure 6.1 Saponify a portion of resin or resin solution in accordance with Test Method D 563. After filtering the potassium phthalate alcoholate (6.3), transfer the combined 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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 Noslrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 250 DUP050296771 # D 1398 tee and washings to the 400-mL beaker with the aid of 25 , of water from a wash bottle. Concentrate to a volume of Iproximately 25 mL on the steam bath under a blanket of progen to prevent oxidation of the fatty acids. (Caution-- sure to use a hood.) Transfer to a 500-mL separatory and with the aid of water from a wash bottle) dilute with fater to approximately 300 mL; and add 10 mL of alcohol. 16.2 Extract the unsapoiiifiable and volatile thinners with jjccessive 50-mL portions of ether (not less than three, or ntil a colorless ether extract is obtained), combining the her extracts in the first separatory funnel and using the jther two funnels for the successive extractions (Note 1). pnally, wash the combined ether extracts with three 15-mL portions of water, adding the water washes to the main fqueous phase. Discard the combined ether extracts. J' 1--If the layers do not separate easily, carefully draw off the fewer, clear aqueous layer and add 2 to 3 mL of alcohol, by means of a jjiipet, to the ether emulsion phases in the separatory funnel. Swirl gently > break the emulsion and continue to draw off the lower layer. This procedure for breaking the emulsion may be repeated on subsequent ractions, if necessary. 6.3 Acidify the aqueous phase to a pH of approximately 2 slowly adding HC1, cooling under running tap water, hen the mixture has cooled to room temperature, extract She fatty acids with successive 25-mL portions (not less than Jthree) of ether until a colorless ether extract is obtained, jjcombining the ether extracts in the first separatory funnel ad using the other two funnels for the successive extraclitions. Wash the combined ether extracts with successive Sj.lO-mL portions of water until free of mineral acid when gjtested with an indicator paper. Discard the aqueous phase Sunless Test Method D 1615 is being followed). | 6.4 Dry the combined ether extracts in the separatory punnel by the addition of successive small quantities of ; anhydrous Na2S04. r 2--The free water has been removed when, by the addition of lii a small quantity of Na2S04 and gentle swirling, the excess Na2S04 is f- seen to disperse as a freely moving powder. 6.5 By either of the following methods, filter the ether J? extract portionwise into a tared (to 1 mg) 250-mL standard- 1 taper flat-bottom flask or 150-mL beaker, containing a small & boiling aid. b 6.6 Method A--Filter the dried ether extract, portionwise through a rapid, low-ash paper by decanting from the top opening of the separatory funnel into the appropriate re ceiver. Cover the filter flannel with a watch glass between each filtration step. & 6.7 Method B: 6.7.1 Invert the separatory funnel and open the stopcock, allowing any water in the bore of the stopcock to run back into the funnel. 3--A small amount of ether applied to and evaporated from the outside of the funnel before the cock is opened will assure that the water will drain back into the funnel. 6.7.2 Close the cock and then shake the contents of the funnel sufficiently for the Na2SQ4 to absorb all the water. If needed, add more Na2S04 and gently swirl the funnel and contents. Swab out the stem of the funnel with a piece of cotton attached to a stiff wire, 4--A small'brass screw soldered to die end of a stiff brass wire will-serve for this purposb. 6.7.3 Insert a clean plug of cotton moistened with ether into the funnel stem and filter the ether solution through the cotton plug into the appropriate receiver. 5--Experience will show how tightly packed the cotton must be to hold back the Na2S04 and still allow a sufficient flow of ether extract 6.8 Evaporate the ether portionwise from the beaker or distill it from the flask on the steam bath, in a hood. Apply a blanket of nitrogen over the beaker during evaporation. Remove the last portions of fatty acids from the Na2S04 in the funnel by washing with successive small portions of ether until a colorless extract is obtained. Remove the final traces of fatty acids from the filter paper or cotton plug by using several successive small portions of ether. 6.9 If a gas chromatographic analysis of the separated fatty acids is to be performed, observe the precautions given in 7.2 of Method D 2245. 6.10 Complete the evaporation of the fatty acid-ether solution on the steam bath, while maintaining a nitrogen atmosphere over the acids. Remove the final traces of ether by heating for successive 20-min periods in a vacuum oven at 60C until minimum weight is obtained. After each heating period, allow the beaker and contents to cool in a desiccator and then weigh to 1 mg. 7. Calculation and Report 7.1 Calculate the percent total fatty adds content, T, as follows, and report the results to 0.1 %: r_= A---s--B x 100 where: A = weight of beaker plus residue, B = weight of beaker, and S - specimen weight taken for analysis. . 8. Precision '' ~ 8.1 On the basis of an interlaboratory study, of this test method, the within-laboratory standard deviation was found to be 0.31 and the between-laboratories standard deviation was found to be 0.50. Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 8.1.1 Repeatability--Two results obtained by same oper ator should be considered suspect if they differ by more than 0.9 % absolute. 8.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 1.5 % absolute. DUP050296772 The American Society tor Testing and Materials takes no position respecting the validity ofanypatenf 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 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 forrevision 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 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., Phlladelphte, PA 19103. 252 DUP050296773 Designation: D 1439 - 83a (Reapproved 1989)L'1 Standard Test Methods for Sodium Carboxymethyicellulose1 This Standard is issued under the fixed designation D 1439; 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 die year oflast reapproval. A superscript epsiton (0 indicates an editorial change since the last revision or reapproval. e> Section 2 was added editorially subsequent sections were renumbered in November 1989. ;i These test ;methods cover the testing of sodium iaoxymethylcellulose.. : 1.2 The test procedures appear in the following order: Sections isiuie 4 to 8 4peg^e of Etherification: %-Test Method A--Acid Wash 9, 10 tb IS AT Test.Method B--Nonaqueous Titration 9,16 to 21 'jiviscosity 22 to 27 SjPunty 28 to 34 Ipaium Glycolate i 35 to 42 |gdium Chloride 43 to 49 Sfcnsity 50 to 54 f1.3 This standard may involve hazardous materials, oper- htions, and equipment. This standard does not purport to 'Address all ofthe safety problems associated with its use. It is Jp responsibility of the user of this standard- tQ establish Appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For pacific hazard statements, see Notes 1 and 2. Referenced Documents . 2.1 ASTM Standards: D1347 Test Methods for Methylcellulose12 E 1 Specification for ASTM Thermometers3 Purity of Reagents 3.1 Reagent grade chemicals shall be used in all tests. lUnless otherwise indicated, it is intended that all reagents Ishall conform to the specifications of the Committee on fAnalytical Reagents of-the? American Chemical Society, t| where such specifications are available.4 Other grades may be i 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 distilled water. 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 DO1.36 on Ceilulosics. Current edition approved June 24, 1983. Published September 1983. Originally published as D1439 - 56 T. Last; previous edition D 1439 - 83. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annua! Book a}ASTMStandards, Vol 14.03. 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., Nfew York, NY, and the "United States Pharmacopeia.'' MOISTURE 4. Scope 4.1 This test method covers the determination of. the volatile content of sodium carboxymethyicellulose. 4.2 The results ofthistestare used for calculating the total solids in the sample; and, by common usage, all materials volatile at this test temperature are designated as moisture. 5. Apparatus , 5.1 Oven--Gravity convection oven, capable*of main taining a temperature of 105 3C. 5.2 Weighing Bottles, low-form, 50-mm inside diameter by 30-mm height, or equivalent. 5.3 Analytical Balance. 6. Procedure 6.1 Weigh 3 to 5 g of the sample to the nearest 0.001 g in a tared andjcovered weighing bottle. 6.2 Place the bottle in an oven at i05CTfor 2 h with the Cover removed. Cool the bottle in a desiccator, replace the cover, and weigh. 6.3 Replace the sample in the oven for 30 min, cool, and reweigh. . --- 6.4 Continue this procedure to'a mass loss of riot more than 5 mg for 30 min drying time. 7. Calculation --- 7.1 Calculate-the percent moisture, M, as follows: M = (A]B)x 100 where: A = mass loss on heating, g and B = sample used, g. ,. (I). 8. Precision 8.1 Statistical analysis of interlaboratory test results on samples containing 2 to 10 % moisture indicates a precision of 0.2 % absolute at the 95 % confidence level. DEGREE OF ETHERIFICATION 9. Scope 9.1 These test methods cover the determination of the degree of etherification (D.E.) of sodium carboxymethyi cellulose. 9.2 Two test methods are included as follows: 9.2.1 Test Method A (Acid Wash), for crude and purified grades of sodium carboxymethyicellulose with degrees of 253 DUP050296774 # D 1439 i ; etherification up to 0.85. Above 0.85 degree ofetherification, slightly low results may be obtained. 9.2.2 Test Method B (Nonaqueous Titration), for purified grades of sodium carboxymethylcellulose of all degrees of etherification. It is not applicable to the crude grades. Test Method A--Acid Wash 10. Summary of Test Method 10.1 The water-soluble sodium carboxymethylcellulose is converted to the insoluble acid form, purified by washing, dried, and then a weighed sample is reconverted to the sodium salt with a measured excess of sodium hydroxide. 11. Apparatus 11.1 Stirrer, air-driven. 11.2 Buchner Funnel, 75-mm, fitted with a 70-mm finetexture, heavy-duty filter paper. A 60-mm medium-porosity, fritted glass fhnnel may also be used. 11.3 Drying Oven, maintained at 105'C. 12. Reagents 12.1 Diphenylamine Reagent--Dissolve 0.5 g ofdiphenylamine in 120 mL of sulfuric acid (H2SO4, 9+2). The reagent should be essentially water-white. It wiU give a deep blue coloration with traces of nitrate or other oxidizing agents. 12.2 Ethyl Alcohol (95 volume %)--Denatured ethyl al cohol conforming to either Formula 2B, 3A, or 30 of the U. S. Bureau of Internal Revenue. 12.3 Ethyl Alcohol (80 % by volume)--Dilute 840 mL of Formula 2B, 3A, or 30 denatured alcohol to 1 L with water. 12.4 Hydrochloric Acid, Standard (HC1, 0.3 to 0.5 N). 12.5 Methanol, anhydrous. .12.6 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 12.7 Sodium Hydroxide, Standard Solution (0.3 to 0.5 N)--Prepare and standardize a 0.3 to 0.5 N solution of sodium hydroxide (NaOH). 12.8 Sulfuric Acid (9+2)--Carefully mix 9 volumes H2S04 with 2 volumes of water. 13. Procedure 13.1 Weigh approximately 4 g of the sample into a 250-raL beaker and add 75 mL of ethyl alcohol (95 %). Stir the mixture with an air-driven stirrer until a good slurry is obtained. Add 5 mL of HN03, while agitating, and continue agitation for 1 to 2 min. Heat the slurry and boil for 5 min. (Warning--See Note 1.) Remove the heat and continue agitation for 10 to 15 min. 1: Warning--Exercise care to avoid fire. 13.2 Decant the supernatant liquid through the filter and transfer the precipitate to the filter with 50 to 100 mL of ethyl alcohol (95 %). Wash the precipitate with ethyl alcohol (80 %) that has been heated to 60C, until all of the acid has been removed. 13.3 Test for the removal of acid and salts (ash) by mixing a drop of the acid carboxymethylcellulose slurry from the filter with a drop of diphenylamine reagent on a white spot plate. A blue color indicates the presence of nitrate and the necessity for further washing. If the first drop of reagent does not produce a blue color, further drops should be added until an excess of reagent is known to be present, noting the color i after each drop. Four to six washings will usually suffice to " give a negative test for nitrate. j 13.4 Finally, wash the precipitate with a small amount of | anhydrous methanol and draw air through it until the ; alcohol is completely removed. Transfer the precipitate to a glass or aluminum weighing dish provided with a cover. Heat ; the uncovered dish on a steam bath until the odor of alcohol can no longer be detected (in order to avoid fires due to methanol fumes in the oven), then dry the dish and contents, uncovered for 3 h at 105C. Place the cover on the dish and ,, cool to room temperature in a desiccator. 13.5 The sulfate ash content of the sample at this point J should be less than 0.5 % when determined on 0.5 g of the sample by the procedure given in the Ash as Sulfate section i of Test Methods D 1347. If the ash content is greater than jj 0.5 %, rewash the sample with ethyl alcohol (80 %). If I necessary, repeat the procedure described in 13.1 to 13.4. 13.6 Weigh, to the nearest 0.01 g, about 1 to 1.5 g of the j dried acid carboxymethylcellulose (depending on the nor- | mality of the acid and base to be used) into a 500-mL 3 Erlenmeyer flask. Add 100 mL ofwater and 25.00 mL of0.3 | to 0.5 N NaOH solution, while stirring. Heat the solution to 1 boiling, and boil for 15 to 30 min. J 13.7 Titrate the excess NaOH, while the solution is hot, I with the 0.3 to 0.5 N HCI to a phenolphthalein end point. J 14. Calculation j 14.1 Calculate the degree of etherification, G, as follows: A = (BC -- DE)/F - ' (2>.,; G = 0.162,4/(1 - 0.058,4) (3) where: A = milliequivalents of acid consumed ` per gram of sample, B = NaOH solution added, mL, -- C -- normality of the NaOH solution, . !j D = HCI required for titration of the excess NaOH,- mL, I E -- normality of the HCI, I F = acid carboxymethylcellulose used,, g, -j 162 = gram _molecular mass of the anhydtoglucose unit of f cellulose, and , J 58 = net increase in molecular mass of. anhydroglucose i unit for each carboxymethyl group substituted. * 1 f 15. Precision j 15.1 The precision of this test method is estimated to be 3 0.03 D.E. units. Test Method B--Nonaqueous Titration 16. Summary of Test Method 16.1 This measurement is based upon a nonaqueous acid-base titration. The sample is refluxed with glacial acetic acid, and the resulting sodium acetate is titrated with a standard solution of perchloric add in dioxane, to a potentiometric end point. Impurities containing alkaline sodium will also be titrated under these conditions. Sodium chloride does not interfere. ;j { j 254 DU P050296775 D 1439 ^Apparatus J7.1 pH Meter, equipped with a standard glass electrode P'a calomel electrode modified as foEows: 17.1.1 Discard the aqueous potassium chloride solution, fn rinse and fill with the calomel electrode solution as 11 eribed in 18.2. 117.1.2 Add a few crystsils of potassium chloride and silver jfjoride or silver oxide to the electrode. |7.2 Buret, micro, 10-mL capacity. JgUj. Reagents 8.1 Acetic Acid, glacial. 8.2 Calomel Electrode Solution--Add 2 g of potassium bride (KC1) and 2 g of silver chloride (AgCl) or silver ide (Ag20) to 100 mL of methanol and shake thoroughly ^saturate. Use the supernatant liquid. 18.3 1,4-Dioxane.5 18.4 Perchloric Acid (0.1 N)--Add 9 mL of concentrated erchloric acid (HC104,70 % to 1 L ofdioxane, with stirring 'aiming--See Note 2). Store in an amber glass bottle. Any it discoloration that appears on standing may be disre- ded. i 2: Warning--The solution of perchloric acid in dioxane IJiould never be heated or allowed to evaporate. 18.4.1 Standardize the solution as follows: Dry potassium lacid phthalate for 2 h at 120C. Weigh 2.5 g to the nearest 10.0001 g into a 250-mL volumetric flask. Add glacial acetic rid, shake to dissolve, and then make up to volume and mix [thoroughly. Pipet 10 mL into a 100-mL beaker and add 50 jnL of acetic acid. Place on a magnetic stirrer and insert the electrodes of the pH meter. Add nearly the required amount |of HC104 from a buret, then decrease the increments to 0.05 fmL as the end point is approached. Record the miUihtres of titrant versus millivolts, and continue the titration a few ; millilitres beyond the end point. Plot the titration curve and I read the volume of titrant at the inflection point. Calculate t the normality, N, as follows: : 1V=(AX 10 X 1D00)/(B x 204.22 x 250) (4) j. where: A = potassium acid phthalate used, g, B - HC104 added, mL, .* 204.22 = gram molecular mass of potassium acid phthalate, 10 = potassium acid phthalate solution added, mL, and 250 = glacial acetic acid used to dissolve potassium acid i* phthalate, mL. 18.5 Potassium Acid Phthalate, primary standard, Na tional Institute of Standards and Technology Standard Sample No. 84. 19. Procedure 19.1 Weigh 0.2 g of the sample, to the nearest 0.0001 g, into a 250-mL Erlenmeyer flask with ground-glass joint. Add 75 mL of acetic acid, connect to a water-cooled condenser, and reflux gently on a hot plate for 2 h. 19.2 Cool, and transfer the solution to a 250-mL beaker 5 1,4-Dioxane available as Eastman Kodak Catalog No. 2144 or Mateson, Coleman, and Bell Catalog No. CB 368 has been found satisfactory for this purpose. with the aid of 50 mL of acetic arid. Place on the magnetic stirrer and titrate to a potentiometric end point with 0.1 N HC104 in accordance with 18.4. 20. Calculation 20.1 Calculate the degree of etherification, H, as follows (Note 3): M = (AN x 100)/(G x (100 - B)) H = 0.162 M/(\.000 - (0.080 M)) (5) <6) where: M = milliequivalents of acid consumed per gram of sample, A = HQ04 added, mL, N = normality of HCIO4, . G = sample used, g, B = percent moisture, determined on a separate sample, in accordance with Sections 4 to 7, 162 = gram molecular mass of an anhydroglucose unit of cellulose, and 80 = net increase in molecular mass of an anhydroglucose unit for each sodium carboxymethyl group added. 3--The result calculated in accordance with Section 18 in cludes the alkaline sodium from sodium glycoiate; however, ifthe latter is less than 0.5 %, the interference is negligible. 21. Precision 21.1 Statistical analysis of interlaboratory test results indi cates the precision of this test method as shown below: Approximate D.E. Level 0.40 0.80 1.35 Precision, D.E. Units (95 % Confidence Level) 0.010 0.012 0.038 VISCOSITY 22. Scope ~~ _ ' 22.1 This is an arbitrary test method for determining the viscosity of aqueous solutions of sodium carboxymethyl-.. cellulose in the viscosity range from lOto 10 000cPat25C. 22.2 The concentration to be used for the test should be agreed upon between the purchaser and the seller. It should be such that the viscosity of the solution will fall within the range of this test. 22.3 The results for the viscosity of sodium carboxymethylcellulose by this test method will not necessarily check with results from other types of instruments used for viscosity measurements. 22.4 The determinations are run on a calculated dry basis; that is, the amount of sodium carboxymethylcellulose re quired for the desired concentration on a dry basis is calculated from the known moisture content. 22.5 This test method is intended for referee purposes. The Brookfield spindles and speeds given in Table 1 are recommended for this purpose, but slight derivations from the table may occasionally be found convenient for indi vidual application. DUP050296776 TABLE 1 Viscometer Spindles Required for Given Speeds Viscosity Range, cP 10 to 100 100 to 200 200 to 1000 1000 to 4000 4000 to 10000 Spindle No. 1 i 2 3 4 Speed, rpm 60 30 30 30 30 Scale 100 100:. 100 100 100 Factor 1 2 10 40 200 23. Apparatus 23.1 Viscometer, Brookfield type.6 23.2 Container--Glass jar, approximately 2%-in. (60mm) in diameter and 5`A in. (133 mm) deep, uncqnstricted at the top, capacity 8 oz (2.3 m3). 23.3 Analytical Balance. 23.4 Mechanical Stirrer--Stirrer constructed of either stainless steel or glass (Fig. I)7 attached to a variable speed motor capable of operating at 800 100 rpm under varying load conditions. 23.5 Water Bath, constant-temperature, set at 25C and capable of maintaining that temperature within 0.2C. 23.6 Thermometer--ASTM Saybolt Viscosity Thermom eter having a range from 19 to 27C and conforming to the requirements for Thermometer 17C, as prescribed in Speci fication El. 24. Procedure 24.1 Determine moisture in accordance with Sections 4 to 7. . 24.2 Calculate the dry-basis sample mass, M, in grams necessary to make 240 g of test solution as follows: M= 100A/(100 - B) (7) where: A = desired dry mass of sample, g, and B = moisture in the sample as received, %. 24.3 Calculate the quantity of distilled water required as follows: V = 240 - 5 (8) where: V = volume of distilled water, mL, and 5 = mass of sample, g. 24.4 Add the calculated quantity of water to the jar. Position the stirrer in the jar allowing minimum clearance between the stirrer and the oottom of the container. 24.5 Begin stirring and slowly add the sodium carboxy- methylcellulose specimen. Adjust the stirring speed to ap proximately 800 100 r/min and mix for exactly 2 h. Do not allow the stirring speed to exceed 900 r/min since higher speeds tend to affect viscosity on certain grades of sodium carboxymethylcellulose. A--If the specimen is added too rapidly, agglomeration will occur. This may prevent complete dissolution within the required mixing time. 6 Model LVG, Brookfield Engineering Laboratories, Inc., Stoughton, MA or equivalent, has been found satisfactory for this test method. 7 Stirrers made with t'/a-in. three-bladed propellets available from A. H. Thomas Co., P.O. Box 779, Philadelphia, PA 19105, Catalog No. 9240K have also been found satisfactory for this purpose. PROPELLERS-4 5' PITCH, DOWNDRAFT In. mm In. ~~ mm Vie 1:5 442 7 % 3 " Vie ' 7.9 Vie 4a 94 15.8 14 6.4 IVa 36 914 an FIG. 1 Stirrer Blade 24.6 Remove the stirrer and transfer the specimen con tainer to tiie'constant-temperature bath for 1 h, Check the specimen temperature with a thermometerjit the end-of 1 h to ensure that the test temperature has been reached. 24.7 Remove the specimen container from the bath and shake vigorously for 10 s. Measure the viscosity with the Brookfield viscometer, selecting the proper spindle and speed from Table 1. Allow the spindle to rotate until a constant reading is obtained. 25. Calculation 25.1 Calculate the viscosity, V, in centipoises as follows: V = reading x factor (9) 26. Report 26.1 Report the results as Brookfield viscosity at 25 C, stating the solution concentration and the spindle and speed used. 27. Predsion 27.1 The difference between the average of the results 256 DUP050296777 # D 1439 ,obtained by a given operator using a given viscometer and ' average of the results obtained by a different operator ' u^ing a different viscometer should not exceed 10 % of the Kean of the averages. PURITY OF CRUDE SODIUM CARBOXYMETHYLCELLULOSE 8. Scope 28.1 This test method covers the determination of purity |py percent of active ingredient in crude sodium carboxy- Sethylcellulose containing no phosphate. The test method is been standardized on materials having a degree of | etherification of about 0.85 or less. 28.2 For determination of purity of refined sodium carjboxymethylcellulose (purity approximately 98 % or higher), { analysis for individual or combined impurities and calcula tion of purity by difference will give more reliable results. i 29. Summary of Test Method 29.1 A 3-g sample is stirred mechanically in a beaker for 15 min with each of two 150-mL portions of ethanol (80 % ll)y volume) at a temperature of 60 to 65'C. The supernatant S liquid is decanted through a tared filtering crucible after each treatment The undissolved matter is transferred quantita! tively to the 'crucible, dried, weighed, and calculated as percent of sodium carboxymethylcellulose. The temperature of the ethanol during the leaching need not be closely controlled, but the concentration of the ethanol must be closely controlled (sp gr within 0.001). 30. Apparatus 30.1 Filtering Crucible, fritted glass, medium-porosity, 50-mL capacity. 30.2 Mechanical Stirring Motor, electric or air-driven, with any convenient stirrer of appropriate size. 30.3 Water Bath, constant-temperature, maintained at 60 to 65*C. 30.4 Cover--A lid to keep a 400-mL beaker substantially covered during mechanical stirring in bath. A flanged lid, preferably of stainless steel, with a slot, wide enough to pass the shaft of the mechanical stirrer, cut from the rim to the center, has been found satisfactory. The center should be cut out somewhat larger than the shaft of the stirrer to permit free rotation of the stirrer. Such a lid serves to weight down the beaker as well as to minimize the evaporation losses during leaching. 31. Reagents 31.1 Ethanol (95 volume %)--Undenatured or specially denatured ethanol conforming to Formula 2B (Note 5) of the U. S. Bureau of Internal Revenue. 5--Other grades of denatured alcohol, such as Formula 3A, are not satisfactory for this purpose, 31.2 Ethanol (80 volume %)--Dilute 840 mL of 95 % ethanol (30.1) to 1 L with water. The specific gravity should be 0.857 0.001 at 25/25C. If necessary, add water or 8 Coming No. 416120 available from A. H. Thomas Co., P. 0. Box 779, Philadelphia, PA 19105, Catalog No. 4142-C50M, has been found satisfactory for this purpose. ethanol until the specific gravity is within the specified limits. 31.3 Ethyl Ether, anhydrous, ethanol-free. 32. Procedure 32.1 Weigh 3 to 5 g of the sample into a tared low-form, 65-mm diameter glass weighing dish fitted with a cover. Dry to constant mass at 105 l'C in either a gravity or a mechanical convection oven. Weigh at the end of an initial 2-h heating period, then continue with 30-min heating periods until the change in mass during a 30-min heating period is not more than 0.10 %. If there is an increase in mass of the sample during one or more drying periods, record the lowest mass observed as the mass for use in the calculation of moisture content. Calculate the loss in mass as the percent of moisture in the sample. 32.2 Weigh 3 0.1 g of the sample, in the "as-received" condition, to the nearest 0.001 g and transfer to a 400-mL beaker. 32.3 Add 150 mL of ethanol (80 %) that has been heated to between 60 and 65'C, and immediately place the beaker in a constant-temperature water bath maintained at 60 to 65'C. The level of the water in the bath should be somewhat higher than the level of the liquid in the beaker. Cover the beaker as completely as possible with a lid that wifi permit mechanical stirring. Lower a mechanical stirrer almost to the bottom of the beaker, and stir for 10 min at a rate suitable to provide good agitation without spattering material on the walls of the beaker above the liquid level. 32.4 Stop the stirrer. Allow the undissolved matter to settle with the beaker still in the bath, and then decant the hot supernatant liquid as completely as possible through a tared, fritted-glass filtering crucible. 32.5 Add 150 mL of ethanol (80 %), at 60 to 65'C to the beaker and proceed in accordance with 32.3 and 32.4. 32.6 After decanting the supernatant liquid as completely as possible, transfer the insoluble matter to the crucible with the aid ofethanol (80 %) at 60 to 65C in a wash bottleJjeing careful tp; scrape all insoluble matterfrom the lid, the stirrer, and the beaker. A total of about 250 mL of ethanol (80 %) will normally be required to transfer the insoluble matter to the crucible and to further wash the insoluble matter in the crucible. During the operations prescribed in this paragraph, apply suction only while filtration is in progress. Make every effort to avoid drying-out of the filter cake. If fines appearto pass through the filter, use only gentle suction. 32.7 Wash the residue in the crucible with 50 mL of ethanol (95 %) at room temperature, and finally with several portions of ether at room temperature (Note 6). Without permitting suction to continue longer than necessary, place the crucible in a beaker or weighing bottle on the steam bath until no odor of ether can be detected. 6--Thorough washing with ether is necessary to remove ethanol completely from the insoluble matter. If ethanol is not com pletely removed before oven drying, it may not be completely removed during the oven drying. 32.8 Place the crucible in an oven at 105 l'C for 1 h. Stir the contents of the crucible with a dissecting needle or thin rod (preferably of smooth-surfaced metal) to break up the cake and facilitate complete drying. Again, dry at 105 l'C for 1 h. Place the crucible in a desiccator. Cover it with a flat glass plate, weighing bottle tover, or other suitable cover DUP050296778 0 D 1439 to minimize absorption of moisture from the atmosphere in the desiccator; and cool to room temperature (at least 30 min). Weigh the uncovered crucible as rapidly as possible. 32.9 Dry the crucible for additional 1-h periods, until the change in mass during a 1-h drying period does not exceed 0.003 g.. If increases in mass , aye observed after such additional drying periods, record the lowest muss observed as the mass of the cruoible plus dry sodium carbpxymethylcellulose. 33. Calculation 33.1 Calculate the percent jqdium ; carboxymethylcellulose^iS, on the dry basis as follpws: S=* (Ax 10 000)/CB (100 ^ C)) ' (10) where: `V A = masS of dried residue, g, B = mass of specimen used, g, and C = moisture in the specimen as received, %, 34. Precision '' 34.1 Statistical analysis of interlaboratory test results indi cate a precision of 0.6" % absolute at the 95 % confidence level. SODIUM GLYCOLATE - 35. Scope . -.,,_i. 35.1 This test method covers the determination:of the sodium glycolate content of purified sodium carboxymethylcellulose containing not mote than 2.0'% sodium giycoMe; the dried material, dissolve in water, and make up to volume in a 100-mL volumetric flask. This solution will contain l mg of glycolic acid/mL. The solution is stable for approxi mately 1 month. 38.5 Sodium Sulfate (Na2S04), 38.6 Sulfuric Add (sp gr 1.84)-r-Concentrated H2S04. 39. Preparation of Calibration Curve 39.1,Into a series of fiy,e 100-mL volumetric flasks accu rately introduce 1,2, 3, and 4-mL aliquots ofthe standard glycolic acid solution, reserving the( fifth flask for a blank.. Add'sufficient water to each Jflask.to give a total volume of 5 mL. Add 5 idL of glacial acetic add, make up'to volume with acetone and mix. Thesepolptions will contain'Q, 1, .2,3 and 4 mg of glycolic, acid, respectiveiy. . 39:2 Pipe! 2 mL ofeach ofthese solutions iqto individual 25-xpL yplumetric flasks. Place the uncovered flasks upright in a boiling water bath for exactly 20 mm to remove the acetone. Remove the flasks from the bath and pool... 39.3 To each flask add 20 mL of 2,7-dihydroxy naphtha- fen'e reagent as' follows; Add 5 mL of reagent initially, mix thoroughly, then add the remaining 15 mL of reagent, and mix. CSver tlife mouth of the flasks wit|i a small piepe of aluminum foil and place upright in the boding water bath'for 20 min. Reniove from the bath, cool,' apd make up to volume with H2SO4. ' '.. 39.4 Measure the absorbance of each .solution at 540 pm against the blank solution. Plot the milligrams of glycplic acid in the original 100 mL bf solution against absorbance to give a calibration curve. " * '>: I 36. Summary of Test Method. 40. Procedure 36.1 The sodium carboxymethylcellulose is dissolved in 40.1 Weigh" about 0.5 g of the sample (0.2 g for I acetic acid (50 %), precipitated with acetone and sodium semirefined grades) to the nearest 0.001 g and transfer to a 1 sulfate and the insoluble material'filtered off. 'The filtrate 1 d0-mL b&aker. Moisten the specimen thoroughly with 5 mL I containingthe sodium glycolate (as glycolic acid) is treated to of acetic acid followed by 5mL of water, and stir with a glass remove the acetone and reacted with 2,7-dihydroxy naphtha rod until 'solution is complete (usually about 15 fiain . is lene. The resulting; color is measured at; 540 nm'with'a required). Slowly add 50 mL. of acetone, stirring during spectrophotometer calibrated with knovVii solutions' / adchti'ony fdllowld by approximately 1 g ofNa,Cl. Stir several minutes't6 ensure complete precipitation'of tHe carfroxy- y. 37. Apparatus j mefhylceiiuiose./ ` 37.1 Spectrophotometer or Filter Photometer, suitable for 40.2 FilWbhtough a soft,' open-tbxture i^per, previously measuring absorbance at 540 nm. wetted with a' small amount pf acetone, and collect the 3T.2 Absorption Cells, for spectrophotometer, 1-cm light filtrate in a 100-mL'volumetric flask:. Use an additional 30, i! path. : r mL of acetpne'to facilitate transfer of the solid? and to wash 37.3 Aluminum Foil--Cat to approximately 2-in. (51mm) squares. the filterca'ke. Make up to volume with acetone and mix.' 40.3 Prepare a blank solution containing 5 mL of water and 5 mL of glacial acetic acid in another 100-mL volu 38. Reagents 38.1 Acetic Acid, glacial; 38.2 Acetone. 38.3 Dihydroxy Naphthalene Reagent (0.100 g/L)--Dis solve 0.100 g of 2,7-dihydroxy naphthalene in 1 L of sulfuric acid (H2S04). Before using, allow the solution to stand until the initial yellow color disappears. If the solution is very dark, discard it and prepare a new solution from a different metric flask. Make up to the mark with acetone and mix. 40.4 Pipet 2 mL of the solution from be'speciinen and .2 mL of be blank solution into separate 25-mL volumetric flasks. Develop the color and measure the absorbance in accordance with 39.2 to 39.4. 40.5 Using be observed absorbance, refer to the calibra tion curve and read the corresponding milligrams of glycolic acid. supply of H2S04. This solution is stable for approximately 1 month if stored in a dark bottle. 38.4 Glycolic Acid, Standard Solution (l mg glycolic acid/mL)--Dry several grams ofglycolic acid in a desiccator 41. Calculation 41.1 Calculate the percent sodium glycolate content, C, as follows: at room temperature overnight. Accurately weigh 0.100 g of C=(Bx 12S)!{WX (100 -- A)] (H) 258. j DUP050296779 D 1439 here: = glycolic acid, read from the calibration curve, mg, = sample used, g, = moisture in the sample as received, %, and 2.9 = (gram molecular mass of sodium glycolate per gram molecular mass of glycolic acid)x 10. ' i2. Precision 42.1 Statistical analysis of intralaboratory data on ihatefeal containing less than 0.50 % sdd^tiift'&ycbfete indicate a decision of Q;03 % absolute at the 95 % confidence level. SODIUM CHLORIDE 3. Scope r-M 43.1 This test method covers the determination of the i sodium chloride content of purified sodium carboxymethyljlellulose. 44. Summary of Test Method 44.1 The sodium carboxymethylcellulose is dissolved in jwater and titrated with a standard solution of silver nitrate to fa potentiometric end point. Hydrogen peroxide is added to | reduce the viscosity of the solution. 45. Apparatus 45.1 pH Meter, equipped with a silver electrode and a mercurous sulfate-potassium sulfate electrode. I 45.2 Buret, micro, IO-mL capacity. 46. Reagents 46.1 Hydrogen Peroxide (SO mass %)--Concentrated hy drogen peroxide (H202). 46.2 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 46.3 Silver Nitrate, Standard Solution (0.1 N)--Dissolve 17.0 g of silver nitrate (AgN03) in 1 L of water. Store in an amber glass bottle. Standardize the solution as follows: 46.3.1 Dry the sodium chloride (NaCI) for 2 h at 120C. Weigh 0.65 g to the nearest 0.0001 g, into a 250-mL beaker and add 100 mL ofwater. Place on a magnetic stirrer, add 10 mL of HN03, and insert the electrodes of the pH meter. Add nearly the required amount of AgN03 solution from a buret, then decrease the increments to 0.05 mL as the end point is approached. Record the millilitres oftitrant versus millivolts, and continue the titration a few millilitres beyond the end point. Plot the titration curve and read the volume oftitrant at the inflection point. Calculate the normality, N, as follows: 7V= (A x l000)/(fl X 58.45) (12) where: A = NaCI used, g, B = AgN03 solution added, mL, and 58.45 = gram molecular mass of NaCI. 46.4 Sodium Chloride (NaCI).47 47.Procedure 47.1 Weigh 5 g of the sample, to the nearest 0.0001 g, into a 250-mL beaker. Add 50 mL of water and 5 taL of H202 (30 %). Place the beaker on a steam bath, stirring occasion ally to achieve a nonviscous solution. If solution is not complete after 20 min, add 5 mL more of H202 and heat until solution is complete. "47.2 Cool the beaker, add 100-mL of water .and 10 mL of HN03. Place it on the magnetic stirrer and titrate to a potentiometric end point with 0.1 N AgN03 solution in 46.3. 48. Calculation 48.1 Calculate the percent sodium chloride content, C, as -follows: >- C = {AN x 584.5)/[<r X (100 5)1 (13) where: A = AgN03 solution added* mL, N = normality of AgN03 solution, G = sample used, g, B = moisture, determined on a separate sample, %, in accordance with Sections 4 to 7, and 584.5 < gram molecular mass of NaCI x 10. 49. Precision 49.1 The precision of this test method is estimated to be 0.05 % absolute for material containing less than 0.50 % sodium chloride and 0.10% absolute for material con taining greater than 0.59 % sodium chloride. DENSITY 50. Scope 50.1 This test method covers the determination of the bulk density of sodium carboxymethylcellulose. 51. Summary of Test Method 51.1 A weighed amount of sodium carboxymethyl cellulose is transferred to a 250-mL graduated cylinder and the graduate vibrated to settle the powder. 52. Apparatus ....... 52.1 Vibrator--A magnetic-type electrie-vibrator attached to the vertical support rod of a ring stand approximately 1 ft (0.3 m) above the base. A condenser clamp of sufficient size to hold a 250-mL graduated cylinder also shall be attached to the above rod. The base of the stand should be weighted. 53. Procedure 53.1 Place 50.0 g of sodium carboxymethylcellulose in a 250-mL graduated cylinder and place it in the condenser clamp. Turn on the vibrator and allow the cylinder to vibrate for 3 min. Record the level (in millilitres) to which the specimen has compacted. 53.2 Alternatively, the specimen may be compacted man ually. Tap it on a hard surface by dropping the cylinder repeatedly from a height of about 1 in* (25 mm) until the volume of the specimen remains constant. In order to prevent cylinder breakage, cover the tapping surface with a */s to `A-in. (3 to 6-mm) thick rubber sheet or use a plastic graduated cylinder. DUP050296780 <|) D 1439 54. Calculation 54.1 Calculate the density, D, in grains per millilitre as foHows: D = 50/r where: f " observed reading, mL. TheAmerican Society lor Testing and Materials takes im position respecting the validity ofany patent rights asserted in connection with any Item mentioned In thls 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 sublect to revision at any time by the responsible technicalcommittee and must be reviewed every five years and Ifnot revised, eitherreapproved or withdrawn. Your comments are Invitedeither tor revision ofthlsstandard 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. It you feel that your comments have not received s fair hearing you should make your I v/eivs known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103. 1 (14) DUP050296781 Designation: D 1469 - 73 (Reapproved 1988)1 Standard Test Method for Total Rosin Acids Content of Coating Vehicles1 This standard is issued under the fixed designation D 1469; 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 revision or reapproval. !>- l Note--Editorial changes were made throughout in May 1988. i Scope 0 This test method.' covers the determination of total frosin acids content of rosin esters, varnishes, and alkyd resins, unmodified by such materials as maleic or fumaric acid, or phenols. Total rosin acids determined include free 5 rosin, esterified rosin, and metallic salts of rosin. 1.2 This test method is priniarily designed for material ' containing 0.5 to 5 % rosin on the nonvolatile basis. 1.3 This standard may involve hazardous materials, operTations, '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: D1193 Specification for Reagent Water12 D1259 Test Methods for Nonvolatile Content of Resin Solutions3 D1644 Test Methods for Nonvolatile Content of Var nishes4 ' 3. Summary of Test Method 3.1 The specimen is saponified with potassium hydroxideethylene glycol reagent and acidified with hydrochloric acid. Heat is applied-to hydrolyze metallic driers. This is neces sary, especially when metallic rosinates are present. 3.2 The mixture described in 3.1 is extracted with ben zene (Note l). The rosin and fatty acids and urisaponifiables pass into the benzene layer. The aqueous layer will contain certain dibasic acids, polyhydric alcohols, and other watersoluble products of saponification. 1--While it has not been evaluated for this procedure, toluene has been found to be an acceptable alternative in similar procedures. 3.3 The benzene is removed,by evaporation, the residue weighed, and the rosin acids are determined by a selective 1 This test method is under die jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and & the direct responsibility of Subcom mittee DO i .33 on Varnish and Rosins, Including Shellac. Current edition approved July 27, 1973. Published October 1973. Originally published as D1469 - 57. Last previous edition P.1469 - 70. Discontinued under 3-year tentative rule 1969. Reinstated and adopted as standard in 1970. 1 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book, ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vo! 06.01. esterification and titration method.5 4, Apparatus 4.1 Air Condenser, 30 in. (760 mm), with a 24/40 standard-taper joint. 4.2 Buret, automatic type, having a capacity of 25 mL, for the standard potassium hydroxide solution, fitted with sodalime traps to protect against absorption of atmospheric carbon dioxide (C02). 4.3 Erlenmeyer Flasks, 250 and 500-mL capacity, with 24/40 ground joint. 4.4 Separatory Funnels, three of 1-L capacity. 4.5 Steam Bath, located in a fume hood, for evaporation of volatile solvents. 4.6 Moisture Collection Trap, constructed according to details shown in Fig. 1. Wrap with `/2-in. (12.7-mm) asbestos tape. 4.7 Pipet, automatic, 50-mL capacity. - 5. Reagents and Materials 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,- Other grades may be used, provided, it is firsLascertained 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 as defined by Type II of Specification D 1193. 5.3 Benzene--(Toluene may be an acceptable substitute, see Note 1.) 5.4 Butyl Alcohol-Sulfuric Acid Esterification Reagent-- Add 500 mL of n-butyl alcohol, 500 mL of benzene, and 3.3 mL (6 g) of sulfuric add (H2S04) to a 2-L round-bottom s Linder, A., and Persson, V., "Determination of Rosin Adds in Mixtures with Fatty Acids," Journal, Am. Oil Chemists' Soc., Vol XXXIV, No. I, 1957, pp. 24-27. 6 Pipets obtainable from the Arthur H. Thomas Co., W. Washington Square, Philadelphia, PA 19105 Catalog No. 8212, or from the Scientific Glass Apparatus Co., Catalog No. JP-6000, have been found satisfactory for this purpose. 7 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." DUP050296782 D 1469 TABLE 1 Precision Between Runs Between Days Degrees of freedom Standard deviation 95 % confidence range 17 6.054 0.12 11 0.062 0.11 Between Labs 4 0.166 0.46 FIG. 1 Moisture Collection Trap flask with ground joint, connect to a moisture trap and condenser, and reflux on a hot plate for 30 min to distill out the water and to form butyl-sulfuric acid. Cool and store in a glass-stoppered bottle. 5.5 Ethyl Alcohol, conforming to formula No. 30 or No. 3A of the U.S. Bureau of Internal Revenue. 5.6 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 5.7 Potassium Hydroxide-Ethylene Glycol Solution (132 g/L)--Dissolve 132 g of potassium hydroxide (KOH) pellets in 1 L of ethylene glycol in a 2-L Erlenmeyer flask. Insert a thermometer and boil to eliminate water until the tempera ture of the liquid reaches 190 to 195C. Cool and store in a rubber-stoppered bottle. 5.8 Potassium Hydroxide, Alcoholic Standard Solution (13.3g/L)--Dissolve 13.3 gofKOH pellets in 1 Lof alcohol. Standardize against potassium acid phthalate primary standard. 5.9 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid <H2S04). 5.10 Thymol Blue Indicator Solution (10 g/L)--Mix 1 g of thymol blue indicator with 100 mL of ethyl alcohol.6 6. Procedure 6.1 Transfer to a 500-mL Erlenmeyer flask an amount of sample, weighed to the nearest 0.001 g, containing approxi mately 10 1 g of nonvolatile material (Note 2). Add 150 mL of the potassium hydroxide-ethylene glycol solution and swirl to disperse the sample. Add a boiling stone, attach a condenser, and reflux on a hot plate for 2 h. --Determine the nonvolatile content in accordance with either the foil method given in Test Methods D 1259 or the varnish method given in Test Method D 1644. , 6.2 After refluxing, remove the flask from the hot plate and cool to room temperature under tap water. Add 100 mL of water, and while cooling under tap water, add 40 mL of HQ. Place on the hot plate again, reflux for 5 min, and cool under tap water. 6.3 Transfer the sample quantitatively to a 1-L separatory funnel with the aid of a total of 150 mL of water, followed by two 25-mL rinses with benzene. Shake, allow the layers to separate, and draw off the lower aqueous layer into a second 1-L separatory funnel. Extract the aqueous layer with a second 50-mL portion of benzene, and drain the aqueous layer into a third 1-L separatory funnel. Extract with a third 50-mL portion of benzene. Draw off and discard the water layer. Combine the benzene extracts, and wash with three 50-mL portions of water. Measure the pH ofjhe third water wash. If it is less than 3.8, repeat with a fourth water wash. Discard the wash waters. 6.4 Transfer the washed benzene extract to a weighed (to the nearest 0.001 g) 25Q-mL Erlenmeyer flask, with the aid of 25 mL ofbenzene. Evaporate the benzene on the steam bath, preferably with the aid of a gentle stream of inert gas to a volume of approximately 20 mL. Add 5 mL of anhydrous ethyl alcohol and evaporate to dryness, to remove any water present by azeotropic distillation. .- 6.5 Cool and weigh to the nearest`0.001. g. -To avoid oxidation, do not dry in an oven; also, the retention of a small amount of benzene does not affect the, final calcula tion. .- ' 6.6 Using an automatic pipet, accurately measure 50 mL of the esterification reagent into the flask. Connect the flask to the moisture collection trap and condenser, place on a hot plate, heat to boiling, and reflux for 20 min. At the end ofthe heating period, allow the flask to cool somewhat, then remove and cool to room temperature. 6.7 Add 10 drops of thymol blue indicator solution and titrate with the alcoholic KOH solution to a blue end point. 6.8 Make a blank titration on 50 mL of the esterification solution, after refluxing it in the same manner. 7. Calculation 7.1 In order to apply properly the esterification correction factors to the isolated rosin acids-fatty acids mixture, it is necessary first to calculate the percent of rosin acids in the dried benzene extract, Y, and then to convert this value to the nonvolatile sample basis as follows (Note 3): 262 DUP050296783 [{A - B)Nx 30.24 x 1.018]/5-0.3 alcoholic KOH solution required for titration of the sample, mL, alcoholic KOH solution required for titration of blank, mL, normality of the KOH solution used, dried benzene extract, g, molecular weight of abietic acid multiplied by 100 and divided by 1000, experimentally determined factor to correct for the slight esterification of rosin acids, and experimentally determined factor to correct for unesterified fatty acids. V = (S X Y)/(W X T) = rosin acids in alkyd vehicle, nonvolatile basis, %, = original alkyd vehicle taken for analysis, g, = nonvolatile content of the vehicle, (Note 2) expressed as a decimal, and = dried benzene extract, g. 3--If it is desired to express the total rosin acids as "com mercial rosin," use 35.0 instead of 30.2 as the factor in the calculation. 7.2 Report the results to one decimal place. 8. Precision 8.1 On the basis of an interlaboratory study of this test method in which one operator in four laboratories analyzed three samples containing different quantities of rosin, the within-laboratory standard deviation was found to be 0.05 % absolute at 11 degrees of freedom and the between-laboratory standard deviation was found to be 0.17 % absolute at 4 degrees offreedom. Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at a 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 0.2 % rosin content. 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 0.7 % rosin content. 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 ot any such patent rights, and the risk olinfringement ofsuch 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 live years end ifnot revised, either reapproved orwithdrawn. Your comments areInvitedeitherfor revision ofthisstandard orforadditional 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 mala your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296784 r. (jjjjM Designation: D 1483 - 84 {Reapproved 1989)61 Standard Test Method for Oil Absorption of Pigments by Gardner-Coleman Method1 mmilflt This standard is issued under the fixed designation D 1433; 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. ? INOTE--EditoriaTchanges were made throughout in March 1989. '.** ' 1. Scope ' 1.1. This, test method covers the determination 'of oil absorption 6f pigments by the Gardner-Coleman procedure.*2 1.2 This standard rhay involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is xh pt (250 mL), or a low-form 250-mL beaker. 5.3 Buret, graduated in 0.1-mL divisions. 5.4 Spatula, sharp-edged steel, having a blade Vz or % by 4 in. (15 or 20 by 100 mm). 5.5 Linseed Oil, Raw, conforming to Specification D 234 except tharit shall have an abid number of 3 1. the responsibility of the user of this standard tq establish appropriate safety and health practices and determine the 6 Procedure applicability ofregulatory limitations prior to. use. 6.1 The weight of pigment used should correspond to a, pigment volume of 3.0 0.6 mL. Determine the weight 2. Referenced Documents needed by multiplying 3.0 0.6 mL by the specific gravity of 2.1 ASTM Standards: D 234 Specification for Raw Linseed Oil3' D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out4 ... c the pigment, being tested. Fc| example, a .20 g specimen normally is used for zinc oxide (3.6 mL x 5.6 g/mL = 20.2 g). Transfer the amount, weighed to 0.1 g, to the glass container. 1 '* 6.2 Add oil from the buipt at the rate of about 1 drop per 3. Summary of Test Method 3.1 A soft paste is formed by the dropwise addition of linseed oil to the gently stirred pigment. The amount of oil required to form the paste is used to calculate an oil absorption value. secondKsti.rriijg and "folding" tile.pigment continuously with the spatula during the addition. Try to provide dry pigment for the oil to strike. Do not mb or grind; as the particles ofpigment become wetted, they collect in small lumps that gradually coalesce. As the coalescence proceeds, reduce the rate of oil addition. The end point is reached when the 4. Significance and Use 4.1 The oil absorption value obtained by this test method provides information about the vehicle demand of the lumps, with a rolling action from the spatula, collect into a single ball or the excess of oil smears the wall of the container. pigment when it is used in a pigment paste. Oil absorption 7. Calculation values can be used to characterize batches of a given $ pigment. 7.1 Calculate the oil absorption, Ar^s follows: . - 4.2 This test method differs from Test Method D 281 in - AmMMkxlfn-' that D 281 requires a vigorous rubbing action whereas this test method involves only a gentle stirring and folding ofthe pigment. Because the end points are different, the values obtained from the two test methods generally differ. where: M= oil, mL, and P = pigment, g. ' 5. Apparatus and Materials 0.93 represents density of oil (in grams per millilitre). Express as grams of oil per 100 g of pigment. 5.1 Balance, capable of weighing to 0.01 g. 5.2 Glass Container, round-bottom, having a capacity of 8. Report 8.1 Report the oil absorption of the pigment as pounds J This test method is under the jurisdiction of ASTM Committee D-1 on Paint (grams) of oil per 100 pounds (grams) of pigment., and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.24 on Physical Properties of Liquid Paints and Paint Material 9. Precision and Bias I . Current edition approved Oct. 26, 1984. Published January 1933. Originally published as D 1483 - 57 T, Last previous edition D 1483 - 60 (1979)cJ. 9.1 On the basis of an interlaboratory study of this test 2 See Gardner, H. A. and Coleman, R. E., MOil Absorption of Pigments," method in which one operator in each of 5 laboratories Scientific Section Circular 35, Paint Manufacturers' Assoc, of the United States, February 1920. 3 Annual Book ofASTM Standards, Vol 06,03. 4 Annual Book ofASTM Standards, Vol 06.02. tested 5 pigments with a broad range of oil absorption levels, the within-laboratory coefficient of variation was 3.4 % at 25 df and the between-laboratory coefficient of variation was 5.3 % at 20 df. Based on these coefficients, the following DUP050296785 # 0 1483 flia should be used to judge the acceptability of results at 95 % confidence level: 1.1 Repeatability--Two results obtained by the same ator should be considered suspect if they differ by more 19.9 % relative. 9; 1.2 Reproducibility-Two results obtained by different operators in different laboratories should be considered suspect if they differ by more than 15.3 % relative. 10. Keywords 10.1 Gardner-Coleman Method; oil absorption; pigments (general properties) The American Society for Testing and Materials takes noposition respecting the validity ofany patent rights asserted In connection with any Item mentioned In Oils 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 knot revised, either reapproved or withdrawn. Yourcomments are Invitedeither 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 oommerits have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 265 DUP050296786 jifh Designation: D 1542 - 60 {Reapproved 1988)1 Standard Test Method for Qualitative Detection of Rosin in Varnishes1 This standard is issued under the fixed designation D1542; tbe 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.orreapprovaL This standard has been approvedfor use bp agencies ofthe Department ofDefense to replace Method 5031, 5032 of Federal Test StandardNo. 141. Consult the Dob Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. ' " ' " Editorial changes were trade throughput, including the title, in Way 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 of phenol 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 D01.33 on Varnish and Resins, Including Shellac. Current edition approved Sept. 19, I960. 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 ofwater, 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 acid will mix slowly with the filtrate. If rosin is present, a fugitive violet color develqps immediately. A pink or brown coloration should be ignored. A control specimen containing rosin should be run simultaneously. 4.2 Halphen-Hicks Test--Dissolve a small quantity of the sample in 1 to 2 mL of the 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 solutioirin the other cavity. Sometimes it is necessary to blow a gentle current of air in the proper direction to accomplish this satisfactorily, or both catties 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. Tbe 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 wilt 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 lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 266 I DUP050296787 Designation: D 1544 - 80 (Reapproved 1989)e1 Standard Test Method for Color of Transparent; Liquids (Gardner Color Scale)1 This standard is issued under the fixed designation D1544; 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 brenapprovrdfor use by.agencies.ofthe Department ofDefense to replace Method 4248 ofFederal Test Method Standard No. 141. Cohstiti the DoD 'Index <tfSpecifications andStandardsfor the specific year ofissue which hdsbeen-adopted by the Department ofDefense. .i --Editorial changes were made throughout in April 1989. : Scope 1.1 This test method covers the measurement of the color transparent liquids by means of comparison with arbirily numbered glass standards. It applies to drying oils, dshes, fatty acids, polymerized fatty acids, and-resin lutions. Its application to other materials has not been ted. 11.2 This standard may involve hazardous materials, oper`ions, and equipment. This standard< does not purport to .Idress all ofthe safetyproblems associated'witk its use. It is 2e:.'responsibility of the user-of this standard to establish appropriate safety .and, health practices andi determine the tpplicability ofregulatory limitations prior louse. Referenced Documents ;f 2.1 ASTM Standards: D1545 Test Method for Viscosity of Transparent Liquids by Bubble fime Method2 ^ v, . E 308 Method for Computing the Colors of Objects by Using the CIE System2 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 Dl545, 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 essential ly achromatic. 3.3.3 Field of View--The specimen and one or more TABLE 1 Color Specifications of Reference Standards Gardner Color Chromaticity Coordinates-* Standard Number x y . 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 0.4498 9 0.4343 " 04640 ` 10 0.4503 -0.47&0 tt 0.4842 0.4818 12 . . - . 0.5077 0.4638 . 13 0.5392 ' 0.4458 -;t4 0.5546 0.4270 ' . 15 ., 0.5B57 0.4089. 16 0.6047 0.3921 17 0.6290 0.3701 18 0.6477 0.3521 Luminous Transmittance Transmittance Tolerance, Y,% 80 79 76 75 74 :71 67 64 . 61" 37 45 .36 30 22 :' 16 11 "6 '4 7 7 6 5 ,4 4 '' 4 4 4 4 4 :5. 6 6 2 1 1 1 * A duplicate standard shall, have chromatldty 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 Shan betfoser together than two thirds of, the1 difference In x or y between corresponding reference standards. _ ^' standards should subtend a visual angle- of about 2 deg-and be in the fieldjof 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. 1 This method is underthejurisdiction ofCommittee D*1 on Paint and Related Coatings and is the direct responsibility of Subcommittee DO1.26 on Optical Properties. Current edition approved March 10, 1980. Published May 1980. Originally 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. 267 DUP050296788 # 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 for judging 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. 1--If desired, liquid standards matching the colors given in Table i, 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 D1544 - 58 T." Many Glass Standards in current use do not conform to the values of Table 1. 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. 4 See 1961 Book ofASTM Standards, Part 8. 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 spectrophotom eter during calibration of each standard. XI.3 Obtain spectral transmittance data for each glass reference standard by following Method E 308. XI.4 From the spectral transmittance data for each refer ence standard calculate the CIE tristimulus values, X, Y, Z, and the chromaticity coordinates, x, y,' for CIE IHuminafit C (see Method E 308). ThoAmerican Society tor Testing and Materials takes no position respecting (he 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 6f 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 Itnotrevised, 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 feeI that your comments have not received a fair hearing you should make your views known to tho ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 268 * mmm DUP050296789 Designation: D 1545 - 89 Standard Test Method for Viscosity of Transparent Liquids by Bubble Time Method1 This standard is issued under the fixed designation D 1543; 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 teapproval. This standard has been approvedfor use by agencies of the Department ofDefense to replace Method 42?I of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications andStandardsfor the specific year ofissue which has been adopted by the Department ofDefense. Scope. 1.1 This test method covers the determination of the jjriseosity in babble seconds by timing. The bubble seconds ; approximately equal to stokes for most liquids, 1.2 The test method is applicable to transparent liquids Jt&at are free from crystalline or gel particles, 1.3 This standard may involve hazardous materials, operfpfi'ons, and equipment... This standard does not purport to * ddress all ofthe safety problems associated with its use. It is Ihe responsibility of the user of this standard to establish IIappropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. Terminology ,2.1 Definition: . . 2.1.1 viscosity--the resistance experienced by one portion jlof a liquid moving over another portion of the liquid. The | absolute unit of viscosity in the cgs system is the poise which l is expressed as dyne-seconds per square centimetre. Stokes lare equal to poises divided by density. The absolute SI I viscosity unit is the pascal-second. 13. Apparatus I 3.1 Constant-Temperature Bath--Any suitable bath cafpable of maintaining temperature at 25 0.1C with water jj. as the bath medium. 3.2 Standard Viscosity Tubes,12 3of dear glass and with flat Sif. bottoms, 10.65 0.025 mm in inside diameter, 114 1 mm in outside length. Plainly legible lines shall be located as .ft follows (Note 1): 27 0.5 mm s' 100(T5mm 108 0.5 mm The distance between the first and second lines shall be 73 0.5 mm. |i| 1--All distances shall be measured from the outside bottom of ;?i the tube. 3.3 Reference Standards--A series of standard viscosity 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 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)"'. 3 Empty standard viscosity tubes are available from the R. P. Cargille Laboratories, Inc., 33 Village Park Rd., Cedar Grove, Ni, or Byk-Gardner Inc.. Gardner 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 referenceionly, is the long established series of Gardner-Holdt letter standards, in tubes that do not have the thVee lines and are shorter than the standard viscosity tubes described in 3.2. 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 qr 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. 3--Adequate control of the temperature bath is essential. A variation of 0.lC 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 m 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. 4--For viscosities of liquids 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 269 MifpmHgSqgpi DUP050296790 D 1545 I TABLE 1 Recommended Numerical Standards for Comparator Viscosity Tubes'* 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. I j |j j 5--Positioning of the 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. j 1 5. Report 5.1 Report the following information: 5.1.1 The viscosity obtained by the timing method ex pressed as "bubble seconds" or "approximate stokes;" ' 6--The time in seconds or "bubble seconds" is an approxi- mate measurement of stokes 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 and by surface tension. Other variations on bubble-tube viscometers are described in ASTM ST? 500, Section 3.2.9.3 j j ') :j j j | I j j $ 6. Precision and Bias 1 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% H confidence level: i 6.1.1 Two results obtained by the same Operator should ' j be considered suspect if they differ by more than 4:9 % l relative. '" j 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. - | Gardnar-Holdt letters. Stakes ere shown in logarithmic progression. sThe bubble time, in seconds, of the numerical tubes under 4 s was determined by a technique employing a movie camera. c For reference purposes only. Numbered tubes are no longer commerciajly available. Above 2.65 the bubble seconds as measured by the kinematic method are approximately equivalent for most products. Below 2.65 this relationship does not hold. 5 Paint Testing Manual, ASTM STP 500, 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. 540-543. DUP050296791 # D 1545 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 ot this standard are expressly advised that determination ol 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 ofthis standard or loradditional 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. DUP050296792 Designation: D 1615 - 60 (Reapproved 187) Standard TsfMethods for . Glycerol, Ethylene Glycol, and Pentaerythritol in Alkyd Resins1- *' Tbis standard is issued under the fixed designation D 1615; the numher. immediatdy 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 offast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These methods cover the determination of glycerol, ethylene glycol, and pentaerythritol in alkyd resins and resin solutions. Other polyhydric alcohols that can be oxidized by periodic acid to formaldehyde or formic acid, or both, will interfere with the determination of glycerol and ethylene glycol. Urea, melamine, or phenolic resins interfere and render this procedure inapplicable. 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: D563 Test Method for Phthalic Anhydride Content of Alkyd Resins and Resin Solutions21 D1193 Specification for Reagent Water3 D1398 Test Method for Fatty Acid Content of Alkyd Resins and Alkyd Resin Solutions2 D2456 Test Method for Identification of Polyhydric Alcohols in Alkyd Resins2 D2998 Test Method for Polyhydric Alcohols in Alkyd Resins2 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 specificationsare 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. 3.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specifi cation D 1193.2 1 These methods are under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials. Current edition approved Sept. 19, 1960. Originally issued 1958. Replaces D 1615-58 T. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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 Nostrand Co., Inc., New York, N. Y., and the "United States Pharmacopeia." --The reagents and samples used in these methods may, under some conditions, be hazardous. Refer to the manufacturer's Material Safety Data Sheets for specific handling and safety precautions. Safe laboratory handling procedures and all applicable OSHA regula tions are to be followed. GLYCEROL AND ETHYLENE GLYCOL 4. Summary of Method 4.1 The primary hydroxyl groups of ethylene glycol and glycerol are oxidized to formaldehyde by periodic acid; the secondary hydroxyl group of glycerol is oxidized to formic add. By acidimetric and iodometric titration, the propor tions of formic acid and formaldehyde can be determined respectively, and calculated to glycerol and ethylene glycol by algebraic equations. The equations for the oxidation of the polyhydric alcohols are as follows: 3Hs03 + 2HsIOfi glycerol periodic acid I 2HCHO + HCOOH + 2HIQ3 + SH20 formal- formic iodic water dehyde acid acid o + H5 ethylene periodic giycol arid 1 2HCHO + HI03 + 31^0- - formal- iodic ---water ,_ ___ dehyde acid With pentaerythritol, there is no reaction. 5. Apparatus 5.1 Burets, 50 and 100-mL capacity. 5.2 Pipets, 20 and 50-mL capacity. 5.3 Beakers, two of 400-mL capacity. 5.4 Erlenmeyer Flasks, four of 1000-mL capacity, glassstoppered. 5.5 Volumetric Flasks, two of 100-mL capacity. 5.6 Graduated Cylinder, 10-mL capacity. 5.7 Filter Paper, fast, qualitative grade. 5.8 Watch Glass. 6. Reagents 6.1 Methyl Purple Indicator Solution,5 5 Methyl purple indicator manufactured by the Fleisher Chemical Co Benjamin Franklin Station, Washington 4, D.C,, U.S. Patent No. 2,416,619, ha been found satisfactory for this purpose. 272 DUP050296793 D 1615 Hodic Acid (11 g/L)--Dissolve 11 g ofperiodic arid ; water and dilute to 1 L. Prepare fresh daily and trbrown bottle. yassium Iodide Solution (200 g/L)--Dissolve 200 g iodide (KI) in water and dilute to 1 L. p&tim Hydroxide, Standard Solution (0.1 N)--PreId standardize a 0.1 JV aqueous sodium hydroxide (solution. podium Thiosulfate, Standard Solution (0.2 N)-- |and standardize a 0.2 N aqueous sodium thiosulfate 3) solution. Starch Indicator Solution--Dissolve 5 g of soluble i water and dilute to 1 L. Preserve the solution with 1 yclic arid. Sulfuric Acid (1+5)--Carefully mix 1 volume of jitrated sulfuric acid (H2S04, sp gr 1.84) with 5 des of water. ocedure pDetermine the plfthalic anhydride in accordance with vlethod D 563. Following this, extract the fatty acids in pance with 5.6 through 7 of Method D 1398, except do scard the aqueous phase. Test the remaining water solution containing the ilcohols for glycerol and ethylene glycol in the following oner: ;,J. Transfer the solution to a 400-mL beaker and : to about 60-mL volume, using an electric hot plate puree of heat. Keep the beaker covered with a watch W during boiling. Jp.2 Cool to room temperature, and filter through a lid paper into a 100-mL volumetric flask. (Take the jjfiple for pentaerythritol determination from this same liumetric flask.) Fill to the mark and agitate. |7.2.3 Pipet 20 mL (Vs aliquot) (Note 2) into a 1-L iltenmeyer, glass-stoppered flask. Add 2 drops of methyl pie indicator solution and neutralize with NaOH. Pipet ito the 1-L flask also 50 mL of HI04 solution, stopper, and rl to mix thoroughly. J 2--The aliquot should be so chosen, if possible, that 15 to '1 % of the periodic acid is consumed during the oxidation. Consider ate excess ofperiodic acid is required to complete the oxidation, and in ^ i more than 20 % is consumed the results should be disregarded and Ipimaller aliquot taken. On the other hand, too small an aliquot is not dvisable, for in such a situation the difference between titration and nk is small and any titration errors are magnified. 7.3 Simultaneously prepare two blanks containing 20 mL fjof water. Allow to stand 50 to 70 min at room temperature. 7.4 To the aliquot ofthe sample (7.2.3) and the blank, add fl00 mL of water and 3 drops of methyl purple indicator and titrate with 0.1 N NaOH solution to neutrality. Use the 150-mL buret and record the volume to the nearest 0.01 mL 7.5 To the solution that has just been titrated, add 150 mL of water, 30 mL of KI solution, and 25 mL of H2S04 (1+5). Titrate with 0.2 N Na2S203 solution to faint iodine ' color, add 10 mL of starch indicator and titrate to the disappearance of the blue color. 3--If the end point is not stable, as indicated by return of the blue color in the stoppered flask in 5 min, add water and titrate to a stable end point. Use the 100-mL buret and record the volume to the nearest estimated 0.05 mL. 8. Calculations 8.1 Calculate the percentage ofglycerol, <?, as follows: G = t(4 - B)N X 0.09206)/Wq X 100 where: A = millilitres of NaOH solution required for titration of the sample, B = millilitres of NaOH solution required for titration of the blank, N = normality of the NaOH solution, 0.09206 = grams of glycerol equivalent to 1 mL of 1 N NaOH solution (acidimetric), W -- grams of sample used, and F - aliquot fraction = Vs. 8.2 Calculate the percentage of glycerol and ethylene glycol, T, as a percentage of glycerol as follows: (T = [(JS' - A')N y. 0.02301 S)/WF J x 100 where: A' = millilitres of Na2S203 solution required for titration of the sample, B' -- millilitres of Na2S203 solution required for titration of the blank, 0.023015 = grams of glycerol equivalent to 1 mL of 1 N Na2S203 solution (iodometric), N = normality of the Na2S203 solution, W = grams of sample used, and F = aliquot fraction =`/s. 8.3 If E is the percentage of ethylene glycol, then = 1.348(7-G) When E = O, the sample is free of ethylene glycol. 4--In practice, samples containing .no ethylene glycol have given calculated E values ofup to 1 %. Therefore, samples with E values of 1 % or less should be considered as containing no ethylene glycol, and' samples with higher E values may be corrected by 1 % at the discretion Of the analyst. ..... 9. Repeatability 9.1 The average difference between duplicate runs per formed by the same analyst in the same laboratory should approximate the following values: Percentage of glycerol Percentage of glycol 0.1 0.4 Not more than once in twenty times would the difference be expected to exceed: Percentage of glycerol Percentage of glycol 0.3 1.0 10. Reproducibility 10.1 The average difference between results obtained by different analysts in different laboratories, when reported as the average of duplicate determinations, should approxi mate: Percentage of glycerol Percentage of glycol 0.2 0.5 ip^ass DU P050296794 D 1615 . jpercentage of glycerol Percentage of giycoi 0.6 1.2 PJ2NTAERYTHRITOL 11. Summary of Metlliod 11.1. Monopeptaerythritol reacts with , benzaldehyde to form a dibenzal which is crystalline and can be handled gravimetrically. 12. Apparatus -. 12.1 Beakers, 100-mL capacity. 12.2 Delivery Pipets ifor aliquots), 10 to 50-mL capacity. 12.3 Steam Bath. 12.4 Ice Bath. 12.5 Crucible, medium porosity, fritted glass. 12.6 Suction Flask. 12.7 Water Aspirator. 12.8 Desiccator. 12.9 Drying Oven;'capable of thaiiitaihing a temperature of 105C. ! 12.10 Glass Rod, flat-end. 13. Reagents and Materials 13.1 Benzaldehyde-Methanol Reagent--To, 20 mL of benzaldehyde,7. add 100 mL of technical grade anhydrous methanol (CH3OH). . . *- 13.2 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HQ). ,- 13.3 Methanol-Water Wash Solution (l+l)-r-Mix equal volumes of technical anhydrous CH3OJH and water. (Because of heat of solution, prepare this solution in; .advance.) One fourth of the wash solution, js-to be-stored in a refrigerator and used cold; the remainder is kept at room temperature. 14. Procedure 14.1 Transfer an aliquot ofthe 100-mL of sample solution (7.2.2) containing 0.15 to 0.55 g of pentaerythritPl to a 100-mL bedker. Evaporati on a steam bath to a volume of approximately 5 mL. To the hot solution (incipient toiling) add 15 mL of benzaldehyde-methanol reagent and 12 mL of HC1. Swirl and allow to stand at room temperature. 15 min, swirling occasionally during this time toprevent the precipi tate from adhering to the bottom, of the beaker. Place the beaker in ah ice bath, maintaining the temperatqre at 0 to 2C for 1 h or more. 7 Merck, N. F. grade benzaldehyde has been found satisfactory for this purpose. 14.2 Remove the reaction mixture from the ice bath and immediately filter with suction through a weighed fritted- glass crucible of medium porosity. Rinse the beaker with 25. mL ofthe cold (0 tp.2C) methanol wash solution and add to the crucible. Continue to transfer and. wash the precipitate with 100 mL of methanol-water wash solution at 20 to 25C as follows: ' .. -> 14.2.1 Disconnect the vacuum line, pour a 10-mL portion of the wash solution from the beaker to the crucible, and stir the precipitate to fonn a-homogeneous slurry, using a: short flat-end glass rod. Connect the vacuum line and draw-the wash .solution through the crucible. Repeat this washing operation.six times. With the last 30 mL of methanol-water wash solution, rinse the interior walls of-the crucible and rinse and remove the short stirring rod. , * 14.3 Aspirate thoroughly and dry the precipitate at 105C for 2 h. Cool in a desiccator and weigh. ;; 15. Calculations 15.1 Calculate the percentage of monopentaerythritol, P, of the resin from the precipitate obtained in accordance with 14.3 as follows: :i - ' P=>[W2'+ 0-02691X43.6]/WlF where: .... "' W, = grams of sample, W2 = grams of precipitate, and F = aliquot fraction. . '152 To convert the percehtage pf iribnopehtaeryfriritbl, P, to th'6 percentage of commercial technicalTnbhb'peilta- erythritol, use the following arbitrary formula which is based on (he assumption that the commercial grade contains 85 % monoperitaerythritbi: ' .. Commercial monopentaerythritol, % =/*/0.85_ 16. Repeatability 16.1 The average difference in percentage of mondpentar. erythritol found, between duplicate rpns performed by the same analyst in the same laboratory, should approximate 0.25. 'Nbt more than once in twenty times 'wouhi the difference be expected to exceed 0.6. - ....... ' r 17, Reproducibility 17,1 The average difference in percentage of monopentaerythritol found, between results- obtained by different ana lysts in different laboratories, when reported 4s thWaverage of duplicate' determinations Should approximate 0,5,Not mqre than once in twenty times would the difference be expected to exceed-1.4. 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 arty such patent rights, and the risk of Infringement of such rights, are entirety theirown responsibility. '` This standard is subject to revision at any time,fry the responsible technical committee and must be reviewed every five years and it not revised, either reapproved of withdrawn. Your comments are invited eitherfor 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 mend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, t$10 Raea St., Philadelphia, PA 1ST03. mumimmmmfK* 274 mrm DU P050296795 Designation: D 1648 - 86 Standard Specification for Basic Lead Siiicochromate Pigment1 This standard is issued under the fixed designation D 1648; 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 (e) indicates an editorial change since the last revision or reapproval. ' Scope .1 This specification covers two types of pigment comrcially known as basic lead siiicochromate. {{Referenced Documents .1 ASTM Standards: 1208 Test Methods for Pommon Properties of Certain, Pigments2 / 1366 Practice for Reporting Particle Size Characteristics of Pigments2 " < 1844 Test Methods Tor Chemical Analysis of BaSic Lead ^Shicbchrofhate2 f! 20 Practice for Particle Size 'Analysis of Particulate s Substances in the Range of 0.2 to 75 pm by Optical Microscopy3 Composition and Properties 3.1 Botii "types 'of pigment shall consist of silica coated ilead silicates andlehd chroxhates and Shall conform to i'*requirements in'Table' 1 i'r 3:2 The mate color and character of the tint obtained by 'xing the pigment with a white pigment shall be the same that of n reference sample mutually agreed upon by the' chaser andthe Seller. 3.3 The oil absorption shall be equal, within agreed upon lerances, to that of a reference sample agreed upon by the urchaser and the seller. 3.4 Panicle Size: 3.4.1 Type.1--This grade is characterized by major ounts of,particles in the 6.5- to-28-pm range. Coarse cles retained on a 45-.jus* (No, 325) sieve shall be less an 0.3 %. The maximum specific. surface diameter (SSD) zll be 8;5 jiinu r, r ; r3.4.2 Type -2--This grade is characterized. by major ounts of fine-sized particles. In general, the maximum ~e is essentially below ,1.0 to 2.5 pm. Coarse particles This specification is under the jurisdiction ofASTM Committee D-l on Paint Related Coatings and Materials and is the directresponsibility of Subooci-. tteeDOI.31 on Pigment Specifications. - ` Current edition approved April 25, 1986. Published June 1986i Originally Iblisbed as D 1648 - 59 T. Last previous edition D 1648 - 81. |` 2 Annual Book ofASTM Standards, Vol 06.02. . j 3 Annual Book ofASTM Standards, Vol 14.02. retained on a 45-pm (No.' 325) sieve shall be less than 0.1%. The maximum Specific Surface Diameter (SSD) shall be 2.0 pm. 3.4.3 Where closer control within a grade is required, the fineness requirements shall be as. agreed qpon by the purchaser and the seller.; < 4. Sampling 4.1 Two samples shall be taken at random froni different, packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units ofa.production appear, samples shall be taken from different packages, in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the. same production unit to form a composite sample. 5. Test Methods 1 5.1 Tests shall be conducted in accordance with (he following ASTM test methods. Test procedures not covered by XSTM test methods shall be mutually agreed upofi by the purchaser and the seller. 5.2 Chemical Analysis--1Test Methods D 1844. 5.3 Ignition Loss--Determine the loss on ignition in accordance with the section on Procedure of Test Methods D 1208, but using an ignition temperature of 450 to SSO0. 5.4 Particle Size by Microscopic Methods--Procedures for determining particle , size by microscopic methods are de scribed'iriPracticc E20.' , ,' 5.5 Specific Surface Diameter--Practiced), 1366." TABLE 1 Requirements for_P_ig_fn_e_nts _ Type 1Regular Particle Size Mlri " Max' Lead oxide (PbO) Chromidm trioxide (dr03) Sllfca (SIOe) Moisture and other volatile mat- ' ter, 26. ,' ignition loesat 450 to 550"C, % 46.0 5.1 45.5 49.0 .5.7 48.5 0.2 oi' ' Type 2 Fine Particle Size Min Max 42.5 46.0 6.3 7.2 47.5 60.5 0.2 0.2 The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection I 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 Invitedeitherfor 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. DUP050296796 Designation: D 1649 - 82 (ROapptoved 1987)e1 Standard Specification for Strontium Chromate Pigment1 This standard is issued Under the fixed designation D 1649; 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. ' The title of the specification and paragraph 4.1 were editorially changed in May 1987. 1. Scope . 1.1 This specification covers the pigment commercially known as strontium chromate which is suitable for use in the manufacture of protective or decorative coatings. 2. Referenced Documents 2.1 ASTM Standards: D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 D1845 Test Methods for Chemical Analysis of Strontium Chromate Pigment2 3. Composition and Properties 3.1 Dry Pigment--The pigment shall be commercially pure strontium chromate free of extenders and organic material, except for materials introduced to improve those properties for which the pigment is used. The pigment shall conform to the following requirements: percent Strontium as SrO, min 41 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Figment Specifications. Current edition approved Oct. 29, 1982. Published January 1983. Originally published as D 1649 - 59 T. Last previous edition D 1649 - 77. s Annual Book ofASTM Standards, Vol 06.02. percent Chromium as Cr03, min Chloride as Cl, max Sulfate as S03, max Water content, max Coarse particles {total residue retained on No. 325 (45-pm) sieve), max 41 0.1 0.2 0.2 1.0 3.2 The mass color and character of the tint and tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller when tested in accord ance with Test Method D 387. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test, procedures not cov ered by ASTM test methods shalllie mutually agreed upon between the purchaser and the seller. - 5.1.1 Chemical Analysis--Test Methods D 1845. 5.1.2 Water Content--Test Methods D 1208. The American Soc/etK lor Testing and Materials takes no position respecting the validity oI anypatentrights asserted In connection with any Item mentioned In this standard. Users ot this standard are expressly advised trial determination of the validity ol any such patent rights, and the risk ol Infringement ot 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, eitherreapproved or withdrawn. Your comments are invited either for revision of this 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 feel that your comments riave not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 'ftaoe St., Philadelphia, PA 19103. 276 < * DU P050296797 Designation: D1650 - 91 .HU4KV j S* J l StL. 1 9S- :! m ? r>i, *& Standard Test Methods of Sampling and Testing Shellac Varnish1 This standard is issued trader the fixed designation 0 1650; the number immediately following the designation indicates the year of original adoption or, in the dase ofrevision, the year oflast revision. A number in parentheses indicates the year-oflast reapproval. A superscript epsilon (r) indicates ;an- editorial change since the,last revision or ieapprovaL WkScope 1 -These test methods cover procedures for the sarhpling ; tiffing of orange shellac and bleached lac varnishes. ' |2 The sampling procedures and methods of testappear le following order 1 ` piihi pral Requirements for Test Melhods: irityof Reagents , paration of Sample SiTime olatile Matter |ine Value fiuble Matter ' 1 Value onification Value Sections ' 5 : 6 ,.7 8 to n ' - 12 to 14 15 to. >7 18 and 19 20 to 23 24 to 27 .. 28 and 29 1 30 to 34 . 35 to 37 ' 38 to 40 tt.3 This .standard does not purport to address the safety koblems associated with its use. It is the responsibility qftfie per of this standard to establish appropriate safety and palth practices and determine the applicability ofregulatory ` nitations prior to use. Referenced Documents 2.1 ASTM Standards: t"D 29 Test Methods of Sampling and Testing Lac Resins12 , -:'-D 1193 Specification for Reagent Water3 IH - ' - BiiTerailnology .. . r 3.1 Description ofTerms Specific to This Standard: I 3.1.1 add value--the number of milligrams of potassium (hydroxide required to neutralize 1 g of the nonvolatile Iportion of the lac varnish. ? . 3.1.2 lot--For purpose of sampling, a lot shall consist'of `^1 the entire amount of vamish manufactured as one batch and ' offered for delivery at one time. 3.1.3 saponification value--a measure of the alkali reac- tive groups in lac resins, it is expressed as the number of 1 f milligrams of potassium hydroxide that react with 1 g of the ^nonvolatile portion of the lac vamish. % 4. Significance and Use , 4.1 These test methods; compiles the common measure ft 1 These test methods are under the jurisdiction of ASTM Committee D-l on K Paint and Related Coatings and Materials and are the direct responsibility of 5 Subcommittee D01.33 on Polymers and Resins. Current edition approved Feb. 22, 1991. Published April 1991. Originally | published as D 1650 - 59. Last previous edition D 1650 - 76 (1981). J AnnuaI Book ofASTM Standards, Vof 06.02. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. rnents aiuLprocedureSr for characterizing shellac. 4.2 All shellac varnishes should be tested by the proce dures contained iri these test methods. > .. SAMPLING 5. Procedure . ; 5.1 A single container shall be taken at random from each lot as representative of the whole. 5.2 In case the vamish is packaged in cans dr drums of 5 gal (1&9 L) or more capacity, thoroughly mix the contents of the container and take a number of small samples from the top, bottom,. and.intermediate points by means of sampling tube. Mix these small samples to form a .composite sample and transfer not less than 1 qt (0.94 L) to a clean, dry, glass bottle, securely stopper with a new clean cork or well-fitting cover or cap, seal, distinctly label, and transmit to the laboratory for test. 5.3 When the'vamish. is packaged.in containers of 1-gal (3;8 L) or less capacity, send the original unopened container to the laboratory for test. When this cannot be done, thoroughly mix the' contents of the contain^ and transfer not less than 1 qt to a clean, dry, glass botllef securely stopper with a new clean cork or well-fitting- cover or cap, seal, distinctly- label, and transmit to the laboratory for test. 5.4 Take precautions to ensure that the sampling appa ratus and the samples themselves are neither contaminated with nor altered by any material not representative of the lot being sampled. Test Methods _ ^ V. . ' o GENERAL REQUIREMENTS 6. Purity of Reagents., . -- 6.1 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.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 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specifi cation D 1193, Type IV. ' 4 "Reagent Chemicals, American-Chemical Society Specifications," Am. Chem. 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." - 277 m DU P050296798 # D 1650 7. Preparation of Sample 7.1 Thoroughly mix the sample of varnish received for test by shaking the container immediately before the indi vidual portions are removed for the various tests. Keep the unused portion in a tightly closed container (preferably glass) and in a cool, dark place. COLOR 8. Apparatus 8.1 Glass Tubes, as prescribed in 19.1.1 of Test Methods D29. 8.2 Glass Plate, as prescribed in 19.1.2 of Test Methods D29. 9. Solvent 9.1 Ethyl Alcohol, Denatured, as prescribed in 8.2 of Test Methods D 29. 10. Color Comparison Standard 10.1 A shellac varnish mutually agreed upon by the purchaser and the seller for the color comparison. The varnish shall be stored in a tightly closed glass bottle and kept in a cool dark place. > . *. 11. Procedure 11.1 Weigh, to the nearest 0.1 g, approximately 35 g ofthe sample (Section 7) and the color comparison standard into separate stoppered flasks. Adjust both varnishes to the same nonvolatile matter content (preferably 33.3 %) by adding the proper amounts of the alcohol to the respective flasks. Thoroughly mix the contents of each flask by shaking and then allow the flasks to stand undisturbed for Vi. h. Compare the color of the sample with that of the comparison standard in accordance with the procedure described in 19.4.2 or 19.4.3 of Test Methods D29, as agreed upon by the purchaser and the seller. DRYING TIME 12. Apparatus 12.1 Film Applicator--The applicator shall be made of smoothly finished metal, preferably corrosion-resistant, and accurately constructed. It shall spread a film of uniform width and shall have such clearance that the thickness of the resulting wet film of coating applied will be 1.5 mils (38 pm). 12.2 Glass Plate, as prescribed in 19.1 of Test Methods D 29. 13. Solvent 13.1 Ethyl Alcohol, Denatured, as prescribed in 8.2 ofTest Methods D 29. 14. Procedure 14.1 Varnishes having more than 36 % nonvolatile matter shall be adjusted with the alcohol to a nonvolatile content of 35 1 %. Varnishes having nonvolatile contents of less than 36 % shall be tested as received. 14.2 Place the glass plate in a horizontal position and the film applicator, having a clearance to give a wet-film thickness of 1.5 mils (38 pm) unless otherwise specified, at one end of the plate. Deposit a small quantity of the sample (Section 7) on the glass plate immediately in front of the applicator. Spread the varnish the length of the panel by means of the applicator. Allow the test panel to remain in a horizontal position and dry in a well-ventilated room or chamber free from drafts and dust and in diffused light (not in direct sunlight). The temperature of the air within the room or chamber shall be between 21 and 32C. If the time of drying is not within the specified limits of the product specification; repeat the test in a room or chamber main tained at a temperature of 223 2C and 50 5 % relative humidity. 14.3 Test the film for set-to-touch and dry-hard times at points, not less than 10 mm (`/2 in.) from its edges in accordance with 14.4 and 14.5. 14.4 Set-to-Touch Time--Lightly touch the test film,with the tip of the finger and immediately place the finger tip against a piece of clean clear glass. Observe if any of the varnish is transferred to the glass. For the purpose of this test, the pressure of the finger shall not be greater than that required to transfer a spot of the varnish from Vs to 3/i6 in. (3.2 to 4.8 mm) in cross section. The film shall be considered set-to-touch when it still shows a tacky condition but none of it adheres to the finger. 14.5 Dry-Hard Time--With one end of the thumb resting on the test film and the forefinger supporting the test panel exert a maximum downward pressure (without twisting) of the thumb on the film. Lightly polish the contacted area with a soft cloth. The film shall be considered dry-hard when any mark left by the thumb is completely removed by the polishing operation. NONVOLATILE MATTER 15. Materials 15.1 EthylAlcohol, Denatured, as prescribed in 8.2 of Test Methods D 29. 15.2 Sand--Sand that has. been digested in hot-concen trated hydrochloric acid (HC1, sp gr 1.19) for 1 h, washed with water to remove all acid and soluble impurities,-ignited, cooled in a desiccator, and stored in a' clean-tightly closed container. ' . ; 16. Procedure 16.1 Place a portion of the sdmplev(Section 7) in a stoppered flask or weighing pipet and weigh to the nearest 0.1 mg. Transfer between 1 and 1.5 g of the sample to a weighed flatbottom glass or metal dish (petri dish or frictiontop can plug) 75 to 80 ram in diameter, containing approx imately 10 g of the sand, and a small glass rod. Weigh the container again and by difference obtain the exact weight of sample transferred to the dish. 16.2 Add 1 to 2 ml of the alcohol to the dish and thoroughly mix its contents with the rod. Heat the dish and its contents in a well-ventilated convection type oven main tained at 105 2C for 1 h. Transfer the dish to a desiccator to cool and weigh. 17. Calculation 17.1 Calculate the percentage of nonvolatile matter in the sample as follows: Nonvolatile matter, % = [(x -- y)/S] x 100 278 * Hi DUP050296799 # D 1650 the & weight of dish plus sand, plus rod, plus nonvolatile I matter, in sample used, g, f= weight of dish plus sand, plus rod, g, and 1= weight of sample used, g. IODINE VALUE Reagents '*$( 8.1 See Section 10 of Test Methods D 29. Procedure ||9:1 Flow some of the sample (Section 7) over a 6 by 10 i'{152 by 254 mm) clean glass plate. Place the plate in a arly vertical position and allow the film of varnish to dry |a well-ventilated room at 21 to 32`C for 1 h. Transfer the 1st plate to an oven maintained at 43 2C and allow to dry yemight. Cool to room temperature and scrape the dry lac lih from the plate with a razor blade, being careful not to |e the thick edges or other areas of abnormal thickness. > 19.2 Weigh, to the nearest 0.1 mg, 0.2 0.005 g ofthe dry resin into a 250-mi, glass-stoppered bottle. Determine nd calculate the .iodine value , in accordance with the rocedures described in Section 10 of Test Methods D 29. INSOLUBLE MATTER Solvents 20.1 See 8.2 or 9.2 of Test Methods D29, whichever is applicable. j?.\ 21. Apparatus 21.1 See 8.1 or 9.1 of Test Methods D29, whichever is iapplicable. f!2. Procedure 22.1 Weigh, to the nearest 1 mg, an amount ofthe sample f(Section 7) that will contain approximately 5 g ofnonvolatile C matter from a weighed stoppered flask or weighing pipet into f! a tail-form 200-ml beaker. Determine the insoluble matter in . accordance with the procedure given in either 8.4 or 9.4 of |Test Methods D 29, whichever is applicable. 23. Calculation ^ 23.1 Calculate the percent'of insoluble matter based on the nonvolatile matter content of the varnish as follows: I where: Insoluble matter, % = [R/(S x M)\ x 100 R = grams of insoluble matter obtained, S' = grams of sample used, and M = nonvolatile matter content of the sample, expressed as a decimal fraction. 26. Procedure 26.1 Weigh, to the nearest 1 mg, an amount of the sample (Section 7) that will contain approximately 10 g of nonvola tile matter from a weighed stoppered flask or weighing pipet into a tail-form 200-ml beaker. Determine the wax content in accordance with the procedure given in 16.3 of Test Methods D 29. 27. Calculation 27.1 Calculate the percent of wax based on the nonvola tile matter content of the varnish, as follows: Wax, % = [,/($, X M)] x 100 where: i?[ = grams of wax obtained, St = grams of varnish used, and M = nonvolatile matter content ofthe sample, expressed as a decimal fraction. ASH 28. Procedure 28.1 Weigh, the nearest 1 mg, an amount of the sample (Section 6) that will contain approximately 5 g of nonvolatile matter from a weighed stoppered flask or weighing pipet into an ignited and weighed silica or porcelain dish or crucible. Determine the ash content in accordance with the procedure described in 18.1 of Test Methods D 29. 29. Calculation 29.1 Calculate the percent ash based on the nonvolatile matter content of the varnish as follows: Ash, % - [R2/(S2 x M)] x lt)0 where: R2 = grams of ash obtained, S2 = grams of varnish used, and -- M -- nonvolatile matter content of the sample, expressed as a decimal fraction. ! PURITY------ "-- Qualitative Testfor Rosin 30. Reagents 30.1 See 11.1 of Test Methods D 29. 31. Procedure 31.1 Weigh an amount of the sample (Section 7) that will contain 2 0.1 g of nonvolatile matter into a 2-L Florence flask. Examine the test specimen for the presence of rosin in accordance with the procedure given in 11.2 ofTest Methods D 29. Qualitative Testfor Copal WAX 24. Apparatus 24.1 See 16.1 of Test Methods D 29. 25. Reagents 25.1 See 16.2 of Test Methods D 29. 32. Reagents 32.1 See 12.1 of Test Methods D 29. 33. Procedure 33.1 To an appropriate amount (40 to 50 g) of the sample (Section 7) add a sufficient amount of the denatured alcohol to reduce the nonvolatile matter content of the test specimen 279 'Vi': " VV ' DUP050296S00 to approximately 33 %. Examine the reduced varnish for the presence ofcopal in accordance with the procedure described in 12.2 of Test Methods D 29. Estimation ofAdulteration 34. Procedure 34.1 When the qualitative test shows the presence of either rosin or copal in the sample, estimate their respective contents as prescribed in Section 13 of Test Methods D 29, using the iodine value obtained on the nonvolatile portion of the varnish. ACID VALUE 35. Reagents 35.1 See 21.2 of Test Methods D 29. 36. Procedure 36.1 Weigh, to the nearest 1 mg, an amount ofthe sample (Section 7) that will contain approximately 1 g of nonvolatile matter from a weighed stoppered flask or weighing pipef into a 250-ml Erlenmeyer flask. Add 100 ml of the neutral alcohol and mix thoroughly. Titrate the lac solution with 0.1 N KOH or NaOH solution as prescribed in either 2.1.3.2 or 2.1.3.3 of Test Methods D 29, whichever is applicable. 37. Calculation 37.1 Calculate the acid value ofthe nonvolatile portion of the varnish as follows: Acid value = (VN X 56,1 )/SM where: V = millilitres of KOH or NaOH solution required for titration. N = normality of the KOH or NaOH solution, S' = grams of sample used, and M = nonvolatile matter content ofthe sample, expressed as a decimal fraction. SAPONIFICATION VALUE 38. Reagents . 38.1 See 23.2 of Test Methods D 29. 39. Procedure 39.1 Weigh, to the nearest 1 mg an amount ofthe sample (Section 7) that will contain approximately 1 g of nonvolatile matter from a weighed stoppered flask or weighing pipet into an alkali-resistant, standard-taper, ground-glass joint, 250mL Erlenmeyer flask. Proceed in accordance with 23.3 of Test Methods D 29, also running a blank sample as pre scribed therein. Titrate the sample and blank solutions in accordance with' the procedure given in either 23.3.2 or 23,3.3 of Test Methods D 29, as applicable. 40. Calculation 40.1 Calculate the saponification value as follows: Saponification value = [(5 - VfjN x 56.il/5M where: ;< Kj = millilitres of HC1 required for titration of sample, B = millilitres of HC1 required for titration of Wank, N = normality of the HQ, S = grams of sample used, and M = nonvolatile matter content of the sample, expressed as a decimal fraction. 41 Keywords 41.1 iodine value; saponification value; shellac varnish 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 oI 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 tfietr own responsibility. -- This standard Is subject to revision at any time by the responsible technical committee and must bereviewed every five years.^nd ifnotrevised, either reapproved or withdrawn. Your comments are Invited iithhrforrevision of this Standard or tot additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of theresponsible 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. 280 DUP050296801 Designation: D 1652 - 90 Standard Test Methods for Epoxy Content of Epoxy Resins1 This standard is issued under the fixed designation 0 1652; 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. This standard has been approvedfor use by agencies ofthe Department cfDefense to replace Method 7403 ofFederal Test Method Standard Ho. 141. Consult the DoD Index ofSpecifications andStandardsfor the specific year ofissue which has been adopted by the Department ofDefense. {. Scope s. i.l These test methods cover the quantitative < " pn of the epoxy content of epoxy resins, f 1.2 This standard does not purport to address all of the afety problems associated with its use. It is the responsibility '"'the user ofthis standard to establish appropriate safety and -alth practices and determine the applicability ofregulatory -citations prior to use. For specific hazard statements, see Ttion 6. Referenced Documents , 2.1 ASTM Standards: , D1193 Specification for Reagent Water*2 | E 200 Practice for Preparation, Standardization, and Storage of Standard Solutions for Chemical Analysis3 /. Summary of Test Method | 3.1 The resin is dissolved in a suitable solvent and the esulting solution is titrated with hydrogen bromide either (Erectly or in situ. The hydrogen bromide reacts stoichiojmetrically with epoxy groups to form bromohydrins; ther&fore, the quantity ofacid consumed is a measure ofthe epoxy content. 3.1.1 In Test Method A, the titration is direct with a tandard solution of hydrogen bromide in glacial acetic acid. 3.1.2 In Test Method B, the titration is with standard ijperchloric add in the presence of an excess of tetratethylammomum bromide. Hydrogen bromide generated in situ by the addition of perchloric acid to the quaternary ammonium halide rapidly opens the oxirane ring. 4. Significance and Use 4.1 The epoxy content of epoxy resins is an important ; variable in determining their reactivity and the properties of ' coatings made from them. These test methods may be used to determine the epoxy content of manufactured epoxy resins and confirm the stated epoxy content of purchased epoxy resins. . 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 DOl.33 on Polymers and Resins. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1652 - 59 T. Last previous edition D 1652 - 88. 2 Annual Book ofASTM Standards, Vois 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 15.05. 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.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. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type II of Specification D 1193. 6. Hazards 6.1 Hydrogen bromide and glacial acetic acid are corro sive. Chlorobenzene and chloroform are considered haz ardous. In addition to other precautions, take care to avoid inhalation and skin or eye contact with these chemicals. Use goggles or a face shield, or both. Protect skiin'by use of suitable protective clothing. All specimen preparations shall be done in a well ventilated area, such as a fuine hood. TEST METHOD A 7. Apparatus 7.1 Buret, closed-reservoir type. The buret tip should be fitted with a rubber stopper of proper size to fit the fleck of the Erienmeyer flask and the stopper should have an' additional small hete to permit escape of replaced air during titration. 7.2 Magnetic Stirrer, adjustable speed. * 7.3 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE) coated 8. Reagents and Materials 8.1 Chlorobenzene (Warning--See Section 6). 8.2 Chloroform-Chlorobenzene Mixture (1+1) (Warn ing--See Section 6). 8.3 Crystal Violet Indicator Solution--Prepare a 0.1 % solution of crystal violet in glacial acetic acid. 8.4 Glacial Acetic Acid (Warning--See Section 6). 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, PC. 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., lac., New York, NY, and "United States Pharmacopeia." 281 # D 1652 8.5 Hydrogen Bromide (HBr), anhydrous (Warning--See Section 6). 8.6 Potassium Acid Phthalate (KHC8H404)--Primary Standard grade. 8.7 Hydrogen Bromide in Acetic Acid, Standard Solution (0.1 N) (Warning--See Section 6)--Prepare by bubbling anhydrous HBr at a slow rate through glacial acetic acid until the desired normality is attained (approximately 8 g of HBr/L). Standardize each day used against 0.4 g of potas sium acid phthalate (KHQH4O4) accurately weighed and dissolved by gently heating in 10 mL of glacial acetic acid. Reagent of 0.1 N concentration has been specified. As solutions exceed this concentration they became progressively less stable. 9. Procedure 9.1 Use a quantity of specimen that contains 0.001 to 0.002-g equivalents of epoxy groups; Weigh the appropriate amount, to within 1 mg, into an Erlenmeyer flask. UsC' a 50-mL flask for low-molecular-weight resins (liquid grades) and a 125-hiL flask, for high-molecular-weight resins (solid- grades). 9.2 Dissolve the specimen in a solvent at room tempera- turd. Use 10 mE of cMorob'enzene for liquid grade resins or- 25 mL of a 1+1 mixture of chloroform arid chlorobenzene for solid grade resins. Place a magnetic stirring bar into the flask and mix on the magnetic stirrer to dissolve. 9.3 Add 4 to 6 drops of crystal violet indicator solution and attach te flask to the rubber stopper on the buret tip. Lower the buret tip to appoint just above..the solution and titrate with the hydrogen bromide in acetic ^pid solution tq.a- blue-green end point with, the magnetic stirrer rotating ait a moderate speed to avoid splashing. Slow down the titration near the endpoint to allpw ample time for the reaction to take place. Titrate, as nearly as possible, to the same color at the end point as that obtained during standardization of the reagent 9.4 Make a blank determination on the reagents in aij identical manner. 10. Calculation 10.1 Calculate the normality, N, of the HBr acetic acid"as follow: '; /V = (IV x 1000)/(204.2 x V) .(1) where: W = KHC8H404 used, g, and V = HBr solution used, mL. 10.2 Calculate the epoxy content, E, in gram equivalents of epoxy groups per 100 g of resin as. follows: E = N(V-B)}lQx W (2) where: N - normality of the HBr in acetic acid, V - HBr solution used for titration of the specimen, mL, B = HBr solution used for titration of the blank, mL, and W = specimen used, g. 10.3 Calculate the percent of oxirane oxygen, O, as follows: ' O = 1.6^- B)/W (3) 10.4 Calculate the weight per epoxy equivalent, WPE, that is, grams of resin containing I g equivalent of epoxy groups, as follows: WPE =, 1000 WjN{ V - B) (4) 11. Precision 11.1 Repeatability--The difference between two results obtained by the same analyst will approximate 0.7 % of the epoxy content ofthe resin tested. Two such values should be considered suspect if they differ by more than 2 % absolute. 11.2 Reproducibility--The difference between two results, each the mean of two determinations, obtained by analysts in different laboratories, will approximate 2 % of the epoxy content of the resin tested. Two such values should be considered suspect if they differ by more than 6 % absolute. TEST METHODS 12. Apparatus 12.1 Buret, closed-reservoir type, bottom filling* 25 mL with '/m-mL division, or potentiometric automatic titrator. 12.2 Erlenmeyer. Flasks, 100-mL, 250-mL, and 500-mL. 12.3 Magnetic Stirrer, adjustable speed. 12.4 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE) coated 12.5 Pipets: ' 12.5.1 Measuring Pipet, 25-mL. 12.5.2 Volumetric Pipet, 50-mL. .12.6 Volumetric Flask, (L. , ,. 12.7 Bottle, 2 oz wide-mouth, or 100-mL disposable beaker, or equivalent 13. Reagents 13.1 Glacial Acetic Acid- (Warning-^-See Section 6). 13.2 TetraethylammofUum Bromide, anhydrous crystals. 13.3 Perchloric Acid (HC104), 60 % (Warning--See Sec tion 6). 13.4 Acetic Anhydride (Warning--See Section 6)7" 13.5 Methylene Chloride (Warning--See Section 6). - 13.6 Crystal Violet.Indicator, crystals.; 13.7 Potassium Acid Phthalate (KHQH4O4) primary standard grade. ; "r-- r: ~ 13.8 Digfycidyl Ether ofBisphenol-A. 14. Reagent Preparation - 14.1 Perchloric Acid (0.1 N Solution in . Glacial Acetic Acid) (Warning--See Section 6)--Prepare in the following manner and sequence in order to avoid an excessive rise in temperature. ' 14.1.1 Place approximately 250'tnL of glacial acetic acid into a 1 L volumetric flask. Add 13 mL of 60 % perchloric acid and mix. Add' 50 mL of acetic anhydride, dilute to the mark with glacial acetic acid, and mix thoroughly. 14.1.2 Allow to stand at least 8 h for completion of reaction between the acetic anhydride and water. A- shorter time period may be used if completion of the reaction is analytically verified. 14.2 Tetrdethylammonium Bromide Solution in Glacial Acetic Acid (Warning--See Section 6): 14.2.1 Dissolve, with agitation at room temperature, 100 g of tetraethylammonium bromide in 400 mL of glacial acetic acid. 282 DUP050296803 D 1652 |f4.3 Crystal Violet Indicator Solution--Prepare 0.1 % liution of crystal violet indicator in glacial acetic acid learnings--See Section 6). Standardization of 0.1 N Perchloric Add Reagent 15.1 Procedure A--Standardization with Potassium Acid hthalate: 15.1.1 Dissolve, by gentle heating, 0.4 g of potassium add Ihthalate, weighed accurately to the nearest milligram, in 50 j&L of glacial acetic acid, and add 6 to 8 drops of crystal ilblet indicator solution. Insert a clean stirring bar into the Sfemnle. and adjust the magnetic stirrer to effect solution, j ^Continue agitation throughout the titration procedure. Jfitrate with perchloric add reagent solution to the end point *~--iich is a sharp change in color from blue to green, stabilize pr at least 2 min. 15.1.2 Calculate and record the perchloric acid reagent jJKormalitv as follows: N={WX 100)/(204,2 x V) (5) Inhere. W - normality of perchloric acid reagent, IV = potassium acid phthalate used, g, and tjf'K = volume of perchloric acid reagent required to titrate the standard, mL. 15.2 Procedure B--Standardization with Diglycidyl Ether ofBisphenol-A (DGEBA): 15.2.1 Dissolve 0.25 to 0.40 g of the DGEBA accurately Iweighed to the nearest milligram into a 2 oz wide-mouth jfcottle or 100 mL disposable beaker. Add 10 to 15 mL of flmethylene chloride. Insert a clean stirring bar into the jsample and adjust the magnetic stirrer to effect solution. ^Continue agitation throughout the titration procedure. 15.2.2 Add 10 mL of tetraethylammonium bromide re: agent and 6 to 8 drops of crystal violet indicator solution and 1 titrate to a sharp blue-to-green end point with the perchloric lacid reagent solution. The end point should be stable for at Beast 30 s. 15.2.3 Calculate and record the perchloric acid reagent Uffactor, F, as follows: F=(W^x)/K (6) where: Wd = diglycidyl ether of bisphenol-A standard used, g, E = epoxide ofthe standard used (normally 25.19), weight % The perchloric acid should be standardized initially by Procedure A and thereafter at least twice per week by Procedure A or B. Temperature of the reagent solution must be kept at 25 2'C (77 3"F). 16. Procedure 16.1 Weigh the required amount of specimen into a 2-oz disposable glass bottle or plastic beaker. The amount of specimen weight used is dependent on the expected epoxide equivalent weight (EEW) as follows: EEW Approximate Specimen Size, g 170-375 375-600 600-1000 1000-1500 1500-2000 2000-2500 2500-5000 0.4 0.6 0.8 1.3 1;B 2.3 2.8 16.2 Add 10 to 15 mL of methylene chloride to the specimen. Insert a dean stirring bar and adjust the magnetic stirrer to effect solution. Continue agitation through the titration procedure. 16.3 Add 10 mL oftetraethylammonium bromide reagent and 6 to 8 drops of crystal violet indicator solution. Titrate with 0.1 TV perchloric acid reagent to a sharp blue to green end point which is stable for at least 30 s. Record the volume of perchloric acid reagent used to titrate the specimen. 17. Calculation 17.1 If 15.1 is used for standardization, calculate weight percent epoxide, E, as follows: =4.3x Vx NJW (7) 17.2 If 15.2 is used for standardization, calculate weight percent epoxide, E, as follows: E = FxV/JVc (8) where: We -- weight of epoxy resin spedmen used, g. 17.3 Calculate the epoxy equivalent weight, WEEW, as follows: ! = F 100/2? (9) where 43 = mol weight of the epoxy ring. 17.4 Calculate weight percent of oxirane oxygen, O, as follows: O = 16/43 x E ='1.6 x V x NjW 410) 18. Predsion 18.1 A liquid epoxy resin sample with approximately 24.1 % epoxide was tested by seven laboratories where ten analysts obtained the following results: 18.1.1 Repeatability--The difference between two results obtained by the same analyst should not vary by more than' 1.22 % relative. 18.1.2 Reproducibility--The difference between two re sults, each the mean of two determinations obtained by analysts in different laboratories should not vary by more than 2.97 % relative. 19. Keywords 19.1 epoxide equivalent weight (EEW); liquid epoxy resin; oxirane; weight percent epoxide; weight per epoxy equivalent (WPE) 283 ! [!KWWyWWWWW 4* I DUP050296804 # D 1652 The American Society for Teating 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 andmust be reviewedevery five years and Ifnot revised, eitherreapproved orwithdrawn. Your comments are invited eithertor revision ofthis 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 Race St., Philadelphia, PA 19103. 284 DUP050296805 Designation: D1695 - 77 {Reapproved 1989) Standard Terminology of Cellulose and Cellulose Derivatives1 This standard is issued under the fixed designation D1695; the number immediately following the designation indicates the year of original adoption or, in the case of revirion, 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. --The title was changed editorially in October 1989. phis terminology is divided into thrfee classes as follows: (4) Cellulosic Materials and Constituents, | '(5) Chemical Modifications and Derivatives of Cellulose, nd JC) Properties of Cellulose and Associated Concepts that i applicable to both (A) and (5). (A) CELLULOSIC MATERIALS AND CONSTITUENTS icetylation pulps--pulps used in the. manufacture of cellu lose acetate or other esters, and subject to various specifi cations by the manufacturers, including those of purity, moisture content, sheet properties, and viscosity, jalpha-cellulose--(7) an imprecise and historic term (origif|. nally devised around 1900) that has been used to characfcterize cellulose purity. The currently preferred term is : "Rio-" (2) When used!, alpha-cellulose is the portion of a cellulose pulp that remains insoluble after treatment with aqueous sodium hydroxide at 20C. The term has meaning ' onjy if there is a precise statement of the initial sodium - hydroxide concentration (usually about 18 %>, the subse quent dilution, and other conditions employed in its ...determination, alpha pulps--in a rather indefinite way, all those bleached wood pulps that have an alpha-cellulose content above 88 %, (Where possible, it is desirable to use a more specific term.) araban--a pentosan yielding essentially oply arabinose on hydrolysis. arabinogalactan--a polysaccharide consisting of arabinose and galactose units, like the water-soluble polysaccharide of larch. arabinose--a pentose that occurs as one of the sugar units in some hemicelluloses. arabinomethylglucuronoxylan--a hemicellulose containing arabinose, 4-Ormethylglucuronic acid, and xylose groups in its structure. beta-cellulose--(7) an imprecise and historic term (originally devised around 1900) that has been used to characterize cellulose purity. The currently preferred term is "S,0-S18." (2) When used, beta-cellulose is the portion of a cellulose pulp which is dissolved in the alkaline solution of the 1 This terminology is under the jurisdiction ofASTM Committee D-l on Paiat and Related Coatings and Materials aDd is the direct responsibility of Subcom mittee 1501.36 on Celluloses. alpha-cellulose test and is subsequently reprecipitatwi on . neutralization ofthe alkaline solution. All conditions must be specified exactly. carbohydrates not cellulose--the noncellulosic carbohy drates of a cellulosic material., cellophane pnlps--pulps used in the manufacture of cello phane, and subject to various specifications by the manu facturers, including those, of' purity, moisture content, sheet properties, and viscosity, cellulose--(7)'the main solid constituent .of woody plants; it occurs widely elsewhere in the vegetable kingdom, and to a small extent in the animal kingdom. (2) chemically, cellulose is 0-1-4 glucan of high degree of polymerization. It is desirable to apply "cellulose" to this material only and to designate the predominantly cellulosic residue obtained by subjecting woody tissues to various pulping processes as "cellulosic residues," "cellulosic pulps," or the like, cellulose I--the crystalline modification of cellulose that normally occurs in, nature. cellulose n--the crystalline modification of cellulose that is found in. mercerized cellulose, in regenerated cellulose, and in cellulose produced by, the hydrolysis of various cellulose derivatives. cellulose III--a crystalline modification of cellulose -pro duced by treatment, under certain conditions, with am monia or sometimes by amines. The method of removing the reagent determines the modification produced, cellulose IV--a crystalline modification of_cellulose pro-. duced by heat.treatment of cellulose II. cellulose X--a crystallinemodification ofcellulose produced^ by treatment of cellulose with strong hydrochloric acid or phosphoric acid. cellulose, purified cotton--see cotton cellulose, purified. cellulose^ purified wood--see wood cellulose, purified. . chemical.cellulose--a chemically purified cellulosic material that is intended for chemical treatment to produce deriva tives. chemical cotton--chemical cellulose prepared from cotton; generally, but not necessarily, cotton linters. chemical pulps--in the paper industry, pulps produced by chemical processes, as contrasted to those produced by mechanical processes, (see also chemical wood pulp), chemical wood pulp--a term used in the paper industry for pulps obtained by digestion of wood with solutions of various chemicals. DEE--This term, which refers to pulp produced and purified by chemical processes, should not be confused with chemical cellulose which refers to pulp that is to be used in chemical processes. m DUP050296806 D 1695 cotton cellulose, purified--chemical cellulose from cotton fiber or linters. (see also chemical cotton) cotton linters--see linters. dissolving pulps--see pulps, dissolving, extractives--compounds occurring in plant materials, but not forming part of the structural elements, that are removed with neutral solvents such as ether, alcohol, and water. galactan--a polysaccharide composed essentially ofgalactose units, (see also arabinogalactan) galactoglucomannan--one of the hemicelluloses of softwoods, containing three types of sugar units--galac tose, glucose, and mannose. galactomannan--a. polysaccharide containing galactose and mannose units. Galactomannans usually have a long chain of mannose units with galactose side chains and are found in seed gums (guar, locust bean), gamma-cellulose--(7) an imprecise and historic term (origi nally devised around 1900) that has been used to charac terize cellulose purity. The currently preferred term is "S18." (2) When used, gamma-cellulose is the portion of a cellulosic material that remains dissolved after neutraliza tion of the alkaline solution from the alpha-cellulose determination; all conditions must be specified exactly, glucan--a macromolecular substance that can be hydrolyzed to give almost exclusively glucose, glucomannan--a hemicellulose consisting essentially of glu' cose and mannose. glucuronoxylan--a common designation for the Xylose-con taining hardwood hemicelluloses. (see also methylglucuronoxylan) hemicellulose--any of a number of cell-wall polysaccharides that are removable by extraction with aqueous alkali and that may be hydrolyzed by boiling with dilute acids to give constituent monosaccharide units; any ofthe noncellulosic cell-wall polysaccharides. hexosan--frequently used in contradistinction to pentosan, for a polysaccharide consisting mainly of hexose units, holocellulose--the total polysaccharide fraction of extrac tive-free wood. The method of isolation or of determina tion should always be given. kraft pulp--pulp cooked by the alkaline liquor consisting essentially ofa mixture of caustic soda and sodium sulfide. The make-up chemical is traditionally sodium sulfate, which is reduced to the sulfide in the chemical recovery process; hence the alternative designation, sulfate pulp, lignin--that part of plant material which is not saccharified by the action Of 72 % sulfuric acid or 42 % hydrochloric acid, after the resins, waxes, and tannins have been removed. linters--the short fibrous material adhering to cotton seed after the ginning operation. After removal from the seed it is used to a limited extent as a fibrous raw material for special papers. The principal use, however, is for chemical cellulose, that is, as the raw material for the manufacture of cellulose derivatives. mannan--strictly, a polysaccharide composed entirely of mannose units, but used conventionally to distinguish the hexosan wood hemicelluloses from the pentosans (xylan). (see also galactoglucomannan and glucomannan) mannogalactan--see galactomannan. methylglucuronoxylan--the main hemicellulose of hard wood pulps; a polysaccharide containing xylose and 4- O-methylglucuronic acid groups. In the wood it is partially acetylated. nitrating pulps--pulps used for the manufacture of cellulose | nitrate and subject to various specifications by the manu facturers, including those of alpha-cellulose content and viscosity. oligosaccharides--polymeric carbohydrates containing rela tively few (compared to the polysaccharides) sugar units connected by glycosidal linkages. Two to nine units has been suggested as a suitable Tange. For longer chains the polymers cannot be readily separated into individual molecular species. pectic substrates--complex polysaccharides containing a large proportion of galacturonic acid units. pectins--colorless, amorphous, water-soluble polysaccha rides occurring in plant tissues that yield pectic acid and methanol on hydrolysis. pentosans--one of the groups of amorphous carbohydrates : included under the general term "hemicellulose." i Pentosans yield principally pentoses on acid hydrolysis. ! The principal pentosan in wood is xylan. | polyuronides--polysaccharides containing uronic acid j groups. pulps, dissolving--chemical cellulose from wood pulp, pulps for chemical conversion--chemical cellulose from I wood pulp, J pulps for manufacture of cellulose derivatives--chemical cellulose from wood pulp. purified cotton cellulose--see cotton cellulose, purified. purified wood cellulose--see wood cellulose, purified. R]0--the portion of a cellulose pulp that is insoluble in 10 % sodium hydroxide using Test- Method D 16962 or its j equivalent. --R,0DE$ is considered to be the main commercial long chain length portion ofcellulose, similar to the intent in the imprecise term "alpha-cellulose" (see S]0). rayon pulps--pulps used in the manufacture of rayon, and subject to various specifications- by the manufacturers, including.those' of purity, moisture content, sheet proper ties, and viscosity. Sj o the portion of a cellulose pulp that insoluble in 10 % sodium hydroxide using Test Method D 1696, or its equivalent. Sl0D is considered to contain both hemicellulose and degraded, short chain length cellulose (see R]0). Sig--the portion of a cellulose pulp that is soluble in 18 % sodium hydroxide using Test Method D 1696, or its equivalent. D !,"!! #%--S,s is considered to be mainly hemicellulose, similar to the intent of the imprecise term "gamma-cellulose." ' Si,,-S18--an estimate of the portion of degraded cellulose in a pulp obtained by subtracting Slg from S10. --SeeD&'()''&*+ S|0 and S,8 definitions. S,o-S,j is similar to the intent in the imprecise term "beta-cellulose." sulfate pulp--see kraft pulp. 2 Annual Book ofASTM Standards, Vol 15.04. 286 DUP050296807 D 1695 Ifite pulp--wood pulp produced by cooking with a sulfite p liquor made by dissolving sulfur dioxide in an aqueous Itoase. ViMod cellulose, purified--chemical cellulose from wood, ylan--a pentosan giving almost exclusively xylose on ^hydrolysis. 8) CHEMICAL MODIFICATIONS AND DERIVATIVES OF CELLULOSE rboxymethylcellulose, CMC--the common name for a "cellulose ether of glycolic acid. It is usually marketed as a water-soluble sodium salt, more properly called'sodium carboxymethylcellulose. In the early literature, it is somel-stimes called cellulose glycolate or cellulose glycolic acid. Cellulose acetate--in the broad sense, any of several esters of cellulose and acetic acid, (see also cellulose triacetate) ffcellulose acetate butyrate--a mixed ester of cellulose con taining both acetate and butyrate groups. Icellulose acetate phthalate--a mixed ester of cellulose conI taining both acetate and phthalate groups. | cellulose acetate propionate--a mixed ester of cellulose ft containing both acetate and propionate groups. . cellulose derivative--a substance derived from cellulose by substitution of one or more of the hydroxyl groups with < some other radical. Most derivatives are ethers or esters, cellulose esters--derivatives of cellulose in which one or : more of the hydroxyl hydrogens have been replaced acyl groups. ; cellulose ethers--derivatives of cellulose in which one or , more of-the , hydroxyl hydrogens have been replaced by alkyl groups. cellulose lacquer--a liquid coating composition containing as the basic film-forming ingredients, cellulose esters or ethers and plasticizers with or without resins, cellulose mixed ester--a cellulose ester containing more than one type of acyl group. cellulose nitrate--any of various nitrate esters of cellulose. D/01200/3456ellulose nitrate is often and erroneously called "nitrocellulose" because it was formerly considered a nitro-comv pound, cellulose plastics--plastics based on cellulose compounds, such as esters (cellulose acetate) and ethers (ethylcellulose). cellulose propionate--any ester of cellulose with propionic acid. cellulose sodium glycolate---see ^arboxymethyl cellulose, cellulose triacetate--that form of cellulose acetate in which the degree ofsubstitution approaches 3 sufficiently that the product is not soluble in acetone, cellulose xanthates--the salts of cellulose xanthic acid. Commonly, cellulose xanthate refers to sodium cellulose xanthate, the essential constituent of the viscose solution, from which viscose rayon is spun, dope--a composition, usually a cellulose lacquer, for appli cation on textiles and leathers. Also a very viscous crude reaction product, as acetylation dope.' ethylcellulose--any of several ethyl ethers of cellulose. The one most generally used in industry has-sufficient substi tution to be soluble in organic solvents, hydrocelluloses--water-insoluble products of the hydrolysis of cellulose with acids. They are molecularly heteroge neous in the sense that they are composed of molecules varying in degree ofpolymerization. The average degree of polymerization (DP) and the DP distribution depend on the nature of the acid treatment and of the original cellulose. The term may also be applied to any insoluble polysaccharide so formed and separated as a more or less homogeneous fraction from the mixture of products, but the singular form "hydrocellulose" should not be used without an article, to avoid the implication of a molecu larly homogeneous species. (2-hydroxyethyl)celIulose--any of several cellulose ethers in which some of the hydroxyl groups have been substituted with hydroxyethyl, groups. Hydroxyethyl cellulose, except at very low degrees of substitution, is water-soluble. (2-hydroxyethyl)ethylcellulose--a mixed ether of cellulose containing both hydroxyethyl and ethyl groups. (2-hydroxyethyl)methylceIlulose--a mixed ether of cellulose containing both hydroxyethyl and methyl groups. (2-bydroxypropyl)methylcellulose--a mixed ether of cellu lose containing both hydroxypropyl and methyl groups. ionic cellulose ethers--those water-soluble cellulose ethers which cqntain ionizable groups, in more than trace amounts. Sodium carboxymethyl cellulose is. an example. lacquer--see cellulose lacquer. methylcellulose--any of several methyl ethers of cellulose. Commercially, the water-soluble ether (degree of substitu tion approximately 1.5 to 2.0). methylethylcellulose--a cellulose ether containing both methyl and ethyl groups. microcrystalline cellulose--a commercial name for cellulose that has been hydrolyzed to the limiting DP and that consists essentially of microcrystals. nitrocellulose--see cellulose nitrate. nonionic cellulose ethers--that class of cellulose ethers which does not contain any ionizable groups. -- oxycelluloses--water-insoluble substances formed by the action of oxidizing agents on cellulose. The chemical'' nature of oxycelluloses varies with the oxidant'us^d, and the type is indicated by attaching the name of the'bxidant adjectivally to'^oxycelluloses" as in "hypochlorite oxy celluloses." Any such mixture is "an oxycellulose" and the word should not be used in the singular withoSt either the definite or indefinite article. In many respects, the phrases "oxidized cellulose" or "partially oxidized cellulose" are preferable. propylene glycol ether of methylcellulose--see (2-hydroxypropyl)methylcellulose. regenerated cellulose--cellulose regenerated from a solution of cellulose or from a cellulose derivative. sodium carboxymethylcellulose--see carboxymethylcellu lose. viscose--a solution ofsodium cellulose xanthate prepared by dissolving the reaction product formed by the interaction of carbon disulfide and alkali cellulose in an aqueous solution of sodium hydroxide. Viscose is used mainly in the manufacture of rayon or cellophane, where it is extruded through fine openings of the proper shape into a coagulating bath. I 287 1 DU P050296808  0 1695 (C) PROPERTIES OF CELLULOSE AND ASSOCIATED CONCEPTS accessibility--the fraction of total cellulose present that is accessible to certain reagents under certain specified con ditions. The conditions of determination should always be indicated. acetylation--substitution of an acetyl radical for an active hydrogen. Specifically, formation of cellulose acetate from cellulose. acetyl groups--the characteristic groups of acetic acid; CH3CO--. acyl groups--radicals derived from carboxylic acids by removal of the hydroxyl group, acid groups--functional groups having the properties of acids. In cellulose and its derivatives, these are usually carboxyl groups. aging--in general, the change of properties with the passage of time. Specifically, the changes occurring in shredded alkali cellulose when allowed to stand exposed to air. air-dry--a condition applied to paper or pulp whereby its moisture content is in equilibrium with the atmospheric conditions to which it is exposed. According to trade custom, pulps are generally understood to be air dry when they contain 10 % of moisture, for example, a pound of air-dry pulp contains 0.9 lb of oven-dry pulp and 0.1 lb of moisture (see STP 60-B): alcohol-benzene solubility--solubility of a cellulosic pulp in a mixture of ethanol and benzene. The term is without precise meaning unless complete specification of an ana lytical procedure is attached explicitly or implicitly, aldehyde groups--carbonyl groups to which a hydrogen atom is attached; the first oxidation stage of an alcohol; --CHO. alkali resistance--for a cellulosic pulp, the fraction insoluble in alkali, usually sodium hydroxide, of a fixed concentra tion under specified conditions. The term is without precise meaning unless complete specification of an ana lytical procedure is attached explicitly or implicitly, (see also alkali solubility) alkali splubility--for a cellulosic pulp, the fraction in alkali of a fixed concentration under specified conditions. This term is without precise meaning unless complete specifica tion of an analytical procedure is attached explicitly or implicitly. Some related terms imply at least a partial specification, for example, "ten percent potassium, hy droxide solubility"' or "nondilution alkali solubility." alkali staining--discoloration caused by the presence of an alkali. alkyl groups--monovalent aliphatic radicals derived from aliphatic hydrocarbons by removal of a hydrogen, amorphous regions--those regions within a cellulosic mate rial which, on the basis of X-ray diffraction or other suitable technique, do not show any evidence ofcrystalline structure. The technique, should be specified, anhydroglucose units--the repeating unit of many poly saccharides, including cellulose; since the glucose mole cules have combined with elimination of water, the unit is called "anhydroglucose" rather than "glucose." ash--the inorganic residue obtained by igniting a specimen of pulp, paper, or other cellulosic material in such a way that all combustible and volatile compounds are removed. Conditions of ashing should be specified, bleachability--the capacity of a pulp to bleach to a given whiteness. This is approximately and indirectly related to lignin content. bone-dry--see oven-dry. brightness--as commonly used in the paper industry, the reflectivity of a sheet of pulp or paper for blue light measured under standardized conditions on a particular instrument designed and calibrated specifically for the purpose. carbonyl group--the bivalent radical, --CO--, especially as it occurs in aldehydes or ketones, carboxyl group--the radical --COOH characteristic of most organic acids. CED (cupriethylenediamine) viscosity--see viscosity, cupriethylenediamine. chain length distribution--in a linear polymer like cellulose, the frequency distribution of molecular size, usually ex pressed in units of degree of polymerization, chlorine number--the number of grams of chlorine gas or of bleaching powder (expressed as its equivalent in chlorine) that is consumed by 100 g of ovendiy pulp in a definite time under certain specified conditions. The chlorine number is an indication of the bleach requirement of the pulp and an indirect estimate of the lignin content, color reversion--a process common to almost all bleached cellulose pulps in which the color darkens to a greater or lesser extent on standing. commercial moisture regain--see moisture regain, commer cial. copper number--the number of grams of copper ih the cuprous oxide reduced from a cupric compound by 100 g of pulp or paper (after deduction of moisture, aSh, and sizing materials) treated under specified conditions with an excess of cupric solution. The copper number is an indication of die relative number ofreducing groups in the pulp or paper. cross linking--the reaction of a difunctional molecule with each of two molecules of a polymer. This change of the polymer from linearity produces profound changes in the physical properties. crystalline regions--see crystallinity, crystallinity--a regular arrangement of tile atoms of a solid in space. In most polymers, including cellulose, this state is usually imperfectly achieved. The crystalline regions (or dered regions) are submicroscopic volumes in which there is more or less regularity ofarrangement ofthe component molecules, In these regions there is sufficient geometric order to enable definite X-ray diffraction patterns to be obtained, (see also degree of crystallinity; degree of order) crystallinity index--a number used to represent the state of crystallinity of cellulose as a whole. Unfortunately, it has been differently defined by different investigators and should not be used unless it is clearly stated which crystallinity index is meant, (see also crystallinity) crystallite--a single crystalline region, (see also crystallinity) cuam viscosity--see viscosity, cuprammoniiun. cuene viscosity--see viscosity, cupriethylenediamine. cuprammonium process--a process for making rayon by dissolving cellulose in an ammoniacal copper solution and 288 jljP!.M11 *11!1,'.WIPE*1" I ri 1 111111........ I DUP050296809 <) D 1695 aing the resulting solution into an acid bath, thereby Generating the cellulose as fibers. mmmonium viscosity--see viscosity, cuprammonium. 1sthylenediamine viscosity (cuene or CED)--see vis- pty, cupriethylenediamine. lotion--in general chemical use, the conversion of a aplex compound to a simpler. Specifically for cellulose, I breakdown of the polymer chain, usually by hydrolysis | oxidation. Degradation is usually applied to changes in aical structure, (see also deterioration) ee of crystallinity--the fraction by mass of a cellulose aple occurring in crystalline regions. The method of ffetermining crystallinity must be stated, (see also crystal linity) fee of lateral order--the relative degree of molecular lignment. As for degree of crystallinity, quantitative values must be defined in terms of the experimental fbeasurements. (see also crystallinity) |pfee of polymerization, DP--in general, the average ffiumber ofbase units, or of monomeric units per molecule |jn linear polymers. Specifically, the average number of 'tjnhydroglucose units (or derivative units) per molecule of (cellulose (or cellulose derivative). The type of average obtained depends upon the method used for the determiT nation. Hence, the method must always be specified. |jegree of substitution, DS--in a cellulose derivative, the average number of hydroxyl groups substituted per anhydroglucose unit. DS varies from zero to about 3. ilensity--the mass per unit volume at a specified tempera ture. apparent--the mass per unit volume of a sheet of pulp or paper. It is commonly calculated by dividing the basis weight by the caliper, although it must be recognized that the numerical value thus obtained is dependent upon the definition of the ream. I density, bulk--the mass of a cellulosic material that will fill a unit volume of a container under specified conditions. I deterioration--a permanent impairment of the physical properties, (see also degradation) | dry weight--a term is usually applied to the mass of the ovendry material, but it is ambiguous unless the method of drying is specified. end groups--the functional groups at either end of the cellulose molecule. It is frequently used for the terminal glucose units that contain these groups. It is usually clear from the context which is meant, and the differentiation is seldom important. One end group is reducing (probably a bemiacetal) and one nonreducing (a free hydroxyl in the 4-position). equilibrium moisture content--the percentage mass of mois ture in a material when it has attained equilibrium with water vapor at a specified pressure or partial pressure. It is determined by successive weighings of the sample, either on the adsorption or desorption curve, and plotting moisture content against the logarithm of time. It should be designated as adsorption equilibrium or desorption I equilibrium. exchange capacity--see ion-exchange capacity, fiber--the unit cell of vegetable growth, which is many times longer than its diameter and which consists largely of cellulose. It is the basic unit of pulps and papers. fiber length--when applied to a pulp, this applies to the mean fiber length and both the experimental details and the calculations must be specified, fiber length distribution--the frequency distribution of the individual fiber lengths in a material about the mean fiber length. fiber saturation point--the moisture content in the absorp tion of water by cellulose when the cell walls are saturated, but virtually no free water is present in the grosser capillary structure. The concept is based on the hypothesis that a discontinuity occurs in the sorption curve at this point Some careful studies of the region have Med to show a discontinuity, but it is still possible to define "fiber saturation point" as an extrapolation of the adsorption curve. In any case, it should only be used with reference to the method of determination. fiber structure--the morphological structure of a fiber at the visual or microscopic level, (see also fine structure) fibril--a fiberlike bundle of molecules, oriented in one direction either with the fiber axis or spirally around it. It makes up the fibrous structural unit of the single fiber. The cellulose fibrils are crystalline as shown by X-ray diffrac tion. film--sheeting, including that composed of cellulose or its derivatives, having nominal thickness not greater than 10 mils, (see also films) films--transparent sheeting. If this is used as a generic term, regardless of sheet thickness, the plural should be used and the singular restricted to a specified size, (see also film) fine structure--a generic term denoting the submicroscopic structure that depends on molecular arrangement, fluidity--the reciprocal of viscosity, gamma number--degree of substitution.. (DS) X 100. This term is of widespread use in the cellulose xanthate field, gloss--the geometrically selective reflectance of a surface responsible for its shiny or lustrous appearance. Surface reflectance is commonly at a maximum in or near the geometric directions in which a mirror would reflect light, hardness--a term referring to the degree of cooking of a pulp. A hard pulp is one in which the residual lignin content is relatively high. - . haze--the turbidity produced by the material in some cellulose derivatives that is not completely soluble in the medium. This turbidity may refer to solutions or to the solid plastic. bemiacetal groups--functional groups derived from carbonyl groups by addition of one molecule ofan alcohol, of the general structure: OH -c7 ^OR hornification--the behavior of certain forms of cellulose and related materials on drying, which results in a lowered reactivity. This is apparently caused by the formation of new hydrogen bonds with a corresponding decrease in accessibility. hydrodynamic specific surface--the specific surface of a fibrous material as measured by the filtration resistance of a compacted pad formed from a fiber suspension under specified conditions. 289 DUP050296810 D 1695 hydrophilic--having an affinity for water, hydrophobic--having an antagonism to water, hydroxyl groups--the monovalent group --OH, character istic of hydroxides and alcohols. inherent viscosity--see viscosity, inherent. intrinsic viscosity--see viscosity, intrinsic, ion exchange--a reversible process by which ions are inter changed between a solid and a liquid with no substantial structural changes in the solid, ion-exchange capacity--for cellulosic ion-exchange matei rials, the number- of milliequivalents of ions that can be exchanged by 1 g of the ion-exchange material, ion-exchange materials--insoluble solid materials with the ability1to exchange reversibly certain ions, in the structure or attached to the surface as functional groups, with ions in a surrounding medium. iron-sodium tartrate, EWNN or FeTNa--a complex tartaric acid salt of sodium and ferric iron. Solutions in aqueous sodium hydroxide will dissolve cellulose. Both the German abbreviation, EWNN, and the English, FeTNa, are to be found in English articles. The details of preparation of the solution should always be given, iron-sodium tartrite viscosity--the viscosity of a solution or dispersion of cellulose or pulp under standardized condi tion when dissolved in the iron-sodium tartrate solvent, (see also iron -sodium tartrate) kappa number--the number of millilitres of 0.1 N potassium permanganate solution consumed by 1 g of ovendry pulp under specified conditions. It is an indication of the hardness or bleachability ofa pulp. An indirect estimate of lignin content. lateral order--the degree of regularity of arrangement of atoms and atomic groups in the direction normal to the molecular chain axes in linear polymers. Quantitative evaluation is impossible without further specification and without description of the particular experimental tech nique. leveling-off degree of polymerization, LODP--the nearly constant degree of polymerization of cellulose reached after very prolonged mild hydrolysis or short drastic hydrolysis. limiting viscosity number--see viscosity, intrinsic, luster--in the pulp and paper industry, synonymous with "gloss" or "sheen." (sea also gloss) mercerization--the process of subjecting a vegetable fiber to the action of a fairly concentrated aqueous solution of a strong base so as to produce great swelling with resultant changes in fine structure, dimensions, morphology, and mechanical properties. mesomorphous cellulose--those portions of cellulose in which the segments of the individual molecules have some regularity of arrangement, but not enough to permit strict lattice order to give a distinct X-ray diffraction pattern, methoxyl group--the monovalent group --OCH3, character istic of methyl alcohol and its esters or ethers, moisture content--the moisture present in a cellulosic mate rial, as determined by prescribed methods, conventionally expressed as a percentage of the total mass of the "wet" material. moisture equilibrium--the condition reached by a sample i when it no longer takes up moisture from, or gives up moisture to the surrounding air. moisture equilibrium for preconditioning--the moisture equilibrium condition reached by a sample after free exposure to air controlled at the standard condition for precondi tioning. moisture equilibrium for testing--the equilibrium moisture condition reached by a sample after free exposure to moving air controlled at standard conditions, moisture regain--the moisture present in a cellulosic mate rial, as determined by prescribed methods, expressed as a percentage of the ovendry mass, moisture regain, commercial--an arbitrary figure formally adopted as die regain to be used in calculating the commercial or legal mass of shipments or deliveries ofany specific material. moisture regain, standard--the moisture regain of sample brought from a lower moisture regain into equilibrium with the standard atmosphere, moles of substituent combined, MS--in a cellulose deriva tive, the average number of substituent molecules per glucose unit For most derivatives, MS = DS, hut for a few, such as hydroxyethylcellulose, the substituted group may also be reactive and MS may be greater than DS. , nonreducing end groups--those terminal glucose; units of cellulose or its derivatives which contain a free hydroxyl in the 4-position and do not reduce Fehling's solution or similar reagents. oleoresins--nonaqueous secretions of resin adds, dissolved in terpenic hydrocarbons that are produced, or exudfed from the intercellular resin ducts of living trees, especially the conifers, and accumulated, together with oxidation products, in the wood of weathered limbs or stumps.^ order distribution--see lateral order, orientation--the angle made by the crystallites of-fhe. cellu lose with the fiber axis. This is approximately the same angle as that made by the molecules or the fibrilSs - overdry--the state of a cellulosic material that has been dried to constant mass at a temperature of 100 to 105e. - percent hydrolysis-resistant celluIose-Mhe residue after treatment ofcellulose with add under spedfied conditions, expressed as a percentage of the original. permanganate number--the number of millilitres of 0.1 N potassium permanganate solution that is consumed by 1 g of ovendry pulp under certain spedfied and carefully controlled conditions. It is an indication of the hardness or bleachability of a pulp. It also is an indirect estimate of lignin content. plastic--(I) capable of being deformed continuously and permanently in any direction without rupture, under a stress exceeding the yield value. (2) made of, Consisting of or pertaining to plastics. (2) a material containing as an essential ingredient an organic substance of large molec ular mass, which is Solid in its finished state and, at some stage in its manufacture or in its processing into finished articles, can be shaped by flow, porosity--the existence in a material of connected air voids. It is frequently expressed as the ratio of void volume to total volume. 290 DUPO50296811 # D 1695 tivity--the ability to react. For proper use of the term, ie reaction in question and the conditions should be stated and the parameter used in measuring reactivity idicated, such as rate, uniformity, or the like. 'uced viscosity--see viscosity, reduced. [ucing end groups--those terminal glucose units in cellu lose or its derivative!! in which the 1-position is not ubstituted or involved in a glycosidic linkage. These end ups will reduce Fehling's solution or similar reagents. ain--see moisture regain. Hive viscosity--see viscosity, relative. Crsion--in general, the tendency of pulp or paper properes to return to those of the material at some other stage. : is frequently specifically applied to the loss of brightness :%ith time, after bleaching has produced a high brightness, jening--in the manufacture of viscose rayon, that stage rwhere the cellulose xanthate solution is stored several days under controlled conditions to reach a state from which coagulation is easier. |yer---a continuous strand of loosely assembled fibers that 'is approximately uniform in cfoSs-sectional area and ^Without twist. ipecific gravity--the ratio of the mass of a specimen to the mass of ah equal volume of water; both at the same Specified temperature. Generally, density is more useful, (see also density) [specific surface--the surface per unit mass (or less frequently || per unit volume) of a moisture-free sample. The specific J! external surface is used as a measure of the degree of fineness of fibrillation. jj[specific viscosity--see viscosity, specific. standard moisture regain--see moisture regain, standard, surface area--the total area of the surface. As usually used 1 for reactive pulps, this applies not to external surface, but to the internal surface as well, the total surface available to gases or penetrating liquids. It is useful to express this as specific surface, area per gram, swelling--increase in volume and dimensions caused by penetration of a liquid. total internal-surface--the surface of a cellulosic material available for absorption of a given substance. A useful substance for this purpose is water; the value obtained with water is close to the potential maximum surface that can be developed without disruption of the crystalline struc ture. unit cell--a parallelepiped element of crystal structure, containing a certain number of atoms, the repetition of which-through space will build up the complete crystal, uronic adds--oxidation products of the sugars in which a primary alcohol group has been oxidized to a carboxyl without changing the reducing functional group, viscosity--in general, the resistance of a fluid to flow or motion within itself. As applied to cellulose or its deriva tives, the viscosity of a solution of the substance. viscosity, cuprammonium--the viscosity of a solution or dispersion of cellulose or pulp in cuprammonium hy droxide under standardized conditions, viscosity, cupriethylenediamme--the viscosity of a solution or dispersion of cellulose or pulp Under standard condi tions when dissolved in a solution of copper hydroxide in ethylenediamine. viscosity in absolute units, CGS poises--the force in dynes required to move, at a velocity of 1 cm/s, one surface having an area of l cm2 past another parallel-like surface 1 cm away, overcoming the resistance to shear of the material filling the space between, viscosity index--the ratio of the viscosity of a highly concen trated solution to that of a dilute solution. It is a measure of solvent power and, in derivatives, of uniformity of substitution. viscosity, inherent--the quotient of the natural logarithm of relative viscosity by the concentration, that is, in j ^/78 The concentration should be specified, viscosity, intrinsic--the limiting value of reduced viscosity, ijsp/c, as c (concentration) approaches zero. In the cellu- losic field the concentration is generally expressed as grams per decilitre. The IUPAC Committee of Nomenclature has recommended the expression "Limiting viscosity number" for this and the concentration is generally expressed as grams per millilitre. viscosity number--see viscosity, reduced. viscosity ratio--see viscosity, relative. ; viscosity, reduced--the . specific viscosity divided by the concentration. In the cellulosic field the concentration is generally .expressed as grams per decilitre. The IUPAC Committee on Nomenclature has recommended the ex pression "viscosity number" for this, in which case the preferred expression of concentration is grams per millilitre. viscosity, relative--the ratio of the viscosity of a solution to that of the pure solvent. The IUPAC Committee on Nomenclature has recommended the expression "Vis cosity ratio" for this. - vfecosity, specific--the difference between the viscosity of a solution and that of a solvent, divided by the latter, viscosity, xanthate--for a ceilulosic pulp., the viscosity ofthe viscose that will be obtained as a result ofa specified series of processes; ~ viscous flow--flow, usually at low velocity, in which fluid - elements flow in a straight line parallel to the direction of flow of the liquid in the absence of turbulence.. water vapor permeability--the rate of water vapor transmis sion per unit of thickness and per unit of vapor pressure differential. Test conditions must be specified, whiteness--the degree of approach of the color of a sub stance to that ofthe ideal white, commoiily represented by a standardized preparation of magnesium oxide. xanthate viscosity--see viscosity, xanthate. The American 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 are expressly advised that determination ol the validity oi any such patent rights, and the risk of Infringement of such rights, ere 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. Yourcomments are invitedeither 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. 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. 291 DUP050296812 Designation: D 1696 - 90 Standard Test Method for Solubility of Cellulose in Sodium Hydroxide1 This standard is issued under the fixed designation D 1696; 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*2 1is intended for application to dissolving-type cellulose pulps prepared from cotton or wood. The procedure is not directly applicable to unrefined pulps for use in chemical conversion processes because solubility equilibrium may not be attained within the speci fied extraction 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 ofthe user ofthis 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: D1193 Specification for Reagent Water3 D1347 Test Methods for Methylcellulose4 D1348 Test Methods for Moisture in Cellulose4 2.2 TAPPI Standard: T 429 Method for Alpha-Cellulose in Paper5 3. Summary of Test Method 3.1 Pulp is steeped in a sodium hydroxide solution of a specified concentration for 1 h at 20C. The soluble fraction is estimated by dichromate oxidation of the filtered steeping alkali. The concentration of sodium hydroxide used in the pulp extraction process must be reported as part of the analytical result. Sodium hydroxide concentrations of 10,18, and 21.5 % are most frequently used. Data are reported as percent of dry sample weight. 3.2 The extraction procedure avoids dilution sequences, and therefore, the results are not comparable to data obtained by the alpha, beta, gamma methods of pulp fractionation (see TAPPI Method T 429). The terms "alpha," "beta-," or "gamma-" cellulose must not be applied to any test values obtained by this procedure since they are defined only by the method of their determination. 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 1.36 on Celiuiosics. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1696 - 59. Last previous edition D 1696 - 61(1985)". 1 This test method is an adaptation of the method designated CCA 8:55 by tbe Analysis Committee of the Central Committee of the Cellulose Industry of the Swedish Association of Pulp and Paper Engineers. This test method is also comparable with the TAPPI Tentative Standard T 235 m-58, Solubility of Pulp in Cold Sodium Hydroxide. 5 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.02. 5 Annual Book ofASTM Standards, Vol 15.09. 3.3 The essential feature of the method is . to prepare sodium hydroxide extracts and oxidize the soluble material with dichromate as described Alternative methods of esti mating dichromate by titration with ferrous ammonium sulfate and sodium thiosulfate are described. 4. Significance and Use 4.1 The measurement of soluble oxidizable components ofcellulose in sodium hydroxide is indicative of the purity of the cellulose sample, since pure cellulose is insoluble in sodium hydroxide. The extracted components are typically hemicelluloses, which are naturally present in the wood. Differences in pulp purity can have a dramatic impact on the processing and properties of the cellulose derivatives pro duced from the pulp. 5. Apparatus 5.1 Constant-Temperature Bath--A water bath main tained at 20 0.2C. 5.2 Stirrer--Mechanical stirrer as shown'in Fig. 1. All parts in contact with solutions must be of stainless steel. The stirrer motor shall be a variable speed laboratory motor with 1500 rpm max speed 5.3 Fritted-Glass Filter Crucible--A fritted-glass filter crucible, coarse porosity (pore size 40 to 60 pm), of 3Q;mL capacity. 5.4 Electrometric Titration Apparatus--For estimatiori of dichromate by titration with ferrous ammonium sulfate. An indicator may be used as described in_8.6, but, for rapid, accurate analysis an electrometric apparatus is recom mended. 6. Purity of Reagents 6.1 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,6 where such specifications are available. 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 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specifi cation D 1193. 6 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." i I I i 1 s 292 DUP050296813 In. y mm 3.2 Vt % 1 314 6.4 12.7 19.0 25.4 82.6 FIG. 1 Design Details of Mechanical Stirrer 6V2 165.1 m 219.1 17. Reagents i 7.1 Ferroin (0.025 M)--Dissolve 1.48 g of orthophenan; throline monohydrate (or 1.624 g of the hydrochloride) with 0.695 g of ferrous sulfate (FeSO,,) in water and dilute to 100 mL. It 7.2 Ferrous Ammonium Sulfate Solution (0.1 N)--Dis solve 40 to 41 g offerrous ammonium sulfate (FeS04(NH4)2S04-6H20) in water containing 10 mL of H2S04 and dilute to 1 litre in a volumetric flask. Standardize the solution daily against potassium permanganate (KMn04). 7.3 Potassium Dichromate Solution (20 g/L)--Weigh 20.0 g of potassium dichromate (K2Cr207), transfer to a 2-L beaker, and dissolve in approximately 700 mL ofwater. Add, with constant stirring, 150 mL of H2S04. Allow to cool to room temperature. Dilute to 1 L with' water. 7.4 Potassium Iodide (KI).7 7.5 Sodium Hydroxide Solution--Dissolve solid sodium 7 This reagent is required only for the iodomctric method for measuring dichromate (see 8.7). Thyodene, supplied by Fisher Scientific Co., Pittsburgh, PA is an acceptable substitute. hydroxide (NaOH) in an equal weight of water. Cover and; allow to stand about one week to permit-settling pf sodium carbonate (Na^jCOj). Prepare the dilute NaOH solutions listed below by approximate addition of freshly boiled water to portions of the concentrated stock solution* Use a siphon' to withdraw the required volume of 50 % NaOH solution from the stock bottle; do not disturb the Na2C03 precipitate. The Na2C03 content of the dilute solutions should not exceed 1 g/L. Standardize the final dilute solutions by titration with standard acid. 7.5.1 Sodium Hydroxide Solution (10 %y--Prepare a so lution containing 10.0 0.1 g NaOH per 100 g of solution. Specific gravity at 20/4C is 1.1089. This solution is 2.77 N. 7.5.2 Sodium Hydroxide Solution (18 %)--Prepare a so lution containing 18.0 0.1 g NaOH per 100 g of solution. Specific gravity at 20/4C is 1.1972. This solution is 5.39 N. 7.5.3 Sodium Hydroxide Solution (21.5 %)--Prepare a solution containing 21.5 0.1 g NaOH per 100 g ofsolution. Specific gravity at 20/4C is 1.2356. This solution is 6.64 N. 7.6 Sodium Thiosulfate Solution (0.1 Nf--Prepare and standardize 0.1 N sodium thiosulfate (Na2S203) solution as directed in 23.1 i of Test Methods D 1347. 293 DUP050296814 # D 1696 7.7 Starch Solution (5 g/L).6 7.8 Sulfuric Acid (sp gr 184)- -Concentrated sulfuric acid (H2S04). 8. Preparation of Samples 8.1 Condition the air-dry pulp samples to obtain moisture equilibrium by exposing them to the atmosphere for 24 h in the room where the portions of this sample will be weighed for moisture and solubility analysis. 8.2 If the pulp is in sheeted form, tear it into pieces about 10 mm square. Do not use cut edges. Weigh a portion for moisture analysis and immediately also weigh, to the nearest 1 mg, about 1.6 g of the air-dry sample for the solubility determination. 8.3 Determine the moisture content ofthe air-dry sample in accordance with Test Methods D 1348. Calculate the oven-dry weight of the sample for the solubility determina tion. 9. Procedure 9.1 Precool the NaOH solutions to 20C. Pulp solubility in 18 and 21.5 % NaOH solutions is not affected by a few degrees variation in temperature. Hence, temperatures of 20 2C are satisfactory in this case. However, pulp solubility in 10% NaOH solution is very sensitive to temperature variation. The operator must control temperature to 20 Q.2C in all phases of pulp extraction with 10 % NaOH solution. 9.2 With a pipet or buret, transfer 100 mL of the NaOH solution of the desired concentration (10,18, or 21.5 %) into a 250-mL beaker. Add the 1.6 g air-dry pulp sample to the solution. Allow the pulp to swell for 2 min; then introduce the stirring apparatus into the beaker so that the surface of the liquid coincides with the draft tube top. Disintegrate the pulp by stirring for 3 min (Note 1). Adjust the stirring speed to prevent addition of air to the slurry (about 1500 rpm). Remove the stirrer. Carefully clean the stirring apparatus and walls of the beaker with a glass rod so that all pulp fibers are retained in the alkali. Cover the beaker with a watch glass and leave in the 20<'C bath until a total of 60 min have elapsed from the time of addition of NaOH to the sample. For solubility determinations in 10 % NaOH solution, all extraction operations must be performed with the sample container in the constant-temperature water bath. In work with 18 or 21.5 % NaOH, the sample container may be removed from the bath for the disintegration process. 9:;< 1--Most pulps are completely disintegrated after 3 min. A reasonable increase in the time ofdisintegration does not sensibly affect the solubility. On the other hand, low values are obtained if the disintegration is not complete. The stirrer should, therefore, be run until complete disintegration is obtained, even if the time required exceeds 3 min. 9.3 At the end of the 1-h total extraction time, remove the beaker from the bath and immediately filter the slurry through a coarse fiitted-glass filter. Apply suction but do not pull air through the cellulose mat on the filter. Discard the first 10 mL of filtrate. If suspended fibers are noted in the filtrate, recycle the filtrate through the cellulose mat to clarify. Retain the filtrate in a stoppered Erlenmeyer flask. 9.4 Transfer 10-mL aliquots of the NaOH filtrates to 250-mL Erlenmeyer flasks. Add 10 mL K2Cr207 solution to each flask; then carefully add 30 mL of H2S04 to each flask. After 10 min (Note 2), cool to room temperature. Include a blank test with the original NaOH extraction solution in this operation. =>?@ 2--It is suggested that heat be applied to maintain a tempera ture in the range of 125 to 130'C for the entire 10-min period. A reflux system is highly satisfactory. 9.5 The 10-mL aliquot of the NaOH filtrates specified in 9.4is generally suitable for dissolving-type pulps; however, if the alkali solubility is greater than 16 %, reduce the volume of filtrate to 5 mL and the volume of H2S04 to 25 mL. For pulps with alkali solubility less than 5 %, use 20 mL of filtrate and 45 mL of H2S04. 9.6 After dichromate oxidation, add 50 mL of water to each sample and the blank. Cool again to room temperature. Titrate the excess K2Cr207 with 0.1 N ferrous ammonium sulfate solution. An electrometric titrimeter is preferred for this operation. If this equipment is not available, ferroin indicator may be used to detect the end point. 9.7 An acceptable alternative for measuring dichromate concentration is to use iodometric methods. In this case, transfer the cooled solution with about 500 mL of water to a 1-L Erlenmeyer flask. Add about 2 g of K1 and after 5 min titrate the solution to a visual end point with 0.1 N Na2S203 solution, using starch as the indicator. Make a blank test on the original NaOH extraction solution in the same manner. 10. Calculations 10.1 Calculate the results, when obtained by titration with ferrous ammonium sulfate, as follows: Alkali solubility, % ~[(b -- a)N x 68.5]/mw (I) . where: a = ferrous ammonium sulfate solution required for titration of the sample, mL, b = ferrous ammonium sulfate solution required for titration of the blank, mL, N -- normality of the ferrous ammonium sulfate solu tion, - 68.5 = cellulose equivalent to '1-- milliequivalent of K2Cr.207, times 10 (Note 3), mg, m = filtrate used for oxidation, mL, and w = oven-dry weight of sample used, g.- =ABC 3--The factor 68.5 is the experimental value recommended in method CCA 8:55.2 As an alternative, the problem ofstandardization of ferrous ammonium sulfate can be handled in terms of oxidation of a reference cellulose solution prepared at each occasion for analysis as follows: Dissolve 200 mg (oven-dry weight) ofhigh-quality cotton linters pulp in H2S04 (3+1) (prepared by mixing 3 volumes of H2SQ4 (sp gr. 1.84) with 1 volume of water) and dilute to 100 mL with H2s64 (3+1). Do not use heat in the preparation of this solution. Immediately, after preparation, oxidize 2-mL aliquots of this solution in the procedure described in Section 8 for blank and sample treatment. Compare the cellulose solution and blank to express the concentration of ferrous ammonium sulfate solution in terms of milligrams of cellulose per millilitre of solution. The calculation then becomes: Alkali solubility, % = (10 C(b - a)]/mw (2) where: C = concentration of ferrous ammonium sulfate solution in terms of milligrams ofcellulose per millilitre, and b, a, m, w are defined as in 10.1. DUP050296815 Alkali solubility, % = [{F, - V%)N x 68.5]mw (3) '== Na2S203 solution required for titration ofthe sample, mL, = Na2S203 solution required for titration of the blank, mL, and = normality of the Na2S203 solution, and m and w are Report 1.1 Report the alkali solubility as a percentage of ovenpulp.to one decimal place. Use the symbol S for alkali solubility. Denote the strength of the sodium hydroxide solution by a numerical suffix, for example, designate the soouliubuiluittyj inFGH 1tv0 %/v NilaaOvHii.soovliutuiovnu buyy tihiive soyjmiiibwoil Sxj j oIJDK 11.2 If it is of interest to report the insoluble fraction, subtract the S value from 100. Use the symbol R, with the appropriate subscript, to report this value. For example: Rl0 = 100 - 5,0. 12. Precision and Bias 12.1 Precision--The relative standard deviation ofthe test method for all concentrations of sodium hydroxide is less than 4 %, 12.2 Bias--No statement of bias can be made as no suitable reference material exists for determining bias. The American Society (or Testing and Materials takes no position respecting the validity oi any patent rights assertedin connection with any item mentioned in this standard. Users of this standard are expressly advised that determination oi the validity oi 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 reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or tor additionalstandard? and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting oi 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. 295 DUP050296816 Designation: D 1716 - 62 (Reapproved 1987) Standard Test Method for Cellulose Chain Length Uniformity by Fractional Precipitation of Cellulose Nitrate1 This standard is issued under the fixed designation D 1716; the number immediately following the designation indicates the year or original adoption or, in the case of revision, the year oftast revision. A number in parentheses indicates the year oflast reapproval A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. The committeeresponsiblefor this standard has voted its withdrawal. In the absence ofsubstantial reasons that it should be continued, the Society will approve withdrawalfrom publication in February 1993. 1. Scope 1.1 This test method covers the determination ofthe chaift length uniformity of cellulose by fractional , precipitation of cellulose nitrate. It is recognized that this test method does not give absolute delineation of chain length; however, the curves obtained by this method afford a useful basis for comparing the relative chain length uniformity of different cellulose samples. It is applicable primarily to purified cellu loses. 2. Referenced Documents 2.1 ASTM Standards: D 301 Test Methods for Soluble Cellulose Nitrate12 D1193 Specification for Reagent Water3 3. Summary of Test Method 3.1 This test method is based on the following steps; 3.1.1 Conversion of the cellulose sample into cellulose nitrate by a nitration step that does not degrade the cellulose to any appreciable extent. 3.1.2 Separation of the cellulose nitrate into several vis cosity components through stepwise precipitation by the addition of a nonsolvent to a solution of the sample. 3.1.3 Measurement of the weight and viscosity of each recovered fraction and calculation of its average chain length (degree of polymerisation). 4. Purity of Reagents 4.1 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 available4. 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. 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 DO 1.36 on Celluiosics. Current edition approved Sept. 28,1962. Published November 1962. Originally published as D 1716 - 60 T. Last previous edition D 1716 - 60 T. 2 Annual Book ofASTM Standards. Vol 06.02. 3 Annual Book ofASTM Standards, Vots 06.03 and 11.01. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." . 4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specifi cation D 1193. PREPARATION OF CELLULOSE NITRATE 5. Apparatus, 5.1 Bottles, 2-oz (60-mL), wide-mouth, with plastic caps, 5.2 Constant-Temperature Bath, 0.0 0.5'C (ice water). 5.3 Erlenmeyer Flask, temperature-resistant glass, 200mL, standard-taper 45/50 neck, with glass stopper. 5.4 Filter Funnels, Buchner-type, 50-mm diameter with fritted disk, coarse porosity. 5.5 Mixer.5 5.6 Tamper, stainless steel rod, 40-mm diameter by 100mm. 5.7 Weighing Bottles, 40 by 100-mm, ground-glass stoppears. 5.8 Wire Baskets, 200-mesh stainless screen. 5.9 Oven, forced draft, 50C. 6. Reagents 6.1 Ethyl Alcohol--Neutral 95 % ethyl alcohol or neutral denatured alcohol with 0.5 % benzene (Formula 2B) or 10 % methanol (Formula 30). 6.2 Methanol, absolute. 6.3 Nitrating Acid Mixture (64 % HN03, 26 %H3P04, 10 % P2Oj)--Add very slowly with a- spatula 404 g of phosphoruspentoxide (P205) to 1000 g ofcold-white fuming nitric acid, swirled in a 2-L Erlenmeyer flask. Keep the-acid cold throughout the time of P2Os addition by keeping the flask immersed in the ice-water bath. 6.4 Nitric Acid (sp gr 1.49 to 1.50)--White fuming nitric acid. 7. Procedure 7.1 Place 2.0 0.1 g of the air-dry sample in the mixer and mix dry for about 30 s or until the material is uniformly fluffed. Transfer the fluffed material to a glass weighing bottle and dry for 1.5 h at 50 1C. Remove the sample from the oven, cover, and cool in a desiccator. 7.2 Weigh a 100-g portion of the nitrating acid into a glass-stoppered weighing bottle. Stopper the bottle and place it in the 0C constant-temperature bath. Allow time for the acid to equalize to the bath temperature. 3 An Osterizer or Waring Blender has been found satisfactory for this purpose. 296 DUP050296817 3 Weigh a 1-g portion (Note 1) of the dried cellulose pie to the nearest 0.001 g, and transfer it with stainless 1-forceps to the bottle containing the nitrating acid (0C). I to mix. Allow the bottle and contents to remain in the th for exactly 60 min, swirling at 10-min intervals. LMNOP 1--One gram of cellulose gives sufficient nitrate for viscosity isurement and a single fractionation. If duplicate fractionations, entage nitrogen, or stability tests are desired, use a blend of nitrates m multiple 1-g nitrations. || 7.4 At the end ofthe reaction period, transfer the contents the bottle to the Buchner-type, fritted-glass funnel. Apply cuum, pressing the cellulose nitrate down with the stain- i `steel tamper (Note 2). Continue pressing the cellulose Irate with the tamper while applying suction until excess id has just been removed. With forceps, quickly transfer e nitrate pad to 300 mL of water (0'C) and stir rapidly for veral seconds. Wash the nitrate with at least five 300-mL anges of water (room temperature). QRST 2--The stainless steel tamper is used to provide uniform ressure and to exclude air while removing excess nitrating acids; it also ~ds to form a loose pad of cellulose, which in most cases may be andled quickly and conveniently with tweezers to transfer to the water for drowning. An alternative procedure for removing the excess 'trating acid and drowning the nitrate is to apply vacuum cautiously bile squeezing the cellulose nitrate until oniy the minimum amount of ating acid to cover the sample completely remains. The sample is en flooded in the funnel under vacuum with 50 % aqueous acetic acid previously chilled to --10"G 7.5 Stabilize the cellulose nitrate by subjecting it to at least three 5-min boils in fresh 200-mL portions of water. Transfer the nitrate to the Buchner-type, fritted-glass funnel, and |drain with suction. Place the nitrate in the wire basket and Wry in the oven at 50"C for 1 h. Remove the nitrate from the Soven, transfer to a weighing bottle, cool in a desiccator, and weigh. If the nitrate is to be stored for more than a few days, ^transfer it to a 2-oz (60-mL) wide-mouth bottle, saturate it with ethyl alcohol, seal the bottle with a cap lined with tin !>foil, and place in a cool, dark cabinet. 8. Measurements on Fractionated Nitrate 8.1 Determination ofYield--Determine the moisture con tent for the pulp as nitrated. Consider the dried cellulose nitrate for practical purposes"to be moisture-free. Calculate the yield in percent by multiplying the quotient of nitrate weight divided by pulp weight by 54.6. UVWX 3--Depending on the type of cellulose, the yield value gives some indication ofthe degree ofnitration and the purity ofthe cellulose. As the specified nitration conditions give a high nitrogen content with pure cellulose, low yields should occur only with pulps of high pentosan content (xylan dinitrate) or with pulps of high lignin content. 8.2 Determination of Percentage Nitrogen--When de sired, determine the degree of nitration (percent nitrogen) by Specification and Methods of Test D 301. QYZ[ 4--Nitrates prepared by the procedure described in Section 7, from a pure cellulose, should contain 13.9 0.1 % nitrogen; they should have a stability of 20 to 25 min by Specifications and Methods D 301. It should be noted that the degree ofnitration does affect solution viscosity. and for samples with nitrogen contents outside the limits specified an adjustment must be made in the calculation of intrinsic viscosity.6 MEASUREMENT OF VISCOSITY 9. Apparatus 9.1 Bottles, 4-oz, narrow-mouth, with plastic caps. 9.2 Constant Temperature Bath, 25.0 0.TC. 9.3 Shaker.7 9.4 Stop Watch, reading to 0.1 s. 9.5 Tin Foil, 0.001 in. thick. 9.6 Viscometers, Cannon-Fenske, 0.4 to 0.5-mm bore capillary, 1-mL bulb,8 or Ubbelohde Type 1. \]^_ 5--It should be further specified that the viscometer have a flow time within the range of 70.0 to 100.0 s/mL at 25C for the solvent being used in order to avoid a kinetic energy correction. 9.7 Oven, forced draft, 50C. 10. Materials 10.1 Ethyl Acetate, reagent-grade. 11. Procedure 11.1 For a preliminary check of the viscosity, weigh a 0.0500 0.0001-g sample of nitrate (redried for 1 h at 50C and cooled just prior to weighing), place it in a 4-oz (120-mL plastic capped bottle, add 100 mL of ethyl acetate from a pipet, cover the bottle with a cap lined with tin foil, and place it on the shaker until solution is complete. 11.2 Measure the flow time ofthe solvent and the solution in the viscometer. For the final determination, of viscosity, adjust the concentration of the nitrate solution to a value indicated by the following equation; C X DP - 50 (Section 12) 11.3 If the approximate degree of polymerization {DP) of the sample is known, select the appropriate concentration at the start; the initial measurement will then suffice. \]^_ 6--The time needed to obtain complete solution depends on the degree of polymerization and the degree of subdivision of the sample, usually running from a few minutes for rayon or cellophane to several hours for-very high viscosity wood pulps or raw cotton'. 12. Calculation of Degree of Polymerization fDP) . 12.1 Calculate the degree of polymerization, DP, as fol lows: DP = K[V) where: K = 75, M = intrinsic viscosity = (t?s,,/Q[l/(l + /c'^)], Vrei -- viscosity of solution/viscosity of solvent, ~Vsp Vret k' = 0.35, and, 6 Lindsley, C. H., and Frank, M. B., "Intrinsic Viscosity of Nitrocellulose Related to Degree of Nitration," Industrial and Engineering Chemistry, Vol 45, 1953, p. 2491. 7 A Burrell Wrist Action or International Shaker has been found satisfactory for this purpose. * This viscometer can be obtained from the Cannon Instrument Co., P. O. Box 16, State College, PA 16801. P DUP050296818 Vsp 0.005 0.010 0.015 0.020 0.025 0.030 0.035 0.040 0.045 0.050 0.055 0.060 0.065 0.070 0.075 0.080 0.085 0.090 0.095 0.100 0.105 0.110 0.115 0.120 0.125 0.130 0.135 0.140 0.145 0.150 0.155 0.160 0.165 0.170 0.175 0.180 0.185 foJC 0.0050 0.0100 0.0149 0.0199 0.0248 010297 0.0346 0.0394 0.0443 0.0491 0.0540 0.0588 0.0636 0.0663 0.0731 0.0778 0.0825 0.0873 0.0919 0.0966 0.1013 0.1059 0.1103 0.1152 0.1198 0.1243 0.1289 0.1335 0.1371 0.1425 . 0.1470 0.1615 0.1560 0.1605 0.1649 0.1693 0.1737 1.0 0.190 0.195 0.200 0.205 0.210 lv]C 0.178 0.183 0.187 0.191 0.198 TABLE 1 #8 0.375 0.380 0.386 0.390 0.395 Viscosity-Concentration Relationship MC 0.332 0.335 0.339 0.343 0.347 0560 0565 0.570 0575 0.580 UP 0.468 0.471 0.475 0.479 0.482 0.745 0.750 0.755 0.760 0.765 MC 0591 0593 0.597 0.600 0.603 Vs/? . 0.930 0.935 0.940 0.945 0.950 [v]C 0.702 0.705 0.707 0.710 0.713 0.215 0.220 0.225 0.230 0.235 0.200 0504 0.209 0.213 0.217 0.400 0.405 0.410 0.415 0.420 0.351 0.355 0.359 0.382 0.366 0.585 0590 0.595 0.600 ,0.605 0.486 0.489 0.492 0.496 0.499 0.770 0.775 0.780 0.785 0.790 0.607 0.609 0.613 0.616 0.619 0.955 0.960 0.965 0.970 0.975 0.716 0.7,19 0.721 0.724 0.727 0.240 0,246 0.250 0.255 0.260 0.221 0.226 0.230 0.234 0.238 . 0.425 0.430 0.435 0.440 0.445 0.370 0.374 0.378 0.381 0.385 0.610 0.615 0.620 0.825 0.630 0503 0506 0.509 0513 . 0.516 0.795 0.800 0.805 0.810 0.815 01622 0.625 0.628 0.631 0.634 0.980 0.985 0.990 0.995 1.000 0.730 0.733 0.735 0.738 0.741 0.265 0.270 0.275 0.280 0.285 0.242 0.247 0.251 0555 0.259 0,450 0.455 0.480 0.485 0.470 0.389 0.393 0.396 0.400 0.404 0.635 0.640 0.645 0.650 0.655 0.520 0523 0526 0.529 0533 0.820 0.825 0.830 0.835 0.840 0.637 0.640 0.643 0.646 0.649 1.005 1.010 1.015 1.020 1.025 0.743 0.746 0.749 0.752 0.754 0.290 0.295 0.300 0.305 0.310 0.263 0.267 0.272 0.276 0.280 0.475 0.480 0.485 0.490 0.495 0.407 0.411 0.415 0.418 0.422 0.660' 0.666 0.670 0.675 0.680 0536 0.539' 0.543 0546 0.549 . 0.845 0.850 0.855 0.860 0.865 0.652 0.655 0.658 0.661 0.664 1.030 1.035 1.040 1.045 1.050 0.757 0.760 0.763 0.765 0.768 0.315 0.320 0.325 0.330 0.3?5- 0,284 0588 0.292 0596 ,0500 . 0.500 0.505 0.510 0.515 0520 0.428 0.429 0.433 0.436 0.440 0.685 0.690 0.695 0.700 0.705 0553 0556 0.559 0.562 0.565 0.670 0.875 0.880 0.885 0.890 . 0.667 0.670 0.673 0.676 0.679 . 1.055 1.060 1.065 1.070 " 1.075 0.771- 0,773 0.776 0.778 0.781 0540 0.345 0550 0555 0560 0504 0.308 ; 0.312 Q.316 0.320 0.525 0.530 0535 0540 0545 0.444 0.447 0.451 0.454 0.458 0.710 0.715 0.720 0.725 0.730 0.569 0.572 0.575 0578 0581 , 0.895 0.900 0.905 0.910 0.915 0.682 0.684 0.687 0.690 0593 -.1.080 1.085 1.090 " 1.095 1.100 0.784 , 0.786 0.789 0.792 0:794 0.365 0.370 0.324 0.328 0.550 0555 0.481 0.465 0.735 ` 0.740 0.685 0588 0.920 0.925 0.696 0.699 Iil05 1.110 1.115 0.797 JQ.799 ' 0.802 C = concentration in grams of nitrate per 100 mL of solution. ' 12.2 To facilitate the calculation of intrinsic viscosity the relationship between rssp and [t j ]C is given in Table 1. FRACTIONATION OF CELLULOSE NITRATE 13. Apparatus 13.1 Centrijuge, with head and trunnion cups for 250-mL centrifuge bottles. 13.2 Centrifuge Bottles, 250-mL round-bottom, with tem perature-resistant caps, rubber, 1.5-in. (38.1 mm). 13.3 Constant-Temperature Bath, 25 0.1C. 13.4 Laboratory Stirrer, with a glass auger-type agitator, `/2-in. (12.7-mm) diameter. 13.5 Microburet, 10-mL, with 0.02-mL subdivisions. 13.6 Shaker.6 13.7 Spatula, stainless steel. 13.8 Oven, forced draft, 50C. 14. Material 14.1 Acetone-Water Mixture--Mix 91 volumes of acetone (reagent graide) with 9 volumes of water. TABLE 2 Sample Weight VersusDegree-of-Polymerization Level of Unfractionated Sample Degree=ot-Polymerization Level gof sample/200 mL of Solvent 3000 2000 1000 500 250 0.2 0.4 0.6 1.0 1.2 15. Procedure 15.1 Redry the nitrate sample for 1 h at 50C. Select from Table 2 the appropriate sample weight corresponding to the DP level of the unfractionated sample, and weigh the specified amount to the nearest 0.0001 g. Transfer the specimen to an 8-oz plastic capped bottle, add 200 mL ofthe acetone-water mixture, close the bottle with a cap lined with tin foil, and place it on the shaker to dissolve. `abc 7--The use ofthe 91+9 acetone-water mixture instead of pure acetone in the solution step gives faster dissolving action and at the same time brings the solution to the point ofthreshold precipitation, avoiding the necessity of adding relatively large amounts of water prior to precip- 298 P DUP050296819 D 1716 TABLE 3 Sequence of Water Addition Degree-of-Polymerization Level 3000 2000 1000 500 250 For Precipitation of Fraction Add Mllilitres of Water as Shown 0.5 0.7 1.2 1.7 2.7 0.2 0.2 0.3 0.3 . 0.3 Q.3 0.3 0.35 0.35 0.4 0.4 0.5 0.6 0.4 0.4 0.5 0.5 0.6 0.6 0.7 0.8 0.4 0.6 0.8 1.0 0.6 0.7 0.7 0.9 0.8 0.9 1.2 1.4 1.2 1.0 1.5 2.5 4.0 5.0 6.0 Evaporate to one half initial volume, cool, centrl- fags, decant Evaporate to one fourth Initial volume, cool, cen trifuge, decant Evaporate to dryness |oa ofthe first fraction. Mild, heating (3QC) is sometimes required to t solution, particularly of material of very high degree of polymer- |pn. In such cases, the tendency to gel formation can be lessened by ling the nonsolvent water first followed by addition of the acetone, ise additions would be in place of the 91+9 acetone-water mixture, i the quantities would remain the same. |5.2 Transfer the solution to a 250-mL, round-bottom jitfifuge bottle, and place it in' the constant-temperature ph at 25C. Immerse the tip of a microburet filled with ater in the solution, adjusting the position so that the auger jrrer and buret tip do not make contact. Stir the solution Jbidly and add the desired increment of water slowly from H buret. d efgh 8--The successive increments'of water that need be added in Tier to separate the sample into'about 12 fractions of roughly juivalent weight are critical. As a guide, Table 3 gives sequences of water additions that have been found to give satisfactory weight Separation at several initial DP levels for the sample weights outlined in "Table 2. Experience will help to judge minor adjustments that may be - . needed for various nitrates. Watch the precipitation carefully, and ifany r* precipitate tends to cling to the buret nozzle, remove it promptly to If;prevent the formation of large stringy masses; This tendency is apparent ,< only with,the early fractions of nitrate having a high degree of ?polymerization, particularly if .too high an initial concentration of pirate has been chosen. With proper precipitation technique, the fractions appear as finely divided floe.' . 15.3 After the precipitation of a fraction, cap the centriifuge bottle and centrifuge the dispersion until the precipitate has completely settled (approximately 5 min at 500 g). Decant the supernatant liquor into a second centrifuge bottle and set it aside for precipitation of the next fraction. 15.4 Transfer the settled residue, comprising the first fraction, to a weighing bottle. To facilitate drying, press the gel-like fraction into a thin film using the spatula to squeeze out the excess, liquid. Add 1 to 3 mL of water, to agglomerate (the higher degree of polymerization fractions agglomerate as films, the lower ones as powders). Whenever possible to do so without loss of nitrate, pour off die excess solution. Place the weighing bottle containing nitrate in the SOT oven until constant weight is attained (usually about 2 h). ijkl 9--For all but fractions with very low degree of polymeriza tion, the centrifuged residue can be shaken out ofthe centrifhge bottle in a relatively solid piece that requires no tinting for quantitative transfer to file weighing bottle. The fractions of a low degree of polymerization are somewhat more difficult to transfer, sometimes requiring a rinse for clean removal. 15.5 In a similar manner, precipitate and recover the next eight fractions. To recover fraction No. 10, evaporate on a water bath the supernatant liquor from fraction No. 9 to one half its initial volume, cool, centrifuge, and decant. In a similar manner, evaporate the supernatant liquor from fraction No, 10 to one halfits volume to recover fraction No. 11. Evaporate to dryness the supernatant liquor from frac tion No. 11 to obtain the final fraction. No. 12.-The entire precipitation fractionation should be completed within one 6-h period. 16. Measurements on Cellulose Nitrate Fractions 16.1 Determine for each fraction the weight of cellulose nitrate precipitated and the degree of polymerization fol lowing the procedure described in Sections 9 to 12. 16.2 Plot the integral distribution curve (degree, of poly merization versus cumulative percentage). and differential distribution curve (amount at each chain length versus degree of polymerization). . mfgh 10--To prepare the integral distribution curve, plot the cumulative percent as the abscissa and the degree of poiymerization-as the ordinate. To construct a differential plot draw a smooth curve through the stepwise integral plot, ignoring minor deviations from the mid-point of individual fractions. From this smooth curve pick the amount (in percentage of total) of material falling within successive suitably spaced degree-of-polymerization ranges^ for example, 0 to 25, 25 to 50, 50 to 100;-100 to 200, etc. Divide each percentage by the increment range of degree ofpolymerization covered to give the. average amount of each chain length in that increment. Plot this "amount for" each increment range" agaihst the degree of polymerization to give a stepwise differential curve. Draw a smooth curve through the stepwise curve ignoring minor deviations from the mid-point of individual steps in such a manner that the area under the curve totals 100 %. 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 that determination of the validity of any such patent rights, and the risk ol infringement of such rights, are entirely thaSr 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 invitedeither tor revision ofthisstandard 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 19103i IPPiPiP D UP050296820  Designation: D 1725 - 62 (Reapproved 1989)e1 Standard Test Method for Viscosity of Resin Solutions1 This standard is issued under the fixed designation D 1725; 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. nopq41 --Editorial corrections were made throughout in April 1989. 1. Scope 1.1 This test method covers the measurement of the viscosity of resin solutions. 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 154 Guide for Testing Varnishes42 1 1 D 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method3 3. Summary of Test Method 3.1 Solid resins are dissolved in organic solvents by cold-cut or hot-cut methods in the laboratory. The viscosity of such prepared solutions, or of commercial solutions of resins is then detennined by the bubble time method (Test Method D 1545). The bubble seconds are approximately equal to stokes. 4. Apparatus 4.1 Bath, constant-temperature, consisting of a cylindrical glass jar of about 5 -gal capacity, or an aquarium tank with controls capable of maintaining the temperature at 25 0.1C with water as the bath medium. 4.2 Bottles, 8-oz (225-mL), wide-mouth, screw cap. . 4.3 Cellophane, sheet," cut into 4 or 5-in. (102 or 127mm) squares. 4.4 Corks, No. 2 short taper, to fit viscosity tubes. 4.5 Holder for Viscosity Tubes,4 preferably a mechanical holder with rack and pinion for inverting the tubes. The holder should be checked with a small level and T-square to make certain it holds the tubes in an exact vertical position after being placed in the constant-temperature bath. 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 DO 1.33 on Polymers and Resins. Current edition accepted Sept. 28, 1962. Originally issued 1960. Replaces D 1725-60 T. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. ` A suitable mechanical holder is available from the Gardner Laboratory, Inc, 5521 Landy Lane, Washington, DC, Item 660. 4.6 Bottle Shaker, preferably one which will give endover-end agitation. 4.7 Timing Device, such as a stopwatch or electric stop clock capable of being read to a precision of 0.1 s. 4.8 Viscosity Tubes,5 of clear glass and flat bottoms, having 10.65 0.025-mm inside diameter and 114 1-mm outside length. Plainly legible lines shall be located on the tubes as follows: 27 0.5 mm 100 0.5 mm 108 0.5 mm All distances shall be measured from the bottom outside of the tube. The distance between the first and second lines shall be 73 0.5 mm. 5. Solvent 5.1 The solvent used should be mutually agreed upon between the purchaser and the. mah'Qfacturer. Toluene, xylene, mineral spirits, alcohols, etc., are used for the preparation of solutions of resins. For a given resin, the viscosity obtained will depend on the solvent used. In case of dispute, both laboratories should use portions of the same batch of solvent 6. Preparation of Resin Solutions . 6.1 The procedure employed for dissolving solid resins will be dependent upon the chemical nature of the resin under test.. Some resins will dissolve readily in cold solvent with moderate agitation, while others must be hot-cut in order to effect solution. The method of solution shall be agreed upon mutually between the purchaser and the seller since there may be differences in solubility or viscosity between solutions prepared with and without heat. The solvent concentration may vary from 30 to 90 % and- is generally selected to give a solution having a viscosity between 5 and 300 s. With hard resin use only material taken from freshly broken lumps. Do not use crushed or powdered material from the resin sample container. 6.2 Cold-Cut Solutions--Because it is not ..easy to tell when solution of the resin is complete, proceed exactly in accordance with the following directions, unless experience has shown that short cuts can be safely taken: 6.2.1 Prepare 100 g of solution as follows: Weigh an 8-02 (225-mL), screw-cap bottle, cap, and cellophane sheet to the 5 Viscosity tubes are available from the Gardner Laboratory, Inc, 552 i Land; Lane, Washington, DC, Item 555, or from the R. P. Cargille Laboratories, Inc. ! 18 Liberty St., New York, NY 10805. 300 I531S" DUP050296821 D 1725 -rest 0.05 g. Weigh into the bottle to the nearest 0.05 g the Jpropriate amount of solvent (40 g for a 60 % solution). |j|>2.2 Weigh into a beaker to the nearest 0.05 g the correct ount (60 g for a 60 % solution) of the freshly crushed an, passing a No. 10 (2000'-pm) sieve. li.2.3 Pour the resin slowly into the bottle containing the pvent, swirling gently so as to wet the resin as thoroughly as ssible as it is added. Place the cellophane sheet over the louth of the bottle and screw on the cap tightly. M.2.4 Immediately shake vigorously by hand and place on jphaker to give end-over-end agitation for an overnight Jfriod. 6.2.5 Check the weight of the bottle and solution to make ^ tain that none was lost during the mixing. If appreciable ss has occurred, discard the solution and prepare a fresh 1L.6.3 Hot-Cut Solutions: J|j5.3.1 Prepare 1(K) g of solution as follows: Weigh a JpO-mL Erlenmeyer flask with a ground joint to the nearest (.05 g. Weigh into the flask to the nearest 0.05 g the gppropriate amount of solvent (40 g for a 60 % solution). 6.3.2 Weigh into the flask to-the nearest 0.05 g the correct imount (60 g for a 60 % solution) of the freshly crushed re sin passing a No. 10 (2000-pm) sieve. Connect the flask to a t suitable air or water condenser and warm gently on a hot f; plate with swirling as necessary to prevent any charring or & scorching of the resin. Usually, the solution will be complete Tin 15 or 20 min. 6.3.3 When the solution is complete, cool the flask, jfdisconnect, and weigh. If over 0.1 g of solvent has been lost, jadd the necessary amount and swirl to mix. 6.3.4 If any air bubbles are present, allow the solution to jstand until they disappear. 6.4 Resins Supplied in Solution--ZThese resins ordinarily |can be tested for viscosity as received. However, if modifieaItion is necessary, such as a reduction to a specified solids content, use a solvent or solvent combination suitable for use with resin under test, as agreed upon between the manufac turer and the purchaser. 7. Procedure 7.1 Determine the viscosity of the resin solution in accordance with Test Method D 1545, repeating the timing determination until three readings are obtained that agree within 10 s or 3 % relative, whichever is larger. 7.2 For viscosities of solutions which have a timed bubble travel of 5 s or less, more precise results can be obtained by comparison against reference standards having predeter mined viscosity (Test Method D 154) or timed bubble travel (Test Method D 1545). Report : 8.1 Report the following information: 8.1.1 The mean bubble travel time, in seconds, as the viscosity at 25C, including: 8.1.1.1 Solution concentration, 8.1.1:2 Solvent used, and 8.1.1.3 Whether cold- or hot-cut solutions were used. 9. Precision 9.1 Repeatability and Reproducibility--Two results, each the mean of three readings, should be considered suspect if they differ by more than 7 % relative (95 % confidence level). rstuvThis estimate of precision is based on an interlaboratory study.6 Because the data showed no significant difference for between laboratory and within laboratory variances, the precision estimates for repeatability and reproducibility were pooled and a single value re ported. "For the results of the interlaboratory study, see Report of Committee D-l, Proceedings, ASTM, Vol 60, 1960. The American Society tor Testing and Materials takes no positionrsspecting the validity ot any patent rights assarted 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 at such rights, are entirely their own responsibility. ....... This standard is subject to revision at any time by the responsible technicalcommittee itni must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofOtis 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. 301 DUP050296822  Designation: D 1726 - 90 Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins1 This standard is issued under the fixed designation D 1726; the numberimmediately 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 (s) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the determination of the easily hydrolyzable chloride content of liquid epoxy resins which are defined as the reaction product of a chlorohydrin and a di- or polyfunctional phenolic compound. 1.1.1 In Test Method A, the easily hydrolyzable chloride is saponified with potassium hydroxide and directly titrated with hydrochloric acid. This test method can be used for concentrations of 1 weight % and below. 1.1.2 In Test Method B, the easily hydrolyzable chloride is again saponified with potassium hydroxide, then titrated potentiometrically with silver nitrate. This test method can be used for concentrations of 5 to 2500 ppm hydrolyzable chloride. 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. For specific hazard statements see Sections 8 and 14, 2. Referenced Documents 2.1 ASTM Standards: D841 Specification for Nitration Grade Toluene12 D 1193 Specification for Reagent Water2'3 3. Summary of Test Method 3.1 The sample is refluxed in the presence of a known amount of 0.1 N alcoholic potassium hydroxide. The amount of potassium hydroxide consumed in the hydrolysis is a measure of the hydrolyzable chloride content of the resin. 4. Significance and Use 4.1 The hydrolyzable chloride content of liquid epoxy resins is an important variable in determining their reactivity and the properties of coatings made from them. These test methods may be used to determine the hydrolyzable chloride content of manufactured epoxy resins and confirm the stated hydrolyzable chloride content of purchased epoxy resins. 5. Purity of Reagents 5.1 Reagent grade chemicals shall be used in all tests. 1 This test method is under the jurisdiction of ASTM Committee D-t on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.33 on Polymers and Resins. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1726 - 60. Last previous edition D 1726 - 87. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 11.01. 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,4 | where such specifications are available. 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. f 5.2 Unless otherwise indicated, references to water shall ? be understood to mean reagent water conforming to Type II j of Specification D 1193. | ! TEST METHOD A | 6. Apparatus 6.1 Reflux Apparatus, consisting ofa 250-mL Erlenmeyer flask attached to a reflux condenser and a hot plate with variable heat control. I ! 1 7. Reagents and Materials 7.1 Hydrochloric Acid, Standard (0.1 TV)--Dilute 9 mL of concentrated hydrochloric acid (HC1, sp gr 1.19) to 1 L with water. Standardize against 0.25 g of" sodium carbonate (Na2C03) accurately weighed and dissolved in 75 to 100 mL of water. 7.2 Methyl Ethyl Ketone. _ 7.3 Phenolphthalein Indicator Solution--Dissolve 1 g of phenolphthalein in 100 mL of methanol, ethanol, or isopropanol. .. . 7.4 Potassium Hydroxide, AlicohoL Solution (0J N)-- Dissolve 5.5J2 6.0 g ofpotassium hydroxide (KOH) in 1 L of methanol (99 %) or ethanol conforming to Formula No. SD-30 of the U.S. Bureau of Internal Revenue.-No standard ization of the solution is necessary. 7.5 Toluene (Warning--See Section 8.), conforming to Specification D 841. 8. Hazards 8.1 Hydrochloric acid and potassium hydroxide are corro sive. Toluene and methyl ethyl ketone are flammable and their vapors can be harmful. Precautions should be taken to avoid inhalation and skin or eye contact with these chemi cals. All sample preparations should be done in a well ventilated area, such as a fume hood. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." 302 1,) l"11) DUP050296823 ceduce 'Weigh to the nearest 1 mg, 6 to 8 g of neutral ten into a 250-mL glass-stoppered Erlenmeyer flask, eans of a pipet, transfer 50.0 mL of 0.1 N alcoholic ^solution' into the flask and add 15 mL of toluene. ` the flask and swirl to mix. Add a few boiling aids ach to the reflux conderfser on the hot plate; Allow the solution to reflux gently for 15 1 min. At Jod of the reflux period, remove the flask from the hot I and cool to room temperature with the condenser in Remove the condenser,, add 3 drops of phenolphtha- />}) indicator solution to the specimen, and titrate with 0.1 N The end point is taken when 1 drop changes the solu- wxyz from pink to colorless. - WO'T' E 1--Add 100 m' L of methyl ketone to the specimen if'required ^ ensure a homogeneous solution during titration of the excess KOH "Sion. . . r$A Make a blank determination on the reagents following the same procedure but omitting the specimen. Calculation 10.1 Calculate the weight percent hydrolyzable chloride tontent, H, of the specimen as follows: H=[(V-B)Nx3.55\/W (1) = HC1 required for titration of the blank, mL, = HC1 required for titration of the hydrolyzed spec imen, mL, = normality of the HC1, 55 = grams of chlorine per milliequivalent multiplied by the percentage factor of 100, and MW " specimen weight, g. Precision A 11.1 The following criteria should be used forjudging 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 0.02 % absolute, 11.1.2 Reproducibility--Two results obtained by opera- liprs in different laboratories should be considered suspect if jfhey differ by more than 0.05 weight %. TEST METHOD B 112. Apparatus 12.1 Reflux Apparatus, consisting of a 250-mL ErlenI meyer flask attached to a reflux condensor. 12.2 Hot Plate, with variable heat control. 12.3 Magnetic Stirrer, with polytetrafluoroethylene (PTFE)-coated stirring bar. 12.4 Buret or Automatic Titrator. 12.5 Silver Electrode or equivalent.5 12.6 Boiling Chips. 5 A Mettler DM Ml Silver Electrode, manufactured by Mettler Instruments, Princeton Hightstown Rd,, P.O. Box 71, Hightstown, NJ 08520, or equivalent has been found satisfactory for this purpose. 13. Reagents and Material 13.1 Acetone. 13.2 Bromcresol Green Indicator Solution (0.1 %)--Dis solve 0.1 g of bromcresol green in 100 mL of water. 13.3 Nitric acid, (HN03) (1 + 1), diluted with water. 13.4 Potassium Hydroxide, alcohol solution (0.1 N)-- Dissolve 5.6 g of potassium hydroxide (KOH) in 1 mL of methanol (99 %) or ethanol conforming to Formula No. SD-30 of the US Bureau of Internal Revenue. No standard ization of the solution is necessary. 13.5 Silver Nitrate, alcohol solution (0.0025 N)--Dissolve 0.425 g of silver nitrate (AgNOj), weighed to the nearest 1 mg, in 1 L of methanol (99 %) or ethanol conforming to Formula No. SD-30 of the US Bureau of Internal Revenue. Standardize against hydrochloric acid or sodium chloride solution (with traceability to an NIST standard). 13.6 Toluene. 14. Hazards , 14.1 Nitric acid, potassium hydroxide, arid silver nitrate are corrosive. Acetone and Toluene are flammable and their vapors can be harmful. Precautions should be taken to avoid inhalation and skin or eye contact with these chemicals. All sample preparations should be done in a well, ventilated area, such as a fume hood. 15. Procedure 15.1 Weigh 2 to 3 g of specimen, to the nearest 0.005 g, into a 250-mL Erlenmeyer flask. Add 20 mL of toluene, 20 mL of acetone, and 50 mL of 0.1 N alcoholic.KOH. Swirl or mix until dissolution is complete. 15.2 Add several boiling chips, connect the flask to the reflux condenser, and gently reflux for 15 1 min on a hot plate. 15.3 Remove the hot plate from under the flask and allow the flask and contents to cool to room temperature. Rinse down the condenser with acetone then remove from the flask. 15.4 Quantitatively transfer the contents-of the flask to a 250-mL beaker using acetone as wash-solution. Dilutethe solution to about 125 mL with acetone, insert a stirring bar, and place on a magnetic stirrer. 15.5 Add five drops of bromcresol green indicator. While stirring add 1 + 1 nitric acid dropwise just until the ' permanent color changes from blue to yellow. {|}~ 2--Caution--Do not add excess nitric acid. Do not acidify the solution until ready to begin the titration. Make certain that the solution is at room temperature before acidifying. These cautions are necessary to prevent the chloride results from being low due to recombination with the resin. 15.6 Titrate with 0.0025 N silver nitrate using the combi nation silver electrode and the automatic titrator or buret. 15.7 Reflux a blank, which includes all components except the sample, and titrate with 0.0025 N silver nitrate. 16. Calculation 16.1 Calculate the parts per million hydrolyzable chloride content, H, of the specimen as follows: H = l(V- B)N x 35.5 x Vpyw DUP050296824 # D 1726 where: B = AgN03 required for the titration of the blank, mL, V = AgNQ3 required for the fixation ofthe hydro lyzed specimen, mL, IV, . -- Normality of the AgN03, 35.5 x 103 = grams of chlorine per milliequivalent multi plied by the ppmconversion of 1 x 106, and W = specimen weight,g. 17. Precision ...... 17.1 A liquid epoxy resin, of approximately 150 ppm hydrolyzable .chloride was. sampled to five laboratories and seven analysts obtained the following results. 17.1.1 Repeatability--The difference between two results obtained by the same analyst should not vary by more than 8.32 % at the 95 % confidence level. 17.1.2 Reproducibility--The difference between two re sults, each the mean of two determinations, obtained by analysts in different laboratories should not vary by-more than 15.88 % relative at the 95 % confidence level. 18. Keywords 18.1 hydrolyzable chloride; liquid epoxy resin; saponifi able chloride The American Societyfor 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, are entirely theirown 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 commentsareInvitedeither forrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Yqur comments will receive careful consideration at a meeting of the responsible technical committee, which youMy 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.Rate St., Philadelphia, PA 19103. DUP050296825 Designation: D 1787 - 89 Standard Test Method for Pentosans in Cellulose This standard is issued under the fixed designation D 1787; 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 test methoci covers the determination 'of fans in cellulose by die orcinql colorimetric method, in ^ ge from less than 1 to about 16 %. ms. 1--This test method is an adaptation ofthe method designated 04:56 by the Analysis Committee of the Cellulose Industry of the pb Association of Puip and Paper Engineers. P: This standard may involve hazardous materials, oper as, and equipment. This standard does not purport to mess all ofthe safety problems associated with its use. It is mesponsiblity of the user of this standard to establish mpriate safety and health practices and determine the ficabiity ofregulatory limitations prior to use. Referenced Documents .1 ASTM Standards: 11193 Specification for Reagent Water12 11348 Test Methods for Moisture in Cellulose3 Summary of Test Method . 1 The cellulose is treated with boiling hydrochloric acid proxittiately 12 % or 3 + 7) to hydrolyze the pentosans to tttoses, which are then converted to fbrfural." The furfural distilled and collected. Hydroxymethyl furfural is also produced during the distillation, but does not interfere in the plowing colorimetric determination. L3.2 An aliquot of the distillate is treated with orcinol Jagent, and after standing for 2 h the absorbance is |easured at 630 am. By reference to a calibration curve irepared from known furfural solutions, the percent |entosans is calculated. f|. Significance and Use 4.1 This test method is used for measuring the level of jhemicelluloses in wood pulps. The amount of pentosans, primarily arabinose and xylose, are measures of the purity of fwood pulps used in chemical cellulose applications. 6p. Apparatus if 5.1 Flask, two-neck round-bottom, 500-mL, standardtaper 24/40 joint. 5.2 Dropping Funnel, 500-mL, with standard-taper 24/40 neck. 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 D01.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D1787 - 60. Last previous edition D 1787 - 62(1985)". 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.02. 5.3 Distillation Connecting Tube, with standard-taper 24/ 40 innerjoints to fit the round-bottom flask and the Graham condenser, respectively, with the proper angles to allow for the vertical position of the condenser. If a thermometer is to be used, the adapter should have a standard-taper 10/30 thermometer well. 5.4 Condenser, Graham, water-cooled, with standard- taper 24/40 connections. 5.5 Adapter, with standard-taper 24/40 joints with gas inlet. 5.6 Receiving Flask, 500-mL, with standard-taper 24/40 joint, to collect the distillate. 5.7 Ice Bath, for receiving flask to help prevent loss of furfural. ; 5.8 Heating Mantle, for reaction flask, controlled by a variable transformer. A gas burner may be substithted for the heating mantle. 5.9 Constant-Temperature Bath, capable of maintaining a temperature within 0.5*C of the temperature selected for development of the color with orcinol, which temperature should be between 15 and 30G 5.10 Filter Photometer or Spectrophotometer, suitable for measuring absorbance at 630 nm. 6. Purity of Reagents 6.1 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.4 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 Unless otherwise indicated, references to-water shall be understood to mean reagent water conforming to Specifi cation D 1193. 6.3 Ethanol, 95 %, aldehyde-free. 6.4 Furfural--Distill furftnal immediately before use. Use only freshly-distilled pale yellow material with a boiling point of 162C. It is preferable to distill in vacuum. 6.5 HydrochloricAcid (3 + 7)--Mix 3 volumes of concen trated hydrochloric acid (HCI, sp gr 1.19) with 7 volumes of water. The concentration will be approximately 12 %. , 6.6 Orcinol Solution--Dissolve 0.40 g of orcinol and 0.5 g of ferric chloride (FeCl3-6H20) in 1 L of 11.0 N HCI. Discard solutions more than 2 weeks old. * "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." 305 DUP050296826 # D 1787 1 7. Preparation of Calibration Curve 7.1 Dissolve about 0.5 g furfural, weighed to an accuracy of 0.2 mg, in HC1 (3 + 7) and dilute to 500 mL with HC1 (3 + 7) in a volumetric flask. After mixing thoroughly, pipet 5, 10,15,20,25, 30, and 50 mL of this solution into separate 100-mL volumetric flasks and dilute to the mark with HC1 (3 + 7). This gives solutions with 50, 100, 150, 200, 250, 300, and 500 mg of furfural per litre. 2--Higher or lower concentrations of standards may be prepared to fit specific conditions. 7.2 Pipet 10 mL of each of these diluted solutions into separate 50-mL volumetric flasks, and add 25 mL of orcinol solution to each. Place the flasks in a constant-temperature bath. '. 3--The color intensity is dependent on the temperature during the reaction of furfural with orcinol. Any tempefature.between IS and 30C may be used, provided the temperature is the same during the pentosans determination as in the preparation ofthe calibration curve. If available, a constant-temperature room may be used. 7.3 Prepare a blank containing.all the reagents except the- furfural solution. 7.4 After 60 5 min, almost fill the volumetric flasks with ethanol, mix, bring to the temperature of the bath, fill to the mark with ethanol, and again mix thoroughly. Place in the bath for a second 60 5 min period. Measure the absorbance at 6j30 am, and correct for the reading on the reagent blank. 7.5 Plot absorbance versus milligrams offurfural to give a: calibration, curve. , 8. Procedure . 8.1 The size of specimen to be taken depends- on its: pentosan content. Select the proper size specimen and suitable size aliquot for the subsequent colorimetric mea surement as follows: Pentosans Content, % <1 ! to 3 3 to 5 5 to 10 >10 Specimen Size, g 4 3 2 1 t Size of Aliquot, jnL 10 . fo 10 105 (plus 5 mL of HC1 (3.+7)) . 8.2 Allow the specimen to come to moisture equilibrium with the atmosphere of the balance. Weigh to the nearest milligram and transfer it to the 500-mL round-bottom flask. At the same time weigh aspecimen for moisture determina tion in accordance with Test Methods D 1348. Add 100 mL of HC1 (3 + 7) to the flask, washing down any fibers adhering to the sides of the flask. Assemble the distillation apparatus and mark the flask to indicate the liquid level. ` 4--Ifthe room air temperature is above 20C, cool the receiver with an ice bath. 8.3 Add 300 mL of HC1 (3 +. 7) to the dropping funnel. With a glass-marking pencil or permanent glass-marking ink, divide the volume into six portions, one portion for each 15-min period. (Any convenient number of divisions that will enable the operator to keep track of the amount of HC1 (3 + 7) added with time is satisfactory.) 8.4 Start timing the distillation when the distillate first starts to appear, and distill for 90 min, collecting in that time 300 mL of distillate in the receiver. Allow the acid to drop into the distillation flask from the separatory funnel at such a rate that the original 100-mL level is maintained. It is i important that the proper rate of distillation be maintained 1 and that 300 mL of distillate be collected. The receiver J should be marked at the 300-mL level; 5--It is important to avoid overheating the flask above the f liquid level. 8.5 Transfer the contents of the receiver to a 500-mL volumetric flask. Rinse the receiver (Note 6);with HC1 (3 + 7), and add the rinsings to the volumetric flask. Dilute to the mark with HC1 (3 + 7) and mix well. 6--If a 500-mL volumetric flask, marked at the 300-mL level, is tried as the receiver, transfer ofthe distillate and rinsing ofthe receiver are avoided. Proper choice of specimen size and aliquot will allow the use of a 300-mL volumetric flask as the receiver. The distillation can be stoppedjust short ofthe mark.to allow precise adjustment ofthe volume. j j j j : 1 8.6 Pipet 10 mL of the diluted distillate into a 50-mL volumetric flask, add 25 mL of orcinol solution, and place the flask in the constant-temperature bath; After 60 5 min almost fill the flask with ethanol, mix, bring to the tempera ture of the constant-temperature bath, fill to the mark with ethanol, and mix. thoroughly. Place in the bath for a second 60 5-min period; Measure the absorbancy ofthe blue color at 630 nm, using a blank containing 10 mL (or whatever size aliquot is used) of HC1 (3 + 7), instead of the distillate, as a reference solution. Read the furfural concentratibn of-the distillate from the calibration curve. 9. Calculation , 9.1 The theoretical factor for converting pentosans to furfural is 0.727, which is the quotient-of the molecular weight, of furfural, 96, divided by- the molecular weight of atihydroxylan, 1.32, Assuming that the-pentosans content of wood consists principally of xylan that is converted to furfural with a yield of 88 percent, the empirical factor for. converting furfural values to pentosans is: 1/(0.727 x 0.88) = 1.563 9.2 Calculate the pentosans content of the Specimen as follows: ...... ! Pentosans, % - [A/{B x [(100 - CyiOO])] x 1.563'x "100 where: A -- furfural in the distillate, g, B = specimen used, g, and C = moisture'in the specimen, %. 10. Report 10.1 Report the pentosans content of the cellulose as a percent ofthe moisture-free sample. Make all determinations at least in duplicate, and report the average value. 11. Precision and Bias .. 11.1 A general guide for the agreement between duplicates and the number of significant figures is as follows: Pentosans, % <2 2 to 10 >10 Agreement, % 0.1 0.4 1.0 Nearest Significant Fig ures to be Reported, % 0.1 0.1 0.5 11.2 No statement on bias can be made as no suitable reference material exists for determining bias. 306 DUP050296827 The American Society lor Testingand 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 ot any such patent 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 responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapprovedor withdrawn. Your comments are invitedeither torrevision ot this stendardor 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.,tt you leal 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. 307 HP DUP050296828 Designation: D 1794 - 89 An American National Standard Modification of Technical Association of Pulp and Paper Industry Standard Method T 6 m-69 Standard Test Method for Alcohol-Benzene Soluble Matter in Cellulose1 ,. o This standard is issued under the fixed designation D1794; 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. The committee responsiblefor this standard has voted Us withdrawal. lit the absence ofsubstantial reasons that it shouldbe continued, the Society will approve withdrawalfrom publication in February 1993, 1. Scope 1.1 This test method covers the determination ofalcoholbenzene soluble matter in cellulose and is applicable to dis solving-type cellulose pulps prepared from cotton or wood. 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: D1348 Test Methods for Moisture in Cellulose12 2.2 Other Documents: Occupational Safety and Health Standards and Interpreta tions, Part 19103 3. Summary of Test Method 3.1 A sample is extracted with a 1 + 2 alcohol-benzene solution in a Soxhlet apparatus as a measure of the waxes, fats, resins, and oils present. 4. Significance and Use 4.1 This test method provides an estimate ofwaxes, lipids, resins, and other organic soluble residues that were not removed from the fiber during the pulping process. 5. Apparatus 5.1 Extraction Apparatus, Soxhlet, consisting of a 300-mL flask, an extractor with a 50 by 250-mm body, and a Hopkins type condenser. 5.2 Extraction Thimble' either (/) standard thickness pa per, 43 by 123 mm, (2) Alundum, 45 by 127 mm, mediumporosity, or (3) glass with coarse-porosity fritted-glass disk, 45 by 130 mm. 5.3 Extraction Heater and Support, heater with three-heat switches. 5.4 Oven, gravity-convection, maintained at 105 3C. 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 D01.36 on Cellulosics. Cunent edition approved Oct. 27, 1989. Published December i989. Originally published as D 1794 - 62. Last previous edition D 1794 - 62 (1985)ei. Replaces D 1794 - 60 T. 2 Annual Book ofASTM Standards, Vo! 06.02. 3 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 5.5 Dish, evaporating, milk, aluminum, 75 mm in diam eter by 20 mm deep. 5.6 Desiccator with efficient desiccant such as anhydrous calcium sulfate, activated alumina, or magnesium perchlo rate. Calcium chloride is not satisfactory. 6. Reagent 6.1 Alcohol-Benzene Solvent--Mix 1 volume of Formula 30 ethyl alcohol with 2 volumes of benzene. o t Caution--Benzene is regulated as a "cancer hazard" as outlined in OSHA Regulations. 7. Procedure 7.1 Weigh 8 to 12 g of loose pulp, to the nearest 0.01 g, into an extractor thimble that has previously been extracted with the alcohol-benzene solvent. For sheet pulp, cut a sample into strips about lA in. (6.4 mm) wide and 3 in. (76 mm) long, and weigh about 20 g into a-thimble. Weigh aseparate portion for a moisture determination in accordance with Methods D 1348. 7.2 Place the extraction thimble with specimen in the ex tractor and connect the flask. Pour 250 mL of the alcoholbenzene solvent into the body of the extractor. Connect the assembled extractor to the condenser and place the flask on the extraction heater. Turn on the cooling water to the condenser and adjust the heater to cause the solvent to reflux at such a rate as to cause siphoning 6_to 8 times/h. Continue the extraction for 5 h, beginning the timing when tlie solvent first begins fo drop from the condenser into the extractor. 7.3 When the extraction is complete, turn off the heater. Disconnect the flask at a time when most "bf the solvent has collected in the extractor. 7.4 Heat the evaporating dish in the oven at 105C for 30 min, cool in a desiccator, and weigh to the nearest 0.0001 g. Filter the solution from the flask through a sheet of qualita tive paper into the weighed drying dish. Rinse the flask and filter with three 5-mL portions of the alcohol-benzene solvent. 7.5 Place the dish on a steam bath and evaporate just to dryness. Then place the dish in the oven at 105C for 1 h, . cool in a desiccator, and weigh. 8. Calculation 8.1 Calculate the percent of alcohol-benzene soluble matter, S, on the dry basis as follows: S'" [{A - B)/W x [(100 - M)/100])] x 100 where: 308 mmm P* DUP050296829 # D 1794 = weight of dish and residue, g, = weight of dish, g, Report 9.1 Report the alcohol-benzene, soluble matter to the arest0.01%. 10. Precision and Bias 10.1 At an extractive level of0.13 %, the relative standard deviation is 10 %: 10.2 No statement on bias can be made as no suitable reference material exists for determining bias. The American Society for Testing and Materials takes no positron 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 suchrlghts, are. entirely Mr own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must'be reviewed every rive years end Ifnot revised, eitherreapprovedor withdrawn: Yourcomments are Invitedeitherforrevision ofthis standardorloradditionalstandards 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 Race St., PhlUdelphle, PA 19103. 309 m DUP050296830 4 Designation: D 1795 - 90 Standard Test Method for Intrinsic Viscosity of Cellulose1 This standard is issued under the fixed designation D 1795; 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 test method covers the determination of the in trinsic viscosity of purified celluloses such as bleached, wood . pulps, cotton linters, and regenerated cellulose. It is-appli cable to all cellulose samples with an intrinsic viscosity of 15 dl/g or less. Most native (unpurifledj celluloses have intrinsic' viscosity values too high for measurement by this test method. The use ofcuprammonium hydroxide solution for regular viscosity determination is described in Test Methods D 539, Method T 206 m-55 of the Technical Association of Pulp and Paper Industry on "Cuprammonium Disperse Viscosity of Pulp," and Joint Army-Navy Specifications JAN-C-206. 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. Referenced Documents 2.1 ASTM Standards: D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)21 D 539 Test Methods for Apparent Fluidity of Dispersions of Cellulose Fibers3 D629 Test Methods for Quantitative Analysis of Textiles4 E 1 Specification for ASTM Thermometers5 3. Summary of Test Method 3.1 A weighed sample of the material is dissolved in a 0.5 M cupriethylenediamine hydroxide solution. The viscosity of this solution, and also that of the solvent, is determined at 25C by means of a calibrated glass capillary-type viscometer. The relative viscosity is calculated and the corresponding intrinsic viscosity is read from a table. 4. Significance and Use 4.1 This test is a sensitive measure of the degradation of cellulose resulting from the action of heat, light, acids, alka lies, oxidizing and reducing agents, and the like, used in its 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 D01.36 on CeUulosics. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1795 - 60. Last previous edition D 1795 - 62(198$)*1 2 Annual Book ofASTM Standards, Vols 10.03 and 05.01. 3 Discontinued, see J97S Annual Bock ofASTM Standards, Part 24. * Annual Book ofASTM Standards, Vol 07.01. * Annual Book ofASTM Standards, Vol 14.03. processing or purification. The intrinsic viscosity value may be converied to degree of polymerization {DP) or to intrinsic fluidity, if desired, '4,2 Solutions of cellulose are not Newtonian liquids; that is, their viscosity depends upon the rate-of-shear or velocity gradient during measurement. This effect is smaller for sam ples of low molecular mass (DP) and at low concentrations than for high-DP samples and at high concentrations. For the celluloses and concentrations included within the limits set forth in this test method, the effect of rate-of-shear is assumed to be negligible for referee purposes. For other conditions and for research purposes this assumption may be invalid, but to discuss ways of accounting for this effect is beyond the scope of the present test method. 5. Apparatus 5.1 Viscometer, Glass, Capillary Type--The CannonFenske, Ubbelohde, or similar capillary type instrument as described in Test Method D 445 is recommended. Viscome ters described in Test Methods D539 are also suitable. In order to avoid correction for the kinetic energy effect, choose, a viscometer with a small enough capillary to give an outflow time of 80 s or more for the Cannon-Fenske type. (A size 100 viscometer is normally used for the sample solution and a size 50 for the solvent.) 5.2 Thermometer--ASTM Kinematic Viscosity Ther mometer for use at 25C, having a range from 19 to 2TC and conforming to the requirement for Thermometer T7C as prescribed in Specification E 1. 5.3 Bath--A constant-temperature bath at 25C suitable for immersion of the viscometer so that the reservoir or the top of the capillary, whichever is uppermost, is immersed at least 50 mm, and with provision for visibility of the instru ment and the thermometer. Firm supportsTor the viscometer shall be provided; or the viscometer may be sealed in as an integral part of the bath. Either a liquid bath with thermo static regulation and a stirrer or a vapor bath with pressure regulation is permissible. The efficiency of the stirring and the balance between heat losses and heat input must be such that the temperature of the bath medium does not vary by more than 0.1C over the length of the viscometer, or from viscometer to viscometer in the various bath positiohs. If a vapor bath is used, there must be no temperature gradient over the length of the viscometer greater than that permitted in a liquid bath. 5.4 Timer--A stop watch or other spring-activated timing device or electrical timing device shall be used, graduated in divisions of 0.2 s or less, and accurate to within 0.05 % when tested over not less than a 10-min period. Such electrical timing devices shall be used only on electrical circuits of continuously controlled frequency. Frequency-controlled de- 310 spis? DUP050296831 D 1795 lees of suitable capacity for laboratory purposes, accurate to /ithin 1 part in 10 000 should be used. Errors exceeding Ii05 % of a 10-min interval may occur in timing devices Ictuated by electrical synchronous motors driven by most public power systems, which are intermittently and not ontinuously controlled. f|. Reagent I! 6.1 Cupriethylenediamine Hydroxide Solution (1.00 8.01 M), in copper, with the molar ratio of ethylenediamine to. copper of 2 0.1 to 1. This solvent may be prepared in pe laboratory as described in Test Methods D 539. It is also Commercially available.6 ; Reference Materials 7.1 Viscosity Oil Standards--'Calibrating oils in the spec ified ranges of viscosity.6 Aqueous solutions of glycerol may be used instead of standardized oils; the compositions for various viscosities are- given in chemical handbooks. The applicable viscosity oil standards (Note 2) are listed in Table 1. No t e 2--The viscosity oil standards arc available only as 1-pt (4.7H in3) samples. More than 1 pt of any given oil (for example, duplicate ' samples) are supplied only when it is established that 1 pt is inadequate.6 8. Calibration of Viscometer 8.1 The following directions apply to the Cannon-Fenske | viscometer (Note 3). They should be modified according to Tthe operating instructions for other types of viscometers. The viscometers shall be calibrated (Note 4) by means of liquids : having known viscosities approximately equal to those of the solvent and cellulose solutions respectively (1.2 and 12 cP, f approximately). 3--Detailed specifications and directions' for filling, cali- ` brating, and measurement with types of capillary viscometers most used s are given in Test Method D 445. 4--Calibration of the viscometers may be avoided if both I solvent and solution are measured in the same instrument. Then the t relative viscosity is nearly the ratio of outflow times for solution and solvent, respectively. This simplification involves two assumptions. The I first, that the densities of solution and solvent are equal, holds very well for the dilute solutions used in these tests. The second, that the kinetic energy correction is zero, depends upon the choice of viscometer. If the 1 one used gives convenient outflow times for the solution ofless than 150 s, then it will be too fast for the solvent. The kinetic energy correction is zero, depending upon flow. On the other hand, if one is chosen so that the outflow time for the solvent is large enough (80 s or more), then the times for the solutions will in most cases be inconveniently long. For some work, however, it may be desirable .to make some sacrifice in TABLE 1 Viscosity Oil Standards Viscometer Viscosity OU Standard Size Viscosity Range, cPA SO 0.9 to 3.5 100 3.3 to 13.3 ' For solution with density of 0.9. Designation S-3 S-6 Approximate Absolute Viscosity at770F(25C), cP 3.3 7.7 6 Viscosity oil standards are available from the Cannon Instrument Co., P.O. Box 16, State College. PA 16801. accuracy or in convenience during measurement in order to avoid calibration and using two sizes of viscometers. 8.2 By means of a pipet, add 7.0 mL of the calibrating liquid to the viscometer, in a constant-temperature bath at 25 0.1C (or fill as described in Test Method D445, Appendix A). 8.3 When the liquid has reached temperature equilibrium with the bath (in about 5 min), determine the outflow time t by drawing the top meniscus of the liquid above the mark between the two bulbs and measuring the time required for the meniscus to pass from this mark to the mark below the lower bulb. Take the average of two or more observations, which should differ by not more than 0.2 s. 8.4 Determine the viscometer constant Cby the equation: C=r)/dt (l) where: ij = viscosity of the calibrating liquid, cP, d = density, g/mL, and t = time, s. 9. Preparation of Sample 9.1 To avoid undesirable effects from long heating at high temperature, samples should be air-dried and the moisture content determined on a portion that is not used for mea surement of viscosity. The mass of air-dried samples is then corrected for moisture to obtain the mass of oven-dried cellulose used to calculate concentration. 9.2 Soft, sheeted pulp should be picked apart with tweezers or scraped with a dull knife. Hard-pressed or harsh pulp should be slurried in water, formed into thin sheets on a Buchner funnel, and dried at a temperature below 100C (preferably room temperature). Loose pulp should be picked apart by hand to break up any lumps. Slurried or slush pulps should be formed into thin sheets and dried. Yam and staple should be washed in warm water containing a little detergent to remove the finish, rinsed thoroughly, dried (at low tem perature), and fluffed. (It will be found helpful to cut yam and long staple into short lengths, say lh in. (13 mm), before washing.) Fabrics should be cut into small pieces, desized (see Test Methods D 629, Section 8),7 thoroughly washed, and. dried. Ravelingjyill be helpful before dissolving samples that tend to get in the solvent. Materials containing a consider^ able amount of non-cellulosic matter must first be purifiedT such treatments lie outside the scope of this test method. 10. Preparation of Solution 10.1 The sample size is dependent upon the nature of the material, smaller masses ofhigh-viscosity celluloses and larger masses of low-viscosity celluloses being used in order to keep the viscosity of the solutions within rather narrow limits. (Working at nearly constant viscosity reduces the effect of rate of shear upon the measurements.) The concentration for each sample is chosen according to the rule: Me = 3.09 0.5 (2) where: 1 This solution may be purchased in I-gal (3.8-L) lots from the Ecusta Paper Div., Olin-Mathicson Chemical Corp., Pisgah Fewest, NC or in 5-lb (2-kg) lots from Baker and Adamson, General Chemical Div., Allied Chemical Corp., 40 Rector St., New York, NY 10006. 311 DUP050296832 [j ?] = intrinsic viscosity, dL/g, and c = cellulose concentration, g/dL. Obviously, use of this rule requires knowledge of the approximate intrinsic viscosity of the sample before the concentration can be estimated. In routine control work, such information is available. If it is not, Table 2 will serve as an approximate guide. 10.2 Make up a preliminary solution of about the indi cated concentration, and determine the viscosity as described in Sections 11 and 12. From the relative viscosity thus obtained, find the approximate value of the intrinsic vis cosity by means of Table 3. From this determine the concentration needed to give: [ij]c = 3.0. If this preliminary solution does not give a value of [n]c of 3.0 0.5, prepare a second solution of the indicated concentration for the final viscosity measurement. 10.3 Alkaline solutions of cellulose are known to be sensitive to oxidation. Hence it is usually necessary to exclude air during solution of the sample; several ways of doing this are described in the literature, but the following is simple and adequate: Weigh out the calculated amount of air-dried cellulose (corrected to oven-dry mass) and transfer quantitatively to a suitable glass or polyethylene container (capacity somewhat more than 50 mL) that can be.tightly closed by a stopper or screw cap. Add 25.0 mL of distilled water from a pipet or buret, insert the stopper or cap, and shake in order to wet out and disperse the sample. Sweep the air, from the vessel with a stream of nitrogen and, with the nitrogen still flowing, add 25.0 mL of solvent. Stopper or cap tightly and shake vigorously by hand or in a mechanical shaker until the cellulose is completely dissolved. 5--Most work pulp and regenerated celluloses dissolve within 5 min. Mercerized celluloses do not dissolve as easily in cupriethylenediamine as in cuprammonium solvent and require longer times (up to 1 h). Some operators report difficulty in dissolving native celluloses including cotton liriters with DP as low as that ofwood pulps. The difficulty shows up by much poorer precision ofresults than the 1 to 2 % that is normally obtained between measurements made with two or more solutions ofthe same sample. Even solutions that leave no residue on fritted-glass filters have been observed to give erratic resuits. Inadequate dispersion of the sample is apparently the cause, and two modifications in procedure have been recommended in such cases. One is to add about 0.04 % wetting agent to the water used to wet out the sample.8 The other requires use of cupriethylenediamine solutions of " Lindstey, C. H., "Rapid Dispersion of Cellulose in Cupriethylenediamine," Textile Research Journal, Vol 21, 1951, p. 286. TABLE 2 Intrinsic Viscosities of Typical Samples Type of Material Regenerated cellulose (rayons) Dissolving pulps: Low viscosity Regular viscosity High viscosity Cotton linters, for rayon and acetate Paper (wood) pulps Native celluloses4 Intrinsic Viscosity, dL/g 2to3 3 to 4 4 to 7 7 to 10 6 to 9 3 to 8 15 to 30 Approximate Concentration, 9/dL 1 1 0.5 0.3 0.4 0.4 0.1 to 0.2 4 Serious error may be introduced when this test method, which neglects effects of rate of shear upon viscosity, is used for native celluloses of high intrinsic vfscoslly. two concentrations: The sample is wetted out with one solution that is 0.167 M in copper and dispersion is completed by adding the second solution, 1.000 M in copper, in such volume as to make the final copper concentration 0.500 M (see Section 14 ofTest Methods D 539). 11. Measurement of Viscosity 11.1 Transfer 7.0 mL of the solution by means of a syringe or pipet to a viscometer previously placed in the bath at 25C and flushed with nitrogen (or fill as described in Test Method D 445, Appendix A). Allow at least 5 min for the solution to reach bath temperature. 11.2 By applying either pressure (with nitrogen) or suc tion, draw the solution into the lower bulb of the viscometer until the top meniscus is a little above the mark between the two bulbs. Measure the time t required for the meniscus to pass from this mark to the mark below the lower bulb. Repeat at least twice and average the observations, which should not differ by more than 0.3 %. 11.3 In the same way, measure the outflow time t0 for the solvent. This of course must be determined not for the. 1.00 M solvent as prepared or purchased, but for this solvent diluted with an equal volume of water. 12. Calculations 12.1 Calculate the viscosity, y, in ceniipoises, as follows: y = Ctd where: C = viscometer constant (Section 8), t - Outflow time, s, and . d = density, g/mL. (3) Calculate the relative viscosity,' jrel, as follows: ftrel. t/ifo s where y0 is the viscosity of the solvent. Since the densities of solvent and solution are practically the same, they cancel in determining relative viscosity. Hence a little work may be saved by determining the kinematic viscosity, e, in centistokes, for solution and solvent:. and then 6=0 ' ... - " (4). - 4,,i = dto . (5) If both solution and solvent are measured in the same viscometer (see Note 4), relative viscosity may be obtained directly from the ratio of outflow times: Pre! = f/4> (6) 12.2 By means of Table 3, determine the product [y\c corresponding to the value ofthe relative viscosity. From this value and the concentration, calculate the intrinsic viscosity in decilitres per gram. 6--Table 3 gives values of [tf]c for the indicated values of vi determined by the Martin equation: log[(ijrci - l)/c] = logfo] + me (7) where A = 0.13. More precise values of [t?] can be obtained by finding jjrei for three or more concentrations, plotting log [(tjre] - l)/c] against c and extrapolating the straight line through the points to c = 0. The intercept gives log fo]. 12.3 For some purposes it is desirable to express results as degree of polymerization, since this concept is easily under stood by nontechnical people who must interpret technical 312 mm !fi#S * DUP050296833 D 1795 TABLE 3 Intrinsic Viscosity, fo]c, at Different Values of Relative Viscosity, Me Vnt 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 i.i 0.068 0.106 0.115 0.125 0.134 0.143 0.152 0.161 0.170 0.180 1.2 0.189 0.198 0.207 0.216 0325 0333 0342 0.250 0359 0268 1.3 0.276 0.288 0.293 0.302 0.310 0.318 0.326 0.334 0.342 0.350 1.4 0.358 0.367 0.375 0.383 0.391 0.399 0.407 0.414 0.422 0.430 1.5 ' 0.437 0.445 0.453 0.460 0.468 0.476 0.484 0.491 0.499 0.507 1.6 0.515 0.522 0.629 0.536 0.544 0.551 0.558 0.566 0.573 0.580 1.7 0:587 0.595 0.602 0.608 0.615 0.622 0.629 0.636 0.642 0.649 1.8 0.656 0.663 0.670 0.677 0.683 0.690 0.697 0.704 0.710 0.717 1.9 0.723 0.730 0.736 0.743 0.749 0.756 0.762 0.769 0.775 0.782 2.0 0.788 0.795 0.802 0.809 0.815 0.821 0.827 0.633 0.840 0.846 2.1 0.852 0.858 0.864 0.870 0.876 0.882 0.888 0.894 0.900 0.906 2.2 0.912 0.918 0.924 ' 0.929 0.935 0.941 0.948 0353 0.959 0.965 2.3 0.971 0.976 0.9S3 0388 0.994 1.000 1.006 1.011 1.017 1.022 2A 1.028 1.033 1.039 1.044 1.050 1.056 1.061 1.067 1.072 1.078 2.5 1.083 1.089 1.094 1.100 1.105 1.111 1.116 1.121 1.126 1.131 2.6 1.137 1.142 1.147 1.153 1.158 1.163 1.169 1.174 1.179 1.184 2.7 . 1.190 1.195 1.200 1305 1310 1315 1.220 1.225 1330 1235 2.8 1.240 1.245 1.250 1355 1360 1365 1.270 1.275 1380 1.285 2.9 1.290 1.295 1.300 1.305 1.310 1.314 1.319 1.324 1.329 1.333 3.0 1.338 1.343 1.348 1.352 : 1.357 1.362 1.367 1.371 1.376 1.381 3.1 1.386 1.390 1.395 1.400 ' 1.405 1.409 1.414 1.418 1.423 1.427 3.2 1.432 1.436 1.441 1.446 1.450 1.455 1.459 1.464 1.468 1.473 3.3 1.477 1.482 1.486 1.491 1.496 1.500 1.504 1.508 1613 1.517 3.4 1.521 1.525 1.529 1.533 1.637 1.542 1.546 1.550 1554 1.558 3.5 1.562 1.566 1.670 1.575 1.579 1.583 1.587 1.591 1.595 1.600 3.6 1.604 1.808 1.612 1.617 1.621 1.625 1.629 1.633 1.637 1.642 3.7 1.646 1.650 1.654 1.658 1.662 1.666 1.671 1.675 1.679 1.683 3.8 1.687 1.691 1.695 1.700 1.704 1.708 1.712 1.715 1.719 1.723 3.9 1.727 1.731 1.735 1.739 1.742 1.746 1.750 1.754 1.758 1.762 4.0 1.765 1.7,69 1.773 1.777 1.781 1.785 ' 1.789 1.792 1.796 1.800 4.1 1.804 1.808 1.611 1.815 1.819 1.822 1.826 1.830 1.833 1.837 4.2 1.841 1.846 .1.848 1.852 1.856 1.859 1.863 1.887 1.870 1.874 4.3 1.878 1.882 1.885 1.889 1.893 1.896 1.900 1.904 1.907 1.911 4.4 1.914 1.918 1.921 1.925 1.929 1.932 1.936 1.939 1.943 1.946 4.5. 1.950 1.964 1.957 1.961 1364 1.968 1.971 1.975 1.979 1.982 4.6 1.986 1.989 1.993 1.996 2.000 2.003 2.007 2.010 013 2.017 4.7 2.020 2.023 2.027 2.030 2.033 2.037 2.040 2.043 2.047 2.050 4.8 2.053 2.057 2.060 2.063 2.067 2.070 2.073 077 2.080 2.083 49 2.087 2.090 2.093 2.097 2.100 2.103 2.107 2.110 2.113 2.116 5.0 2.119 2.122 2.125 2.129 2.132 2.135 2.139 2.142 2.145 2.148 5.1 2.151 2.154 2.158 2.160 2.164 2.167 2.170 2.173 2.176 2.180 5.2 2.183 2.186 2.190 2.192 2.195 2.197 2300 203 2306 2209 5.3 2.212 2.215 2.218 2321 2324 2327 230 2333 2336 240 5.4 2.243 2.246 2.249 2352 2355 2.258 2361 2364 2.267 2270 5.5 2.273 2.276 2.279 2382 2385 2.288 . 2391 2.294 2397 300 5.6 2.303 2.306 2.309 2.312 2.315 2.318 320 2.324 2.326 2.329 5.7 2.332 2.335 2.338 2.341 2.344 2.347 350 ' 2.353 2.365 2.358 5.8 2.361 2.364 2.367 2.370 2.373 2.376 379 382 384 "2.387 5.9 2.390 2.393 2.396 2.400 2.403 2.405 2.408 2.411 414 3.417 6.0 2.419 2.422 2.425 2.428 2.431 2.433 2.436 2.439 2.442 2.444 8.1 2.447 2.450 2.453 2.456 2.458 2.461 464 2.467 2.470 472 6.2 2.475 2.478 2.481 2.483 2.486 2.489 2.492 2.494 2.497 2.500 6.3 2.503 2.505 2.508 2.511 2.513 2.516 2.518 2.521 2.524 2.526 6.4 2.529 2.532 2.534 2.537 2.540 2.542 2.546 547 2.550 553 data. A reasonably good approximation to degree of polymation is obtained by multiplying intrinsic viscosity by 190, t values so obtained have relative not absolute significance. j.12.4 The concept of fluidity is used by large numbers of rators in place of viscosity. These two quantities are iiprocals of one another. Intrinsic fluidity, the reciprocal of irinsic viscosity, is useful because it is a nearly linear function of yam or fiber strength; its unit is grams per decilitre. 13. Precision and Bias 13.1 Precision--Based on interlaboratory testing, the re producibility is within 3 % of each other. 13.2 Bias--No statement of bias can be made, as no suitable reference material exists for determining bias. 313 '"MHsaSB! DUP050296834 D1795 TABLE 3 Continued Me tiro) 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 6.5 2.555 2.558 2.561 2.563 2.566 2.568 2.571 2.574 m 2.581 2.584 2.587 2690 2.592 2.595 2.597 2.600 6,7 2.608 2610 2.613 2.615 2.618 2.620 2.623 2.625 6.8 , 2.633 ,2.635 2.637 2640 2.643 2.645 2.648 3.650 6.9 2.658 2.660 2.663 , 2.665 2.668 2.670 2.673 2.675 7:0 2.683 2.685 . 2.687 2.690 2.693 2.695 2.698 2.700 7.1 2.707 2.710 2.712 2.714 2.717 2.719 2.721 2.724 7.2. 2.731 2.733 2.736 2.738 2.740 2.743 2.745 2.748 7.3 2.755 2.757 2.760 2.762 2.764 2.767 2.769 2.771 7.4 . 2.779 2.781 2.783 2.786 2.788 2.790 2.793 2.795 7.5 2.802 2.805 2.807 2.809 2.812 2.814 2.816 2.819 7.6 2.826 2.828 2.830 2.833 . 2.835 2.837 ' 2.840 2.842 7,7 2.349 2.851 2.854 2.856 2.858 2.860 2.863 2.865 7.8 2.873 2.875 . 2.877 . 2.879 2.881 2.884 . 2.887 2.889 7.9 2:895 2.898 2.900 2.902 2.905 2.907 2.909 2.911 8.0 2,918 2.920 2.922 2.924 ,2.926 2.928 2.931 2.933 8.1 2.939 2.942 2.944 . 2.946 3.948 2.950 2.952 2.955 8.2 2.961 2.963 2.966 2.968 : ., 2.970 2.972 2.974 2.976 8.3 2.983 2.985 2.987 2.990 2.992 2.994 2.996 2.998 8.4 ' 3.004 3.006 3.008 3.010 3.012 3.015 3.017 3.019 8.5 3.025 3.027 3.029 3.031 3.033 3.035 3.037 3.040 8.6 3.046 3.048 3.050 3.052 3.054 3.056 3.058 .. 3.060 8.7 3.067 3.069 3.071 3.073 3.075 3.077 3.079 3.081 8.8 3.087 3.089 3.092 3.094 3.096 3.098 3.100 3.102 8.9 3.108 3.1 IQ 3.112 3.114 3.116 3.118 3.120 3.122 9.0 3.128 3.130 3.132 3.134 3.136 3.138 9.1 3.148 3.150 3.152 3.154 3.156 3.158 9.2 3.168 3.170 3.172 3.174 3.176 3.178 9.3 3.188 3.190 3.192 3.194 3.196 3.198 9.4 3.208 3.210 3.212 3.214 3.215 3.217 9.5 3.227 3.229 3.231 3.233 3.23S 3.237 9.6 3.246 3.248 3.250 3252 3.254 3.256 9.7 3.266 3.268 3.269 3.271 3.273 3.275 9.8 3.285 . 3287 3.269 3.291 3.293 3.295 9.9 3.304 3.305 3.307 3.309 3.311 3.313 0.0 0.1 0.2 0.3 0.4 . 0.5 10 3.32 3.34 3.36 3.37 3.39 3.41 11 3.50 3.52 3.53 3.55 3.56 3.56 12 3.66 3.68 3.69 3.71 3.72 3.74 13 3.80 3.83 3.85 3.86 3.88 3.89 14 3.96 3.97 3.99 4.00 4.02 4.03 15 4.10 . 4.11 4.13 4.14 4.15 4.17 16 4.23 4.24 4.25 4.27 4.28 4.29 17 4.35 4.36 4.37 . 4.38 4.39 4.41 18 4,46 . 4.47 4.48 . 4.49 4.50 4.52 19 4.57 4.58 4.59 : 4.60 4.61 4.62 -- '`Swedish Method CCA 27:57, Karin Wilson, Svensk Papparstldning, Vol 60,1957, pp, 513 to 521. 8 Derived from the equation: v,,: - 1 " vp - where ft' = 0.30. 3.140 3.160 3.180 3.200 3319 3339 3.258 3.277 3.297 3.316 0.6 3.43 3.60 3.76 3.90 4.04 4.18 4.30 4.42 4.53 4.63 3.142 3.162 3.182 3.202 3.221 . 3241 3.280 3279 3.298 3.318 0.7 3.45 3.61 3.77 3.92 4.06 4.19 4.31 4.43 ' 4.54 4.64 0.08 2.576 2.603 2.627 2.653 2,678 2.702 2.726 2.750 2.774 2.798 2.821 2.844 2.868 2.891 2.913 2.935 2.957 2.979 3.000 3.021 3.042 3.062 3.083 3.104 3.124 3.144 3.164 3.184 3.204 3.223 3.242 3.262 3.281.. 3.300 3.320 0;8 3.46 3163 3.79 3.93 4.07 4.20 4.33 4.44 4.55 4.65 0.09 2.579 2.605 2.630 2.655 2.680 2.705 2.729 2.752 2.776 2.600 2.823 2.847 2.870 2.893 2.915 2.937 2.959 2.961 3.002 3.023 3.044 3.064 3.085 3.106 3.126 3.146 3.166 3.186 3.206 3.226 3.244 3.264 3.233 3.302 3.321 0.9 3.46 3.64 3.80_ 3.95 4.09' . 422 . 4.34' 4.45 4.56 4.66 The American Society tor Testing and Materials takes noposition respecting the validity of anypatent rights asserted In connection with any Item mentioned In this standard. Users ot this standard are expressly advised that determination ofthe validity of atry such patent rights, and the risk of Infringement of such rights, are entirely theft 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 forrevision 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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103. 314 P DUP050296835 Designation: D 1844 - 86 (Reapproved 1991)61 Standard Test Methods for Chemical Analysts of Basic Lead Silicochromate1 This standard is issued under the fixed designation D 1844; 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 revision or reapproval. " --Keywords were added editorially in April 199.1. Scope ' I.1 These test methods cover the chemical analysis of the igment commercially known as basic lriad silicochromate |nd are applicable, to pigment supplied by the manufacturer d to pigment, .but not mixed pigments, separated from iquid coatings. The presence of basic lead silicochromate jecies shall be confirmed by X-ray diffraction analysis (see Ipecification D 16482). J.2 -For liquid coatings tlte pigment must first be separated from the vehicle before conducting the analysis. : 1.3 The analytical procedures appear in the following M.oj:den . ., ,, Lead oxide , 1 Chromium trioxide iplstoisture and other volatile mhtter `Coarse particles^. . ' 0# absorption , t . , |<;iMass color and tinting'strength' ''' '' " Sections 6 to 14 IS to23. 24 to 27 -28 29 30,. s v 3f 1.4 This-standard does not purport to address the safety | <problems, if any, associated with its use. It Js 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. . . |f 2. Referenced Documents f. .. i" i . a -2. L ASTM Standards: y. . . D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 - D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out2 D387 Test Method for..Color and Strength of Color figments with a Mechanical Muller2 D1193 Specification for Reagent Water4 D1648 Specification for Basic Lead Silicochromate Pig ment2 1 These test method* are under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.2I on Chemical Analysis of Paints and Paint Materials. Current edition approved April 25, I9g6. Published June 1986. Originally published as D 1844 - 61 T. Last previous edition D 1844 - 78. - Annual Book ofASTM Standards, Vol 06.02. ' Annual Book ofASTM Standards, Vols 06.01 and 06.02. ` Annual Book ofASTM Standards. Vols 06.03 and 11.01. D2371 Test Method..for Pigment Content of SolventReducible Paints5 ' - 3. Significance and Use 3.1 These test methods may be used to confirm the stated lead oxide, chromium trioxide and silica content of basic lead silicochromate and is useful for quality control. 4. Purity of Reagents 4.1 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. 4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. ^ 5. Preparation of Sample 5.1 Thoroughly mix liquid coatings and separate in .ac cordance with Test Method D;2371 sufficient pigment.-to enable the required analyses to be carried out. 5.2 Thoroughly mix pigment supplied as such and grind separated, pigment to a fine, powder in a mortar, and pestle before taking portions for analysis. TOTAL LEAI) AS LEAD OXIDE-GRAVIMETRIC METHOD 6. Apparatus 6.1 Glass Filtering Crucible (medium-porosity . fritted disk), dried to constant weight before use. 6.2 Platinum Dish. \ 7. Reagents 7.1 Acetic Acid (Glacial). 7.2 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH40H). -- 7.3 Ammonium Acetate, Acid Solution--To 300 mL of water add an equal volume of NH40H. Neutralize with 5 Annual Book ofASTM Standards, Vol 06.01. 6 "Reagent Chemicals. American Chemical Society Specifications," Am. Chem. 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." 315 DU P050296836 D 1844 glacial acetic acid and add 20 mL in excess. 7.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 7.5 Hydrofluoric Acid (47 %)--Concentrated hydrofluoric acid (HF). 7.6 Hydrogen Sulfide (H2S)--Handle and use H2S in hood. 7.7 Isopropyl Alcohol (50 and 98 %). 7.8 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03) (see 7.4.1). 7.9 Potassium Dichromate Solution (saturated)--Prepare a saturated solution of potassium dichromate (K2Cr207) in water. 7.10 Sulfuric Acid (1+1)--Careflilly mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84) with 1 volume of water (see 7.4.1). PbO, % = (P x 69.06))S where: P = lead chromate (PbCr04) precipitate, g, S = sample used, g, and molecular weight (PbO) _ molecular weight (PbCr04 223 21 22$ 21 ~ x '00 (for percent) = 69.06 69.06 represents the gravimetric factor to convert grams of PbCr04 to grams of PbO. This gravimetric factor has led to high results due to the presence of mixed lead chromates and an empirical, factor can be used to compensate: Empirical factor = 69.06 x 0.9944 = 68.67 8. Procedure ALTERNATIVE METHOD FOR TOTAL LEAD AS LEAD OXIDE--TITR1METR1C METHOD 8.1 Weigh accurately (to 0.1 mg) 1 g of the sample into a platinum dish. Add 5 mL of HN03 and 10 mL of HF. 10. Apparatus Cautiously evaporate to dryness on a steam bath. Repeat the 10.1 Platinum Dish. addition of HN03 and HF and again cautiously evaporate to 10.2 Filter Paper, ashless, medium texture, or paper pulp. dryness. Wash the sides of the dish with a little water and evaporate to dryness. Wet the residue with 5 mL of HN03>' 11. Reagents warm gently, and transfer the residue to a 400-mL beaker using a policeman. Neutralize with NH4OH, and then make the solution just add with HQ, adding 5 mL in excess. 11.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 11.2 Glacial Acetic Acid (min 99.7%)--Concentrated Dilute to 200 mL and heat to just below the boiling point until solution is complete. 8.2 Pass H2S through the solution for about 20 min. Filter, using paper pulp. Wash the precipitate five to six times with water just acid with HC1 and saturated with H2S. glacial acetic acid (CH3COOH). 11.3 Acid Ammonium Acetate Buffer--Mix 400 mL of distilled water and 400 mL of ammonium hydroxide (sp gr 0.90). Add 375 mL of reagent grade glacial acetic acid slowly while stirring. Transfer the paper and predpitate to the original beaker, add 11.4 Cupric Sulfate Solution (0.1 M)--Dissolve 25 g of 25 mL of HN03, boil until the residue is white, then add 10 CuS04 5H20 in distilled water and dilute to 1 L. mL of H2S04 (1+1). Destroy the organic material by 11.5 Disodium Ethylenediaminetetracetate Dihydrate evaporating the solution to dense white fumes, making (0.05 M) (EDTA solution)97--Dissolve 18.6 g of the salt in further additions of HN03 until there is no charring. 8.3 Cool the solution, add 10 mL of water, and evaporate to fumes. Repeat the addition of water and the evaporation. Cool the solution, add 40 mL of water, and bring the solution to boiling. Cool the solution and add 50 mL of isopropyl alcohol (98 %), stir, and allow the solution to stand cold for at least 4 h. Filter, using paper pulp, and wash once with cold isopropyl alcohol (50 %) containing 10 mL of distilled water and dilute to 1 L. Standardize the solution as follows: Transfer 25 mL of lead standard (11.14) to a 400-mL beaker. Add concentrated ammonium hydroxide (11.1) dropwise until a permanent precipitate just forms. Add 25 mL of acid ammonium acetata^l 1.3), dilute .to-200 mL, heat to boiling, add 4 drops of copper EDTA (11.7) and 12 drops ofPAN (11.13) and titrate with the EDTA to a clear yellow. ,,. H2S04 (sp gr 1.84)/100 :mL. 8.4 Transfer the precipitate to the original beaker with 1 mL Na2 EDTA - 0.2790/ Kg PbO 150 mL of water, add 50 mL of the ammonium acetate where: solution, and boil the solution until the lead sulfate dissolves. V = EDTA required for titration, mL Filter while hot through the original paper and wash well (6 g = lead oxide, g, and ii to 8 washes) with hot water. To the filtrate add 5 mL of 0.05 M x 0.22321 = 0.01116 g PbO in 1 mL oflead standard glacial acetic acid, heat the solution to boiling, and add 20 (10.14) (25 mL) (0.05 M) (0.22321) = 0.2790 g PbO in 25 mL of saturated K2Cr207 solution. Boil the solution until the mL of lead standard (10.14). precipitate turns orange, and allow to stand on a warm plate 11.6 Murexide Indicator Tablets--Ammonium salt of for at least 2 h. Filter through a glass filtering crucible purpuric add. (medium-porosity fritted disk), wash three times with hot 11.7 Copper-EDTA Solution--Mix equivalent amounts of water, and finally once with alcohol. Dry in an oven at 105C cupric sulfate solution (11.4) and EDTA solution (11.5) and for 2 h, cool, and weigh. store in a dropping bottle. The cupric suliate EDTA equiva lence may be determined as follows: Pipet 10 mL of cupric 9. Calculation 9.1 Calculate the percent of total lead as lead oxide (PbO) as follows: 7 The standardized solution may also be purchased from Corco Chemical Corp. Catalog No.--Special. 316 DUP050296837 # D 1844 Hftto a beaker, add concentrated ammonium hy- ie dropwise until the precipitate which forms just lives. Dilute to 200 mL with water, add two Murexide |or tablets, and titrate immediately with EDTA to a change from yellow to purple. Hydrochloric Acid {sp gr 1.19)--Concentrated hy- jloric acid' (HO) (see 7.4.1). Hydrofluoric Acid (47 %)--Concentrated hydro- lcacid(HF). TO Hydrogen Sulfide (H-2S)--Cylinder. Handle ahd use aood. JSt-1 Hydrogen Sulfide Wash Solution--Add. 10 mL of fcp gr 1.19) to 1 L of water and saturate with H2S. Ilf2 Nitric Acid (sp gr 1.42)--Concentrated nitric acid Ps). 1.13 Pan Indicator (l-(2-pyridylazo)-2-naphthol)--Disj|o.l g in 100 mL of ethanol. jj,14 Primary Standard (0.05 M lead nitrate)--Dissolve 5515 g of reagent grade lead nitrate in distilled water and Re to 1 L. S' ' 1 mL = 0.01116 g PbO *1.15 Sulfuric Acid (1+1)--Carefully mix 1 volume of jcentrated sulfuric acid (H2S04, sp gr 1.84) with 1 volume water. Procedure 12.1 Dissolve 1 g of pigment in accordance with 8.1 and t. ' ; `' 12.2 Cool, so that the addition of 25 mL ofwater does not lise excessive splattering of the sulfuric acid; the solution at s jpoint should be water white. Add ammonium hydroxide B gr 0,90) until the pH of the solution is 5 to 5.5 (as plicated by pH paper). Add 50 mL of add ammonium etate (11.3), boil 5 min, dilute to 200 mL with water, heat ( boiling, add 4 drops of copper-EDTA (11.7) and 12 drops 1"PAN (11.13) and titrate while hot with standard EDTA to clear yellow. P. Calculation bl 3.1 Calculate the percent lead oxide as follows: 5 Pbo, ^*199 ' r J-j where: *!`V ~ EDTA required for titration, mL, fp L = lead equivalent of EDTA solution, and y S = specimen weight, g. 14. Precision and Bias 14.1 On the basis of an interlaboratory study of the method in which operators in three laboratories analyzed Iy wo paints containing basic lead silicochromate with iron oxide the following criteria should be used for judging the acceptability of the results at the 95 % confidence level: 14:1.1 Repeatability--Two results, each the mean of du plicate determinations obtained by the same operator should be considered stispect if they differ by more than the following: Percent Absolute PbO 0.20 0.30 14.1.2 Reproducibility--A realistic range could not be established for results between laboratories because of the limited number of participating laboratories. 14.1.3 Bias--A bias statement could not be established because of the limited number ofparticipating laboratories. CHROMIUM TRIOXIDE 15. Interference 15.1 Soluble Fe+3 will cause high results. See Section 20. 16. Reagents 16.1 Potassium Dichromate, Standard. Solution (0.1 N)--Weigh 4.904 g of dried potassium dichromate (K2Cr207), dissolve it in water, and dilute to 1 L with water in a volumetric flask. 16.2 Potassium Iodide Solution (150 g/L)--Dissolve 150 g of potassium iodide (KI) in water and dilute to 1 L. 16.3 Hydrochloric Acid Mixture^SaXuT&te water with NaCl (about 350 g/L). To each litre of this solution add 150 mL of water and 100 mL of concentrated HC3 (sp gr 1.19). 16.4 Sodium Thiosulfate Solution (0.1 N)--Dissolve 24.8 g of reagent grade Na2S203 \5H20 in recently boiled water and dilute to 1 L with additional recently boiled water. To standardize, pipet. 25 mL of the standard potassium dichromate solution (exactly 0.1000 IV) into a 250-mL Erlenmeyer flask. Add 100 mL of water, 15 mL ofpotassium iodide solution, and 15 mL of concentrated hydrochloric acid (sp gr 1.19). Titrate the liberated iodine with,sodium thiosulfate solution until the reddish-brown color becomes quite faint. Add 5 mL of starch solution arid continue the titration dropwise until the blue color changes to a pale green. Calculate the normality of the sodium thiosulfate solution-as follows: . 2.5000 /=-- where: " N = normality, and M= sodium thiosulfate solution, mL, 16.5 Starch Indicator Solution--Make a homogeneous paste of 10 g of.soluble starch in cold waterTAdd to this l`L' of boiling water, stir rapidly, and cool. Salicylic acid <(1.25 g/L) may be added to preserve the indicator. Iflor Storage is required, the solution should be kept in a refrigerator at 4 to 10C (40 to 50?F). Prepare fresh indicator when the end point of the titration from blue to colorless or blue to light green fails to be sharp. 17. Procedure 17.1 Weigh to 0.1 mg about 1 g of sample into a 500-mL Erlenmeyer flask. Add 100 mL of NaCl-HCl solution and dissolve the sample without heat, keeping the solution'cold. (Silica will not dissolve, but it does not interfere witlr the analysis.) Add 10 mL of KI solution and titrate with 0.1 N sodium thiosulfate solution until the reddish-brown color is almost gone. Add 5 mL of starch solution and titrate slowly, dropwise, until the blue color changes to a light green. 18. Calculation 18.1 Calculate the percent ofchromium trioxide (Cr03) as follows: DU P050296838 # D 1844 Cr03, % = [(K,Wx 0.03334)/S2] where: Vl = sodium thiosulfate solution required for titration of the specimen, mL N = normality of the sodium thiosulfate solution, = sample used, g, and +6 Cr03 -- Cr+3 _ molecular weight (Cr03 milliequivalent weight 1000 x 3 (valence) 99.99 = 0.03334 1000 X 3 ALTERNATIVE METHOD FOR CHROMIUM TRIOXIDE 19. Scope 19.1 This test method determines total chromium as chromium trioxide. Iron oxide interference is masked by the Use of EDTA. This procedure is not applicable when chromium oxide green (Cr203) is present. This test method is limited to basic lead silicochromate pigments with or without iron oxide. 19.2 The perchloric acid is employed as an oxidizing agent to ensure complete oxidation of any reduced chro mium. When perchloric acid is used, concentrated nitric acid must also be used. The use of a perchloric acid hood is optional since the specimen is covered with a watch glass and is being oxidized, not wet ashed. 20; Reagents 1 20.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 20.2 Disodium. Ethylenediaminetetracetate Dihydrate (0.05 M) (EDTA)--Dissolve 18.6 g of the reagent, grade salt in distilled water and dilute to 1 L. See 11.5 for standardiza tion. 20.3 Hydrochloric Acid Mixture--See 16.3. 20.4 Hydrofluoric Acid (47 %)--Concentrated hydro fluoric acid (HF). 20.5 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 20.6 Perchloric Acid (sp gr 1.67)--Concentrated per chloric acid (HC104). 20.7 Potassium Dichromate, Standard Solution {0A N)-- See 16.1. , 20.8 Potassium Iodide Solution (150 g/Litre)--See 16.2. 20.9 Sodium Thiosulfate Solution (0.1 N)--See 16.4. 20.10 Starch Indicator Solution--See 16.5. 21. Procedure 21.1 Transfer 0.5 g of pigment to a 500-mL high-silica Erlenmeyer flask.8 Add 10 mL of nitric add (sp gr 1.42), and 10 mL of perchloric acid (sp gr 1.67) and cover with a watch glass. Evaporate to fumes (flask will fill with white vapor) of perchloric add, cool, add 15 mL of water, and evaporate to fumes. Continue fuming for 15-20 min (the spedmen should be red-orange color). Cool immediately by placing the flask in a cold water bath. 21.2 Wash down the cover glass and sides ofthe flask with 8 Vycor has been found suitable for this purpose. water. Add 50 mL of HC1 mixture and 50 mL of 0.05 M EDTA solution. Adjust to pH 8 (determined with pH paper) with ammonium hydroxide (sp gr 0.90) and add 50 mL of HQ mixture (16.3). Cool the flask to 20 to 25C, add 10 mL of potassium iodide solution, 10 mL of starch solution, and titrate immediately with standard sodium thiosulfate solu tion to a sharp change in the starch indicator. (The final solution color may be lavender or green depending on the composition of the sample). 21,3 Add 2 to 3 mL of HF, (20.4) stir for lh min and ifthe indicator changes color titrate to the endpoint. 22. Calculation 22.1 Calculate the percent chromium trioxide (Cr03) as follows: Cr03, % = [(KjjV] X 0.03334)/,] X 100 where: V2 = sodium thiosulfate solution required for titration of the specimen, g, JVj = normality of the sodium thiosulfate solution, and S3 = sample used, g. 23. Precision and Bias 23.1 On the basis of an interlaboratory study of this test method in which operators in three laboratories analyzed two paints containing basic lead silicochromate with iron oxide the following criteria should be used for judging the acceptability of the results at the 95 % confidence level. 23.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator should be considered suspect if they differ by more than the following: .^ . 3 % C1O3 5 % Ct 03 . Percent Absolute OO3 0.15 0.40 23.1.2 Reproducibility--A realistic range could not be established for results between laboratories because of the limited number of participating laboratories; -- ~: 23.1.3 Bias--A bias statement could not, be-established because of theJimited number of participating laboratories. SILICA 24. Apparatus 24.1 Platinum Crucible. 25. Reagents 25.1 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric add (HQ). . 25.2 Hydrofluoric Acid (47 %)--Concentrated hydro fluoric acid (HF). .. 25.3 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 25.4 Nitric Acid (1+19)--Mix 1 volume of concentrated HN03 (sp gr 1.42) with 19 volumes of water. 25.5 Perchloric Acid (sp gr 1.67)--Concentrated per chloric add (HCIO4). 25.6 Sulfuric Acid (1+4)--Carefully mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84)6 with 4 volumes of water. 318 *wmmm S8PPPW" DU P050296839 0 1844 K. Procedure f 26.1 Weigh 0.5 g of pigment and transfer to a 400-mL laker. Add 10 mL each of HC1 (sp gr 1.19) and HN03 (sp gr 42). Warm slightly, if necessary, to dissolve the chromate. ||d 50 mL of HC104 and fume for 15 to 20 min. Wash the des of the beaker down with 30 to 40 mL of water, vaporate, and fume for 10 min. Cool and dilute to 200 mL fth water. Filter through a double acid-washed quantitative Siper and wash eight times with hot water, once with HN03 JJ+19) and finally again with hot water. C26.2 Dry and ignite the paper and precipitate in a platinum crucible. Cool in a desiccator and weigh the iicible and contents. To the crucible add 2 drops of H2S04 H+4) and 15 mL of HF. Evaporate cautiously on a hot plate iid ignite at 100dC for approximately 5 min. Cool in a lesiccator and weigh to constant weight. w S7. Calculation r 27.1 Calculate the percent of silica (Si02) as follows: Si02, % = [(Wi - wy/SJ x 100 |where: ? Wl = weight of crucible and contents before HF treatment, S> pF2 = weight of crucible and contents after HF treatment, g, and jp4 = weight of Sample used, g. ' MOISTURE AND OTHER VOLATILE MATTER 28. Procedure 28.1 Determine moisture and other volatile matter in accordance with Method A of Test Method D 280. COARSE PARTICLES 29. Procedure 29.1 Determine the percent coarse particles in the pig ment as received in accordance with Test Methods D 185. OIL ABSORPTION 30. Procedure 30.1 Determine the oil absorption of the pigment in accordance with Test Method D 281. MASS COLOR AND TINTING STRENGTH 31. Procedure 31.1 Determine the mass color and tinting strength in accordance with Test Method D 387. 32. Precision and Bias 32.1 Precision and bias have not been determined. 33. Keywords 33.1 basic lead silicochromate; chromium in basic lead silicochromate; lead in basic lead silicochromate; lead oxide; pigment; silica in basic lead silicochromate The American Society for Testing and Materials takes no position respecting the validity ofanypatent 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 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 yclir comments have not received a fair hearing you should make your views known to the ASTM Committee oh Standards, 1916 Race St., Philadelphia, PA 1S1Q3. wmm 319 DUP050296840 Designation: D 1845 - 86 (Reapproved 1991)e1 Standard Test Methods for Chemical Analysis of Strontium Chromate Pigment1 This standard is issued under the fixed designation D 1845; 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. " Non--Keywords were added editorially in January 1991. 1. Scope 1.1 These test methods cover the chemical analysis of strontium chromate pigment. 1.2 The analytical procedures appear in the following order: Sections Strontium by the Strontium Sulfate Method Chromium by the Thiosulfate Method Chloride Content Sulfate Content Moisture and Other Volatile Matter Coarse Particles Mass Color and Tinting Strength 7 to 10 . 11 to 14 15 16 17 18 19 Jshall conform to the specifications of the Committee on | Analytical Reagents of the American Chemical Society, where such specifications are available.5 Other grades may be | used, provided it is first ascertained that, the reagent is of 1 sufficiently high purity to permit its use, without lessening I the accuracy of the determination. 1 4.2 Unless otherwise indicated, references, to wafer shall be understood to mean Type II of Specification D 1193. j 5. Apparatus 5.1 Gooch crucible. 5.2 Electric Furnace, capable of 800C. 1 1 1 1.3 This standard does not purport to address the safety 6. Preparation of Sample I ; 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, ' 6.1 Mix the sample thoroughly.' Take a sufficient .quantity I for chemical analysis and pass it through a No. 325 (4-p.m) I s limitations prior to use. sieve. 'j STRONTIUM BY THE STRONTIUM SUEPATE METHOD HI 2. Referenced Documents ' 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in -Pig ments3 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller3 D444 Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow)3 D1193 Specification for Reagent Water4 7. Reagents -j o?Il Acetic Acid (glacial). - 1 7.2 Ammonium Hydroxide (1+3)--Mix 1 volume of j Concentrated ammonium hydroxide (NH4OH, sp gr 0.90) I with 3 volumes of water. * I 7.3 Ethyl Alcohol, conforming to Formula No. 2B or No. 1 30 of the U.S. Bureau of Alcohol, Tobacco, and Firearms. J 7.4 Hydrochloric Acid (1+1)--Mix-equal volumes ofcon- j centrated hydrochloric acid (HC1, sp gr 1.19) and water. | 7.5 Suffiiric Acid (1+19)--Mix 1 volume of concentrated I sulfuric acid (H2S04, sp gr 1.84) with 19 volumes of water, j 3. Significance and Use 3.1 These test methods may be used to confirm the stated strontium oxide and chromium oxide content of strontium chromate. 4. Purity of Reagents 4.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents 1 These test methods are under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and are under the jurisdiction of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved April 25, 1986. Published June 1986. Originally published as D 1845 - 61 T. Last previous edition D 1845 -65 (1979)*2. 2 Annua! Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 8. Procedure 1 8.1 Weigh to 0.1 mg about 0.5 g of the sample into a J 400-mL beaker. Add 40 mL of HCi (1+1) and heat the j solution to dissolve the pigment. Add 40 mL ofethyl alcohol ! until the chromium is reduced, as this is indicated by a dark : coloration of the solution. Add to the solution 100 mL of ` water and sufficient NH4OH (1+3) to form a slight persistent f precipitate. -j 8.2 Add HCI dropwise until the precipitate just redissolves 5 (Note 1). Heat the solution to just under boiling and add 20 j mL of H2S04 (1+19). Add 100 mL of ethyl alcohol and | 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Cheroical 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." s 320 DUP050296841 _w the precipitate to settle for several hours or overnight. K 1--For a cleaner precipitate, add HC1 until a pH of 2.0 is ched, instead of adding HC1 dropwise until the precipitate is just -olved. Then add 25 mL of acetic acid to minimize the tendency of sulfate to form a complex with tiivalent chromium. Finally, heat the .jtion, and add H2S04 (1 + 19). 18.3 Filter the precipitate through a Gooch crucible that as been previously dried to constant weight. Wash the tecipitate several times with a solution of equal volumes of Jtyl alcohol, water, and H2S04 (1+19). Dry the crucible in | oven and then ignite for Vi h at 800C or until constant feight is attained (weight loss less than 0.1 mg). Cool and ieigh the crucible. 1: Calculation | 9.1 Calculate the percent of strontium oxide (SrO) as bllows: ' SrO, % = [(/x 0.56416)/5] x 100 Ivhere: f = SrS04 precipitate, g, and |j = pigment specimen, g. I n '.{A C n>0^ecu^ar weight of SrO 103.63 ' molecular weight of SrS04 163.70 10. Precision 10.1 Within Laboratory~Jbs usual difference between duplicate runs performed by the same analyst is approxipnately 0.2 % of the SrO content of the pigment tested. 'f 10.2 Between Laboratories--The average difference be tween two determinations performed by different analysts in (different laboratories is approximately 0.5 % of the SrO content of the pigment tested. CHROMIUM BY THE THIOSULFATE METHOD II. Reagents 11.1 Hydrochloric Acid (1+5)--Mix 1 volume of concen trated hydrochloric acid (HQ, sp gr 1.19) with 5 volumes of water. r 11.2 Potassium Iodide Solution (150 g per L)--Dissolve 150 g of potassium iodide (KI) in water and dilute to 1 L. 11.3 Sodium Thiosulfate Standard Solution (0.1 N)-- Dissolve 24.8 g of reagent grade Na2S203 5H20 in recently i boiled water and dilute to 1 L with additional recently boiled f water. To standardize, pipet 25 mL of the standard potassium dichromate solution (exactly 0.1000 N) into a 250-mL ' Erlenmeyer flask. Add 100 mL ofwater, 15 mL ofpotassium iodide solution, and 15 mL of concentrated hydrochloric acid (sp gr 1.19). Titrate the liberated iodine with sodium thiosulfate solution until the reddish-brown color becomes quite faint. Add 5 mL of starch solution and continue the titration dropwise until the blue color changes to a pale green. Calculate the normality of the sodium thiosulfate solution as follows: ,, 2.5000 Nm -- where: N = normality, and M - sodium thiosulfate solution, g. 11.4 Starch Indicator Solution--Make a homogenous paste of 10 g of soluble starch in cold water. Add to this 1 L of boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L) may be added to preserve the indicator. If long storage is required, the solution should be kept in a refrigerator at 4 to 10C (40 to 50`F). Prepare fresh indicator when the end point of the titration from blue to colorless or blue to light green fails to be sharp. 12. Procedure 12.1 Weigh accurately approximately 0.2 g of the sample into a 250-mL iodine flask. Add 50 mL of water and 50 mL of HC1 (1+5); swirl the flask to complete solution. Add 20 mL of KI solution and allow the solution to stand for several minutes. 12.2 Titrate the liberated iodine with 0.1 N Na2S203 'solution until the reddish brown iodine color becomes faint. Add 1 mL of starch solution and continue the titration cautiously to the end point which is easily discernible when the color changes from blue to a light green with no blue tinge. 13. Calculation 13.1 Calculate the percent of chromium as chromic oxide (Cr03) as follows: Cr03, % = [{VH x 0.03334)/5'J x 100 where: V = Na2S203 solution required for titration of specimen, mL, N -- normality of the Na2S203 solution, and S = sample used, g. 14. Precision and Bias 14.1 Within Laboratories--The usual difference between duplicate runs performed by the same analyst is approxi-- mately 0.3 % of the C1O3 content of the pigment tested. 14.2 Between Laboratories--The average difference be tween two determinations performed by different analysts in different laboratories is approximately 0.5'% of the Cr03 content of the pigment tested. 0 0334 - molecular weight CrP2 __ 99.99 U,U " 1000 x 3 (volume) 1000 x 3 = milliequivalent weight CHLORIDE CONTENT 15. Procedure 15.1 Determine the chloride content in accordance with Test Methods D 444. SULFATE CONTENT 16. Procedure 16.1 Determine the sulfate content in accordance with the Test Methods D 444. DUP050296842 MOISTURE AND OTHER VOLATILE MATTER D 1845 MASS COLOR AND TINTING STRENGTH. [i 17. Procedure ' 17.1 Determine moisture and other volatile matter* in accordance with Method A of Test Methods D.280. COARSE PARTICLES 18. Procedure 18.1 Determine the percentage of coarse particles-in the pigment as received in accordance with Test Methods D 185. 19. Procedure 19.1 Determine mass icofor and tinting strength in accord^ ; ance with Test Method D 387. 1 20. Keywords 20.1 chromium, thiosulfate method; strontium chromate pigment The American Society for Testing andMaterials takes no position respecting the validity a!anypatentrights assertedIn connection with any Item mentioned In this standard. Users of this standard are expressly advised, that domination 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 V not revised, either reapprovedor withdrawn, Yourcomments are Invited either lorrevision ofthis standard or toradditional standards 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 s views known to the'ASTM'Committee on Standards, Race St., Philadelphia, PA 19103. f DU P0502 96843 Designation: D 1847 - 87 Standard Test Methods for brd-; Total Chlorine Content of Epoxy Resins1 This standard is issued under the fixed designation D 1S47; 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. iate scope .1 These test methods cover the determination of the chlorine content, in concentrations below 1 weight ircent, of epoxy resins. Both organic and inorganic chlorine apounds contained in the resin are determined. Epoxy i is defined as the reaction product ofa chlorohydrin and or polyfunctional phenolic compound, ft 1.2 Two alternative test methods for determining chloride In concentration resulting from combustion of the sample fe included as follows: l Method A--Potentiometric Titration Pst Method B---Gravimetric Determination Sections 6 to 10 11 to 15 1l3 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 ' M responsibility' of tM user of this standard to establish tAfopriate safety qhfi health, practices, and determine the \SpfiliccibUUy of regulatory limiiatiShs prior ip itse. .Specific ' hazards are given in Section 12. 5. Purity of Reagents 5.1 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.3 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 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. TEST METHOD A--POTENTIOMETRIC TITRATION 6. Apparatus 6.1 Combustion Apparatus--Ah oxygbii bomb4 apparatus for combustion of the sample. ' 6:2 Titration Apparatus*--A suitable pH meter equipped with a glass-silver electrode system and' titration stand, stirrer, beakers, and 10-mL buret. ,7/ 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 3. Summary of Test Methods 3.1 The resin is oxidized by combustion in a bomb containing oxygen under pressure. The chlorine compounds thus liberated are absorbed in a sodium carbonate solution. In Test Method A the amount of chlorine present is determined by potentiometric titration with standard silver nitrate solution.' In Test Method B the amount of chlorine present is determined gravimetrically by precipitation as silver chloride. ' 4. Significance and Use 4.1 The total chlorine content of epoxy resins is an important variable in determining reactivity of epoxy resins and performance ofcoatings prepared from them. These test methods may be used to determine the total chlorine content of manufactured epoxy resins to confirm specification limits. 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 D 01.33 on Resins and Varnishes, Including Shellac. Current edition approved Nov. 27, 1987. Published January 1988. Originally published as D 1847 - 61 T. Last previous edition D 1847 - 73 (1980)*'. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 7. Reagents 7.1 Methyl Red Indicator (0.2 % alcohol solution)--Dis solve 0.2 g of methyl red in 100 mL of methanol, ethanol or wopropanol. 7.2 Nitric Acid (sp gr 1.42)--Concentrated, nitric acid (HN03). 7.3 Oxygen, free of . combustible materials and hMogen compounds, available at a pressure of 40 atm. .7.4 Silver Nitrate, Standard Solution (0.01 N)--Dissolve in water 1.70 0,01 g of crystalline silver nitrate (AgN03)... which previously has been pulverized, dried at 150C for 1 h, and stored in a glass-stoppered bottle, and dilute to 1 L. Standardize against an accurately weighed amount of so dium chloride (NaCl) dissolved in 75 to 100 mL of water. 7.5 Sodium Carbonate Solution (20 g/L)--Dissolve 20 g of sodium carbonate (NaiC03) in water and dilute to 1 L 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 Slates Pharmacopeia." 4 The Pair, double-valve, self-sealing oxygen bomb equipped with a safetyrelief-type Oxygen filling connection, ignition circuit, rase wire, sample cups, and water bath, available ftom Parr Instrument Co., 209 53td St., Moline, IL 61265, has been found satisfactory for this purpose. s The Dual Titrimeter manufactured by the Precision Scientific Co., 3737 W. Cortland St, Chicago, IL, and the Beckman pH meter (Model M or G) manufactured- by Beckman Instruments, Inc., 2500-T Harbor Blvd., Fullerton, CA, have been found satisfactory for this purpose. 323 DUP050296844 # D 1847 8. Procedure 8.2.5 Plot the cumulative volumes of 0.1 N AgNOJ; 8.1 Combustion ofSpecimen: 8.1.1 Place 25 mL of Na2C03 solution in the bottom of the bomb. Incline the bomb and rotate it in such a manner that the interior surface is moistened by the solution. 8.1.2 Weigh to 1 mg 0.8 to 1.2 g of sample into the metal sample cup. Grind solid resins to pass a No. 60 (250-pm) solution added against the corresponding cell potentials. Select as the end point the midway point on the steepest portion ofthe inflection curve. 8.2.6 Make a blank determination in accordance with 8.2.1 through 8.2.4, but omit the specimen. This procedure will give a measure of the chlorine in the reagents used. sieve and moisten with a few drops of acetone before combustion. 9. Calculation 8.1.3 Insert the cup containing the sample in the loop 9.1 Calculate the chlorine content of the sample as electrode and attach the fuse wire so that it hangs slightly follows: above the specimen. Assemble the bomb and tighten the Chlorine, %={(V-B)Nx 0.0355/S) X 100 cover securely; however; do not use auxiliary tools to tighten the cover. 8.1.4 Attach the filling connection to the oxygen-filling valve and admit oxygen slowly (to avoid blowing the sample from the cup) until a pressure of 35 atm is indicated bn the gage; then close the control valve. Open the relief valve to reduce the pressure in the tube and in the connection to where: V = AgN03 solution required for titration ofthe specimen, mL B = AgN03 solution required for titration ofthe blank, mL N = normality of the AgN03 solution, and S = specimen weight used, g. atmospheric pressure. Detach the filling connection from the bomb and replace with the bomb thumb nut Tighten the thumb nut with finger pressure. 8.1.5 Immerse the bomb in the water bath, then connect the terminals to the electrical circuit. Ignite the charge within the bomb by closing the switch for not more than 5 s, or until the pilot light goes out. Allow the bomb to stand in the water bath for 10 min while cooling. 8.1.6 Remove the bomb from the water bath, and invert and rotate it so that maximum washing of the inside surface is achieved. Release the pressure at a uniform rate over a 10. Precision 10.1 The following criteria should be used for judging the acceptability of 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 0.02 weight %. 10.1.2 Reproducibility--The results, each the mean of two determinations, obtained by operators in different labo ratories should be considered suspect if they differ by more than 0.05 weight %. period of not less than 1 min. 8.2 Titration: TEST METHOD B--GRAVIMETRIC DETERMINATION 8.2.1 Transfer the absorbing solution from the combus tion of the sample to a 250-mL tail-form titration beaker. Wash all the inside surfaces ofthe bomb with a fine stream of water and transfer the washings to the beaker. Adjust the 11. Apparatus 11.1 Combustion Apparatus--See 6.1. 11.2 Fritted-Glass, medium porosity. volume of the solution to 150 to 200 mL with water. Add three drops of methyl red indicator solution and neutralize 12. Reagents If with HN03; then add 6 drops in excess. 12.1 Warning--Nitric Acid (sp gr 1.42)--Concentrated 8.2.2 Place the beaker on the titration stand and adjust its nitric acid (HN03). position so that the electrodes are about half immersed; Fill 12.2 Caution--Nitric Acid (1+99)--Mix 1 volume of the buret with 0.01 N AgN03 solution, and place the buret in HN03 (sp-gr l.42) with 99 volumes of water. position on the titration assembly so that the tip extends 12.3 Oxygen--See 7.3. __ approximately 25 mm below the surface of the liquid in the 12.4 Potassium Iodide Solution (300- g/litre)--Dissolve beaker. Adjust the speed of the stirrer to give vigorous 300 g of potassium iodide (KI) in water and dilute to 1 E. stirring without splattering. Record the initial buret and 12.5 Silver Nitrate Solution (100 g/L)--Dissolve 100 g of meter (cell potential) readings. silver nitrate (AgN03) in water and dilute to 1 L. 8.2.3 Add small portions of 0.01 N AgN03 solution and, 12.6 Silver Nitrate, Standard Solution (0.01 N)--See 7.4. after waiting until a constant potential has been established, 12.7 Sodium Carbonate Solution (20 g/L)--See 7.5. record the buret and meter readings. In regions between inflections where the potential change is small for each 13. Procedure increment of AgNG3 solution, add volumes as large as 0.5 13.1. Oxidize the specimen by combustion in accordance mL. When the rate of change of cell potential becomes with 8.1.1 to,,8.1.6. greater than 5 mV per 0.1 mL, use 0.1-mL increments of 13.2 Transfer the absorbing solution from the combustion 0.01 IV AgN03 solution. of the specimen to a 250-mL beaker. Wash all the inside 8.2.4 Continue the titration until the rate ofChange of cell surfaces ofthe bomb with a fine stream ofwater and transfer potential is less than. 2 mV per 0.1 mL of AgN03 solution. the washings to the beaker. Add 1 mL of HN03 (sp gr 1.42) Remove the titrated solution, rinse the electrodes well with to the solution; then, with stirring, add 1 mL of AgN03 water, wipe with a dry cloth, and burnish the silver electrode solution (100 g/L). Heat the solution to boiling as rapidly as lightly with a fine emery cloth. Between determinations, possible. Allow the mixture to cool in a dark cabinet for at immerse the electrodes in water. least 1 h. 324 DU P050296845 D 1847 13.3 Filter the precipitate by suction on a clean, fritted,,s filter funnel. Wash the silver chloride (AgCl) precipitate proughly with HN03 (1+99). Dry the filter and precipitate ii| I0C for 1 h. Cool in a desiccator and weigh accurately to mg. 13.4 Dissolve the AgCl from the filter, using KI solution, 'ash the filter thoroughly with HN03 (1.+99). Dry the filter t 110C for 1 h, cool in a desiccator, and reweigh. The ight of AgCl obtained from the sample is the difference tween the weight of the filter funnel containing the redpitate and the weight of the filter funnel obtained at this ae. 13.5 Make a blank determination in accordance with 13.2 'fid 13.4, but omit the specimen. This procedure will give a " easure of the chlorine in the reagents used. 4. Calculation 14.1 Calculate the chlorine content of the spedmen as follows: Chlorine, % = [(/- B) x 0.2474/S] x 100 where: P - AgQ precipitate from the spedmen, g, B -- AgQ found in the blank, g, and S *= specimen used, g. 15. Precision 15.1 The following criteria should be used forjudging the acceptability of results at the 95% confidence level. 15.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.05 weight percent 15.1.2 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 0.05 weight percent. 77is American Society tor Testing and Materials takes no position respecting the validity of arty patent rights asserted in connection with any item mbntionechin 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 auoh 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 'Ifhotrevised, eitherreapproveddr withdrawn. Your comments anaInvitedeither forrevision ofthis standard or loradditional standards end should be addressed to ASTM Headquarters. Yourcomments will receive careful consideration at e 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. 325 DUP050296846 Designation: D 1915 - 63 (Reapproved 1989) Standard Test Method for Chromatographic Analysis of Chemically Refined Cellulose1 This standard is issued under the fixed designation D1915; 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 --Editorial changes were made throughout, including the title, in October 1989. 1 i ii $ 1. Scope requires quantitative handling of the carbohydrate portion f 1.1 This test method covers the determination of the throughout the entire sequence of chromatographic opera- jj composition of chemically refined cellulose by chromato tions. In the case of purified celluloses, where the carbohy- i graphic analysis. This test method is suitable for rapid and drate fraction comprises all but a minor part of a given routine testing of large numbers of samples with high sample, it is convenient to express composition on the basis j accuracy and precision. of the ratios of the carbohydrate constituents; that is, the j 1.2 This standard may involve hazardous materials, oper quantity of each isolated sugar is expressed as a percent of f ations, and equipment. This standard does not-purport to the combined sugar content of the sample. Quantitative address all ofthe safety problems associated with its use. It is handling is thus not required until application of the J the responsibility of the user of this standard to establish hydrolyzate to the paper. Proper correction for conversion of 1 |: appropriate safety and health practices and determine the polysaccharide to monosaccharide and for decomposition j applicability ofregulatory limitations prior to use. are of course required in any method of analysis. These may j conveniently be accounted for by calibration. j 2. Referenced Document 5. Purity of Reagents 2.1 ASTM Standard: D1193 Specification for Reagent Water2 5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents 3. Summary of Test Method i* shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,' : 3.1 Quantitative paper chromatographic analysis of where such specifications are available.3 Other grades may be polysaccharides by the chemical method involves the fol used, provided it is first ascertained that the reagent is of lowing operations: (/) total hydrolysis, (2) neutralization, sufficiently high purity to permit its use without lessening the (5) concentration, (4) chromatographic separation, (J) accuracy of the determination. elution, (6) analysis of separated sugars, and (7) calibration 5.2 Unless otherwise indicated, references to water shall and calculation. be understood to mean reagent water conforming to Specifi- . 4. Significance and Use cation D 1193. 4.1 While this test method involves a chemical determina tion of separated sugars, it is recognized that direct photom etry of the chromatogram can also be capable of good precision. All of the steps involved, up to the actual determination, are the same for both techniques. Direct chemical measurement is of more general applicability in a chromatographic laboratory, however, since it involves no special instrumentation and it is adaptable to the determina tion of a variety of materials. 4.2 The carbohydrate composition of a cellulosic material may be expressed either on the basis of the total initial sample or on the basis of the carbohydrate portion of the sample. The former establishes composition on an absolute basis. It requires precise information concerning all compo nents present in the starting material, or lacking this, it 6. Sampling -- 6.1 Take samples from not less than 10 % of each lot in the shipment. Then composite these samples to represent each lot or latch. TOTAL HYDROLYSIS 7. Summary of Procedure 7.1 The total hydrolysis of a cellulose requires a primary hydrolysis with strong mineral acid followed by a secondary hydrolysis in dilute acid. The primary hydrolysis results in the formation of a mixture of oligosaccharides. It is the function ofthe secondary hydrolysis to complete the conver sion to monomeric sugars (l).4 1 This test method is under the jurisdiction of ASTM Committee D-23 on Cellulose and Cellulose Derivatives and is the direct responsibility of Subcom mittee D23.20 on Cellulose. Current edition approved Nov. 19, 1963. Published January 1963. Originally published as D 1915 - 61. Last previous edition D 1915 - 61T. 3 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." 4 The boldface numbers in parentheses refer to the list of references at the end of this test method. 326 WWPbM DUP050296847 D 1915 apparatus I Shell Vials, 25 by 90-mm. Stirring Rods, 5 by 150-mm. 3 Water Bath, controlled at 30 0.1C. J$ Pipet, 3 0.005-mL (preferably syringe pipet for safe, pse pipetting of the sulfuric acid; see Fig. 1). Laboratory Sterilizing Autoclave, preferably with tier to provide clean steam, and fitted with time clockiiiated steam and water valves. .6 High-Speed Mixer to disintegrate tough pulp sheets. f.7 Analytical Balance, with a capacity of 200 g and a iitdvity of 0.1 mg iReagent 9.1 Sulfuric Acid{72.0 0.1 weight %)--To 1 volume of |ter add slowly while stirring vigorously 2 volumes of jjpcentrated sulfuric acid (H2S04, sp gr 1.84). When cool, todaidize against a standard alkaline solution. Adjust the Id strength to 72.0 0.1 weight %. Procedure 40.1 Primary Hydrolysis--Weigh 0.30 g of loose pulp lote 1) into a 25 by 90-mm shell vial and add 3.0 mL of 2S04 (72 %) (Note 2). Using a 5 by 150-mm rod, stir at ntervals as required to dissolve the pulp , rapidly and ompletely (Notes 3 and 4), leaving the stirring rod in the dal at all times. Maintain the mixture at 30.0 0.1'C for a ptal of 1 h. Then dilute by washing the contents of the vial jtto a 250-mL, tared, wide-mouth bottle with 84 mL of ater measured in a 100-mL graduate. The bottles should be |f such size as to fit the cups of a laboratory centrifuge. 1--Precise weighing is necessary if the determination is to be [ion an absolute basis; it is not necessary if the final determination is [based on the ratios of the component sugars. 2--The use of a hypodermic syringe pipet, equipped with [suitable stops, greatly facilitates the precise pipetting of replicate 3-mL portions of H2S04 (72 %) with an accuracy of 0.005 mL. One design Of such a pipet is shown in Fig. 1. An aluminum button on the end of the plunger and a brass band around the barrel are bonded to the glass with epoxy resin. The projection on the brass band is slotted, so as to serve as a guide as well as a stop for the volume adjusting rod. Accurate dispensing of acid facilitates neutralization on a routine basis. 3--Sheeted specimens may prove difficult to dissolve. They should be dispersed in a water slurry by means of a high-speed stirrer or blender, then filtered on a Buchner funnel, washed with acetone, and air-dried. 4--When many specimens are being handled, primary hydrolysis of successive specimens should begin and end at 2-min intervals. 10.2 Secondary Hydrolysis--Cover the bottles containing the diluted hydrolyzates from the primary hydrolysis with 50-mm watch glasses and place them in a preheated autoclave. Admit live steam to the autoclave and continue heating for 4 h (Note 5) at the boiling point of water (saturated steam at atmospheric pressure) (Note 6), following which cool the autoclave to room temperature. A total of 50 specimens can be processed simultaneously in a standard 20 by 30-in. (508 by 762-mm) laboratory sterilizer. 5--For routine use, it is convenient to control the duration of the incoming steam by means of a solenoid valve actuated by a time clock. At the end ofthe steamingcycle, a second clock-operated solenoid valve can be used to admit cooling water to a coil of copper tubing in contact with the metal rack supporting the sample bottles. In this way, the 4-h secondary hydrolysis can be completed overnight and the specimens are ready for neutralization next morning. 6--It is possible to reduce the time required for secondary hydrolysis by going to higher steam pressures in the autoclave (2). Because of increased rate of sugar decomposition, however, it then ' becomes necessary to exercise rigid control over each step in the autoclaving operation so as to maintain a high level ofaccuracy. On this basis, the use ofatmospheric steam pressure in an autoclave fitted out as described above would seem to present fewer problems. In addition, recent work has shown that complete hydrolysis can be accomplished with less net destruction at the lower temperature.' - NEUTRALIZATION - 11. Apparatus 11.1 pH Meter. 11.2 Titration Assembly, with stirrer, as shown in Fig. 2. 11.3 Balance, sensitive to 0.1 g. 11.4 Centrifuge. ' ? 3 frafcc / j jHk FIG. 1 Adjustable Syringe Pipet l 327 DU P050296848 # D 1915 TO CARBOY OF 11.5 Calibrated Pipets, 200-mL, for quantitative transfer of hydrolyzate to the evaporator. These pipets are required only when the sugar ratio method is not adequate. 12. Reagents 12.1 Barium Hydroxide Solution (70 g/L)--Dissolve 70 g of barium hydroxide (Ba(OH)2-8H20) in water, dilute to 1 L, and protect suitably from atmospheric carbon dioxide. 12.2 Ion-Exchange Resin, anion exchanger, weakly basic, granular form, 20 to 50-mesh.5 13. Procedure 13.1 Neutralize the hydrolyzates by direct titration with a saturated barium hydroxide (Ba(OH)z) solution, as follows (Note 7): Affix an individual specimen in its tared bottle to the titration assembly shown in Fig. 2. Admit the Ba(0H)2 solution directly from the stock carboy, while the bottle contents are under vigorous agitation, to a pH of approxi 5 Araberlite 1R-4B, manufactured by Rohm & Haas Co., Philadelphia, PA, has been found satisfactory for this purpose. mately 5.5. Put the bottle aside until.aU other specimens in the series are neutralized. The barium sulfate (BaS04) formed in these relatively concentrated solutions occludes H2S04, which is slowly released, resulting .in a decreasing pH. By allowing the solution to stand for about 1 h and then readjusting the pH to the desired 5.3 with additional Ba(OH)2 solution, the problem of drift is eliminated. 7--Many laboratories prefer to neutralize sugar hydrolyzates with ion-exchange resins, using both anion and cation-exchange col umns. When handling large numbers of specimens, however, columns are inconvenient, and.simple batch neutralization with anion resin only has been found adequate (2). Neutralization is accomplished by mixing the cooled hydrolyzates with approximately 25 g of the freshly washed ion-exchange resin. This quantity of resin is such as to raise the pH to 3.8 to 4.0 in the convenient time of 25 to 30 min, following which the solution is recovered by filtration and washing. Here again, quantitative sugar recovery from the resin is necessary only if the determination is to be made on an absolute basis. The need for prewashing the resin arises from the fact that relatively large amounts ofwater-soluble materials are released by the resin during storage. 13.2 Adjust the bottles containing the neutralized hydrolyzates to a net weight of 258.4 g by the addition of 328 mum BiPW*""1 DUP050296849 D 1915 ater. Each bottle now contains 250 mL of solution and 8.4 pf BaS04, 13.3 Centrifuge the bottles to settle the BaS04 and take a E00-mL aliquot ofthe clear supernatant liquid from each for gjyaporation. ; 8--To avoid sugar losses by yeast or microbial action, storage if neutralized hydrolyzates should be done under refrigeration. The dition of a few drops of toluene affords added protection. 9--If, as in the usual case, it is sufficient to measure ratios of lie carbohydrate constituents, the 200-mL aliquot and the prior adjustment to 250-mL need not be done accurately. If, however, it is desired to determine composition on an absolute basis, exact volumes must be used. CONCENTRATION 14. Apparatus 14.1 Evaporator and Condenser---A simple, inexpensive evaporator that is rapid in operation, permits high recovery ofproduct, and causes a minimum ofsugar decomposition is 329 wpsr DUP050296850 # D 1915 siawa:ia Fig. 3 (2) (Note 10). With a bank of three such units, one operator can conveniently evaporate 50 specimens a day from 200 mL of 3 mL (Note 11). --The evaporators shown in Fig. 3 can be made by a glass blower from the indicated design. The main critical feature of tbe evaporator is that ofproviding a smooth tangential entry from the boiler section to the liquid reservoir. NOTE 11--In unbuffered systems, a 100-fold concentration of solu tions containing a nonvolatile strong acid results in a drop of 2 units in pH. On complete solvent removal, much greater pH changes result. Because of the buffering action of materials dissolved from the resin, resin-neutralized solutions show much less pH change on evaporation than do those neutralized with barium hydroxide. Regardless of the neutralization or evaporation technique employed, it must be kept in mind that excessive pH changes can lead to serious error in the sugar content ofhydrolyzates. Too low a pH causes reversion, while too high a pH results in epimerization. Adjustments in technique should be made as necessary to ensure that tbe pH ofthe concentrate will be maintained in tbe 3.5 to 5.0 region. 14.2 Vapor Washing Unit, consisting of a 3-L flask with ground joint fitting the evaporator and arranged for boiling water rapidly. This unit is required only when the sugar ratio method is not adequate. 14.3 Pressure Controllers for the water and steam supply to the evaporators. 14.4 Aspirator, one for each evaporator. 15. Procedure 15.1 With the aspirator turned on and the-condenser in operation, draw the entire 200 mL of hydro'lyzate into the evaporator through the capillary stopcock, taking care to admit the last portion slowly and to close the cock just as air enters the bore. Tbe solution should have been previously cooled to a temperature below the boiling point at the pressure used for evaporation (Note 8). Then adjust the stopcock to provide a very slow stream of air bubbles into the evaporator. This promotes smooth ebullition. Turn on steam into the boiler jacket. The addition of pressure controllers to the steam and water supply greatly facilitates the operation of the evaporators. With pressure control, no individual adjustment ofsteam to the evaporator or water to the condenser is necessary. Pressures of 5 psi (30 kPa) for steam and 15 psi (100 kPa) for water have proven satisfactory. 15.2 Carry out the last stages ofevaporation cautiously, in fact, this can be accomplished with the small amount of warm condensate left in the heater jacket as the steam is turned off. The concentration required at this point depends on the composition of the pulp, but a final volume of 2 to 4 mL is common. This final volume can be read with sufficient accuracy by using calibration marks on the evaporator. The concentrate is recovered in high yield by draining it from the stopcock into a small plastic-capped vial (Note 13). The solutions are now ready for chromatography. They should be kept under refrigeration until so used. 13--Quantitative removal of sugar concentrate from the evaporator may be effected by removing the evaporator from the condenser and fitting it to a flask containing rapidly boiling water. The vapors condensing on the cold inside surfaces wash out the sugars with a minimum ofdilution. CHROMATOGRAPHIC SEPARATION 16. Summary of Procedure 16.1 In this separation procedure the previously prepared sugar concentrates are applied to filter paper by streaking, the paper is irrigated by descending chromatography, and the sugar-containing areas are cut out for chemical analysis. 17. Apparatus 17.1 Plywood Jig for folding paper to conform with requirements of the paper holders in the chromatographic cabinets. 17.2 Chromatographic Streaking Device, as shown in Fig. 4. - 17.3 Chromatographic Cabinets for 18`A by 22VWn. (463.6 by 571.5 mm) paper. 17.4 Separate Chromatographic Room held at 30 0.TC (Note 15). 17.5 Steel Template, 7.5 0.1 by 60 cm (any convenient thickness). 17.6 Paper-Cutting Knife. 17.7 Circulating Oven for heating guide strips at 105C. 17.8 Filter Paper--Special filter paper for paper chroma tography, in 18'/4 by 22!/2-in. sheets. Two grades are required, a normal high grade, rapid paper for general work, and a thick, strong paper of medium filtering speed with smooth surface. 18. Reagents 18.1 Irrigation Solvent--Mix 10 volumes of butanol with 3 volumes of pyridine and 3 volumes of water. Also needed when arabinose is present is a solution of 9 volumes of ethyl acetate, 2 volumes of acetic acid, and 2 volumes of water. 18.2 IndicatingSolution--Mix 800 mL ofbutanol, 40 mL of water, 8 mL of aniline, and 14.7 g of phthalic acid. This may be used as a spray. For use as a dip, mix equal volumes of this solution and ethyl ether. 19. Procedure 19.1 Sample Application--Carry out chromatographic separations on 18>4 by 22`/2-in. (463.6 by 571.5-mm)jsheets of chromatographic paper, normal, rapid filtering type,6 having folds made on a jig in positions to suit the reqiiirements of the paper holders in the chromatographic cabinet. The long dimension of the paper is-the machine direction and is the direction used for solvent flow. "Hang the folded paper over the supporting bar of the streaking device illustrated in Fig. 4 (Note 14). Move the.wooden holder bearing the syringe loaded with sugar concentrate down the steel bar to apply a uniform streak ofspecimen to the starting line. With the normal chromatographic paper, the maximum loading is limited to about 6 pL ofsolution per centimetre of streak, or about 400 pg of total sugar per centimeter of streak. Loading on heavier papers can be increased in proportion to paper weight. Air-dry the streaked papers. 14--The application of specimen to the paper as a continuous streak rather than as spots has the advantage, in direct photometry, of providing a uniform band of specimen; and when chemical methods are used, it has the advantage of loading the paper to the limit of its capacity, thereby providing the most favorable ratio of applied sugar to paper blank. Tbe streaking device shown in Fig. 4 is simple to construct, and its precision and utility have been proven in extensive use. The only 1 I 4 6A Beckman Model DU spectrophotometer, manufactured by Beckman Instruments, Inc., 2500 Harbour Blvd., Mail Station E 31D, Fullerton, CA 92634, has been found satisfactory for this purpose. 330 u.rnmuisvmmmmtMium | DUP050296851 D 1915 Paper Holder '/2"x l"x 25'/2" 24 GA. Stainless Angle ^4Ml. Tuberculin Syringe Cemented to Hardwood Slider. (Plunger End Meltdd to Spherical Shape and Needle Bent for Proper Contact with Paper) Paper (Chromatograhic Paper Support Bar 5/g''x |"x 261/2" Hardwood Slope 1724" Spoce Bar " I "x 5" Steel-Plated / Paper Support Rod 3/o 265/8 Stainless Rod End Plate'' 3/s"x 5i/2"x4i/2" Hardwood Plywood 2 Required Straightedge 1/4'x 2"x 24" Steel- 0.0002" or Plated 2 Required Base l'/4 x 9 x 26!/2' Hardwood - Finished Space Bar v 8'' |'' 7" Steel-Plated t in: ,25.4 mm. FIG. 4 Device for the Precise Unear Application of Pulp Hydroiyzates to Chromatographic Paper S critical details of construction are the two straightedges whose angular ''separation governs the loading of sugar concentrate on the paper. The ! indicated slope and syringe size are suitable for the normal chromatojpgraphic paper. 19.2 Solvent'irrigatibn and Isolation ofSugars--Tot irri gation, hang the streaked papers from the supporting tods in 3dhe chromatographic cabinet (Note 15), then add approxi; mately 5()0 tnL of'solvent directly to'the bottom pf the icabinet or to a shallow tray resting on the bottom. Close the' cabinet for about 1 h to permit vapor equilibration. Add solvent to the troughs into which the starting edges of the papers project. Continue irrigation for a period of time i||\sufficient to move xylose neatly to the bottom of the sheets, i'g IWheri using the butanobpyridine-water solution (Note |6), Bj this time period is approximately 55 h for the normal |l|chrpmatographic paper (Note 17) at 30C. Iii 19.3 papers After completion of the irrigation period, dry the in a suitably ventilated space. Cut four strips spaced about equally apart vertically from the starting line of each chromatogram, using a steel template 75 1 mm wide by. 600 mm long and a paper knife. (With a little experience, this cutting can be done accurately to a fraction of a I millimetre.) 1 19.4 Next dip the guide strips remaining into a solution made by mixing equal volumes of ethyl ether and indicating Vt solution. Allow the strips to drip dry, then heat in a circulating oven at 105C for 15 min to color the sugar- containing areas. Match the previously cut out vertical strips with the guide strips, and remove the areas containing the' glucose, manriose, and xylose. At this point, individual sugar components of the initial pulp hydrolyzate are present-on four replicate tabs of paper, each 75 mm wide by approxi mately 2 in. (50 mm) long in the initial-length direction of the sheet. "' 15--Temperature differences across a cabinet cab have a serious effect onthe'parallelism of the separating sugar zones. For this reason, it is desirable to locate the cabinets in a small thermostattetf room. By means of a mercury regulator, operating'one or more, household circulating Ian heaters, room, temperature can be controlled to approximately 0.1C. Auxiliary fans directed at the cabinets enhance air circulation. Cabinets should be supported several inches offthe floor on wooden blocks. Because ofthe Obnoxious odor ofpyridine, adequate ventilation facilities should he provided to remove solvent vapors when papers are being removed from the cabinets and air-dried. 16--Purified wood pulps generally contain only glucan, mannan, and xylan as their carbohydrate components. The butanolpyridine-water system has proved entirely adequate for such separations:litis system fails to resolve mannose and arabinose, however, and in the presence of large amounts of glucose, galactose cannot be cleanly separated from glucose. In pulps yielding these other sugars, the hydroiyzates are streaked on narrower sheets of paper which are first irrigated in chromatographic jars with an ethyl acetate-acetic acid-water system (9 + 2 '+ 2) for 28 h then dried and irrigated in the cabinets with a butarioi-pyridine-waier system (10 + 3 + 3) for 32 h. This double irrigation separates mannose, arabinose, and xylose into well defined bands. Galactose may be isolated by extending the irrigation with butanol-pyridine-water to the point where glucose is at the bottom ofthe sheet, all the other sugars being off. Galactose then occupies a separated DUP050296852 # D 1915 FIG. 5 Elution Rack + Calibrated Plpet (or Recovering Sugars Irani Chromatogram band between glucose and the starting line. The ethyl acetate-acetic acid-water system provides rather clean separation of all five sugars in small jars, but its performance in cabinets has been disappointing. ELUTION 20. Summary of Procedure 20.1 The determination of small quantities of sugar by chemical analysis requires that individual sugars be isolated from their respective 2 by 3-in. (51 by 76-mm) tabs ofpaper. This can be done quantitatively with little solvent and little manipulation by a combination of techniques (3,4). 21. Apparatus 21.1 Elution Rack, as illustrated in Fig. 5. 21.2 Cabinet for elution rack (a simple glass-covered box lined with Wotting paper). 21.3 Elution Pipets, 0.7S-mL, constructed from 3-mm (inside diameter) tubing as described in Note 20. 21.4 Glass Plates (2 by 2-in. (51 by 51-mm) transparency cover glasses) for holding paper in the elution rack. 21.5 Adapter Plate (optional) for use in elution of heavier paper, constructed as described in Note 18. 22. Procedure 22.1 Barely catch the tabs of paper containing mannose and xylose between the edges of a pair of 2 by 2-in. (51 by 51-mm) glass plates and hang them in an elution rack as shown in Fig. 6, with the 3-in. (76-mm) dimension vertical (Note 18). Position the elution pipets so as to touch near the bottom edge of the tabs. To prevent excessive evaporation of water, the entire assembly should be contained in a glasscovered humidified box (Note 19). 22.2 Start elution by filling the trough with water, which rises by capillarity between the plates and then flows down the paper and into the pipets. When a pipet is filled, capillary forces prevent flow through the pipet, and surplus water flows past the tip. The volume provided by a 0.75-mL pipet (Notes 20 and 21) is more than adequatedo remove all ofthe sugar from the tab, so that the last water to enter is sugar-free. Quantitative transfer of sugar to a test tube for analysis is achieved by draining the pipet through the end not in contact with the paper. -- 22.3 Soak the paper tabs containing glucose in 25 mL of water for about 15 min with occasional swirling. Filter the eluates through glass wool to remove fibers,' following which take replicate 0.75-mL aliquots of the'supematant solutions for analysis.-- 17--Uniformity of performance and of .gaper blank .are of critical importance in the selection of a chromatographic paper for quantitative work. The normal inexpensive, high grade, rapid paper used for general work6 has been widely used for this purpose and can be purchased in a grade especially selected for chromatographic work. For high-purity pulps and for cotton where minor constituents are present in very small quantities, the use ofa thick, strong paper ofmedium filtering speed with smooth surface7 may be advantageous, sinceit can be loaded with three times as much solution. 18--With thicker papers, the 2 by 2-in. (50.8 by 50.8-mm) glass plates may become separated to such an extent that water wilTnot rise between them. A stainless steel adapter plate, 2 in. in width and of length equal to that of the elution rack, can be made to solve tbis problem. The thickness ofone edge of this plate is reduced by milling a cut lh in. (3.2 mm) wide by 0.008 in. (0.20 mm) deep the full length of the plate. The paper tabs can now be caught in the space between this milled depression and a covering 2 by 2-in. glass slide. Elution is carried out in the usual way. 7Whatman No. 3MM paper, available from. Whatman Inc., 9 Bridewell Place, Clifton, NJ 07014, has been found satisfactory for this purpose. 332 am DUP050296853 D 1915 FIG. 6 Combination Steam Bath-Test Tube Rack for Sugar Analysis 19--Humidification of the elution cabinet is easily accont- i- plished by lining the walls with strips of wet blotting paper. || 20--The elution pipets are made from 3-mm (inside diameter) Jjbbrosilicate glass tubing and calibrated to deliver 0.75 0.005 mL of Jwater. This volume is suitable for use with either paper described in Note 17. Draw down the ends of the pipets to an inside diameter of [japproximately 0.020 in. (0.51 mm), bending one end up at about a 60 Fah|le as illustrated in Fig. 5. Grind the tips flat and then give them a |F slight bevel to reduce chipping. Capillary forces are now such that eluate is.readily drawn into the straight end of the pipet but does not flow out of the bent end. 21--After every use, wash.the pipets by drawing through them, j: in succession, dilute sodium hydroxide, add dichromate, and water. Dry ? by leaving them for 'fi h in a bottle evacuated with an aspirator. Clean | the 2 by-2-in. slide cover glasses in dichromate and keep wet until use. ANALYSIS OF SEPARATED SUGARS 23. Significance and Use 23.1 The chemical method of-analysis is well adapted to work in which the major emphasis is on the Accurate determination of minimal quantities of "extraneous" carbo hydrates present in a cellulose. The best reagents are those which provide a maximum discrimination against the sol uble polysaccharides of the paper. The copper reagent (5) and the arsenomolybdate chromogenic reagent (6) have proven quite suitable from this standpoint.24 24. Apparatus 24.1 Combination Steam Bath--Test Tube Rack (Fig. 6). 24.2 Glass Marbles, 15 to 16 mm in diameter. 24.3 Calibrated Syringe Pipets, 1.00 0.001 mL and 2.25 0.002 mL (Fig. 1 and Note 2). 24.4 Spectrophotometer6 using 3-mL borosilicate glass cuvettes with a 1-cm light path. 25. Reagents 25.1 Copper Reagent (5)--Dissolve 24 g of anhydrous sodium carbonate (Na2C03) and 12 g of Rochelle salt (NaKC4H406) in about 250 mL of boiled and co.oled water. Add to this solution 4 g of hydrated copper sulfate (CuS04- 5H20) dissolved in 40 mL ofboiled water and mix. Add 16 g of sodium bicarbonate <NaHC03), and when dissolved, pour the combined solution into a 1000-mL graduated cylinder. Dissolve 180 g of anhydrous sodium sulfate (Na2S04) in about 500 mL of.hot water, and boil the solution to expel air. When cool, add this solution to the. cylinder. Dilute the combined mixture to the mark and mix thoroughly. 22---It is preferable to prepare a' 10-L stock of the copper reagent several weeksts advance of its use. This allows impurities and a slight amount of cuprous oxide (CiksQ) to settle. The supernatant solution may then be siphoned into a clean bottle. 25.2 Arsenomolybdate Chromogenic Reagent (6)--Dis solve 25 g of ammonium molybdate ((NH4)2Mo04) in 450 mL of water, add 21 mL of concentrated sulfuric acid (H2S04, sp gr 1.84) mix, and add 3 g of monobasic sodium orthoarsenate (Na2HAs04-7H20) dissolved in 25 mL of water. Place this solution in an incubator at 37*C for 24 to 48 h before use and store in brown bottles. 23--For routine use, this solution should also be made up in 10-L quantities. 26. Preparation of Calibration Curves 26.1 Glucose Calibration Curve--As will be seen later, it is convenient to express all sugars in terms of glucose equivalent. Prepare a calibration curve for this purpose by pipetting 0.75 mL of glucose solutions, containing from 0 to 210 jxg of sugar, into % by 6-in. (15.9 by 152-mm) test tubes and processing as described in Section 27 (Note 24). This is 333 rn,m,S: ' DUP050296854 most accurately done by dissolving 0.2800 g ofglucose in 1 L of water (210 p.g/0.75 mL) and diluting this to give the desired number of calibration points. A plot of absorbance versus glucose concentration provides the desired calibration curve. 24--The use of individually calibrated syringe pipets greatly facilitates the multiple pipettings encountered in this sugar analysis procedure. 26.2 All sugars undergo measurable destruction when subjected to the acid conditions employed for saccharifica tion. Sugar degradation products can migrate at the same speed as the sugars. Each sugar exhibits a characteristic reducing powder toward the copper reagent Sugar values must be converted to sugar anhydride. Appropriate indi vidual corrections for these matters are troublesome. It is possible, however, to account in one operation for all conversion and correction factors involved in paper chro matographic analysis by the use of empirical calibration curves. Such a correction is especially adapted to high-purity pulps where mannan and xylan represent the only significant nonglucose carbohydrates present. It is advised that calibra tion curves be established specifically for the system under study. This is illustrated by the procedure described in 26.3, which is adapted to purified pulps with mannan and xylan contents up to 5 %. 26.3 Empirical Calibration Curvesfor Mannan and Xylan in Purified Pulps--Prepare 0.300-g quantities of mixtures of glucose, mannose, and xylose containing, respectively, 0.00, 1.00, 2.00, 3.00, 4.00, and' 5.00 % bf both mannose apd xylose. These specimens will have respective mannan equiv alents of 0.00, 1.00, 2.00; 3.00, 4.00, and 5.00% and respective xylan equivalents of 0.00, 0.98, 1.96, 2.94, 3.92, and 4.90 %. To avoid weighing such small quantities of mannose and xylose, solutions of the desired mixtures may be prepared and suitable aliquots (containing 0.300 g of total sugar) pipetted into the vials used for primary hydrolysis and dried in a vacuum desiccator. 26.3.1 Hydrolyze these sugar mixtures in duplicate, neu tralize, concentrate, chromatograph, and analyze exactly in accordance with the procedures described for cellulose pulp analysis. This yields the glucose, mannose, and xylose content of each mixture in terms of micrograms of glucose equivalent. From these values subtract the amount, in micrograms, of apparent reducing sugar due to the paper blank (Note 25). Then total the corrected quantities, in micrograms, of glucose, mannose, and xylose. By dividing the corrected quantities of xylose (as glucose) by this total (all sugars as glucose), obtain the apparent percent of xylose in each mixture. Calculate the apparent percent of mannose similarly. 26.3.2 Construct two curves, one in which the app^ percent of xylose is plotted against the calculated content of the original mixtures as listed above, second, in which the apparent percent of mannose is p1 against the calculated mannan content of the original1 tures (Note 26). These are the master calibration curves" should serve as long as the defined technique is follow-* 25--All chromatographic papers contain traces of so*' reducing substances which constitute a source of error in the L determination.' Since the absolute amount of these materials v widely with the different papers and may also vary appreciably 1 different lots ofthe same paper, it is not feasible to account for them the master calibration curves. For a given lot of paper, the correction apparent reducing sugar may be obtained by irrigating several rando selected sheets in the usual way with spots of mannose and xyl applied to the starting line in the guide-strip regions. Two by tbree- (51 by 76-mm) tabs of paper are then cut from the sugar-free re- adjacent to the mannose and xylose areas, and eluted. The eluates analyzed for their apparent reducing sugar content The mean values obtained (in micrograms) provide the desired corrections for pape blank. It has been found that there is a small but significant difference in the blank correction for the mannose and xylose regions. The uncer tainty in the blank between successive tabs of a given lot of paper is otf the order of 1 pg. 26--The described calibration procedure was designed ta accommodate pulps having a mannan and xylan range between 0 and' 5 %. By strict adherence to the prescribed techniques and with adequate '< replication, errors can be held to a level of about 0.1 % of a minor '' constituent, based on the total carbohydrate. For highly purified pulps ' with mannan and xylan contents in the 1 to 1.5 % range, the master1 calibration curves can be made more sensitive by selecting a series offiy- or more calibration points over the range of 0 to 1,5 % mannan and xylan. This illustrates the principle of calibrating specifically for thej system under study. . T^ 27. Procedure i 27.1 To each of the 0.75-mL sugar "eluates (Section 22) contained in % by 6-in. (15.9by 152-mm) test tubes add 1.00 * mL of copper reagent. Cover the tubes with the glass marbles and heat them by direct steam for 20 min in the combination steam bath and test tube rack illustrated in Fig. 6. Connect. { the steam bath to a water line to provide rapid cooling Next, add 1.00 mL of the chromogenic reagent to each tube and shake the contents to expel carbon dioxide. Finally, add 2.25 mL of water-to each tube and thoroughly'mix the contents (Note 24). 27.2 Determine absorbances at 520 jim with 3-mL cuvettes and a spectrophotometer.6 Use a reagent blank in the reference cell. In cases where absorbance exceeds 1.0, dilute both sample and blank with an additional 5 00 mL of water. 27.3 From the glucose calibration curve obtain the glu cose equivalent (see 26.1), and from the master calibration curves (see 26.3) determine the composition of the pulp. REFERENCES (1) Fetzer, W. R,, Crosby, E. K., Engel, C. E,, and Kirst, L. C., "Effect of Acid and Heat on Dextrose and Dextrose Polymers," Industrial & Engineering Chemistry, Vol 45, 1953, p. 1075. (2) Saeman, J. F., Moore, W. E, Mitchell, R. L., and Millett, M. A., "Techniques for the Determination of Pulp Constituents by Quantitative Paper Chromatography," Tappt, Vol 37,1954, p. 336. (3) Hawthorne, J. R., "Micro-estimation of Sugars Separated on the Filter Paper Chromatogram," Nature, Vol 160, 1947, p. 714. (4) Dimler, R. J., Schaefer, W. C., Wise, C. S., and Rest, C. E., "Quantitative Paper Chromatography of D-Glucose and Its Oligosaccharides," Analytical Chemistry, Vol 24, 1952, p. 1411. (5) Somogyi, M., "Notes on Sugar-Determination," Journal ofBiolog ical Chemistry, Vo! 195, 1952, p. 19. (6) Nelson, N., "A Photometric Adaptation of the Somogyi Method for the Determination of Glucose," Journal of Biological Chem istry, Vol 153, 1944, p. 376. 334 saV.-jO-T. *. .. DUP050296855 D 1915 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 aublect 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 eitherfor 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 SI, Philadelphia, PA 19103, 335 DUP050296856 (jOTh Designation: D 1926 89 Standard Test Methods for Carboxyl Content of Cellulose1 This standard is issued under the fixed designation D 1926; 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. 1. Scope L.l These test methods cover the determination of the carboxyl content, or ion-exchange capacity, ofcellulose from any source. Two test methods are described, the sodium chloride-sodium bicarbonate method (l)12 and die methylene blue method (2). The test methods must be used within their limitations, and it must be recognized that there is no way of determining the accuracy of any method for the determina tion of carboxyl. The precision of the sodium chloridesodium bicarbonate method is low in the lower range of carboxyl values. The methylene blue method can be used over the whole range of carboxyl values; it is especially useful in the low range. It is not applicable to the determination of carboxyl in soluble carbohydrate material. Although these test methods may be used to determine the ion-exchange capacity of unbleached pulps, the residual lignin will cause an undetermined error, especially the sulfonic acid groups in unbleached sulfite pulps (3). 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safely 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: D1193 Specification for Reagent Water3 3. Significance and Use 3.1 These test methods measure the amount of carboxyl groups present in wood or cotton linter pulp. Carboxyl groups are indicative of the surface charge of the pulp which is a very important quantity for use in the papermaking industry. 4. Purity of Reagents 4.1 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, 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 D01.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 1926 -61. Last previous edition D 1926 - 63 (1985)41. 2 The boldface numbers in parentheses refer to the list of references at the end of these test methods. y Annual Book ofASTM Standards, Vols 06.03 and 11.01. where such specifications are available.4 Other grades may bei| used, provided it is first ascertained that the reagent is olf sufficiently high purity to permit its use without lessening the! accuracy of the determination. 4.2 Unless otherwise indicated, references to water shall ;! be understood to mean reagent water conforming to Specification D 1193. SODIUM CHLORIDE-SODIUM BICARBONATE METHOD 5. Summary of Test Method 5.1 In the sodium chloride-sodium bicarbonate method : the specimen is deashed with hydrochloric acid, washed, soaked in sodium chloride-sodium bicarbonate solution, filtered, and an aliquot of the filtrate titrated with 0.01 N1 hydrochloric acid to a methyl red end point. The difference between the concentration of the filtrate and of the sodium chloride-sodium bicarbonate solution is a measure of the ion-exchange capacity of the cellulose. 6. Reagents 6.1 Hydrochloric Acid, Standard (0.01 N)--Prepare and standardize a 0.01 N solution of hydrochloric acid (HQ). 6.2 Hydrochloric Acid (1 + 99)--Dilute 1 volume of concentrated HCI (sp gr 1.19) with 99 volumes of water. 6.3 Methyl Red Indicator Solution. 6.4 Sodium Chloride-Sodium Bicarbonate Solution--Dis solve 5.85 g of sodium chloride (NaCl) and 0.84 g of sodium bicarbonate (NaHC03) in water and dilute to 1 L. 6.5 Sodium Hydroxide Solution (0.4 g/L)--Dissolve 0.4 g of sodium hydroxide (NaOH) in waterjind dilute to ,1 L. 7. Procedure ' 7.1 Condition the specimen in the atmosphere near the balance for at least 20 min before weighing duplicate portions of 2.5 0.01 g. At the same time, weigh specimens for the determination of moisture. Disintegrate the specimen in water, filter through fritted glass, and disperse to about 1 % consistency in HCI (1 +99) at room temperature. After 2 h collect the specimen on a fritted-glass filter funnel and wash with water saturated with carbon dioxide (C02). Continue the washing until the filtrate, after boiling, does not require more than 1 or 2 drops of NaOH solution to give an alkaline color with methyl red. 7.2 Weigh the wet pulp pad, transfer it immediately to a 250-mL glass-stoppered Erlenmeyer flask, add 50 mL of the 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., 3nc., New York, NY, and the "United States Pharmacopeia." 336 DUP050296857 D 1926 ? f'J NaCl-NaHC03 solution with a pipet, and shake to obtain a jpdniogeneous sltnry (Note 1). Allow the mixture to stand for || h at room temperature. Filter through a clean, dry, frittedIglass funnel, pipet a 25-mL aliquot of the filtrate into an ||rlenme,yer flask, and titrate with 0.01 N HC1, using methyl pied solution as an indicator. When the first change in color Sbccurs, boil the solution for about 1 min to expel the carbon jpioxide and continue the titration to a sharp end point. I Nora 1--If the cation-exchange capacity is very low, use a solution pjpntaining about S.85 g of NaCi and 0.42 g of NaHC03 per litre. It is important, that ;the excess of NaHC03 be large enough that the pH does ipst fall below 7.0, 7.3 Pipet 25 mL of the Naa-NaHC03 solution into- an fjjjiienmeyer flask and titrate as described in 7.2. |8. Calculation I 5 8.1 Calculate the cation-exchange capacity, c, of the Specimen in milliequivalents per 100 g as follows: 2 G 0) pere: fe = weight of oven-dry specimen, g, p = weight of water in the wet pulp pad, g, k = millilitres of0.01 iVHCl consumed by 25 mL offiltrate, ; arid !b = millilitres of 0.01 ATHC1 consumed by 25 mL of the ii r NaCl-NaHC03 solution. Report , 9.1 Until more data are obtained on the precision of this est method, it is suggested that the ion-exchange capacity be irted to 0.01 milliequivalent/lOG g of pulp. |0. Precision and Bias 10.1 The precision of this test method varies with the [carboxyl content and from laboratory to laboratory. Preci sion data is available in Ref (4). i : 10.2 No statement on bias can be made as no suitable reference material exists for determining bias. if? METHYLENE ( |l. Summary of Test Method r 11.1 In the methylene blue method the specimen is treated f'ith 0.0002 M methylene blue solution buffered to a pH of 8 with diethylbarbituric add (barbital). The decrease in meth'[lene blue concentration, measured photometrically, is a function of the ion-exchange capacity of the cellulose. ylbarbituric acid (barbital) in water, add the equivalent of 0.16 g of sodium hydroxide using a standard solution and buret, and dilute with water to 1 L in a volumetric flask. 13.2 Hydrochloric Acid (1 + 99)--Dilute 1 volume of concentrated hydrochloric add (HC1, sp gr 1.19) with 99 volumes of water. 13.3 Methylene-Blue, Stock Solution (0.002 M)--Dissolve 0.640 g of methylene blue in water, making allowance for moisture, and dilute to 1 L in a volumetric flask. --Information on the determination of the purity of methylene blue is given in the literature (5). 13.4 Methylene Blue--Buffer Solution (0.0002 M)--Mix I volume of methylene blue stock solution with 1 volume of buffer stock solution and dilute to a total of 10 volumes in a volumetric flask. The volume of solution to be prepared will vary with the requirements. For example, pipet 10 mL of each solution into a 100-mL volumetric flask, dilute to the mark with water, and mix thoroughly. Prepare a fresh solution for each determination. 14. Preparation of Calibration Curve for Ordinary Size Specimens 14.1 In order to prepare a calibration curve, make up a series of methylene blue buffer solutions containing the same amount of buffer but different amounts of methylene blue, to cover the desired range. Add 50 mL of. the stock solution of buffer to each of nine 500-mL volumetric flasks. Add to these flasks 10, 15,20,25,30,35,40,45, and 50 mL, respec tively, of the 0.002 M stock solution of methylene blue. Di lute each solution to the mark with water and mix thoroughly. ! 3--The concentrations suggested for preparing calibration curves need not be followed exactly as long as enough points are obtained to allow construction ofah acceptable calibration curve. 14.2 Pipet 10 mL of each solution into 100-mL volu metric flasks, add 10 mL of HC1 (1 + 99), dilute to the mark with water, and mix (Note 4). Measure the absorbance of the' solutions and prepare a plot of absorbance at 620 nm against , concentration (Note 5). "#$ 4--The procedure described for the colorimetric determina tion of methylene blue is based on Ihe use of the Beckman PU spectro photometer5 with l-cm-absorption cells. The dilution procedure may have to be modified for use with filter photometers or for cells with a longer tight path. .. %&') 5--It has been reported (5) that Beer's law is obeyed at 620 nm, and it is recommended that measurements be made at this wave length. Measurements may also be made at 675 nm, which is close to the absorption peak, but Beer's law is not obeyed at this wavelength. 15. Preparation of Calibration Curve for Small Specimens |2. Apparatus 12.1 Spectrophotometer or Filter Photometer, capable of jfaeasuring absorbance near 620 mm. : 12.2 Shaker or Mixer for agitating the specimens in the methylene blue solution. A wheel or rod, to which the imen vials can be attached, that rotates at about 15 J/min, has proven satisfactory. 12.3 Centrifuge, capable of settling the cellulose from the ethylene blue solution. 15.1 In order to prepare a calibration curve, pipet 1 mL of each of the nine solutions mentioned in Section 14 into 10-mL volumetric flasks, add 1 mL of HC1 (1 + 99), dilute to the mark, mix, and measure the absorbance at 620 nm. Iffhe volumetric apparatus is sufficiently precise, this calibration curve should be identical with the one described in Section 14 (Note 6). Obviously, any specific procedure that gives solutions in the right concentration range for the colori metric measurements should be satisfactory. |3. Reagents 13.1 Buffer, Stock Solution--Dissolve 1.151 g of dieth- 5 Manufactured by Beckman Instruments. Fnc., 2500 Harbour Blvd., Mail Station 31D, Fullerton, CA 92634. 337 DUP050296858 D 1926 T*+,- 6--Since methylene blue solutions have a tendency to form droplets on glassware,, this can seriously impair the accuracy in transferring small volumes of solution. For this reason the 1-mL automatic pipet should be coated with silicone tb make it nonwetting. The point should be completely emptied during Use, and should be calibrated in the same way in which it is used. An automatic pipet is highly desirable for the precise delivery of l mL of solution. The pipet should be thoroughly cleaned before coating with silicone. Ifelectrolytes are likely to be on th? surface, the pipet should be boiled in water for 30 mini dried, and then degreased by heating to 400*C for 1 h or more, or by the use of some solvent, such as carbon tetrachloride or methylene chloride. The pipet is coated with a fresh 2 weight % solution of silicone6 in methylene chloride, carbon tetrachloride, or perchloroethylene, allowed to drain, and air-dried or heated for 1 h at 100C to remove the solvent. The film must then be cured by heating for 1 h at 300"C or for 2 h at 275"C. 16. Procedure for Ordinary Size Specimens 16.1 Determine the approximate carboxyl content in a preliminary experiment. Weigh out three specimens, one estimated to give 50 % exhaustion of the dye solution, one 10 to 15 % smaller, and one 10 to 15 % larger, making allowance for the moisture contents Weigh the specimens into 125-mL glass-stoppered flasks (any other convenient size flask may be used), and add 50 mL of 0.0002 M methylene blue-buffer solution from a pipet., Lubricate the stoppers with a little petroleum jelly and secure, them with rubber bands. Place,the flasks on a device that will turn them end over end or otherwise agitate the solutions, 16.2 After overnight agitation, centrifuge the solutions and pipet a 10-mL aliquot of the supernatant liquid, into a 100-mL volumetric flask. Add 10 mL of HC1 (1 + 99), and fill the flask to the mark with water. Measure the absorbance of the solutions at 620 ntfl.' 16.3 Using the observed absorbances, refer to the calibra tion curve and read the concentration of methylene biue present for each of the three portions of specimen. 16.4 Plot the specimen size against the concentration of methylene blue in the supernatant liquid, and read from the plot the specimen size that gives 50 % exhaustion of the dye solution. : ./01 7--It is not absolutely necessary to plot the specimen size against methylene blue concentration in order to calculate dye absorp- 6 Dow Coming 200 silioone solution manufactured by Dow Coming, Midland, MI, has been found satisfactory for this purpose. tion. The dye absorption may be calculated from two slightly differed 1 weights of cellulose that will give, approximately 50 % exhaustion, and I the mean of the two results taken. H 17. Procedure for Small Specimens I 17.1 The'general procedure is the same Us for ordinary*j| size specimens (Section 16). Weigh the specimens into 1 glass-stoppered weighing bottles of about ;iO-mL capacity 1 jand add 5 mL of 0.0002 M methylene blue-buffer solution, After overnight agitation, centrifuge the solutions, remove a 1 1-mL aliquot with an automatic pipet, and transfer to a 10-mL volumetric flask. Add about 1 mL of HO (1 + 99), J dilute to the mark, and measure the absorbance at 620 nm. I Determine-the specimen size that gives 50 % exhaustion of f the methylene blue solution as described in 1614. 18. Calculations > "i;j 18.1 Ordinary Size Specimens--The size specimen that gives 50 % exhaustion of 50 mL of0.0002 M methylene blue> I solution has used 0.005 millimole of methylene blue in ion f exchange with carboxyl groups. Therefore the millimoles of If carboxyl per 100 g of cellulose, JWj, is calculated as follows: j M, = (0.00.5/W0 x 100 (2), I where W = specimen to give 50 % exhaustion of 50 ,mL of j 0.0002 M methylene blue solution,'g. f 18.2 Small Specimens--The size specimen that gives 50% exhaustion of 5 mL of 0.0002 M methylene blue j solution has used 0.0005 millimole of methylene blue in ion 1 exchange with carboxyl groups. Therefore the millimoles of j carboxyl per 100 g of cellulose, M2, is calculated as follows: M2 = (0.0005/7 x 100 ' (3) where W - specimen to give 50 % exhaustion of 5 mL of 0.0002 M methylene blue solution, g. 19. Report 19.1 Until more data are obtained on the precision of this test method, it is suggested that the ion-exchange capacity be reported to 0.01 meq/100 g ofpulp. 20. Precision and Bias 71 20.1 The precision of this test-method ,varie with the carboxyl content arid from laboratory fo laboratory. Preci sion data is available in Ref (4). 20.2 No statement of bias can be made as no suitable reference material exists for determining bias. REFERENCES (1) Wilson, K., "Bestamming av, Karboxylgrupper i Cellulosa," Svensk Papperstidn, Vol 51, 1948, p. 45. (2) Davidson, G. F.,."The Absorption of Methylene Blue," Journal, Textile Institute, Vol 39, 1948, p. T65. (3) Jayme, G., and Neuschaffer, K., "Uber die Bestimmung des Carboxylgruppengehaltes von Zellstoffen," Das Papier, Vol 9, 1955, p. 143. (4) Wilson, W. K., and Mandel, J., "Determination ofCarboxyl in Cel lulose; Comparison of Various Methods, Report of TAPPI-ACS-. ICCA Subcommittee on Carboxyl," Tappi, Vol 44, 1961, p. 131. (5) Davidson, G. F., "The Determination of Methylene Blue," Jour nal, Textile Institute, Vol 38, 1947, p. T408. (6) Anti-Wuorinen, O., and Visapaa, A., "Application of an Auto matic Titration Method in the Study of the Behavior of Cellulose Towards Different Salt Solutions," Paper and Timber, Vol 38, 1956, p.327. (7) Davidson, G, F., and Nevell, T. P., "A Comparison of Various Methods Proposed for the Determination of Carboxyl Content,5 Journal, Textile Institute, Vol 39, 1948, p. T102. 338 DUP050296859 # D 1926 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any hern 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 orforadditional standards arid 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. 1 339 DUP050296860 Designation: D 1979 - 91 Standard Test Method for Free Formaldehyde Content of Amino Resins1 This standard is issued under the fixed designation D 1979; 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 (2) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of free formaldehyde in amino resins and their aqueous and nonaqueous solutions. Amino resin-free formaldehyde levels from about 0.02 to 5.0 % can be determined by this test method. The applicability of this test method to other matrices is unknown. 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 consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 5. Apparatus 5.1 Analytical Balance, 0.1 mg. 5.2 Magnetic Stirrer and Stir Bar--A "heavy duty" mag netic stirrer is necessary. 5.3 Buret, 50 mL manual or electronic. Manual burets should be of the type designed to minimize the exposure of reagent to air. Electronic burets are preferred. 5.4 Beakers, glass, 100 mL, 600 mL, and 1500 mL. 5.5 Stopwatch or Timer. 5.6 Graduated Cylinders, glass, 50 mL and 250 mL. 5.7 Glass Pipet, 2 mL. 5.8 Thermometer, subdivision 1C. ; 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water12 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 3. Summary of Test Method 3.1 Specimens are mixed with borate buffer solution and ice water, then kept cool in an ice bath. Excess sodium sulfite is added to consume free formaldehyde as follows: CH20 + Na2S03 + H20 - H0CH2S03Na + NaOH (1) 3.2 The excess sodium sulfite is removed by titration with iodine using starch as the indicator as follows: Na2S03 + I2 + H20 -> Na2S04 + 2 HI (2) 3.3 The sodium sulfite-formaldehyde complex is then decomposed with sodium carbonate to quantitatively regen erate sodium sulfite and formaldehyde as follows: HOCH2S03Na + Na2CD3 - CH20 + Na2S03 + NaHC03 (3) 3.4 The liberated sodium sulfite is titrated with iodine (Eq 2) and free formaldehyde" is calculated from this second iodine titration. 4. Significance and Use 4.1 The amount of free formaldehyde in amino resins may be of concern to both producer and user, as its presence in air above threshold amounts may produce objectionable odors and irritant effects. This test method can be useful for evaluating suppliers' products and for quality control. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be ; used in all tests. Unless otherwise indicated it is intended that j all reagents 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 j sufficient high purity to permit its use without lessening the \ accuracy of the determination. "f 6.2 Purity of Water--Unless otherwise indicated, refer- j ences to water shall be understood to mean reagent water as { defined by Type II of Specification D 1193. I 6.3 Acetic Acid Solution (1.0 M)--Dissolve 60 mL of j glacial acetic add (CH3CO2H) in water and dilute to-1 L. j 6.4 Boric Acid Buffet" Solution--Prepare a sodium hy-. j droxide solution (1.0 M) by dissolving 40 g of sodium hydroxide (NaOH) in water and diluting to 1 L. Dissolve ; 12.39 g of boric acid (H3B03) in 100-mL of 1.0 M NaOH, j then dilute-to 1 L. Maintain temperature at 0C in an ice j bath. The pH at 0C should be 9.4 (glass electrode). 6.5 Ice, finely crushed. 6.6 Iodine Solution (0.1 N)--Dissolve 40 g of iodate free potassium iodide in 25 mL of water in a 100-mL beaker. Weigh out 12.6905 g of dry re-sublimed iodine and add to the beaker. Stir until the iodine is dissolved and dilute to 1 L with water. Store iodine titrant in the dark. This reagent can be purchased as a standardized solution or must be standard ized against sodium thiosulfate. 6.7 Methylene Chloride (CH2C12)--Cool to 0C in an ice bath. 6.8 Sodium Carbonate Solution (1.0 M)--Dissolve 106 g of sodium carbonate (Na2C03) in water and dilute to 1 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 1.33 on Polymers and Resins. Current edition approved Feb. 22, 1991. Published April 1991. 2 Annual Bock ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards* Vol 06.03. 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," 340 DUP050296861 6.9 Sodium Sulfite Solution (1.0 M)--Dissolve 126 g of um sulfite (Na2S03) in water and dilute to I L. This ent is unstable and must be prepared fresh daily. 6.10 Starch--0.2% aqueous (weight/volume) or 1.0% ueous (weight/volume). This indicator can be purchased as ^stabilized solution or prepared in accordance with Test "^Method D 1959.-Store in a cool, dark place. J*:6.11 Water (H20)--Cool Type II water to' 0C in an ice m .^Procedure A-blank determination is nipToilowpig; this, proce dure, omitting 7.2 (addition of sample). . :;,s. j;'7.2 Taking the appropriate specimen size from Table 1, igh the specimen to the nearest mg into a 600rmL beaker. .7.3 . Placevthe beaker into the ice bath that rests upon a leavy-duty magnetic stirrer. , . Jf 7.4 Place a stirring, bar. in the beaker and immediately isplve the specimen as described .in 7.4.1 (for aqueous cimens) or 7,4.2 (for non-aqueous specimens). Maintain ie temperature of the specimen solution at 0C by adding The temperature must not rise above 2C during . bsequent steps. Note that bqric acid buffer (6.4), pethylene chloride (6.7) and water (6.11) should be pre- poled to 0C. : . 7.4.1 Aqueous Specimens--Rapidly mix the specimen jjwith 150 mL of ice water and 25 mL of boric acid buffer Mution.. . ........ ; ;* mp.4.2 Ufon-dqueous Specimens--Rapidly mix . the spec- ~ien with 50 mL of methylene chloride,cooled to QC. Stir to Sxssolve' specimen. Add 150 inL of ice water and 25 mL of boric acid buffer. Continue extraction for 5 min. Uninter- p-upted stirring must be maintained through 7.5 to 7.10. 7.5While constantly stirring the specimen solution, pipet 2 mL of 1.0 ATsodium sulfite' Solution into the beaker. ^)7,6. Cbntinue 'stinirig.for i3 min.. .` "7:7 Add, i 0 mL of\ .Q M acetic acid solution and'10 mL 6f the starciisolution. ' TABLE. 1 Specimen Size According tp Expected Forrpa|d$hyde. jp-"1 M*- Free Formaldehyde, weight,, * ' 6.02-0.05 , 6.5-1.6 - < ' 1.0-2.0- ' 2.0-3.0 3.0-5.0 ! .,. Specimen Weight, . " Vs ' '' . .- 3-8 r ih 1.0 'iP-5 , 0.25 ' , . 7.8 Titrate the excess sodium sulfite with 0.1 N iodine solution to a green-blue color that persists for 10 s. Re-zero the buret. . ;\ 7.9 Add 30 mL of 1.0 M sodium carbonate solution. 7.10 Titrate the'liberated sodium sulfite with 0.1 N iodine solution to a constant blue color that persists for 1 min. The shade of blue varies with the sample under test and may appear slightly different in emulsions when compared to the blank. Record the volume of the iodine solution used in this step for use in the calculation, Section 8. 8. Calculation .8.1 Calculate the weight percent free formaldehyde in the. sample as follows: - vFormald,,eh, yd,e, ,,% ----------. . , W x 20 where: .. " ,'s.' A = volume T of iodine solution for specimen titration . ' (7.10), mL, ` t \' B = volume of'iodine,solution for blank titration (7.10), mL, and W = sample weight, g. ' ' 9. Precision and Bias 9.1 Precision--The precision statements are based upon an interlaboratory study in which one analyst in each of five different laboratories analyzed three samples of commercial melamine resins with free formaldehyde contents between 0.2 and 2.7% , in duplicate on. twq: different days. . The within-laboratory coefficient of variation was found to be 4.07 % at 12>df,.and,the between-laboratories; coefficient of variation was found to be 13.69 % at 9 df. Based on these coefficients of variation, the following criteria should be used in judging the acceptability of results at the 95 % confidence level. ... ^ .. ... .,. 9.1.1 Repeatability--Twp results* each the means of du plicates, obtained by the same operator on different days should; , be, .considered suspect if .they, differ by-more, than. 12,5,% relative. [. , - .., 9.1.2 Reproducibility--Two results, each the means of duplicates,; obliged by operators in different laboratories should be considered suspect, if they differ by more than 43,8 % .relative.,.... ... / ;9.2 . J/'as--Bias, has. not been established; for, this test method. , 10" Keywords ' ^ 10.1. amino resins; formaldehyde; sodium sulfite " Tho American/Sodety 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,.arid 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 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. Youf 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 yow views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 341 DUP050296862 Designation: D 2090 - 88 Standard Test Method for Clarity and Cleanness of Paint and ink Liquids1 This standard is issued under the fixed designation 0 2090; 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 (s) indicates an editorial changesince the last revision or reappFoval. 1. Scope 1.1 This test method covers a procedure for the visual examination of any unpigmented liquid for use in paints and inks, including fatty oils and acids, drier solutions, solvents, miscellaneous chemicals, varnishes, resin solutions, clear lacquers, and other clear coatings for the presence or absence of undesirable components. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associatedwith 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 1003 Test Method for Haze and Luminous Transmit tance of Transparent Plastics12 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method4 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 There are various terms for clarity or cleanness of liquids, which are established as trade vernacular in de scribing undesirable components of a liquid. The following seven are preferred over the other terms (in bold face) related to them; 3.1.2 foreign matter--any visible material unrelated to the true origin of the liquid specified. 3.1.3 sediment--any solid which can settle or be centri fuged from the main portion of the liquid, for example, foots, meal, grain, gum. 3.1.4 skins--partial solid layers of material which may form, from the material itself or otherwise. 3.1.5 turbid--a relatively great amount of nonsettling floe, gels, suspended matter, particles, droplets, or other insoluble or separated matter, even though the liquid is translucent and transmits at least a little light. 1 This test method is under the jurisdiction of ASTM Committee 0-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D 01.33 on Polymers and Resins. Current edition approved Oct. 31, 1988. Published Oecember 1988. Originally published as D 2090 - 62 T. Last previous edition D 2090 - 70(1981)'' Discon tinued under 3-year tentative rule 1969. Reinstated and adopted as standard in 1970. 2 Annual Book ofASTM Standards. Vol 08.01. 1 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 3.1.6 hazy--a relatively small amount of nonsettling, finely dispersed matter which is not visibly homogeneous with the mass of the liquid specified, even though the liquid is transparent and transmits most of the light incident upon it. 3.1.7 clear--a complete lack of any visible nonuniformity when viewed in mass, in bottles or test tubes, by strong transmitted light. 3.1.8 clean--a complete lack of any visible nonuniformity sometimes referred to as seeds, when viewed in thin films by any macroscopic or microscopic use of visible light. 4. Summary of Test Method 4.1 The sample is visually examined in its original container, in the specified sample containers, and then in a film thin enough to show any nonuniformity. j j 5. Significance and Use 5.1 The results of the clarity and cleanness examinations are used as controls in production, and for specification acceptance of any nonpigmented liquid used in paints and inks. 6. Sampling ^ 6.1 Sampling of one or more containers of a .liquid is especially important for the validity of a clarity or cleanness test, and each type of container, such as tank car, tanktruck, drum, carboy, etc., requires 'its own detailed sampling procedure. Temperature conditions and periods_ affect amounts of solidified matter which may-form,- or volatilized matter lost, such as phosphatidespwaxes, or high melting acids solidified from fatty oils or acids, or low boiling solvents volatilized from varnishes, resin solutions, etc. Therefore, the precise mechanics, the date, time and temper ature of sampling, the type of sample container and the temperature of the container, light, and any . other critical sample storage conditions shall be specified. 7. Conditioning Sample 7.1 Because limits may be desired on the amounts of gums or other solids which will separate from a liquid very slowly at various temperatures, specify limits of a time and temperature schedule for conditioning the specimen arid for making the examination. When not stated otherwise, the sample is presumed to have been stable for any period of time and observed at 77F (25C). 8. Procedure 8.1 Examine all parts of the sample and its containei under at least 50 ft-candles (53.8 lx) of light for an; nonuniformity. 342 DUP050296863 D 2090 12 Transfer some of the sample to fill a clean Gardner- plt tube as specified in Test Method D 1545 to leave an jjbubble under a clean stopper. Tilt the tube at a small [}e from the horizontal so that the air bubble will move and permit observation in the moving liquid of any I particles that may produce a haze in the specimen. 1.3Drain the tube of 80 to 90 % of its contents, replace |:`stopper, let stand vertically for 15 min or other time ailed to allow a highly viscous specimen to complete its to the bottom, while leaving a very thin film of the |pimen over the upper walls of the tube, and while still ected from extraneous dust and from evaporation, fine the drained, vertical tube by both transmitted and |ected strong light to detect particles of any sort in the thin j. A liquid may appear clear in mass, yet not clean in a in film. vfcTE--Many variables influence the choice of details of specimen |ditioning and examination, such as:' lighly colored bitumen solutions, driers, varnishes, etc., that never;less may be judged to be clear and dean when examined in a very ifilm. Relative pure fatty acids may have narrow melting ranges of aperature, and their cleanness is easily observed at a temperature of jffeF(27.8PC) above their melting point, whereas gross or dark mixtures Ratty acids may have such a wide range of melting temperature that ijedfication of time and temperature for specimen conditioning and for iissing a clean test may constitute a convenient, proximate method of Ifiiting their composition. I Glyceride oils may contain small amounts of fatty acids, hosphatides, waxes, and high melting glycerides, for example, stearin in phroil; specification of time, temperature, and air and moisture posure for specimen conditioning and for passing a dean test may constitute a convenient, proximate method of limiting their composi tion. Solutions of varnishes, resins, driers, soaps or polymerized oils may contain tiny gel partides which spoil the appearance of high gloss paints and enamels made from them. The drained tube technique is particu larly useful in detecting these partides when their index of refraction makes them difficult to detect in mass. Test Method D 1210, may also be used for semiquantitative determi nation of particle size and frequency in unpigmented liquids. However, the films prepared by either Test Method D 1210 or by simple drainage on clean, vertical glass plates are more susceptible to contamination by extraneous matter during the course of the test. 9. Report 9.1 Report the following information: 9.1.1 Name of original or specimen container examined and any significant details of sampling procedure, 9.1.2 Temperature range and time period of specimen conditioning. 9.1.3 Temperature of specimen at time of observation, and 9.1.4 Term or terms, selected from Section 3, which describe the clarity or cleanness of the specimen. 10. Precision 10.1 No numerical statement of precision is possible in this qualitative method. 11. Index Terms 11.1 This test method is indexed under the following terms: foreign matter content; sediment; skins content. APPENDIX (Nonmandatory Information) XI. INSTRUMENTAL DETERMINATION This instrumental test method is offered for comment, and without cooperative testing, because it utilizes an existing IpASTM test method to fill a recognized need. It is published as information only and offered without prejudice,against other Best methods. 11.1 Summary of Test Method XL 1.1 A specimen of liquid js placed in a curette and a jjparallel beam of light shining through it is measured at the Inormal (sere) angle of emergence and also at an angle 10 |ifrom normal. The ratio of intensities of the emergent beams |is a measure of clarity. Xl.2 Procedure ijj X 1.2.1 Test the specimen in accordance with Procedure A l of Test Method D 1003. Use the Hazemeter, but in place of the solid specimen of plastic specified therein, pour the thoroughly mixed specimen into a 10-mm glass cell with parallel walls and place it in the specified positions on the integration sphere. XI .3 Calculation X 1.3.1 Calculate percent haze IT as follows: H = {TJT,) x 100 . where: Td = diffuse transmittance, and Tt = total transmittance. 343 DUP050296864 REFERENCES (1) Nimeroff, L, "Status of ASTM Methods and Standards for Appear ance Valuation," Symposium on Visual Aids for Standardizing and Communicating Product Appearance, STP 258, Am. Soc. Testing Mats. 1959. (2) Billymer, Jr., F. W., "Measurement of Optical Clarity by Low- Angle Light Scattering," Journal, Optical Soc. Am., Voi. 49* April 1959, pp. 368-371, a method for measuring scattered light photoelectrically at a 10" angle, with an angular resolution of 1*. It is suitable for plant control applications. (3) Rieger, C. J., and Carpenter, F. G., "Light Scatfering by Commer cial Sugar Solution," Journal ofResearch, Nat: Bureau Standards Vol 63A, November 1959, pp. 205-211. (4) Method D 871, sections on determination of haze by comparison with arbitrary standards based on aqueous suspensions of fdller'i earth; when balloted in Committee D-23 on Cellulose and Cellu lose Derivatives, and adopted by the Society. (5) Coleman Nephelometer method used by L. V. Anderson in ASTM 1 Committee D-l, Subcommittee II, Group II, on Gum Determina tions in Linseed Oil. Tito 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 tNs 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. 344 DUP050296865 Designation: D 2218 - 67 (Reapproved 1989)t Standard Specification for Molybdate Orange Pigments1 1 This standard is issued under the fixed designation D 2218; 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 of the Department ofDefense to replace Method 7133 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. 3 45678Editorial changes were made throughout in March 1989. TScope Jl.l This specification covers the pigment known as oiybdate orange, jgl .2 The following hazard caveat applies to the test method |rtion of this specification only. This standard may involve qzardous materials, operations, and equipment. This iard does not purport to address all of the safety Wblems associated with its use. It is the responsibility ofthe fer of this standard to establish appropriate safety and iealtk practices and determine the applicability ofregulatory Wpiitations prior to ttse. . Referenced Documents 2.1 ASTM Standards: D126 Test Methods for Analysis of Yellow, Orange, and ; Green Pigments Containing Lead Chromate and Chro mium Oxide Green2 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2,3 I,,, D 235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)4 5 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D 523 Test Method for Specular Gloss3 D600 Specification for Liquid Paint Driers4 D 822 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light and Water Exposure Apparatus3 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry3 2.2 Federal Specification:6 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint I and Related Coatings and Materials and is the direct responsibility of Subcom[ mittee DO 1.31 on Pigment Specifications. Current edition accepted Sept. 8, 1967, Originally issued 1963. Replaces jp D 2218 - 63 T. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. " Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards. Vols 06.01 and 14.02. 6 Available from Standardization Documents Order Desk, Bldg. 4 Section D, ; 700 Robbins Ave., Philadelphia, PA 19111-5094. TT-R-266 Resin, Alkyd; Solutions 3. Composition and Properties 3.1 Dry Pigment--The pigment shall be a product made by the chemical coprecipitation of lead chromate and lead molybdate, with or without admixtures of other insoluble compounds of lead or other materials used in manufacture to control certain properties. The pigment shall conform to the requirements for chemical composition as prescribed jn Table 1. 3.2 The mass color and character of the tint formed by a mixture with a white pigment shall be the same as, and the strength shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller. 3.3 When mutually agreed upon between the purchaser and the seller as being essential to the end use of the pigment, resistance to loss of gloss, chalking, and color change shall be tested as specified in 5.1.6 The exposed panel shall show no chalking, a loss of not more than 10 % of the original gloss, and a color change difference of not more than three units. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, _or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb (4540 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, or samples from the same production unit may be blended in equal quantities to form a composite sample. TABLE 1 Requirements for Chemical Composition Chromium (calculated as PbCrOJ Molybdenum (calculated as PbMo04) Total of all substances (including moisture and water soluble compounds) other than insoluble compounds of lead Moisture and other volatile matter Coarse particles (total residue retained on a 45-pm (No. 325) sieve Matter soluble in water * Min Max 70 8 12 1.5 1.0 1.0 345 DU P050296866 D2218 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods: 5.1.1 Chemical Analysis of Lead Chromate--Proceed in accordance with the Lead Chromate section of Test Methods D 126. The alternative procedure is not applicable. 5.1.2 Chemical Analysis of Lead Molybdate and Total Molybdenum--Weigh to l mg about 1-g sample of pigment into a 250-mL beaker. Add 20 mL of sulfuric add (H2S04, 1+1) and heat to light fumed Cool the solution, dilute to 150 mL, filter, and wash with water. To reduce chromate, add freshly prepared sulfurous acid (H2S03) until the solution turns green, and then add several millilitres in excess. Boil the solution until excess H2S03 is removed. Cool the solution to 5 to 10C, and add 30 mL of a 2 % solution of alphabenzoinoxime in alcohol slowly, with stirring. Add sufficient bromine water to tint the solution a pale yellow, and then add a few more millilitres of the alphabenzo inoxime reagent. After 15 min at 5 to 10C, filter the solution through very thin, medium paper. Then wash the solution with cold H2S04 (1+100) containing 25 to 50 mL of prepared alphabenzoinoxime reagent per litre. Place the pretipitate in a platinum crucible, char cautiously, then <9ignite to constant weight at 500C, and weigh as molyb denum oxide o 03). Calculate weight percent lead molybdate (FbMoQ4), M, as follows: M = (Ax 255)/S ' where.:. A = weight .of Mo03 obtained, g, and S - specimen weight, g. 5.1.3. Coarse Particles--Test Methods D 185. 5.1.4 Mass Color and Tinting Strength--Test Method D387. 5.! .5 Moisture and Other Volatile Matter--Test Methods D126. , . . :. 5.Jl,6 Resistance to Loss of Gloss,, Chalking, and Color Change;, '. 5.1.6.1 Prepare a test enamel consisting of ingredients conforming to the applicable specifications in the following proportions: Ingredient Molybdate orange sample Alkyd resin solution A Mhilral spirits4 Lead naphthenatec dobalt naphthenatec Total Weight % 29.51 61.72 8.37 0.25 0.15 100.0 * Conforming to Type 111 of U.S. Federal Specification TT-R-266. 4 See Specification D 235. c See Class B of Specification D 600. 5.1.6.2 Give the enamel three passes through a moder ately tight roller mill setting to give a fineness of grind, as determined following Test Method D 1210, of 1.5 mils (40 pm) or less. Apply the enamel to duplicate flat metal panels by spray or applicatorto complete hiding, and allow to dry 72 h. Measure the gloss at 60 in accordance with Test = Method D 523. Measure the directional reflectance of the. coating in accordance with Test Method E 971 Subject the ? coated panels for 168 h to accelerated weathering ufader the'? conditions' prescribed in Practice D 822. Examine the ex posed coating for chalking. Wash the exposed panel under running water with a thoroughly degreased lamb's wool pad5 to remove scum or' dirt: Wipe off the water with clean; cheesecloth and dry the panel for 2 h. Calculate the. loss of glbss from gloss measurements made bfefore and after expofj sure. After exposure, determine the directional reflectance for each panel as described in Test Method E 97. Estimate the color change or lightness-difference estimate (A L) asj follows: AL = K{Y2'/2 -- r//2) f where: - j F, = ICuiiinous directional reflectance of the panel mea- . sured before exposure, . -s Y2 ~ reflectance measured after exposure, and K -- 100 when the reflectances are expressed in decimal; fractions or. 10 if reflectances are expressed in per cent. ' - The color change for the coating shall be the mean obtained for the two panels.7 7 The tnethod of determining the lightniss-difference' estimate is described in detail in example 4; "Photoelectric Tristimulus Colorimetry witb.J'hree Filters," Circular C429, NBSCA, Nat. Bureau Standards. - 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 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. 346 DUP050296867 m Designation: D 2350 - 90 Standard Test Method for n Antimony Oxide in White Pigment Separated From U Solvent-Reducible Paints1 This standard is issued under the fixed designation D 2350;- the number immediately following the designation indicates the year of origin^ 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 ijeen approvedfor use by agencies ofthe Department ofDefense to replace Method 7016 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor tfib specific yearofistue which has been-approvedby the Department pfDefense. . ' scope fill 'fhis'test method covers the determination of the total jtimofty oxide in white pigment separated frdm solvent- ucible paints. 1.2 This standard does not purport to address the safety ,:oblems associated with its use. It is the responsibility ofthe er of this standard to establish appropriate safety and akh practices and determine the applicability ofregulatory mitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for- Reagent Water12 D2371 Test Method for Pigment Content, qf Solvent- Reducible Paints3 3. Summary of test Method 3.1 The'pigment is dissolved in hydrochloric add (HC1). 'Svdfuric acid (H2S04) ii added. The'mixture is titrated with ; potassium permanganate (KMn04) and calculated to anti- i mony oxide (Sb203) which gives antimony in the ous condition. 3.2 The pigittient is dissolved in H2SO4 with potassium sulfate (K2S04) and reduced. Sodium sulfite (Na2SQ3) is added and sulfur dioxide gas (S02) is expelled. The solution is diluted and HG1 added after which the solution is titrated with KMn04, which gives total, antimony calculated to Sb203. ..,. 3.3 Sb203 from ous condition is subtracted from total Sb203 and residual Sb203 is calculated to Sb205. 3.4 The procedure is also described for antimony oxide in presence of large amounts of iron. 4. Significance and Use 4.1 Antimony trioxide is often used in fire-retardant paints, so it is useful to formulators and users to be able to monitor the amount of this compound in whole paints. 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 D01.2I on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990. Originally published as D 2350 - 65 T. Last previous edition D 2350 - 85. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.01. 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shati coiiform 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, provide^ ft is firt ascertained that tiife reagent is qf sufficiently high purity to permit its use without lessening the accuracy ofthe determination. 5.2 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. 5.3 Hydrochloric Acid (sp gr 1.19)--Concentrated HC1. 5.4 Hydrogen Sulfide (H2S). 5.5 Potassium Permanganate^ Standard Solution (0.1 N)--Dissolve 3.2 g of pure potassium permanganate (KlCln04) in 1 L pf water, let stand 8 to 14 days, and siphon off the clear solution (or filter through a glass filter). For use in determining antimony, the KMnQ4 solution is best standardized as follows: To 0.25 g of pure metallic antimony in a 500-mL resistant-glass Erlenineyer flask, add 12 tb 1,5 mL of H2S04 (sp gr 1.84) and 10 to 12 g of K?S04. Heat until all the antimony is dissolved, cool, dilute to 100 nrL with water, add 1 to 2 g of sodium sulfite (Na2S03), and boil until all the S02 is expelled. This expulsion, is evident when no blue color is obtained with starch-iodate paper (5.7). The volume will be reduced about one half. "Dilute to 250 mL with water, add 2ft mL of HC1 (sp gr 1.19) and titrate to a faint pink tint'with 0.1iVKMnO4 solution. :;=> 1---For '.normal routine control-work, the reduction with sodium sulfite may be eliminated. The material may be diluted to 250 mL, 20 mL of HC1 added, and titrated immediately after cooling the sulfuric acid-potassium sulfate digestion. 5.6 Potassium Sulfate (K2S04). 5.7 Starch-iodate Paper--Impregnate filter paper with a solution obtained by heating 2 g of starch with i 00 mL of water, and, after solution, adding 0.2 g of potassium iodate (KI03) dissolved in 5 mL of water. 5.8 Sulfuric Acid (sp gy 1.84)--Concentrated sulfuric'acid (H2S04). 5.9 Tartaric Acid. 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." 347 DUP050296868 # D 2350 6. Preparation of Sample 6.1 Separate and prepare the pigment in accordance with Test Method D 2371. 7. Procedure 7.1 Transfer 0.3 g of a straight Sb203 pigment, or 0.5 g of a mixed pigment, to a 500-mL resistant-glass Erlenmeyer flask, add 15 mL of water and 25 mL of HCl (sp gr 1.19). Cover with a watch glass, warm on the steam bath for 10 to 15 min to dissolve the antimony oxide, wash off the cover, add 250 mL of water, and 15 mL of H2S04 (sp gr 1.84). Boil 2 min, cool to 10 to 15C, and titrate to a feint pink tint with 0.1 iVKMn04 solution. Calculate to Sb203. 7.2 The procedure described in 7.1 gives only the anti mony in the ous conditions. The following method gives the total antimony (ous and ic forms): Transfer 0.3 g ofa straight Sb203 pigment, or 0.5 g of a mixed pigment, to a 500-mL resistant-glass Erlenmeyer flask, and add 15 mL of H2S04 (sp gr 1.84), 10 g of K2S04, and a 9-cm filter paper (to furnish carbon to act as a reducing agent). Place a funnel in the neck of the flask and heat until the solution becomes colorless. Cool, wash off the funnel, dilute to 100 mL with water, add 1 to 2 g of Na2S03, and boil until all the S02 is expelled. This expulsion is evident when no blue color is obtained with starch-iodate paper (5.7). The volume will be reduced about one half. Dilute to 250 mL with water, add 20 mL of HCl (sp gr 1.19), and titrate, to a feint pink tint with 0.1 JVKMn04 solution (Nqte 1). 7.2.1 Calculate total antimony to Sb203. Subtract the Sb203 found using the procedure ,given in 7.1 from the total Sb203 and calculate the residual Sb203 to Sb2Qs (multiply by the factor 1.1098). 7.3 Procedure in Presence ofAppreciable Amounts ofIron: 7.3.1 Treat 1 g of the mixed pigment, or 0.3 g of a tinted Sb203 pigment, in a covered 250-mL beaker with 5 mL of water and20 mLofHCl(spgr 1.19). Heat on the steam bath for 15 min, cool, wash off the cover, add 3 g of tartaric add s and 100 mL of hot water, and digest a few minutes. Filter, catching the filtrate in a 500-mL resistant-glass Erlenmeyer flask. Wash thoroughly with hot water, dilute to 300 mL with ; hot water, and pass in H2S until the precipitation is i complete. (If the sample. contains no insoluble matter, dissolve directly in a 500-mL resistant-glass Erlenmeyer flask, add tartaric add, dilute, and pass in H2S.) 7.3.2 Filter, wash with water containing H2S until free from HCl, return paper and predpitate to the Erlenmeyer flask, add 15 mL of H2S04 (sp gr 1.84) and 10 g of K2S04, place a funnel in the neck of the flask, and heat until the solution is colorless. Cool, wash off the funnel, dilute to 100 mL with water, add 1 to 2 g of sodium sulfite (Na2S03), and boil until all the S02 is expelled. This expulsion is. evident when no blue color is obtained with starch-iodate paper } (5.7). The volume will be reduced about one-half. Dilute to ` 250 mL with water, add 20 mL of HCl (sp gr 1.19), and j titrate to a feint pink tint with 0.1 N KMn04 solution (Note 1). ,, ' 8. Calculation 8.1 Calculate follows: the percent antimony, B, asSb203 as j f AV 5 = ~x 100 ' | where: A - Sb203 equivalent of the KMn04 solution, g/mL, V == KMn04 solution required, mL, and S = sample used, g j \ 9. Precision ^ j 9.1 Data are not available to determine the precision of j 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. . 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 that determination of the validity of spy such' patent rights, and the risk of infringement of such rights,.are entirely their own responsibility. --1 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 areinvited 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 respor&lbie 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. 348 DUP050296869 Designation: D 2351 - 90 Standard Test Method for Sulfide in White Pigment Separated from Solvent-Reducible Pairjts1 This standard is issued under the fixed designation D 2351; 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. jjvScope . .,$.1 This* tes\ method covers the.determination of sulfide tifur in white pigment separated from solvent-reducible i'1.2 This standard does not purport to address the safety 'roblems associated with its use. It is the responsibility ofthe iser of this standard to establish appropriate safety and ealth practices and determine the applicability ofregulatory imitations prior to use. l! Referenced Documents . !i2.1 ASTM Standards: D215 Test Methods for Chemical Analysis of White Linseed Oil Paints12 D1193 Specification for Reagent Water3 D2371 Test Method for Pigment Content of Solvent- Reducible Paints2 Summary of Test Method 3.1 The extracted pigment is placed in a flask with mossy ihc and the sulfide generated by addition of HC1 reacts with lead nitrate in an absorption flask forming lead sulfide. The lead sulfide is dissolved with nitric add (HN(>3) and the lead stermined as lead sulfate in accordance with Test Methods 215. *' j3.2 A rapid method is also described. Significance and Use 4.1 Sulfide containing pigments such as lithopone have been used in paints in varying degrees in the past, years. As such it is useful to formulators and users to be able to monitor the amount of this compound in whole paints. 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 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 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990, Originally published as D 2351 - 65T. Last previous edition D 2351 -85. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Yols 06.03 and 11.01. 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. 5.2 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. 5.3 Ammoniacal Cadmium Chloride or Zinc Sulfate Solu tion-Dissolve 8 !g of cadmium chloride (CdQ2-2H20) in 200 mL of water and add 200 mL of ammonium hydroxide (NH4OH, sp gr 0.90); or, dissolve 200 g of zinc sulfate (ZnS04- 7H20) in 1080 mL ofwater and 920 mL'of NH4OH (sp gr 0.90). 514 Hydrochloric Acid (sp gr 1.19)---Concentrated HC1. 5.5 Lead Nitrate, Alkaline Solution--Into 100 mL of potassium hydroxide (KOH) solution (56 g in 140 mL of water) pour a saturated solution ofJlead nitrate (Pb(N03)2) (250 in 500 mL of water) until the precipitate ceases to redissolve, stirring constantly while mixing. Let settle- filter through a glass filter, and dilute the clear filtrate with an equal volume of water. About 3 volumes of the Pb(NQ3)2 solution will be required for 1 volume of the KGH solution. 5:6 Mossy Zinc. 1 5.7 Nitric Acid (1+4)--Mix 1 voliime of concentrated HN03, (sp gr 1.42) with 4 volumes of water. 5.8 Potassium Iodate, Standard Solution--Dissolve 3.6 g ~ of potassium iodate (KI3) and 39 g of potassium iodide (KI) in 1 L of water. For general work the theoretical sulfur, titer of this solution should be used; for special work the solution may be standardized against similar material, such * as a Kthopohe of known sulfide sulfur content. The'theoret ical titer is based on standard sodium oxalate (Na2C204) and is obtained as follows: To 300 mL of water in a'fcOO-mL flask,'preferably glass-stoppered, add 10 mL of HC1 (sp gr 1.19) and 1 gofKI. Cool and add lOmLofO.l AT potassium permanganate (KMn04) solution which has been standard ized against Na2C204. Swirl gently, stopper, and let stand for 5 min; Titrate the liberated iodine with standard sodium thiosulfate (Na2S203) solution until'the color fades. Then add 10 mL of starch solution and continue the titration until the blue color is destroyed. Repeat the titration, except substitute 10 mL of the KI03 for the KMn04 solution. Calculate the normality of the KI03 solution as follows. 4 "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." 349 DUP050296870 D 2351 5.8.1 Standardization Calculation for Theoretical Sulfur Titer: where: B = normality of KI03, Vl ~ standard Na2S203 solution, mL, required to titrate 10 mL of KMn04 solution, N -- normality of standardized KMn04 solution, and V2 -- standard Na2S203 solution, mL, required to titrate 10 mL of KI03 solution. 5.8.2 Standardization Against Known Pigment: C= (AXS)/(FX 100) (2) where: A - sulfur in known pigment, % C - sulfide equivalent of the KI03 solution, g/mL, S - pigment, g, and. V -- KI03 solution required to titrate known pigment, mL. 5.9 Starch Indicator (for Sulfur Titration)--To 1 L of boiling water add a cold suspension of 6 g of starch in 100 mL ofwater and boil vigorously for 5 min. Cool the solution, add 6 g of zinc chloride (ZnCl2) dissolved in 50 mL of cold water, thoroughly mix, and set aside for 24 h. Decant the clear supernatant liquid into a suitable container, add 3 g of KI, and mix thoroughly. 5.9.1 {Optional) Prepare an emulsion of 6 g of soluble starch in 25 mL of water, add a solution of 1 g of sodium hydroxide (NaOH) in 10 mL of water, and stir the solution until it gels. Dilute to 1 L with water, add 3 g. of KI, and mix thoroughly. , 6. Preparation of Sample. 6.1 Separate and prepare the pigment for this determina tion in accordance with Test Method D 2371.7 7. Procedure 7.1 Place 0.5 to 1 g ofthe pigment in a flask with about 10 g of "feathered" or mossy zinc and add. 50 mL of water; insert a stopper carrying a separatory funnel and an exit tube. Run in 50 mL of HC1 (sp gr 1.19) from the funnel, having previously connected the exit tube to two absorption flasks in series; the first flask containing 100 mL of alkaline lead nitrate solution, the second flask, 50 mL ofthe same solution as a safety device. After all of the acid has run into the evolution flask, heat slowly, finally boiling until the first appearance of steam in the first absorption flask. 7.2 Disconnect, let the lead sulfide (FbS) settle, filter, and wash with cold water, then with hot water until neutral to litmus paper and until the washings give no test for lead. Dissolve the PbS precipitate in hot HN03 (1+4) and determine the lead as lead sulfate (PbS04) in accordance with Test Method D 215. 7.3 For very rapid work, the evolved hydrogen sulfide (H2S) may be absorbed in an ammoniacal Cdd2 or ZnS04 solution (5.3) contained in two flasks connected in series, the contents of the absorption flasks washed into a vessel with cold water and diluted to about 1 L, acidified with HC1 (sp gr 1.19), and titrated with standard KI03 solution using starch indicator (5.9). 8. Calculation 8.1 Calculate the percent of sulfide sulftir, E, as follows: ?@ABCThe percent of sulfide sulfur can be calculated from the percent of total zinc and zinc soluble in acetic acid (2 to 3 %), assuming the sulfide to be zinc sulfide (ZnS). See section on Total Zinc of Test Method D 215. =[(/,x0.1054)/5,JX 10C (3) where: P = PbS04 formed, g, and S = sample used, g. E~{AV/S)X 100 (4) where: A = sulfide equivalent of the KI03 solution, g/mL, V = KI03 solution required for titration of specimen, mL, and S = sample used, g. 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. The American Society tor Testing and Material takes no position respecting the validity ot anypatent rights asserted in conmhtioh with any Item mentioned in this standard. Users of this standard are expressly advised that determination d 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 at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprmed or withdrawn. Your comments are Invited either lor revision oi this standard orlor additional 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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 350 DUP050296871 Bl> Designation: D 2352 - 85 (Reapproved 1990)'61 Standard Test Method for Sulfur Dioxide in White Pigment Separated from SolventReducible Paints1 This standard is issued under the fixed designation D 2352; the number immediately following the designation indicates the year of original adoption or, in the ease ofrevision, 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. DEFGei --Section 10 was added editorially in May 1990. Scope 1.1 This test method covers the determination of sulfur lioxide in white, pigment separated from solvent-reducible iaints. 1.2 This test method is not applicable in the presence of ilfides decomposable under the conditions given. || 1.3 This standard does not purport to address the safety foblems associated with its use. It is the responsibility ofthe $er of this standard to establish appropriate safety and Mtilth practices and determine the applicability ofregulatory limitations prior to use. Referenced Documents $2.1 ASTM Standards: D1193 Specification for Reagent Water*2 . fP"D2371 Test Method for Pigment Content of SolventReducible Paints3 Summary of Test Method 3.1 The extracted pigment is placed in a flask and readily liable sulfur dioxide (S02) is released by addition of ydrocloric acid (HC1) and bubbled through an absorption ask containing iodine solution and potassium iodide (KI). he solution is titrated with sodium thiosulfate (Na2S203). lising starch indicator. 3.2 A blank is run as directed in 3.1 with the pigment aided. The blank is then subtracted from the figure obtained for the sample titration and S02 is calculated. Significance and Use |;|f*4.1 Calcium sulfate pigments-such as titanium-calcium ' ave been used in paints in varying degrees in the past years. i such it is useful to the formulator and the user to be able to monitor the amount of this compound in whole paints. jp. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be 'used in all tests. Unless otherwise indicated, it is intended Irjthat 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. 5.2 Unless otherwise indicated, references to water shall be understood to mean Type II reagent grade water, con forming to Specification D 1193. 5.3 Hydrochloric Acid (1+3)--Mix 1 volume of concen trated hydrochloric acid (HCI, sp gr 1.19) with 3 volumes of water. 5.4 Iodine, Standard Solution (0.05 N) (for S02)--Place 15 to 20 g of pure potassium iodide (KI) in a 1-L flask, dissolve in as little water as possible, and then add about 6.4 g of resublimed iodine. Shake until the iodine is all dissolved, dilute to the mark with 'water, and mix. Standardize the solution against 0.05 N Na2S203 solution to obtain its true normality, 5.5 Potassium Iodide Solution (100 g/L)--Dissolve 100 g of potassium iodide (KI) in water and dilute to 1 L. 5.6 Sodium Thiosulfate, Standard (0.05 N) Solution (Car S02)---Dissolve pure sodium thiosulfate Na2S203 in water . (that has been well boiled to free it from carbon dioxide) in the proportion of 12.42 g of Na2S203 5H20 to 1 L of the solution. It is best to let this solution Stand for about twcr weeks before ..standardizing. Standardize3 with pure resublimed iodine, pure potassium biiodate, or pure potas sium iodate. This solution will be approximately ft.05 N, and it is best to leave it as it is after determining its exact iodine value, rather than to attempt to adjust it to exactly 0.05 N. Preserve in a stock bottle provided with a guard tube filled with soda lime. 5.7 Starch Indicator Solution--Make a homogenous paste of 10 g of soluble starch in cold water. Add to this 1 L of boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L) may be added to preserve the indicator. If long storage is required, the solution should be kept in a refrigerator at 4 to 10C (40 to 5QF). Prepare fresh indicator when the end T ` 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint i 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 Nov. 29, 1985. Published January 1986. Originallv iWished as D 2352 - 65 T. Last previous edition D 2352 - 73 (1979)sl. 1:1Annual Book ofASTM Standards, Vols 06.03 and 11.01. f,.3 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" by Joseph Rosin, D. Van Nostcand Co., Inc., New York, NY, and the "United States Pharmacopeia." 3 Buehrer, T. F,, and Mason, C. M., "Thiosulfate, Standardization of," Analytical Chemistry, Vol 2, 1930, p. 138. 351 DU P050296872 # 0 2352 point of the titration from blue to colorless or blue to light green fails to be sharp. 6. Preparation of Sample 6.1 Separate and prepare the pigment for this determina tion in accordance with Test Method D 2371. 7. Procedure 7.1 Transfer 10 g of the pigment to a suitable flask, insert a stopper fitted with a separatory funnel and a spray trap delivery tube (Note I), and attach the latter to a condenser. Place about 150 mL of HC1 (1 +3) in the funnel, the stopcock being closed (Note 2), and connect the other end of the condenser with a delivery tube that passes through a twohole, stopper and extends nearly to the bottom of an absorption flask; through the other hole of the stopper connect a tube or flask to serve as a safety device. Place 25 mL of 0.05 N iodine solution (5.4) in the absorption flask (dilute with water if necessary) and 20 mL of KI solution (100 g/L) in the safety tube; fit the stopper in the absorption flask. Open the stopcock and allow the acid to slowly enter the flask. Before all of the acid is admitted, force air (washed with sodium hydroxide (NaOH) solution) through the top of the separatory funnel (about 2 bubbles per second in the KI solution). Boil the solution 3 min with air passing through then remove the source of heat and pass air through for 30 min,. HIJK 1--A Knorr C02 apparatus is very convenient. In this case, the vertical condenser may be connected with an absorption tower con taining the iodine solution, followed by the KI solution in a suitable LIJKtube. 2--To minimize, if not'eliminate, any possible oxidation by the air, add about 1 g (in one piece) ofsodium bicarbonate (NaHC03) to the evolution flask, then add the acid directly to the flask, omitting tb.s separatory funnel and the current ofair. Boil the solution until about 56 H mL of distillate has passed over. 7.2 Disconnect the absorption vessels, wash the KI solti. ! don ihto the iodine solution, and titrate at once with 0.05 M Na2S203 solution using starch indicator. "Run a blank f determination in exactly the same manner except for the* omission of the pigment. Subtract the figure obtained for the blank determination from the figure obtained for titration of the sample and calculate the final result to S02 (1 mL 0.05 N iodine = 0.0016 g S02). 8. Calculation 8.1 Calculate the percent of sulfur dioxide. A, as follows: A =* [(V,-- B)I/Sl x 100 where: V = 0.05 N iodine solution required for titration of spec imen, mL, B = 0.05 N iodine solution required for titration of the blank, mL, I = S02 equivalent of the 0.05 N iodine solution, g/mL, and ... S == sample used, g. 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 sulfate analysis; sulfur dioxide; white pigment The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with arty Item mentioned in this standard. Users of this standard am 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 s subject to revision at any time by the responsible technical committee and must be reviewed every five years and tthot 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 fee! that your comments have not received a fair hearing you ahoukUnake your views known to the ASTM Committee On Standards 1916 Race St.. Philadelphia, PA 19103. i 352 DUP050296873 Designation: D 2354 - 91 Standard Test Method for Minimum Film Formation Temperature (MFFT) of Emulsion Vehicles1 i This standard is issued under the fixed designation D 2354; the number immediately following the designation indicates the year of s 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. 3. Scope 1.1 This test method covers the determination of the minimum temperature at which emulsion vehicles coalesce to form continuous films. The term "emulsion" in this test method includes latex vehicles. 1.2 This test method is limited to emulsions having minimum film formation temperatures below 25"C. 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 ofregulatory limitations prior to use. 2. Summary of Test Method I 2.1 In this test method the minimum film formation I temperature (MFFT) is determined by visual observation of ' cracking or whitening in films that have dried over a 1 substrate having a controlled temperature gradient. ] 3. Significance and Use j 3.1 The satisfactory film integrity of emulsion coatings 1 requires that as the aqueous phase evaporates the resinous I portion of the vehicle coalesces into a continuous film. Low temperature impairs the fluidity of the resin particle and thereby their ability to coalesce. Vehicles that can withstand low temperatures are therefore required, and MFFT is an I important quality feature of emulsion vehicles. 1 4. Apparatus | 4.1 Minimum Film Formation Temperature Bar--At l j MFFT unit12 such as is illustrated in Fig. 1. The bar f represented in Fig. 1 is designed to j>e used with thermocou| pies. The thermocouple leads used with the assembly are j iron-constantan with an external resistance of 10 ft. Also I included is a pyrometer (not shown in Fig. 1). MNOPi I--Thermometers can be used as an alternative way of measuring temperature.3 It is noted that larger holes (%2 in.) (4 mm) will have to be drilled in the bar to accommodate the thermometers. If 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 1.42 on Architectural Finishes. Current edition approved Sept. 15,1991. Published November 1991. Originally published as D 2354 - 65 T. Last previous edition D 2354 - 86. 2 A unit manufactured by Custom Scientific Instruments Inc., 13 Wing Dr., Cedar Knolls, NJ 07927, has been found suitable for this purpose. 3 An example of such a thermometer is Prince No. A-011044, 90' angle, red-reading, range from -5 to +50"C, having an accuracy of > 0.5*C and manufactured by Princo Instruments Inc., 1020 Industrial Hwy., Southampton, PA 18966. thermometers are selected, all holes are drilled on the same side of the bar, as opposed to the system of alternate placement of holes when using QRSUthermocouples. 2--A self-contained unit eliminating the need for external cooling and requiring only an electrical outlet, piped water and an air or nitrogen supply has been developed by ICI Paints Division.4 4.2 Dry Air or Dry Nitrogen Supply, with a regulating valve and flow meter. 4.3 Film Caster, having a 6-mii (150-pm) clearance. 5. Reagents and Materials 5.1 Dry Ice. 5.2 Isopropanol, anhydrous. 6. Procedure 6.1 Set up the MFFT bar in a level position with the lower temperature leg ofthe bar immersed in a dry ice-isopropanol bath. It is important that the surface of the bar be smooth and plane to ensure uniform film thicknesses. Use a Vi-gal (2-L) container for this purpose. (The container can be insulated with any suitable material to reduce heat loss.) Adjust the height of the dry ice-isopropanol bath as needed to bring the temperature of the bar to approximately 0C at the lowest temperature-measuring stage ofthe unit. Lower or higher temperatures can be obtained, if needed, by adjusting the bath height: The bath height needed to obtain 0C will vary depending on the heat conductivity ofthe metal used in the construction of the bar. Expose the higher temperature end of the bar at approximately 25C by either conducting the test in a constant-temperature room at this temperature or by thermostattirig the leg. 6.2 Immediately after imposing the temperature.,gradient on the bar, place the cover over it and start the flow ofdry air (or nitrogen) at a rate of 3000 cm3/min from the lowtemperature end to the high-temperature end of the bar, controlling the rate by a simple flow meter. Allowing the air to retain moisture by warming up prevents water condensa tion at the cold temperature end that would interfere with film drying. Approximately 1 to 1 Vi h is needed for the temperature gradient to reach equilibrium once the bar is placed in operation. The air manifold holes must be clean and free of frost before starting a test. VWXY 3--A mixture of ethylene glycol and surfactant applied to the air outlet alleviates the frosting condition temporarily. 6.3 Once a constant-temperature gradient is established, 4 The unit identified as an MFFTBAR, Model SS-3000, manufactured by Sheen Instruments, Ltd., 8 Waldegrave Rd., Teddington, Middlesex TW11 8LD, England has been found suitable for this purpose. j 353 f DU P050296874 ft D 2354 Note--Ijn. -25.4 mm.; > FIG. 1 Minimum Film Formation Temperature Bac remove the cover and cat the films using the 6-mil appli cator (Note 3). Cast films from the low to the hightemperature end of the bar because the extension at the high-temperature end is designed to permit overflow to fall into a container below the bar. After the film is cast and the cover put in place, approximately 1 to 2 h are required for the film to dry. Check the air flow and isopropanol bath height before any tests are started and then maintain them at their respective levels until the test is completed. Z[\] 4--If desired, a `/2-mil (13-p.m) polyethylene terephthalate sheet of 5-in. (125-nun) width can be placed on the bar surface before casting the film. Tests show that' there are no differences between minimum filming temperatures determined with and without the sheet. The polyethylene terephthalatefilm permits riot only easier clean-up of the apparatus, but also a semi-permarient record of the test. Special care must be exercised To ensure good contact'of the sheet with the bar. Accomplish this by either of the following techniques: (1) Wipe the sheet with a dry cloth to develop a static charge before placement on the.bar. (2) Coat the sheet with silicone oil before placement on the bar. 6.4 After the film has dried, observe For discontinuity as evidenced by whitening or cracking or both. Record the lowest temperature on the bar at which the film is still continuous as the minimum film formation temperature. 7. Report . - 7.1 Report the following information: 7.1.1 MFFT iti degrees Celsius, and ' 7.1.2 Description of the discontinuity indicating degree of whitening and cracking. .__ 8. Precision and Bias .8,1 Precision--Information for a formal precision state ment has not yet been obtained, but it is reported that MFFT values obtained by this test method can be .expected to fall within 2,C of their mean. 8.2 Bias--Bias; has not yet been determined. 9. Keywords 9.1 emulsion vehicles; film formation; minimum film formation temperature, MFFT 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 oi 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 live years and ifnotrevised, either reapproved or withdrawn. Your comments are invited either tor revision ofthis standard pr 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. 354 DUP050296875 Designation: D 2363 - 79 (Reapproved 1989)1 Standard Test Methods for Hydroxypropyl Methylcellulose1 This standard is issued under the fixed designation D 2363; 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 epsildn (0 indicates an editorial change since the last revision or reapproval. 'i . - ' `------ **1 ^_`a*l --Editorial changes were made throughout, including the title, in October 1989. - - . --------- Scope | ] These test methods cover the testing of hydroxypropyl ithylceUulose. The test procedures appear in the following order: Sections Moisture Ash (as Sulfate) Chlorides (as NaCl) Alkalinity (asNa2C03) Irbn Heavy Metals Methoxyl Content Hydroxypropoxyl Content Viscosity PH Solids Density 4 to 6 7 to 10 U to 14 15 to 18 19 to 24 25 to 29 30 to 35 36 to 41 42 to 46 47 1 48 to 51 . Si to 56 ,1.3 This standard may involve hazardous materials, oper!turns, and equipment. This standard does not purport to hress all ofthe safetyproblems associated with its use. It is ^Responsibility of the user of this standard to .establish Tpropriate safety and health practices and determine the pplicability of regulatory limitations prior to use. For a ll^cificVazard statement,. se,e Note 1. Referenced Documents teILl ASTM Standards: 10,96 Test Methods for Water and Sediment in Crude Oil by Centrifuge Method (Field Procedure)2 jJi 70 Test Method for pff.of Aqueous Solutions With the Glass Electrode3 1,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, here such specifications are available.4 Other grades may be 1 These test methods are under the jurisdiction of <\STM Committee D-I on Paint and Related Coatings* and Materials and are the direct responsibility of Subcommittee DG1.36 on Celhilosics. Current edition approved May 25, 1979. Published July 1979. Originally published as D 2363 - 65 T. Last previous edition D 2363 - 72. 2 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 15.05. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing ofreagents not listed by American Chemical Society, see "Reagent Chemicals and Standards," by feph Rosin, D. Van Nostrand Coj Inc., New York, NY, and the "United States Pharmacopeia." . 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 distilled water. MOISTURE 4. Scope 4.1 This test method covers the determination of the volatile content of hydroxypropyl methylcellulose and, by common usage, designated xnoisture. 5. Procedure 5.1 Transfer 2 to 5 g of the sample weighed to the nearest 0.01 g to a tared dish (fitted with a lid) and dry for 2 h in an oven at 100 to 105C with lid removed. Remove the dish from the oven, cover with a lid, cool in a desiccator, and weigh. 6. Calculation " 6.1 .Calculate the percent of moisture as follows: Moisture, % = (A/B) x 100 where: ' ' ' ' A = mass loss on heating, and B = sample used, g. ASH--AS SULFATE ~~ , (1) 7. Scope 7.1 This test method covets the determination of the amount of residue left from igniting a sample of hydroxypropyl methylcellulose after being moistened with sulfuric acid. 8. Reagents 8.1 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 8.2 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric add (H2S04). 9. Procedure 9,1 Weigh to the nearest 0.01 g about 2 g of the sample (previously dried for >/2 h at 105C) into a tared Coors No. 1, high-form, porcelain crucible. Add 5 drops of H2SC>4 around the. inside surface of the crucible. Place the crutible inside of a loosely fitting aluminum ring (approximately 1`A in. (32 mm) high, with l/t-in. (6.4-mm) sidewall, and 1%-in. (44- 355 DUP0502 96876 D 2363 1 mm) inside diameter, cut from a piece of aluminum pipe) on a hot plate. Loosely cover with a crucible cover. Carefifily char the hydroxypropyl methylcellulose until all the volatiles are removed. 9.2 Cool the crucible, add 1 ml of H2S04 and 2 ml of HNOj so that it completely wets the charred residue. Cautiously heat to dense white fumes on a hot plate. Place the uncovered crucible in a muffle furnace at 600C and ignite until all the carbon is gone (for about 1 h). Transfer to a dessicator until cool, then weigh. (Save the residue for the Heavy Metals determination.) 10. Calculation 10.1 Calculate the percent of ash, C, as follows: C= (A/B) x 100 where: A = sulfated ash, g, and B = sample used, g. (2) CHLORIDES--AS SODIUM CHLORIDE 11. Scope 11.1 This test method covers the determination of the total percent of chloride (bromide included if present) calculated as sodium chloride (NaCl) in hydroxypropyl methylcellulose. The sample is dispersed and the chloride titrated volumetrically with 0.100 N stiver nitrate solution. 12. Reagents 12.1 Ferric Alum Indicator Solution--Add 100 g of ferric ammonium sulfate FeNH4(S04)2- 12H20 to 250 mL of water. Heat to boiling and add NH03 (sp gr 1.42) slowly until the red color is removed. This will usually require about 6 to 15 mL of HNOj. Filter the solution and store in a glass bottle. 12.2 Nitric Acid (sp gr 7.42)--Concentrated nitric acid (HN03). 12.3 Potassium Thiocyanate Standard Solution (0.1 N)--Dissolve 10 g of potassium thiocyanate (KCNS) in 1 L of water. By means of a pipet, measure 25 mL of 0.100 N silver nitrate (AgN03) solution into a 400-mL beaker. Add 100 mL of water, 10 mL of HN03 (sp gr 1.42), and 5 mL of ferric alum indicator solution. Titrate with the KCNS solution, while stirring, until a faint persistent red color is produced. Calculate the normality, N, of the KCNS solution as follows: N= (A/B) X 0.1 (3) where: A =0.100 N AgN03 solution added, mL, and B = KCNS solution required for the titration, mL. 12.4 Silver Nitrate-Standard Solution (0.100 N)--Grind silver nitrate (AgNOa) crystals fine enough to pass through a No. 20 (850-pm) sieve and then dry for 2 h at 110C. Prepare a 0.100 N solution by dissolving 16.989 g of dry AgNQ3 in chloride-free water and diluting to 1 L in a volumetric flask. 13. Procedure 13.1 Weigh to the nearest 0.01 g about 1.0 g ofthe sample (previously dried for lh h at tOO to 105C) and transfer to a 500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hot water and swirl for a few minutes; then cool to dissolve. 13.2 Add 5 mL of 0.100 N AgN03 solution and 5 mL of ferric alum indicator solution, and back-titrate with 0.1 N KCNS solution to the first appearance qf a faint pink color. 14. Calculation 14.1 Calculate the percent of chlorides as NaCl as follows: Chlorides, % = ([(AB - CD) x 0.0585]/) X 100 (4) where: A = AgN03 solution added, mL, B = normality of the AgN03 solution, C = KCNS solution required to back-titrate the excess AgN03, mL, D = normality of the KCNS solution, and E -- sample used, g. ALKALINITY--AS SODIUM CARBONATE 15. Scope 15.1 This test method covers the determination of the total alkalinity of hydroxypropyl methylcellulose expressed as sodium carbonate (Na2C03). 16. Reagents 16.1 Methyl Purple Indicator Solution. 16.2 Sulfuric Acid, Standard (0.01 N)--Prepare and stan dardize a 0.01 N solution of sulfuric acid (H2S04). 17. Procedure 17.1 Weigh to the nearest 0.01 g about l.frg of the sample (previously dried for xh h at 100 to 105C) and transfer to a 500-ml, widemouth Erlenmeyer flask. Add 250 mL of hot water and swirl for a few minutes; then cool to dissolve. 17.2 Add 4 drops of methyl purple indicator solution and titrate to the first faint pink color with 0.01 TV H2S04. 18. Calculation 18.1 Calculate the percent alkalinity as Na2C03, S, as follows: -~ ._ ----- S= [(AB x 0.053)/C] x 100 (5) where: A = H2S04 required for titration of the sample, mL, B = normality of the H2S04, and C = sample used, g. IRON 19. Scope 19.1 This test method covers the determination of total iron content in samples of hydroxypropyl methylcellulose. The iron is converted to ferric sulfate which reacts'with the indicator to form a pink color that can be quantitatively measured. 20. Apparatus 20.1 Photometer--Any photoelectric filter photometer or spectrophotometer suitable for measurements at 430 nm. 20.2 Kjeldahl Flasks--Calibrated to contain 50 mL, and made of heat- and chemical-resistant glass. 356 DUP050296877 D 2363 1. Reagents | 21.1 Ammonium Hydroxide (sp gr 0.90)--Concentrated ('ammonium hydroxide (NH4OH). i .21.2 Buffer Solution--Dissolve 20 g of sodium bicar bonate (NaHC03) and 10 g of sodium carbonate (Na2C03) in water and dilute to 1 L. 21.3 Disodium-l,2-Dikydroxybenzene-3,5-Disulfonate So lution5--Prepare an aqueous solution containing 25 g/L. 21.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HC1). 21.5 Hydrogen Peroxide (30 %)--Concentrated hydrogen peroxide (H202). 21.6 Iron Standard Solution (0.0001 g Fe/ml)--Dissolve 0.01 g of iron powder containing not less than 99.9 % iron in ;HC1 (sp gr 1.19). Oxidize the solution with bromine water and expel the excess by boiling. Dilute to 1 L in a volumetric flask. 21.7 Phenolphthalein Indicator Solution (1 g/100 mL)--Dissolve 1 g ofphenolphthalein in 100 mL of ethanol (95%). 21.8 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04). 21.9 Sulfuric Acid (1+4)--Carefully mix 1 volume of H2S04 (sp gr 1.84) with 4 volumes of water, adding the tt2S04 gradually while mixing. 22. Preparation of Calibration Curve 22.1 Following the procedure given in Section 23, and | using varied amounts of the standard iron solution prepared | in accordance with 21.6, prepare a calibration curve showing I iron content in parts per million and the corresponding 1 photometer readings. ` * 23. Procedure 23.1 Weigh to the nearest 0.01 g about 2 g of the sample |t(previously dried for lA h at 100 to 105C). Transfer by jj means Of a funnel to a Kjeldahl flask. Place the flask at a 20 angle in the furnace at 500C and heat until some charring of lithe sample has taken place. (Care must be taken not to char jjtoo much.) Remove and allow to cool. 23.2 Add 3 mL of H2S04 to the flask. Place on the digestion rack and digest. Cool and add H202 dropwise until the solution is clear. Heat Over a Mekei burner to a volume of 2 mL. Cool, and wash the sides of the flask with water. jAdd 3 drops of phenolphthalein indicator solution. Add NH4OH to a red end point. Wash the neck of the flask. The solution should be clear and not greater than 20' mL in volume. 23.3 Add 2 mL of the color-forming solution described in 21.3, and mix. Adjust pH to 7.0 and then dilute to mark with buffer. Transfer a small portion to an absorption cell and determine the photometer reading at 480 hm. 23.4 Blank--Make a blank determination, using the same amount of reagents and the same procedure as for the sample. [ 24. Calculation 24.1 Read the iron content, in parts per million, directly s A suitable prepared solution ofthis reagent, known as "Tiferron" or "Tiron," is supplied by the LaMotte Chemical Products Co., Baltimore, MD. from the calibration curve (Section 22). Subtract the parts per million of iron due to iron in the blank. HEAVY METALS 25. Scope 25.1 This test method covers the determination of whether or not. the heavy metals content of hydroxypropyl methylcellulose is below a given level based on a lead standard. 26. Summary of Test Method 26.1 The ash residue from the sulfated ash test is digested with dilute hydrochloric acid. A standard containing a known amount of lead is prepared, and the heavy metals content is determined qualitatively by comparing the sample to the standard. 27. Apparatus 27.1 Nessler Tubes, 50-mL. 27.2 Volumetric Flasks, 50-mL. 28. Reagents 28.1 Acetic Acid--Glacial acetic acid. 28.2 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 28.3 Ammonium Hydroxide (2+3)--Dilute 400 mL of NH4OH (sp gr 0.90) with sufficient water to make 1000 mL. 28.4 Buffer Solution--Dissolve 60 mL of acetic acid in about 500 mL of water, add 10 mL of NH4OH, and dilute to 1 L. ` 28.5 Hydrochloric Acid (1+2)--Dilute 1 volume of con centrated hydrochloric acid (HC1, sp gr 1.19) with 2 volumes of water. 28.6 Hydrogen Sulfide TS--Saturate a convenient volume of water with hydrogen sulfide (H2S) in a narrow-neck, glass-stoppered, amber bottle. This solution must be made fresh, 28.7 Hydroxylamine Hydrochloride Solution (200 g/L)--Dissolve 20 g of hydroxylamine hydrochloride (NH2OH-HCl) m 100 mL of water. 28.8) Lead Nitrate Stock Solution-r-Dissolve 159.8 mg of lead nitrate (Pb(N03)2) in 100 mL of water containing 1 mL of HN03 (sp gr 1.42). Dilute with water to 1000.0 mL and mix. This solution should be prepared and stored in glass containers that are free from lead salts. 28.9 Lead Standard Solution (1 mL -- I pg Pb)--Dilute 10 mL of the lead nitrate stock solution, accurately mea sured, with water to 100.0 mL. Each millilitre ofthe solution so prepared contains 10 pg of lead. 29. Procedure 29.1 Pipet into a 50-mL Nessler tube 0.15 mL of HC1 (1+2), 2 mL .of the buffer solution, and a volume of the standard lead solution containing the quantity of lead equivalent to the specified heavy metals limit. Add water to make 40 mL and label as Solution A. The final pH of these solutions should be between 3 and 4. This can be tested by pH indicator paper or pH meter. For visual comparison the optimum lead content should be between 20 and 40 pg. 29.2 To the crucible containing the sulfated ash residue 357 DU P050296878 # D 2363 I add 4 mL of HC1 (1+2). Cover and carefully digest on a steam bath for 10 min. Uncover and slowly evaporate to dryness. Moisten the residue with 0.15 mL of HC1 (1+2), 0.5 mL of hydroxylamine hydrochloride solution, and 10 mL of hot water. Carefully digest for 2 min. Add 2 mL of the buffer solution. Filter if necessary. Thoroughly wash the crucible and filter with water into a 50-mL Nessler tube that matches the one used for Solution A. If necessary, adjust the pH to 3 to 4 with NH4OH (2+3) Or HC1 (1+2) using pH indicator paper. Dilute to 40 mL and label this Solution B. 29.3 Add 10 mL of H2S solution to each tube: Solution A and Solution B. Mix and view downward over a white surface. The color of Solution B shall be no darker than that of Solution A. Make the comparison within 10 min. METHOXYL CONTENT 30. Scope 30.1 This test method covers the determination of the methoxyl content of hydroxypropyl methylcellulose. Total alkoxyl is first determined and the methoxyl content found by subtracting the hydroxypropyl content from the total alkoxyl figure. 31. Summary of Test Method 31.1 The hydroxypropyl methylcellulose is heated with a strong solution .of hydriodic acid to form an alkyl iodide, which by means of a carbon dioxide stream is swept through a condenser and finally absorbed in a mixture of bromine, acetic acid, and sodium acetate, The alkyl iodide absorbed in the aforementioned mixture is oxidized to an alkyl iodate. The excess bromine is reduced with formic acid, and the iodate is determined iodometrically rising potassium iodide and standard thiosulfate. 32. Apparatus 32.1 Distillation Apparatus, as illustrated in Fig. 1, con sisting of a boiling flask with a side arm for admission of carbon dioxide or nitrogen, an air condenser with a trap, and a receiver. 32.2 Oil Bath, equipped with a heating device, preferably electrical, so that the bath can be maintained at 145 to 150*C. 33. Reagents 33.1 Bromine Solution--Dissolve 5 mL of bromine in 145 mL of the potassium acetate solution. Prepare the bromine solution fresh daily in a hood to remove bromine vapors. 33.2 Carbon Dioxide--This may be obtained by the interaction of marble and hydrochloric acid (HC1, 1+1) in a Kipp generator or preferably from a cylinder of the gas equipped with a suitable needle valve. The carbon dioxide (C02) shall be passed through a bubble counter and a dry trap, and then through a pressure regulator consisting of a glass tee whose vertical arm extends almost to the bottom of a 10-in. (254-mm) column of water. A screw clamp shall be attached to the thin-walled rubber tubing connecting the horizontal arm of the tee with the boiling flask. This arrangement permits regulation of the flow of gas and allows any excess gas to escape. Nitrogen may be used in place of Wk C02. fll 33.3 Formic Add (90 %). i8 33.4 Gelatin Capsules--Gelatin capsules of a suitable size 31 to hold 50 to 60 mg of the dried sample. M 33.5 Hydriodic Acid (57 %, sp gr /. 70)---Hydriodic acid '8 (HI) forms with water a constant-boiling mixture (boiling m point 126 to 127C) that contains 57 % HI. The concentra- m tion of Hl in the reagent used should be not less than 56.5 %. The blank determination, which is affected primarily by free: iodine in the reagent should require not more than 0.5 mL of ? 0,1 N sodium thiosulfate (Na2S203) solution.6 If necessary, j the acid may be purified by adding to it a small amount of j red phosphorus and boiling for 20 to 30 min in a hood, while passing a stream of C02 into the liquid Distillation shall ' then be earned out behind a safety glass shield in a hood, ; using an all glass apparatus with a slow stream of C02 i running through the receiver. (Warning--See Note 1) Put j the purified HI in small, brown, glass-stoppered bottles, j previously swept out with C02, and seal the stoppers with i molten paraffin. Store in a dark place. To minimize decom- f position of HI due to contact with air, run CO2 into the j bottle while withdrawing portions of the acid for .use. 1 bcde fg Warning-- Under some conditions the poisonous gas phosphine (PH3) is formed during distillation, and this may unite with molecular iodine to form phosphorus triodide (PI3), which may. explode on contact with air. It is, therefore, advisable to keep the current ofOOj' going after the distillation is ended and until the apparatus has cooled. I f 1 j I 33.6 Phosphorus Slurry--Add about 0.06 g of red phos- j phorus to 100 mL of water. Shake well before using. j 33.7 Potassium Acetate Solution (100 g/L)~Dissolve 100... g ofanhydrous potassium acetate crystals in 1 L ofa solution J containing 900 mL of glacial acetic acid and 100 mL of ] acetic anhydride. i 33.8 Potassium Iodide (KI). 33.9 Sodium Acetate Solution (220 g/L)--Dissolve 220 g of anhydrous sodium acetate in. water and dilute to 1~. i 33.10 Sodium Thiosulfate Standard Solution (0.1 N)-- i Dissolve 25 g of sodium thiosulfate (Na^^ 5HzO) in 200 ml of water and dilute to 1 L. Use freshly boiled and cooled water. It.i$ preferable to allow the solution to stand for a few days before standardization. Standardize the solution against 0.1000 N potassium dichromate (K2Cr207) prepared by dissolving exactly 4.9037 g of K2Cr2Q7 (National Institute of Standards and Technology Standard Sample No. 136) in water and diluting to a 1 L in a volumetric flask. By means of a buret, measure accurately 35 to 45 mL of the K2Cr207 solution into a 250-mL Erlenmeyer flask. Add 2 g of KI and 50 mL of H2S04 (1+9) and allow to stand for about 5 min. The flask should be stoppered during the standing period to avoid loss of iodine. Titrate the liberated iodine with the Na2S203 solution, using starch indicator solution near .the end point. At the end point, the blue color of the starch indicator will be destroyed, leaving the pale green color ofthe chromate ion. The normality ofthe Na2S203 solution should 6 Hydriodic acid suitable for methoxyl determination may be prepared by the method ofSamsel, E. P,, and McHatd, J. A., "Determination ofAlkoxyl Groups in Cellulose Ethers," Industrial and Engineering Chemistry, Analytical Edition, IECHA, Vol 14, 1942, p. 750. Hydriodic acid available from Merck and Co. has been found satisfactory for this purpose. 358 DUP050296879 # D 2363 be checked at least once a week. Calculate the normality of the Na2S203 solution, N, as follows: N - (A/B) x 0.1 (6) where: A = 0.1000 N K2Cr207 solution added, mL, and : B = Na2S203 solution required for the titration, mL. As an alternative procedure, the Na2S203 solution may be standardized against arsenic trioxide (As^) (National Insti tute of Standards and Technology standard sample No. 83) or potassium iodate (KI03). 33.11 Starch Indicator Solution. 33.12 Sulfuric Acid (7+9)--Carefully mix 1 volume of concentrated H2SQ4 (sp gr 1.84) with 9 volumes of water, adding the H2S04 gradually while mixing. 34. Procedure 34.1 Dry the sample at 105C for at least 30 min. Through the condenser, add to the trap in the distillation apparatus (Fig. 1) enough of the phosphorus slurry to make the trap about half full (Note 2). Add 19 to 20 mL of the bromine solution to the receiver. Weigh 50 to 60 mg of the dry sample, to the nearest 0.1 mg, into a gelatin capsule and drop it into the boiling flask. (The weighing should be done as rapidly as possible without 'sacrificing accuracy, since dry hydroxypropyl methylcellulose picks up moisture rapidly.) hijk l--Water may be used in the trap to scrub out entrained vapors of iodine quite successfully. If the test method Ts to be used as sf routine control test, tbis-may be advisable for safety purposes. If so, check the accuracy of the apparatus with the water trap against samples that have been run using the phosphorus slurry trap. 34:2 Add a few small glass beads or chips ofclay plate and then 6 mL of the HI. Moisten the ground-glass joint with 2 drops of the HI, then fasten to the distillation assembly. Connect the source of C02 to the side arm of the flask. Pass a current of C02 into the apparatus at the rate of about 2 bubbles/s. Immerse the flask in the oil bath, maintained at 150C, and heat for 40 min. 34.3 Add 10 mL of sodium acetate solution to a 500-mL Erlenmeyer flask and wash into it the contents of the re ceiver; dilute to 125 mL with water. Add formic acid dropwise, with swirling, until the brown color of bromine is discharged, and then add about 6 drops more. A total of 12 to 15 drops is usually required. After about 3 min add 3 g of KI and 15 mL of H2S04 (1+9) and titrate immediately with 0.1 N Na2S203 solution to a light straw color. Add a little starch indicator solution and continue the titration to the disappearance of the blue color. 359 DUP050296880 # D 2363 34.4 Blank--Make a blank determination, using the same amounts of reagents and the same procedure as for the sample. (Usually, about 0.1 mL of0.1 7VNa2S203 solution is required.) 35. Calculation 35.1 Calculate the percent of methoxyj as follows: M = ([(A - B)C x 0.00517]/Z>) x 100 . (7) where: M= Methoxyl, total (methyl + hydroxypropyl groups calcu lated as methoxyl), A = Na2S203 solution required for titration of the sample, mL, B = Na2S203 solution required for titration of the blank, mL, C = normality of the Na2S203 solution, and D = sample used, g. 35.2 In 35.1 the percent OCH3 represents the total of methyl and hydroxypropyl groups calculated as methoxyl. To obtain the corrected methoxyl content, the total alkoxyl must be corrected for the percent OC3H6OH obtained in Section 41. The percent OC3H6OH shall be first corrected by a factor of 0.93 (an average obtained by running Morgan determinations on a large number of samples) for the' propylene produced from the reaction of HI with the hydroxypropyl group as follows: A = B -- (CX 0.93 X 31/75) (8) where: A = corrected OCH3, %, B = total OCH3, %, and C = OC3H6OH, %. HYDROXYPROPOXYL CONTENT7 36. Scope 36.1 This test method covers the determination of the hydroxypropoxyl content of hydroxypropyl methylcelluIos&. The figure obtained from this analysis is used.in determining the corrected percent methoxyl content. 38. Apparatus 38.1 Chromic Acid Oxidation Apparatus, as illustrated in Fig. 2.8 38.2 Oil Bath, equipped with an electrical heating device so the bath can be maintained at 155"C. 38.3 pH Meter, expanded scale, capable of giving repro ducible results within 0.1 pH units and equipped with glass and calomel electrodes. 39. Reagents 39.1 Chromium Trioxide Solution {30 %)--Dissolve 60 g of chromic trioxide (Cr03) in 140 mL of organic-free water. 39.2 Nitrogen. 39.3 Potassium Iodide {KT). 39.4 Sodium Bicarbonate (NaHCOs). 39.5 Sodium Hydroxide, Standard Solution {0.02 N), carbon dioxide-free--Standardize against primary standard potassium hydrogen phthalate (KHC8H404) using a pH meter to an end point of pH 7.0 0.1. 39.6. Sodium Thiosulfate Standard Solution {0.1 N)-- Dissolve 24.8 g of sodium thiosulfate (Na2S203) and 0.2 g sodium bicarbonate (NaHC03) in freshly boiled water. Dilute to L L with water. Standardize against potassium iodate (KK>3) using starch indicator to determine the end point 39.7 Sodium Thiosulfate Standard Solution {0.02 N)-- Dilute 200 ml of 0.1 TV sodium thiosulfate standard solution to 1 L with.water. Prepare fresh solutions daily as needed. 39.8 Sulfuric Acid {1+165)--Carefully add, while stirring 10 mL of concentrated H2S04 (sp gr 1.84) to 165 mL of distilled water. 39.9 ' Methylcellulose, free of foreign material such as other substituted celluloses or glycols that will break down to acetic acid. 39.10 Propylene Glycol. 39.11 Water, organic-free, obtained by distillation or by ion-exchange treatment and to pass the following test: To, 100 mL ofwater add 10 mLofdiltiteH2S04 (1+165), heat to boiling, and add 0.1 mL of potassium permanganate (KMn04) solution (approximately 0,1.N). The water must retain a pink coloration after boiling for*10 min.' 37. Summary of Test Method 37.1 The hydroxypropoxyl group of hydroxypropyl methylcellulose is oxidized by hot chromic acid to acetic acid and this in turn is titrated with 0.02 N sodium hydroxide solu tion. Procedures are also given for (7) eliminating the error resulting from oxidation of the cellulose, backbone, which yields an apparent hydroxypropyl value, and (2) preparing a synthetic hydroxypropyl methylcellulose standard using methylcellulose and propylene glycol. 7 References for the hydroxypropoxyl determination are as follows: Dow Method No. MC-15, "The Determination of the Hydroxypropyl Group in the Presence of an Alkyl Group in Hydroxypropyl Methylcellulose." Lemieux, R. U., and Purves, C. B., "Quantitative Estimation as Acetic Acid of Acetyl, Ethylidene, Ethoxy, and Hydroxyethyl Groups," Canadian Journal of Research, Vol B-25, 1947, p. 485. Morgan, P. W., "Determination of Ethers and Esters of Ethylene Glycol," Industrial and Engineering Chemistry, Analytical Edition, 1ECHA, Vol 18, 1946, p. 500. 40. Procedure 40.1 Weigh to the nearest 0.0001 g abouAOO mg of the sample (previously dried at 105C for Vz h) and transfer (o flask, D, and add 10 mL of 30 % Cr03 solution. Fill the steam generator, B, to the bottom;of the standard-taper joint and then assemble the apparatus as shown in Fig. 2. Immerse the steam generator and sample, flask in the oil bath to the level of the Cr03 solution. Start the condenser cooling water and pass nitrogen gas through the flask at a rate of 1 bubble per second. Raise the temperature of the bath to, 155C within l/2 h and maintain it at this temperature untiithe end ofthe determination. Too rapid an initial rise in temperature results in high blanks. Distill until 5Q mL of distillate has * The following parts, manufactured by Ace Glass, Inc., Vineland, NJ 08360 (properly modified), have been found satisfactory for this test method: Steam generator, trap vacuum. No. 8753; Reaction flask, 25-mL, No. 9293 P; Vigneaux column, 100-mL, No. 9224; Adapter bleeder tube. No. 9222; Condenser, micro, 100-mL, No. 9.195. 360 DUP050296881 # D 2363 M--Oil bath equipped with an electric heater capable of heating the bath at the desired rate and maintaining the temperature at 155C. 9--Steam generator consisting of a 25 by 150-mm test tube and a gas Wet tube with a % to IV-t-mm capillary tip. Q--Adapter bleeder tube with a % to 1 'A-mm capillary tip. D--Reaction flask consisting of a 25-tnL conical bottom micro boiling flask modified to provide a sldearm cutlet. B--Vlgroaux column, 95 mm long, wrapped with aluminum foil. F--Micro condenser with a 100-mm jacket. ! 0--Beaker, 150-mL, Berzelius, graduated. FIG. 2 Oxidation and Distillation Apparatus. been collected. Detach condenser, F, from the Vigreaux column, E, and wash with water, collecting the washings in the beaker containing the distillate. Titrate the solution jvith standard 0.02 N NaOH solutidn to a pH of 7.0 0.1 using the expanded-scale pH meter. Record the volume, V, of standard NaOH used. Add approximately. 0.5 g of NaHC03 followed by 10 mL dilute H2S04 (1+165). After evolution of carbon dioxide (C02) has ceased, add 1 g of KI, mix well, and allow the solution to stand in the dark for 5 min. Titrate the liberated iodine with 0.02 jVNa2S203 to the disappearance of the yellow color. Record the volume, Y, of standard Na2S203 used. This titration, Y mL, when multi plied by the empirical factor, K, appropriate to the particular apparatus and reagents in use, gives the acid equivalent not causfcd by acetic acid. The acetic acid equivalent is (V - KY) mL of 0.02 N NaOH solution. 40.2 Empirical Factor, The-empirical factor, K, for each apparatus is obtained by running a blank determination in which the cellulose ether is omitted. The acidity ofa blank run for a given apparatus and given reagents is in a fixed ratio to the oxidizing equivalent of the distillate in terms of Na2S2C>3 solution as follows: K = {Vb x NJ/lYt, X Ay (9) where: I Vb = 0.02 N NaOH solution required in blank run, mL, N, = normality of the 0.02 A NaOH solution, Y,, = 0.02 N Na2S203 required in blank run, mL, and N2 -- normality of the 0.02 N Na2S203 solution. 40.3 Methylcellulose Blank--Conduct several determina tions using methylcellulose according to the given procedure. 40.4 Hydmxypropoxyl Standard--Since, primary stand ards of hydroxypropyl methylcellulose are not available, a synthetic standard may be prepared by weighing 100 mg of methylcellulose into the reaction flask and adding 1.0 mL of .an aqueous solution containing 1.0 g of propylene glycol in 100 mL. Thus, a secondary standard hydroxypropyl methyl cellulose can be established by repeated analysis by this method using properly standardized conditions. 41. Calculation 41.1 Calculate the percent of uncorrected hydroxypro-poxyl as follows: a v ([(jyv,. - KYJtJ x 0.0751/WO X 100 (10) where: > .... r Au = OC3H6OH (uncorrected), % Va = 0.02 N NaOH solution required for titration of the sample, mL, Nv = normality of the 0.02 N NaOH solution, K = empirical factor, Ya = 0.02 N Na2S203 solution required for titration of the sample, mL, N2 -- normality of the 0.02 N Na2S203 solution, and W = sample used, g. 41.2 Calculate the percent of corrected hydroxypropoxyl as follows: . Ag ~ Axj -- B . (11) where: Ac = 0C3H60H (corrected), %, and B = OC3H6OH obtained from the methylcellulose blank determination, % (40.3). VISCOSITY 42. Scope 42.1 This test method covers the determination of the DU P050296882 # D 2363 VISCOMETER FOR 3 LOW VISCOSITY J Heavy well tubing approx, range of sizes 8S follows: Viscosite, cps I.D.. mm 1500 4000 8000 t5000 0000 5J 6.0 7.5 10.0 . '1&0 Precision bore cap. or tubing-V" (3.12 mm or smaller) 25 mm O.D.- Heavy wall tubing approx, range of sizes as follows: IS cps 25 cps 100 cps 400 cps viscosity viscosity viscosity viscosity 1.6 mm 1.8 mm 2.4 mm 3.2 mm i.Q. 1.0. ID I.D _____ NOTES 1. Bore of cap. .above 21 mm O.D. buIb approximately .2,fr more than bote cf cep. below bulb 2. Grind size of precision bore on 2*2 mm O.D. bulb 3. Etch and red enamel 2 lines 32 mm O.D. VISCOMETER FOR HIGH VISCOSITY NOTES ; 1. Bore of cap. above 22 mm O.D. bulb approximately .2 nun more than bore of cap. below bulb 2. Grind'size of precision bore on 21 mm 0.0. bulb 3. Elch and red enamel 2'lines FIG. 3 Hydroxypropyl Methylcellulose Viscometers apparent viscosity of 2 % water solutions of hydroxypropyl methylcellulose. The viscosities found by this test method do not necessarily correspond to values obtained from other possible test methods.43 44 45 43. Summary of Test Method 43.1 A 2% water solution of hydroxypropyl methylcellulose is measured by use of an Ubbelohde tube vis cometer. This 2 % solution is based on a dry mass of the product, for example,- corrected mass for moisture found in the moisture analysis. 44. Apparatus 44.1 Viscometer, as shown in Fig. 3. mnop 3--If a viscometer has been repaired, it should be recalibrated before it is used again. Even minor repairs can cause significant changes in the K value. 44.2 Mechanical Stirrer. 45. Procedure 45.1 Determine the moisture content of a portion of the sample. Since cellulose and its water-soluble derivatives are hygroscopic, exposure of the sample to the atmosphere should be kept to a minimum. Changes in moisture content can introduce large errors into the accuracy of the determi nation, and this step should never be omitted if precise results are desired. The suggested method is to weigh out a 2-g portion in a suitable dish, dry at 105C for 1 h, or until constant mass is obtained after cooling in a desiccator! 45.2 Correcting for the moisture content, weigh out enough of the undried' sample to give 2.000 g of solids, calculated as folows: ' ' ) ' ' Z-' Mass of sample, g = (100/( 100 - moisture content, %)J X 2 (12) Place the sample in an 8-oz (250-mL) wids-moutittbottlelThis weighing step is critical in obtaining good checks, and should be done on a good balance sensitive to.l mg. "Masses to the nearest 0.01 g will be sufficiently accurate. 45.3 Add 98.0 g of hot. water (85 to 90"C) to the-S-oz (250-mL) bottle containing the 2-g sampIe. 45.4 Agitate with a mechanical stirrer for. 10 min, then place , the bottle, in an ice bath (0 to 5Q until solution is complete (at least 20 min). The stirrer assembly, should be equipped with a one-hole stopper-or bottle cap so that no water vapor is lost during, agitation. De-ajr..the solution by some means such as centrifuging. 45.5 When solution is complete as evidenced by the absence of partially swollen or undispersed particles, deter mine the viscosity in a methylcellulose viscometer at 20 O.rC. Two precautions should be observed at this point: (1) the solution should be essentially free of air bubbles, and (2) the temperature of the material in the tube should be checked to make certain that it is actually at the bath temperature. The methylcellulose viscosity tube (Fig. 3) consists of three parts: a large filling tube with a reservoir at its lower extremity, A; the orifice tube, B; and an air vent to the reservoir, C; when B is filled, C should be closed to 362 DUP050296883 # 0 2363 prevent the sucking of air bubbles into the orifice tube, gefore the sample is allowed to flow through the orifice for jje viscosity determination, the vent C should be opened so hat the column of solution in B will flow into the reservoir linst atmospheric pressure. Failure to open C before runling the viscosity will result in false values. Calculation 46.1 Calculate the viscosity as follows: V = Kdt (13) vhere: = viscosity; cP, = viscometer constant (Note 4), = density of the sample solution at 20/20'C (Note 5), and = time for the solution to pass from the upper to the Ifii; lower mark of the viscometer, s. qrst 4--The viscometer constant is determined by passing a ndard' oil of known viscosity1 through the tube and determining the me of flow. The above equation- can then be solved for K. u vwxy <5--For routine work; the density of solutions of hydroxy- hpyl methylcellulose may be assumed to be 1.00. , v , ' ' ;- 47. Procedure 1^47.1 Determine the"pH of the viscosity solution from 15.4, using any suitable pH meter which is standardized "" bordihg to Test Method 70. ', SOLIDS! Scope Ir48;l This test method covers the determination of the fflevel of water-insoluble matter in hydroxypropyl |?hnethylcellulose. 9. Summary of Test Method 49.1 Hydroxypropyl methylcellulose is dispersed in hot l!iater and then cooled to complete sdutiori. Water-insoluble atter is settled by centrifugal force and measured volumetlly. Apparatus 150.1 Oil Tubes, graduated, long-form, 100-mL tapered KSTM, conforming to the requirements prescribed in Sec tion 3 and Fig. 1 of Test Methods D 96. 50.2 Centrifuge, capable of whirling filled centrifuge tubes at a speed that will produce a centrifugal force of 725 times gravity. 51. Procedure 51.1 Add 1.50 g of bonerdry hydroxypropyl methylcellulose to 148.5 g of 90C water in a 2>/4' by 6-in. (57 by 152-mm) bottle and agitate vigorously for about 15 min or until the material has become finely divided. Place an ice bath around the bottle and agitate the mixture until the solution is effected. This usually requires about 15 min. 51.2 Place 100 mL ofthis 1 % solution in an oil tube, cool to 10C, and centrifuge at 725 times gravity for 5 min. The solution temperature should be below 20`C when finished. Read the percent by volume of solids from the graduations on the tube. DENSITY 52. Scope 52.1 This test method covers the determination of the bulk density of hydroxypropyl methylcellulose. 53. Smnmary of Test Method 53.1 A weighed amount ofhydroxypropyl methylcellulose. is transferred to a 250-mL volumetric graduated cylinder and the graduate vibrated to settle the powder. 54. Apparatus 54.1 Vibrator--A magnetic-type electric vibrator attached to the vertical support rod of a ring stand approximately l ft (0.6 n) above the base. A condenser damp of sufficient size to hold a 250-mL graduated cylinder also shall be attached to the above rod. The base of the stand should be weighted. 55. Procedure 55.1 Place 50.0 g of powdered hydroxypropyl methyF ' cellulose in a 250-mL graduated cylinder and clamp to the ring stand support. Allow the cylinder to yibrate for 3 min; then observe the level to which the powder has contracted. 56. Calculation -* ,56.1 Calculate the density, D, as follows: . D = 50/r where r -- observed reading. "* (14) - (: * I:-. The American Society for Testing and tAaterlals 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 thoir 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 orwithdrawn. Your comments are invited either forrevision of this standard or for additionalstandards and should 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 views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 363 DUP050296884 Designation: D 2364 - 89 Standard Test Methods for Hydroxyethylcellulose1 This standard is issued under the fixed designation D 2364; 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 testing of hydroxyethyl cellulose. 1.2 The test procedures appear in the following order; Moisture Ash Viscosity Density Molar Substitution Sections 4 to 9 10 to 17 18 to 24 25 to 30 31 to 40 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: D1193 Specification for Reagent Water12 D1347 Test Methods for. Methylcellulose3 D1695 Terminology of Cellulose and Cellulose Deriva' fives3 D2363 Test Methods for Hydroxypropyl Methylcellulose3 E 1 Specification for ASTM Thermometers4 3. Purity of Reagents 3.1 Reagent grade chemicals shall be used in afi 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.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. 3.2 Unless otherwise indicated, reference to water shall be understood to mean reagent water, conforming to Specifica tion D 1193. 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 1.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2364 - 65 T. Last previous edition D 2364 - 75( 1985). 2 Annual Book ofASTM Standards, Vote 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 14.03. 1 "`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." MOISTURE 4. Scope 4.1 This test method covers the determination of the volatile content of hydroxyethylcellulose. : 5. Significance and Use 5.1 The results ofthis test are used for calculating the total solids in the sample; and, by common usage, all materials volatile at this test temperature are designated as moisture, 5.2 Moisture analysis (along with sulfated ash) is a mea sure of the amount of active polymer in the material and must be considered when determining the amount of hydroxyethyl cellulose to use in various formulations. 6. Apparatus 6.1 Ovew, gravity-convection, capable of maintaining a temperature of 105 3*C. 6.2 Weighing Bottles, low-form,. 50 mm in inside diam eter by 30 mm in height, or equivalent 6.3 Analytical Balance. 7. Procedure 7.1 Weigh 5 g of sample to the nearest 0.001 g in a tared and covered weighing bottle. 7.2 Place it in an oven at 105C for 3 h with the cover removed. Replace the cover, cool in a desiccator, and Weigh. 8. Calculation 8.1 Calculate the percent moisture, M, as follows: M=(A/B)x 100~ - " where: A -- mass loss on heating, g, and B -- sample used, g. - (1) 9. Precision and Bias 9.1 Statistical analysis of intralaboratory test results on samples containing from 1 to 6 % moisture indicate a precision of 0.2 % absolute at the 95 % confidence level. 9.2 No statement on bias can be made as no suitable reference material is available as a standard. ASH--AS SULFATE 10. Scope 10.1 This test method covers the determination of the residue on ignition of hydroxyethylcellulose after a specimen has been treated with sulfuric acid. 11. Summary of Test Method 11.1 A specimen is moistened with sulfuric acid, the 364 DUP050296885 IP! '! cess acid evaporated, the carbonaceous matter burned off, ^d the residue ignited in a muffle furnace, cooled, and eighed. Significance and Use 112.1 Excessive ash can affect solution clarity and film roperties. The ash (along with moisture) is a measure ofthe aount of active polymer in the material and must be jpnsidered when determining the amount of hydroxyethyl llulose to use in various formulations. j|. Apparatus ...................... *13.1 Dishes, platinum, 50 to 75-ml capacity, r 13.2 Muffle Furnace, maintained at 575 25C. Reagents 14.1 Sulfuric Acid (sp gr 1.84)- -Concentrated- sulfuric Icid (H2S04). 15. Procedure 15.1 Weigh, to the nearest 0.001 g, about 5 g of the dried aple into a taied platinum dish. Moisten the entire |pecimen with about 2 mL of H2S04. Then cautiously heat Over a small flame until sulfur trioxide (S03) fumes cease to ! evolved. i| 15.2 Increase the heat, ignite the specimen, and heat as |necessary to bum off the volatile matter. 15.3 Place the dish in a 575C muffle furnace for 1 b, or longer if required, to burn all of the carbon, f 15.4 Remove the dish, allow to cool somewhat, place in a desiccator, and cool to room temperature. Weigh the dish and residue to the nearest O.OQ1 g. 16.. Calculation 16.1 Calculate the percent ofash (as sulfate), C, as follows: C = (ME) x 100 (2) (where: IA = ash, g, and 12? = sample used, g. 17. Precision and Bias . 17.1 Statistical analysis of interlaboratory test results on , samples containing 2 to 5 % ash (as sulfate) indicates a precision of 0.3 % absolute at the 95 % level. I7'2 No statement on bia%cari.be made as no suitable reference material is available as a standard. VISCOSITY 18. Scope I,; 18.1 This test method, is an arbitrary method of deter mining the viscosity of aqueous solutions of hydroxyethyl- TABLE 1 Viscometer Spindies Required for Given Speeds Viscosity Range, CP 10 to 100 100 to 200 200 to 1000 1000 to 4000 4000 to 10 000 Spindle No. 1 1 2 3 4 Speed, rpm 80 30 30 30 30' Scale 100 100 100 : 100 100 Factor 1 2 10 40 200 ' cellulose in the viscosity range from 10 to 10 000 cP at 25C. 18.2 The concentration to be used for the test shall be agreed upon between the purchaser and the seller. It shall be such that the viscosity of the solution will fall within the range of this test. 18.3 The results for the viscosity of hydroxyethylcellulose by this test method will not necessarily check with results from other types of instruments used for viscosity measure ments. 18.4 The determinations are run on a calculated dry basis; that is, the amount of hydroxyethyicellulose required for the desired concentration on a dry basis is calculated from the known moisture content. . 19. Significance and Use 19.1 This test method is intended for referee purposes. The Brookfield spindles and speeds giyen in Table 1 are recommended for this purpose, but slight deviations from Table 1 may occasionally be found convenient for individual application. 19.2 This test method determines the relative ability of the polymer to thicken aqueous solutions and is therefore related to the concentration required in various formulations to achieve the desired finished product viscosity. 20. Apparatus 20.1 Viscometer, Brookfield-type.6 20.2 Container, glass jar, 12-oz (350-cm3) approximately 2 Vi in. (64 mm) in outside diameter and 6 in. (152 mm) high. 20.3 Mechanical Stirrer--Agitator as shown in Fig. I7, attached to a variable-speed motor capable of 1500 r/min. 20.4 Water Bath, constant-temperature, set at 25C and capable of maintaining that temperature ta within 0.2"G. 20.5 Thermometer--An ASTM Saybolt Viscosity Ther mometer having a range from 19 to 27*C and conforming to the requirements for Thermometer 17C, as prescribed in Specification E 1. 21. Procedure , . 21.1 Determine the moisture in accordance with Sections 4 to 9. ----- 21.2 Calculate the dry-basis specimen mass, M, in grams necessary to make 250 g of test solution as follows: M* = mA/(m-B) ' (3) where: A = desired dry mass of specimen, g, and B = percent moisture in the weighed specimen. 21.3 Add the specimen to the jar. Then add sufficient distilled water to make a total of250 g of solution. Calculate the mass of water, Afw, in grams as follows: Mw -- 250 -- S (4) where S' = sample mass, g. 21.4 Place the agitator in the solution allowing a min- 6 Model LVF, available from Brookfield Engineering Laboratories, Inc., Stoughton, MA has been found satisfactory for this purpose. 7 An agitator made with 1 Vi in. (38 mm), three-bladed propellers, No. 9240K, available from A. H, Thomas Co., P.O. Box 779, Philadelphia, PA 19105 has been found satisfactory for this purpose. 365 DU P0502 96886 < D2364 in. mm Vie 1.5 Vie 4.8 V* 6.4 9/32 7 in. Via . % IVs 9Va mm 7.9 15.8 38 241 FIG. 1 Agitator imum clearance between the agitator and the bottom of the container. Stir at approximately 1500 r/min until the spec imen is completely dissolved.' 21.5 Remove the agitator from:the motor and transfer the specimen container, with the agitator in it, to the constant temperature bath. Allow it to stand for 30 min. At frequent intervals, check the specimen temperature with a thermom eter and mix by hand with the agitator to ensure that the test temperature is reached within the 30-min time interval. 21.6 Remove the specimen container from the bath and measure the viscosity with the Brookfield viscometer, fol lowing the Brookfield operating instructions, selecting the proper spindle and speed from Table 1. Allow the spindle to rotate until a constant reading is obtained. z{|} 1--Ifthe room temperature is considerably greater or less than 25"C, the entire operation ofstirring, standing,, and measurement should be conducted with the specimen suspended in the water bath. 22. Calculation 22.1 Calculate the viscosity, V, in centipoises as follows: f=rx/ (5) where: r = reading and / = factor. 23. Report 23.1 Report the following information: 23.1.1 Results, as Brookfield viscosity at 25C, 23.1.2 Solution concentration, 23.1.3 Spindle used, and 23.1.4 Speed used. 24. Precision 24.1 The difference between the averageL of the results obtained by a given operator using a given viscometer and the average of the results obtained by a different operator using a different viscometer should not exceed 10 % of the mean of the averages. DENSITY 25. Scope 25.1 This test method covers the-determination .of the bulk density ofbydroxyethylcellulose. 26. Summary of Test Method -` 26.1 A weighed amount of hydroxyethylcellulose. is trans ferred to a 250-ml graduated cylinder and the graduate vibrated to settle the powder. 27. Significance and Use 27.1 Density can relate to dry .flow properties, rate of dissolution, lumping, packaging, and storage space require ments. ~ 28. Apparatus 28.1 Vibrator--A magnetic-type electric vibrator at tached to the vertical support rod of a ring stand approxi mately 1 ft (0.3 m) above the base. A condenser clamp of sufficient size to hold a 250-ml graduated cylinder also shall be attached to the above rod. The base ofthe stand should be weighted. 366 DUP050296887 D 2364 p| Procedure ^ 29.1 Place 50.0 g of hydroxyethylcelhilose in a 250-mL gaduated cylinder and place in the condenser clamp. Turn . the vibrator and allow the cylinder to vibrate for 3 min. |cord the level (in millilitres) to which the specimen has ipacted. 29.2 Alternatively, the specimen may be compacted manlly. Tap it on a hard surface by dropping the cylinder Jpeatedly from a height of about 1 in. (25 mm) until the jpume of the sample remains constant. In order to prevent ffinder breakage, cover the tapping surface with a Vs to -in. (3 to 6-mm) thick rubber sheet, or use a plastic aduated cylinder. Calculation IT 30.1 Calculate the density, D, in grams per millilitre as follows; it D = 50/r0 (6) Mfeie Ra = observed reading, mL. MOLAR SUBSTITUTION 31. Scope 31.1 This test method covers the determination of the molar substitution (MS) of hydroxyethyloxyethylene pen dant groups in purified hydroxyethylcellulose (HEC).8 32. Terminology 32.1 Definition: 32.1.1 molar substitution, MS--the average number of oxyethylene groups substituted onto each anhydroglucose unit (see also Terminology D 1695). 33. Summary of Test Method 33.1 In this test method, the pendant groups are cleaved from the cellulose by hydriodic add and converted to volatile 8 This test method was first published by Morgan, P. W. in Industrial and Engineering Chemistry, Analytical Edition, Vol 18,1946, p. 500. Hi' if 367 DUP050296888 0 2364 ethyl iodide and ethylene. These volatile products are col lected in alcoholic silver nitrate and bromine-bromide scrub bers, respectively. The total hydroxyethyl content is calcu lated on .the basis of the sum of both products. 34. Significance and Use 34.1 This test method determines the amount of substituent groups added to the cellulose backbone. The level can affect solution properties, rheology, solubility parame ters, and film properties. 351 Interferences 35.1 Interfering materials include glycols, low molecular weight alcohols, and salts of oxidizing acids. Presence of glycols or alcohols, or both, leads to high MS values since reaction ofthese compounds with hydriodic acid is similar to that of HEC. If present, they must be either removed dr determined separately with the results being included in the MS calculations. Large amounts .of salts of oxidizing acids also interfere giving low MS values. Ifany. such salt is,present in the HEC, its individual permissible level must be deter mined. Salts of other acids do not interfere chemically. In either case, the amount of the salt in the sample must be determined separately, in accordance with Method D 2364 69, and its percent included in the MS calculations in Section 39. 36. Apparatus 36.1 Assemble the apparatus as shown in Fig. 2- The main parts in the drawing are designated as follows: 36.1.1 Reaction Flask (A). 36.1.2 Condenser Trap (B). 36.1.3 Side Arm Absorber (C), containing silver nitrate solution to scrub out ethyl iodide. 36.1.4 Twin Spiral Tube Scrubber (D), containing bro mine-bromide solution to scrub out ethylene. 36.1.5 Test Tube (E), containing potassium iodide solu tion. 36.1.6 Heat Gun9 (not shown). 36.2 All equipment must be clean, dry and free of leaks. Use clamps or springs at all glass joint connections. 37. Reagents - 37.1 Ammonium Thiocyanate, Standard Solution (0.05 N)--Prepare 0.05 N solution using distilled water, and standardize in accordance with 8.2 of Test Methods D 1347.' 37.2 Bromine-Bromide Reagent (0.12 N)--Thoroughly mix 12 mL of liquid bromine and 60 g of sodium bromide (NaBr) in about 3600 mL of acetic acid. The resultant solution should be about 0.12 N. Store in an amber bottle in a dark cabinet. 37.3 Ferric Nitrate Indicator Solution--Prepare by dis solving 5.0 g of ferric nitrate [Fe(N03)3 9H20] in 100 mL of distilled water. 37.4 Hydriodic Acid (sp gr 1.7)--Methyoxy grade 57 % hydriodic acid (HI), without preservative. 9 Model HG50ILa, 14A, available from the Maswter Appliance Co. or its equivalent has been found satisfactory for this purpose. 37.5 Inert Gas Purge--Commercial grade nitrogen or carbon dioxide (C02). 37.6 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 37-7 Potassium Iodide Solution (100 g/L)--Dissolve, 100,, g of potassium iodide (KI) in distilled water and dilute to i L. 37.8 Red Phosphorus. 37.9 Silver Nitrate, Alcoholic. Solution (33 g/L)--Dissolve 33 g of silver .nitrate (AgN03j in 110 mL of distilled,water, and acidify with a few drops of concentrated nitric add (HN03, sp gr 1.42). Dilute the resultant aqueous solution to a total volume of 1 L using absolute ethanol.. . ~ 2--Denatured alcohol formula S.D.2B maybe used. 37.10 Sodium Thiosulfate Solution (0.1 N)--Prepare a 0.1 N solution using distilled water and standardize in accordance with Test Methods D 2363. 37.11 Starch Indicator Solution (10 g/L)--Prepare a solu tion of starch in water with a preservative. 37.12 Sulfuric Acid (1+16)--Add. 60 mL of concentrated sulfuric acid (H2S04, sp gr 1.84) to 940 mL of distilled water. 38. Procedure . 38.1 Dry the sample at 105 to 110C for 1 h; store in desiccator. . 38.2 Add approximately 0.1 g of red phosphorus to condenser trap B and add suffident water to cover the tip of the capillary (Note 3). Pipet exactly 10 mL of the alcoholic AgN03 solution to side arm absorber C. Pipet exactly 20 mL of 0.12 N bromine-bromide solution into die spiral scrubber D with the T-bore stopcock turned so that the solution will flow to both spirals. Fill the 6-in. (152-mm) tube at position E with 30 mL of the Kl solution. ~ 3--The presence of a sulfur chemical in the HEC will cause a blackening of the precipitate in the AgN03 trap. This can be overcome by using a cadmium sulfate solution (50 g/L) in place of water for suspending the red phosphorus In trap 5. - 38.3 Weigh, to, the nearest 0.1 mg, the appropriate amount of dried HEC specimen (Note 4) into reaction flask A. Pipet approximately 10 mL of HI into the reaction flask (Notes 5 and 6). Attach the flask to the assembly. Adjust the flow fate of-fire purge gas to one bubble per second or preferably to 5 cm3/min, as measured by a rotameter (not shown in drawing). Heat the reaction flask A with any suitable heat.;source to art internal temperature of 127 2C. Allow the reaction to continue to completion at this temper ature for 90 min or until the liquid in trap C is essentially dear, whichever is longer. 4--The specimen of HEC should contain about 0.0010 to 0.0015 mol of oxyethylene. Thus, approximate specimen weights for given MS levels are as follows: 0.45 g for 0.5 MS HEC; 0.26 g for 1.0 MS HEC; 0.15 g for 2 to 2.5 MS HEC; and 0.1 g for 3 or 4 MS HEC. 5--Purge the HI bottle with nitrogen during the entire time the bottle is open in order to exclude oxygen. 6--Occasionally, erratic, low MS values are obtained when a sample apparently fails to dissolve in the hot HI. This can be overcome by adding 3 g of molten phenol (USP grade, without preservative) after the HEC sample has been added. 38.4 When the specimen decomposition in flask A is completed, heat the AgN03 trap to 50 to 60C with a heat gun. Do not boil. Continue reaction conditions for 15 min maintaining a 127 2C temperature in flask A. 368 DU P050296889 d Designation: D 2438 - 89 Standard Test Method for Silica in Cellulose1 : Tfiis standard is issued under the fixed designation D 2438; the number immediately fbUowing^he designation indicates the yearbf original adoption or, in the case of revision, the year of iksl revision. A nuhaberin parenthesesindicates the year oflast 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 Silica m cellulose and is applicable to all pulps. It is designed to measure up to 200 jig of silica ($i02) in 50 mL of solution. 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 Document ;2.1 ASTM. Standard: D 1348 Test Methods for Moisture in Cellulose52 1 : 3. Summary of Test Method 3.1 The cellulose is ashed and hydrochloric acid (HC1)- soluble compounds are extracted. The ash is then fused with sodium carbonate (Na2C03) to form soluble silicates. The salt is dissolved^ acidified, and converted to a yelldw-colored complex of silicomolybdic acid. The complex is reduced to silicomolybdenum blue by treatment, with aminonaphthol sulfonic acid plus sodium sulfite (NririS03). Thri concentra tion of silica' Is determined spedrophotometrically.' When compared with gravimetric procedures for silica, the spectro- photometric method has better specificity, sensitivity, arid precision. ^ 4. Significance and Use 4.1 Low-silica specifications are required by viscose rayon processors. The general clajms are .that (I) silica may affect the filterability of viscose by: forming insoluble silicates, (2) silica and the formation of insoluble silicates can contribute to spinneret crater formation during spiiining (deposits which build up around spinneret holes to deform yam cross section and ultimately block the holes; these deposits occur on the acid-wet face), and (3) particulate silica can blind spinneret holes or pass through and cause partial or complete discontinuity in yam. 5. Apparatus 5.! Dish, platinum. 5.2 Stirring Rod, plastic. ;5.3 Spectrophotometer; for measuring,absorbance at 700 - nm. V v.,; , > ; j . .. >; f * r > 6^ Regents - ' < a 6.TPurity ofReagkttis--Reagent grade chemicals shrill be . lise'd in all teste. Unless otherwise indicated,"it-is intended I that all reagents 'Shall conform to the specifications of the 1 Committee on Analytical Reagents of the Ainericari Chefn- ical Society, where such specifications are available.3 Other ' grtides may be hsed; provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its iite without lessening the accuracy of the determination. ` 6.2 Purity of Water--U&ess otherwise itidibated, refer ences to water shall be understood to mean distilled water. 6.3 In some'cates, it may be necessary to select specific ft lots of chemicals' to avoid high blank'corrections. Minimhe ; the use of glassware; particularly avoid ft holding alkaline | solutions in glasswafe.'Storri rill reagfents in plastic bottles. ; 6.4 l-Arhino-2-Naphthol-4-Suifomc Acid Solution--Dk-- ft solve 7 g of anhydrous sodium sulfite (Na2S03) in 10U mL Of ft! water. Add 1.5 g of l-amino-2-naphthol-4-sulfonic acid, ft Dissolve 90 g of sodium bisulfite (NaHSO~3) in 800 mL of 'ft water. Blend the two solutions and filter through'a double 3 thickness of an acid-washed general purpose .filter paper into | a 1000-mL volumetric flask. Dilute to volume. . . -.. W . 1.--Some batches of commercial arninonaphtholsalfonic acid) * are incompletely soluble or produce dark-colored solutions. These are a not satisfactory fot silica analysis. The reagent solution should always be M discarded jf .a dark colqrappeajs with age.. Stability of the solution is jfl improved, by refrigeration and protection from-light.-- - ft ,, 6,5 Ammonium Molybdate Solution--Dissolve 100 g of 1 ammonium heptamoiybdate"((NH4)6' Mo7b23'4H20) in ap- f proximately 800 mL of water.- Adjust to a pH of 8 by adding | Sodium hydroxide (NaOH)i Dilute to lOOOTriL. | If necessary, filter the ammonium molybdate solution. With the pH adjusted to 8, the reagent is stable indefinitely. If the pH adjustment is not made, a precipitate will form on standing and the solution must be discarded. The added NaOH can be a significant source of Si02 contamination. Use a 50 % NaOH solution that has not been in glassware. About 35 mL of this solution are required for 1000 mL of molybdate solution. 6.6 Hydrochloric Acid Solution A--Dilute 1 volume of concentrated hydrochloric acid (HC1, sp gr 1.19) with 1 volume of water. Determine the volume of this acid that is required to adjust the pH of a solution of 1 g of sodium I ;j | j ft i; 1 This test method is under the jurisdiction of ASTM Committee D-! on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.36 on Cellutosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2438-65. Last previous edition D 2438 - 68 (1985)ei. 2 Annual Book ofASTM Standards, Vol 06.02. 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." DU P050296890 0 2438 iarbonate (Na2C03) In 15 mL of water of 4. 6.7 Hydrochloric Acid, Solution B--Dilute 150 mL of incentrated HC1 to 1000 mL with watet. Determine the _ olume of this acid that is required to adjust the pH of a ^solution of 1 g of Na2C03 in 15 mL of water to 4. 6.8 Oxalic Acid Solution (100 g/L)--Dissolve 10 g of |xalic acid (H2C204-2H20) in water and dilute to 100 mL. lj 6.9 Silica, Standard Solution--The standard solution imay be prepared from Si02 or silicic acid (ri2Si03). In either Jfcase, add about 0.5 g of material to a platinum crucible and ^dehydrate by heating in a muffle furnace at 1050 to 1100C, * ir 1 h. Cool in a desiccator and, without delay, weigh 0.1000 of the dry sample into a platinum crucible. Add 1.00 g of ja2C03 to the dish, and fuse in a muffle furnace at 850 to $tOOC. Hold in the melted state for at least 5 min and swirl Iccasionally to ensure complete mixing of the silica and the .. (used carbonate. Allow to cool, add water to dissolve the * laelt, and transfer quantitatively to a 1000-mL volumetric (flask. Dilute to volume, and transfer to a plastic bottle for lorage. Discard after 7 days. The standard solution contains i` the equivalent of 100 pg of Si02/mL. ; 6.10 Sodium Carbonate--Granular solid anhydrous so lium carbonate (Na2C03). Select a lot that does not contain pore than 20 ppm of Si02 by this test method. ||7. Test Specimen l 3 7.1 Select a specimen weight, on the basis of the anticipated silica level in the pulp, to provide 500 jog, or more, of Si02. Weigh out a second specimen for determination of inoisture in accordance with Test Methods D 1348. 8. Procedure ; 8.1 Weigh the specimen into a platinum dish. Ash in a Imuffle furnace at 575 25C. Cool the ash, add 10 mL of |HC1 Solution A, and simmer on a hot plate (under a hood). ilContinue heating until all of the acid has evaporated and the $|dry residue has been baked for at least 10 min. Add a small volume of water to dissolve the soluble chlorides. Heat, and Jstir with a rubber-tipped or plastic stirring rod. Filter through Jgn ashless, medium-speed filter paper and discard the filtrate. fSlace the filter paper in the original platinum dish, and ignite |ln the muffle furnace at 575C. 8.2 Cool the dish, add 1.00 g of solid Na2C03, and melt in 1 a muffle furnace at 850 to 900C. Swirl gently to wet all the Bash with the melt. Hold in the melted state for 5 to 6 min. I Remove the melt from the furnace, allow to cool, and add |approximately 15 mL of water. Stir with a plastic rod until isolution is complete, transfer quantitatively, without filtra|tion, to a 50-mL flask, and dilute to volume. There may be a (small amount of insoluble carbonate which will settle rapidly. Without delay, transfer an aliquot that is expected to ^contain not more than 200 pg of Si02 to a 50-mL volumetric ** |flask. The volume of this aliquot must not exceed 25 mL. ^Immediately add 5 mL of HC1 Solution B plus the calculated ijvolume of HC1 Solution A or B that would be required to til. adjust the amount of carbonate contained in the test aliquot Li- to pH 4. The total volume at this stage must not exceed 35 mL. When small specimen aliquots are used, add water to bring the volume to 25 to 35 mL. 8.3 A reagent blank is required. Prepare for the blank by ladding 5 mL of HCl Solution B to approximately 25 mL of water in a 50-mL volumetric flask. 8.4 For each series of analyses, prepare a color standard equivalent to 200 pg of Si02. Prepare for the standard by adding 2 mL of the standard silica solution to a 50-mL .yplumetric flask. Dilute to approximately 25 mL and add 5 mL of HCl Solution B. 8.5 A correction fbr silica in Na2C03 is also required. Fuse 1 g of Na2C03 as though it were a specimen. After cooling, dissolve in a small volume of water and transfer to a 50-mL volumetric flask. Immediately add HCl Solution A to adjust to pH 4, then add 5 mL of HCl Solution B. Do not dilute beyond 35 mL. Develop color in this flask as described in 8.6. 8.6 Develop color in the blank, Na2C03, standard, and test solutions as follows: 8.6.1 Add 5 mL of ammonium molybdate solution and allow to stand at room temperature for 20 min. 3 A yellow-colored complex of silicomolybdic acid forms at this stage. If this color does not occur in the presence of silica, the pH control is not correct. Solutions must be at a pH of 0.9 to I before addition of the ammonium molybdate reagent and a pH of 1.1 to 1.3 following addition of this reagent. 8.6.2 Add 2 mL of oxalic acid solution, followed by 5 mL of amino naphthol reagent, dilute to volume with water, and mix well. 8.6.3 Allow to stand at room temperature for 20 min. 8.7 Within 1 h after color development, read the absorbance of all solutions against the reagent blank with a spectrophotometer at 700 nm. 8.8 Prepare a standard curve of absorbance versus con centration by drawing a straight line through the origin and the observed value of the 200-pg standard. Convert all absorbance values for test solutions to Si02 weight units by reference to this curve. 9. Calculation 9.1 Calculate the parts per million of Si2 in the pulp as follows: ----- Si02, ppm = [(50/1/5) - C]/W where: A - Si02 in the aliquot, pg, B = aliquot, mL, C = Si02 in the Na2C03, ppm, and W = dry specimen, g. 10. Report 10.1 Report the result to the' nearest part per million. Random replicate determinations should not differ by more than 10 % of the observed value. 11. Precision and Bias 11.1 A precision of less than 10 % relative is found by replicate runs by a single analyst. 11.2 No statement of bias can be made as no suitable reference material exists for determining bias. 371 DUP050296891 # D 2438 The American Society tor Testing amt 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 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, eitherreapproved or withdrawn. Your comments are Invitedeither forrevision ofthis standard or for additional standards and should ba addressed to ASTM Headquarters. Your comments will receive careful consideration at a meettng 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, 191B Race St., Philadelphia, PA 19103. he 372 DU P050296892 Designation: D 2448 - 85 (Reapproved 1989) Standard Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment1 This standard is issued under the fixed designation D 2448; 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 rcapprqval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. j Scope jjl-.l This test method covers, the, determination of the gecific, resistance of the aqueous leachate from a pigment as index of water-soluble salt content This test method is iplicable to white pigments and colored pigments (organic nd inorganic). The water-soluble salts content is a function ' the specific resistance of the solution formed by extracting pigment with water. 1.2 Ibis test method is based on a water to pigment ratio if 9+1. The leachate yield (minimum 160 mL) sufficient for insing the cylinder dip, cell and thermometer plus the aimmurn 80 mL required for the measurement to deteriine the quantity Of pigment to be used. 1.3 This standard may involve hazardous materials. Oper ations, and equipment. This standard does not purport to ddress all ofthe safety problems asso'ciated withits use: It is *<ie responsibility Of the user of ihiZ standard W establish Impropriate safety and health practices and deterrfiinethe t'Ouse.' - Referenced Document ,,, 2.1 ASTM Standard: D1193 Specification for Reagent Water2 . Summary of Test Method , 3.1 A weighed quantity of pigment is added to water and oiled. For hydrophobic pigments methyl alcohol'is used to7' adlitate wetting. After filtration, the specific resistance of he filtrate is determined using a conductivity bridge. Significance and Use - * 4.1 This test method provides a reliable means for the etermination of the relative amounts of these salts when Comparing different lots of the same pigment grade. Water|oluble salts also affect the water resistance and blister resistance of coatings, especially primers for steel. Conduc tivity measurements, however, cannot be used as the only bethod to determine and compare the amount of water Soluble salts of pigments with the same chemical composi tion but produced by different manufacturing processes. 5. Apparatus 5.1 Centrifuge (optional), having a 500-mL capacity per cup. ` 5.2 Filter Paper (Note !) --For high reliability avoid use of filter paper containing soluble material. Each filter should be washed with reagent water in the funnel until resistance of the filtrate is greater than 200 000 ft cm. I--The, size of the filter paper wifi be determined by how voluminous the pigment is. Some organic pigments require at least a 1`85-mm paper fob'proper filtering. 5.3 Filter Aid(optional)--The use.of a filter aid may be desirable with sprite jp%iheftts to improve filtration. How ever, the filter aid must' be treated to meet the same specifications for filter paper as given in 5.2. 5.4 Ungraduated Cylinders, approximately 35 mm wide by 125 mm deep. 1 5.5 Thermometer, graduated in 0.2C intervals. . 5.6 Conductivity Bridge? 5.T Conductivity tCd/A3 having a cell constant, K; of 1. The ttell constant recommended for various ranges of electrolytes is*as follows: " 5.7.1 For specific resistances' of less than 250 ft cm, use a cell with a constant of 10 or more. t 5.7.2 For specific resistances from 250 to 200 000 ft-cm, use a cell with a constant.of 1. This covers the range for most pigments. 5,7-3 For specific resistances of reagent water or of over 200 000 Q-cm, use'a cell with a constant of Q,J. 6. Reagents 6, f Purjty 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 *O*ther 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 grade water as defined by Type II of Specification D 1193. 6.3 Methanol. \ 1 This test method is under the jurisdiction.of ASTM Committee D-L on Paint fnd Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.3I on Pigment Specifications. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 2448 - 66 T. Last previous edition D 2448 - 73 (1979)'1. 2 Annual Book ofASTM Standards, Vols 06.03'and 11.01. 3 Any commercially produced conductivity bridge and conductivity ceil is satisfactory. 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." 373 DUP050296893 0 D 2448 6.4 Potassium Chloride, Standard Solution (0.02 N)-- Prepare a 0.02 N potassium chloride (KC1) solution with water by dissolving 1.491 g of KC1 (heated before weighing for 1 h at 105C) in water, followed by dilution to 1 L. 7. Determination of Cell Constant 7.1 Prepare a 0.002 N solution of KC1 by diluting the 0.02 N KC1 solution described in 6.4 with water. Cool and measure the specific resistance, Rm, at 25 0.5C as described in 8.2.2. 7.2 Calculate the cell constant, K, as follows: K2S = {RJRS) where: Rm = specific resistance at 25C (see 8.2.2), and Rs = specific resistance in ohm centimetres of an 0.002 N KCI solution at 25C (Table 1) = 3427 Q*cm. 2--In general the "cell constant" is not greatly affected by variations in the strength of the K.C1 solution, but for greatest accuracy, measurements should be made at or near the specific resistance of the solution to be measured and at values that utilize the medium range of the scale of the conductivity bridge, using the same multiplier tap. 7.3 The specific resistances of KCI solutions are shown for concentrations from 0.001 N to 0.073 iV at 25 C in Fig. 1. This curve, almost a''straight line, was made from published values of specific conductances aind equivalent conductances of KCI solutions at 25 C. Table 1 gives values of the specific resistances of KCI solutions for those concentrations useful for pigment testing. 8. Procedure ' 8.1 Hydrophobicity Test--Test a small amount of pigment with boiling water to see if it ii^water-wettable. Pigments that do not wet well with water are probably hydrophobic and should be treated as described in 8.3. If, the pigment wets TABLE 1 Specific Resistances of Solutions of Potassium Chloride at 25C Normality !2-cm 0.001 0.002 0.005 0.01 0.02 6802 (1) 3427 (1) 1393 {1) 707,3 (1,2) 361.5(3) easily, proceed as described in 8.2. 8.2 Hydrophilic Pigments: 8.2.1 A 20.0-g specimen weight is usually sufficient for pigments easily wet with water. Add 20.0 g of the pigmeht to 180 g ofboiling water in a tared, 400-mL beaker with stirring rod. (Usually a 250-mL beaker is sufficient for white pig ments. Some white pigment, because of tendency to foam and crawl, can be handled better in a larger beaker. Usually 20-g specimens of organic pigments require a 600-mL beaker to allow adequate room for foaming. Boil slowly for 5 min with occasional stirring. Cool to about 60"C and add water to bring the net weight back to 200 g. Stir thoroughly. Filter directly through fine-texture paper (Note i) or separate the solids by centrifuge using clean, dry cups, or cups washed with some of the slurry, followed by decanting the superna tant liquid through a filter. In either case discard the first 10 mL through the filter. 8.2.2 Cool the filtrate to about 20C. Rinse the footed, cylinder and the conductivity cell, previously rinsed with water, with, the leachate. Fill the footed cylinder with the leachate to be measured anfi place the conductivity cell into the leachate. Move the dip cell up and down to remove all air bubbles. Adjust the temperature slowly to 25C and, with the cell submerged so that the vent is `A in. (12.7 mm) beldw the FIG. 1 Specific Resistance of Potassium Chloride at 25C 374 DUP050296894 0 2448 ace of the liquid and centered upright in the cylinder, ake at least five measurements of the specific resistance at 0.5C, using the conductivity bridge with the multiplier ' to give a reading near the center ofthe scale, following the actions supplied with the instrument to obtain a balCe. J8.3 Hydrophobic Pigments--A modification of the proce- : given in 8.2 is necessary for organic pigments that are |t easily wet with water. Wet 30.0 g of pigment with 5 to 20 pf alcohol, as required, to produce a smooth wet paste, mplete the addition ofwater to bring the net weightto 300 by diluting with boiling water in a tared beaker (1000 mL 1 been found satisfactory), with a stirring rod. Boil, cool, "er, and determine the reading as outlined in 8.2.2. Calculation 9.1 Calculate the specific resistance, R25, in ohm centi metres, of the pigment at 25C by taking the mean Ra, of the five or more readings made and divide by the cell constant, K, determined in accordance with Section 7. 10. Precision and Bias 10.1 On the basis of a laboratory study ofthis test method, the following criteria should be used for judging the accept ability of 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 5 % for white pigments and 7 % for colored organic pigments. 10.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 10 % for white pigments and 15 % for colored organic pigments. 5 10.2 Bias--Bias has not been determined for this test method. 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 (his 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. : W- 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 commentsare 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 corrimltfea, 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. 375 DUP050296895 Designation: D 2455 - 89 Standard Test Method for identification of Carboxylic Acids in Alkyd Resins1 This, standard is issued under the fixed designation D 2455; 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 qualitative determination of the carboxylic acids ;in alkyd resins, including resinmodified alkyds. It may be used for analyzing polyesters but additional peaks may appear from monomers such as styrene.. 1.2 The constituents of three resin samples have been correctly identified in collaborative work by three laborato ries. It is apparent that quantities as low as 1 % can readily be detected. 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: D1193 Specification for Reagent Water12 D2245 Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints3 3. Summary of Test Method 3.1 The resin specimen is subjected to rapid transesteri fication with lithium methoxide to form methyl esters that are separated by programmed temperature gas-liquid chro matography on polar and nonpolar columns, then identified by their retention relative to a standard. If the presence of maleic or fumaric acids is indicated, an alternative trans esterification with boron trifluoride is necessary. 4. Significance and Use 4.1 The presence of carboxylic acids in alkyd resins has a direct effect on the crosslinking capability of the resin. This test method helps the user determine the reactivity of the resin. 5. Apparatus 5.1 Linear Programmed Temperature Gas Chromato graph--Any instrument with programming features should be suitable if equipped with a hot-wire type of detector and 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 D01.33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally published as D 2455 - 66. Last previous edition D 2455 - 69 (1981)**. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Bock ofASTM Standards, Vol 06.03. adaptableto the following operating conditions: Detector cell temperature, *C Detector cell current, mA Injection port temperature; *C Helium flow at exit, cm3/min Programmed temperature details: Approximate column heating rate, 7min Starting column temperature, C: Polyesfef-Carbowax Silicone grease, DC-11 Finishing.column temperature, C: Pdyester-Carb'dwax.. ' Silicone greate, DC-11 3<kl . ISO--" 330. 85 4.0 125 75 225 250 5.2 Columns: 5.2.1 Polar---Bend a 6-ft (1.8-m) length of`A-in. (6.4-mm) copper tubing into a U*shape and fill one side with 20 % Carbowax 20M4 on acid-washed 60 to 80-mesh Chromosorb WA and fill the other side with 20 %. diethylene glycol succinate on the same solid support. Maintain constant vibration during the filling and add small amounts of the packing material alternately to each side. Condition at 225C until "bleeding" reaches a minimum. Mount this column so that the sample passes first through the polyester section. Two 3-ft (0.9-m) sections, packed separately and joined together may be used if preferred. ^ 5.2.2 Nonpolar--Pack a 6-ft (1.8-m)Tength of `A-in. (6.4- mm) copper tubing with 20 % silicone grease on acid-washed 60 to 80-mesh Chromosorb W.s Condition at 250C until "bleeding" reaches a minimum. 5.3 Syringe, having a fixed needle, 10-pL capacity. 5.4 Separatory Funnel, 250-mL. 5.5 Steam Bath. - 6. Reagents' 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests (See Section 7). Unless otherwise indicated, it is intended that all reagents shall conform to the specifica tions 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 determi nation. 6.2 Purity of Water--Unless otherwise indicated, refer- 4 Carhowax 20M is a trademark of Union Carbide Corp., 39 Old Ridgebury Rd,, Danbury. CT 06817. s Chromosorb W is Manviile Sales Corp., Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108. 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." 376 DUP050296896 # D2455 ; TABLE 1 Relative Retention Data for Methyl Esters of Some Carboxylic Acids (Formed by Lithium Methoxide Transesterification) m Triacetin -- 1 -Methyl Ester of Acid 6-ft (1.8-m) Poly- 6-ft (1.8-m) Silicone ester-Carbowax Grease 'elargonlc Succinic ienzolc jrthotoluta Tumaric laielc luric idipic laconic pycolio rtertiary butyl benzoic Syriatic etrahydrophthaiic ifeWe ffllmltlc Sebaclc rerephthalic Srthophthalic iophthalic Stearic leic jnoleic Inolenic 0.23 0.44 0.47 0.49 0.63 (0.38)* 0.64 (0.52)'* 0.66 0.71 0.74 0.79 0.83 0.90 0.97 1.08 1.14 1.19 122 126 1.26 1.3$ 1.41 1.49 1.60 0.33 0.49 0.62 0.76 0.69 (0.49)A 0.68(0.47)* 1.29 0.63 0.83 0.70 1.16 1.55 1.07 1.31 1.79 1.43 1.23 1.17 1.26 2.02 1.98 1.98 1.98 < * When transesterlfiecl with boron trtfluoride in methanol. Ices to water shall be understood to mean reagent water as Mined by Type IV of Specification D 1193. i 6.3 Boron Trifluoride Gas. 6.4 Lithium Methoxide in Methanol--AM small pieces of Metallic lithium, about the size of a small pea, one at a time 0 a flask containing absolute methanol which is chilled in an be bath. Periodically titrate a few millilitres with standardbed add until the normality reaches 0.5 or more. If the formality exceeds 0.5, add a calculated amount of absolute nethanol to adjust the reagent to 0.5 N. Filter before each lie. Keep tightly stoppered; it may be necessary to discard liter one month. 1 6.5 Methanol, absolute. 16.6 Methylene Chloride. 6.7 Sulfuric Acid (1+5)--Carefully mix 1 volume of conlentrated sulfuric add (H2S04, sp gr 1.84) with 5 volumes of ^ater. 6.8 Triacetin. f. Hazards 7.1 The reagents and samples used in this test method pay, under some conditions, be hazardous. Refer to the manufacturer's Material Safety Data Sheets for specific fandling and safety precautions. Safe laboratory procedures and all applicable OSHA regulations are to be followed.I I Procedure | 8.1 Pour into a 125-mL flask, a spedmen of resin Containing approximately 0.3 g of nonvolatile material (Note | and add 15 mL of the 0.5 N lithium methoxide reagent. Idd an antibumping stone, attach a short air condenser, and )lace on a steam bath. Swirl constantly until solution is Ifected; then boil for 2 min. Remove the flask from the bath fomptly at the end of the timed 2-min period, remove the Condenser, and add 5 mL of H2S04 (1+5) at once. Transfer the contents of the flask to a separatory funnel and dilute to 50 mL with water. Add 35 mL of methylene chloride and shake vigorously. Separate and wash the solvent layer with 15-mL portions of water until all sulfuric acid is removed; then withdraw the solvent into a small beaker. Place the beaker in a warm water bath and remove as soon as all ofthe solvent has been expelled. If solid methyl esters are present, add tetrahydrofuran dropwise with warming until all or most of the specimen has dissolved. 1--Drying of the resin solutions is not usually necessary, but interference may come .from a few high-boiling mineral solvents. They can he removed by dissolving the specimen in 3 mL of chloroform or acetone, drying the specimen with a current of air in a warm water bath, redissolving, and redrying about three times. 8.2 Mount the 6-ft (1.8-m) polyester-Carbowax column in position so that the specimen will pass first through the poly ester side and heat the column to starting temperature. Pick up about 5 pL of specimen in the syringe followed by approximately 0.2 pL of triacetin and introduce onto the column. Engage the mechanism for increasing column temperature immediately. When maximum column temper ature is reached, maintain the temperature until all compo nents emerge. Obtain a chromatogram in like manner with only the triacetin. 8.3 Repeat the chromatographic separation with the 6-ft (1.8-m) silicone grease column following the operating con ditions described for this column in 5.1 and obtain a separate chromatogram with only the triacetin. 9. Identification 9.1 Calibration is always recommended and can be made directly with known methyl esters or by treating known esters as described in 8.1 (Note 2). In most cases, the peaks can be identified by their relative position on the chromatograms from the data given in Table 1, in which relative retention is calculated from the position of triacetin which should emerge between 20 and 25 min from the air peak under the condi tions described. 2--The acids maleic, fumaric, and itaconic do norform true methyl esters when treated as described in 8.1 so that their esters cannot be used directly for calibration; treatment with boron triiluoride will be necessary. Adducts of maleic and fumaric acid will not be "detectable under any conditions. 9.2 Since maleic and fumaric acids have the same relative retention, distinction can be made only by repeating the transesterification and substituting concentrated boron tri fluoride in methanol as the catalyst, using 5 mL of reagent and boiling for 5.0 min. Prepare the catalyst by bubbling the gas into a flask containing chilled absolute methanol until the titration of 1 mL ofthe reagent, when diluted with 2-5 mL of methanol, uses 11 to 12 mL of 0.5 N KOH in methanol, titrating to the yellow end point with thymol blue indicator solution. At the end of the 5-min reflux, transfer the specimen to a separatory funnel with 50 mL of water and 35 mL of methylene chloride and shake vigorously. Filter the methylene chloride layer (no washing is necessary) and evaporate. Obtain a chromatogram of the resultant mixed esters as before and calculate their retention relative to triacetin. Identify from Table 1. 377 DUP050296897 #: D2455 9.3 Since fatty acid .methyl esters are eluted it may sometimes be possible to identify the drying oil present in the sample, but a more precise method. Method D 2245, based on quantitative calculation of the fatty acid composition is recommended, 10. Precision and Bias 10.1 No statement is made about either the precision or bias since the results of this test method are qualitative rather than quantitative. 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 lime by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved,or withdrawn. Your comments are invited either forrevision ofthis standardor 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., 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. 378 DUP050296898 Designation: D 2458 - 91 Standard Test Method for identification of Polyhydric Alcohols in Alkyd Resins1 This standard is issued under the fixed designation D 2456; the number immediately following this 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 reappravai. Scope 1.1 This test method covers the qualitative determination the polyols in alkyd resins, including resin-modified ds. It may be used for analyzing polyesters, but addi- bnal peaks may appear from monomers such as styrene. 1.2 The constituents of three resin samples have been fbrrectly identified in collaborative work by five laboratories. Jiiantities as low as 1 %, obtained by blending samples of ittown composition, were readily detected. fe'1.3 This standard does not purport-to address the safety piblems associated with its.use. It is the responsibility ofthe per of this: standard to. establish appropriate safety and iealth practices and determine the applicability ofregulatory `imitations prior to use. For a specific hazard statement, see lection 7. it;- '. 2. Referenced Document 2.1 ASTM Standard: ,sD 1193 Specification for Reagent Water2 , Summary ofTest Method ,, 3.1 The. resin specimen is subjected to aminolysis to form pnides of the carboxylic:acids and to release the.polyols, resent, followed by direct acetylation with acetic anhydride, 'he acetates are extracted and then separated by application of programmed;temperatUre gas chromatography. Significance and Use " . .. i 4.1 The types of polyhydric alcohols used in the synthesis of alkyd resins has a direct effect on crosslinking capabilities 'Of the resin. This test method helps determine the reactivity Of the resin. 5. Apparatus 5.1 Linear Programmed Temperature Gas Chromate- . graph--Any instrument with programming features should be suitable if equipped with a thermal conductivity detector (TCD)3 and adaptable to the following operating conditions: Detector cell temperature, 'C Detector ceil current, mA Injection port temperature, "C Helium flow at exit, cm3/min 300 150 330 60 Programmed temperature details:. Approximate column heating rate, deg/min Starting cohmurtemperature, C Finishing column temperature, C ... 7.9 50 22$ 5.2 Columns (Note ' 1)--A 4-ft (1.2-m) length of `A-in. (6.4-mm) outside diabfeter copper tubing packed with 10 weight % of Carbowax 20M4 on 60 to 80 mesh Chromosorb W-AW,5 and conditioned at 240C until "bleeding" reaches a minimum. 1--Commercially available columns may be selected mid used provided they are capable of performing operations equivalent to the columns specified in this test method. 5.3 Syringe, having a fixed needle, 10-pL 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 available6 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 as defined by Type IV of Specification D 1193. 6.3 Acetic Anhydride. 6A n-Butylamine, boiling-point 76 to 78C. 6.5 Chloroform. 7. Hazards ~ 7.1 The reagents and samples used in this test method may, under some conditions, be hazardous. Re% to the manufacturer's Material Safety Data Sheets for specific handling and safety precautions. Safe laboratory handling procedures and all applicable OSHA regulations are to be followed. 8. Procedure 8.1 Weigh a sample of resin containing not less than 1.0 g of nonvolatile material into a 125-mL flask (Note 1) and add 6 mL of n-butylamine. Reflux under a water-cooled con- 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 D01.33 on Polymers and Resins. Current edition approved Jan. 8, 1991. Published February 1991. Originally published as D 2456 - 66. Last previous edition D 2456 - 89. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 'Thermal conductivity detector is adequate 'within the scope of this test method. However, a flame ionization detector (HD) may be used if desired without compromising results of the analysis. 4 Carbowax 20M is a trademark of Union Carbide Coip-, 39 Old Ridgebury Rd,, Danbury, CT 06817. 5 Chromosorb W-AW is manufactured by Manville Products Corporation, Lompoc, CA and is available from most sources of chromatography supplies. 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." 379 DUP050296899 denser for 1 h. Cool and add 25 mL of acetic anhydride slowly and cautiously through the top of the condenser and reflux the mixture for 90 min. Cool, add 35 mL ofwater, boil for 5 to 10 min, and cool. Transfer to a separatory funnel, filtering if necessary, using water sparingly for the transfer. Extract twice with 25-mL portions of chloroform, shaking vigorously for each, extraction. Combine the chloroform extracts and wash with SO-mL portions of water until acid-free. Filter through rapid paper freshly dampened with chloroform, collecting the filtrate in a 250-xnL beaker. Reduce the volume to 5 or 10 mL by evaporating the solvent with a current of air in a warm water bath (Note 3). 2--Drying of the resin solution is not usually necessary but interference may come from a few high-boiling mineral solvents. They can be removed by dissolving the specimen-in 3 mL of chloroform or acetone, drying the specimen with a current of air in a warm water bath, redissoiving, and, redrying about three times. 3--If ail the chloroform is expelled, there is a danger of losing some of the lower-boiling polyol acetates. 8.2 Inject approximately 5 pL of the remaining specimen into the chromatograph, using the operating conditions tabulated in 5.1 and holding the temperature at 225C at the completion of the program until all the volatile components have emerged. 9, Identification 9.1 Calibration is always recommended and can be made with polyol acetates or by treating known polyols in accord ance with 8.1. In most cases, the peaks can be identified by their relative position on the chromatogram from the data given in Table 1, in which the relative retention is calculated TABLE 1 Relative Retention Data for Polyol Acetates Acetate of Polyot Relative Retention Time (Second Reagent Peak = i) 2.3- Butylene glycol Propylene glycol Ethylene glycol 1,34jutylene glycol Neopentyl glycol 1.4- Butanediol Dipropylene glycol Diethylene glycol Glycerol Trimethylol ethane Trimethylol propane Triethylene glycol"' (o-Phthalic add derivative) Pentaerythritol Mannitol Sorbitol 0.70 0.72 0.78 0.82 0.84 0.98 1.05 1.16 1.24 1.33 1.37 1.43 (1.54) 1.81 3.08 3.24 from the second of the two peaks that are produced by the r-e--a--g-e--n.-ts---w- :h--i-c-h----ajppear bjetweein-~14 iandi 16 min under the 10.1 The precision and bias for this test method has not been determined, 11. Keywords 11.1 alkyd resin; aminolysis; gas chromatography; ester resin; polyhydric alcohol; polyol; polypi acetates 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 ifnetrevised, either reapprovedor withdrawn. Yourcomments 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 19703. .. 380 DUP050296900 1 Designation: D 2572 ~ 91 Standard Test Method for isocyanate Groups in Urethane Materials or Prepolymers1 This standard is issued under the fixed designation D 25-72; 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 ;i: superscript epsildn () 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 7421 ofFederal Test Method f- ' StandardNo. MlA. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been-adopted by tr the Department ofDefense. h Scope I' 1.1 This test method covers the determination .of the isocyanate group (NCO) content of a urethane intermediate or prepolymer. 1.2This standard does not purport to address all of the Safety problems, if any, associated with its use. It is the iresponsibility ofthe user ofthis 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 8. 2. Referenced Document 2.1 ASTM Standard: D 841 Specification for Nitration Grade Toluene2 3. Summary of Test Method : 3.1 The urethane prepolymer is allowed to react with an excess of di-H-butylamine in toluene (Note 1). After the Ireaction is complete, the excess of di-n-butylamine is deter mined by back titration with standard hydrochloric acid. 1--Solvents other than toluene may be needed in some cases, for example, anhydrous dimethylformamide (DMF), but the procedure `has not been evaluated using them. 4. Significance and Use .. 4.1 The percent NCO is used to establish unit ratios for stoichiometric reactions with co-reactants. |5. Interferences I 5.1 Phosgene, the carbamyl chloride of isocyanate, hydroJ |en chloride, or any other acidic or.basic impurities of suffi- 1 icient strength will interfere. The concentration of these com- I pounds is usually sufficiently low that their effect on the I determination is negligible. 6.Apparatus 6.1 Polyethylene Stoppers (or corks) covered with alumi num foil to fit 250-mL Erlenmeyer flasks. 6.2 Magnetic Stirrer with TFE-fluorocarbon-covered stir ring bar. 6.3 Pipet,3 25-mL. 6.4 Buret,3 50 or 100-mL. 6.5 Analytical Balance. 7. Reagents 7.1 Purity ofReagents--'Rsaigenx 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 that it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the deter mination. 7.2 Bromphenol Blue Indicator, prepare solution 0.1% by mixing 0.10 g of acid, nonwater soluble bromphenol blue with 1.5 mL of0.1 N sodium hydroxide solution and diluting to 100 mL with distilled water. 7.3 Di-n-butylamine Solution, 0.1 N in dry toluene. Not standardized. 7.4 Hydrochloric Acid Solution, 0.1 N standardized using bromphenol blue indicator solution. 7.5 Isopropyl Alcohol. 7.6 Toluene, anhydrous, conforming to Specification D 841 or equivalent dried with molecular sieve pellets. 8. Hazards 8.1 Diisocyanates are strong skin irritants and sensitizers: They are also hazardous to the lungs. (TLV for toluene 2,4diisocyanate is 0.02 ppm.) Avoid contact with skin, eyes, and clothing, and avoid breathing these substances. -Use with adequate ventilation. In case of contact, wash with plenty of water and flush eyes for 15 min. Call a physician before re use. See Supplier's Material Safety Data Sheet for additional information. 9. Procedure 9.1 Weigh to 0.1 g a specimen containing approximately 1.1 milliequivalents ofNCO (for example, 1.0 g ofprepolymer containing approximately 5 % NCO) in a 250-mL Erlen meyer flask. 1 This test method is under the jurisdiction of ASTM Committee D-J 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. 15, 1991. Published December 1991. Originally `published as D 2572 - 67 T. Last previous edition D 2572 - 87. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Burets and pipets shall conform to National Institute of Standards and Technology tolerances. 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." 381 " DUP050296901 # D 2572 9.2 Add 25 mL of dry toluene (Note 2), place a stopper in the flask, and swirl by hand or on a mechanical agitator to dissolve the prepolymer. Solution may be aided by warming on a hot plate. 2--If the polymer is insoluble, add 10 mL' of dry, analytical grade acetone to the toluene. 9.3 Using a pipet, add 25.00 mL of 0.1 Ndi-n-butylamine solution and continue swirling for 15 min with stopper in place. 9.4 Add 100 mL of isopropyl alcohol and 4 to 6 drops of bromphenol blue indicator solution. Titrate with 0.1 N hydrochloric add to a yellow end point. 9.5 Run a blank titration including all reagents above but omitting the specimen. 10. Calculations 10.1 Calculate the NCO content as follows: NCOi - x^.x 0:0420] x 1QQ where: B = volume of HCI for titration of the blank, mL, V = volume of HCI for titration of the specimen, mL, N = normality of HCI, 0.0420 = milliequivalent weight of the NCO group, and W = grams of spedmen weight, g. 11. Precision and Bias 11.1 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 0.11 % absolute NCO. 11.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 0.4 % absolute NCO. 12. Keywords 12.1 Toluene, 2,4-diisocyanate based intermediate; tol uene, 2,4-diisocyanate based prepolymer, urethane interme diate; urethane prepolymer The American Society tor 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 infrlngsment 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 onStandards, 1916 Race St., Philadelphia, PA 19103. 382 DUP050296902 p IS lb Designation: D 2641 - 39 Standard Test Method for Chlorine in Cellulose*1 This standard is issued under the fixed designation D 2641; 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 This test method2 covers the determination ofchlole in cellulose. Procedures for total chlorine, water insolle chlorine, and alcohol-benzene insoluble chlorine are scribed. The range is 5 to 1000 ppm on cellulose. Total lorine determinations (including ashing) can be performed a rate of one determination every 30 min. 1.2 This standard may involve hazardous materials, operIitions, 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. I I. Referenced Document I 2.1 ASTM Standard: J D1794 Test Method for Alcohol-Benzene Soluble Matter in Cellulose3 : 1. Summary of Test Method j 3.1 The total chlorine determination is a measure of the rater soluble chlorides as well as the chlorine bound in the pulp. 3.2 This test method makes use. of the oxygen flask technique for the combustion of the pulp sample. After combustion, the chloride ions are absorbed in dilute sodium hydroxide, the solution is evaporated to dryness, and the residue is redissolved in a small amount ofdilute nitric acid. Ihe solution is diluted with acetone and titrated with 0.0025 M silver nitrate solution using a potentiometric titrator. 4. Significance and Use 1 4.1 Measurement of total chlorine levels gives the sum of water soluble chlorides and the Organically bound chlorine compounds present in a pulp sample. Inorganic chlorine is known to be detrimental to the performance of many types of cellulose derivatives such as in viscose manufacturing. 4.2 Organic chlorine compounds are of interest from the environmental standpoint. The levels of organic chlorine compounds in pulp mills and in pulp products is under investigation in light of the suspected toxity of these com pounds to aquatic life. I 1 This test method is under the jurisdiction of the ASTM Committee D-! on jPaint and Related Coatings and Materials and is the direct responsibility of ^Subcommittee D01.36 on Cellutosics. 1 Current edition approved Oct. 27, 1989. Published December 1989. Originally {published as D 2641 - 67. Last previous edition D 2641 - 70(1985)cl. j 2 See Rioux, J. P., and Hurtubise, F. G., "Determination of Chloride Ions in 'Pulp and Paper," TAPPl, Vol 48, January 1965, pp. 11-14. ] 3 Annual Book ofASTM Standards, Vol 06.02. 5. Apparatus 5.1 Potentiometric Titrator, preferably equipped with a recorder. The use of a recorder is considered essential at low levels of chlorine.4 5.2 Electrodes, glass or mercurous sulfate reference elec trode and silver-silver chloride indicator electrode: 5.3 Combustion Flasks, 1000-mL conical, borosilicate glass, with 35/25 ball and joint stopper and 5000-mL round bottom, borosilicate glass, with 65/40 ball and joint stopper. The flasks are equipped with perforated platinum sample carriers sealed into extended stem of flask stopper. 5.4 Igniter, suitable for igniting the sample in the flask. An "infrared igniter" is preferred.5- 5.5 Specimen Wrappers, black paper. 6. Reagents 6.1 Purity ofReagents1--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. 6.2 Water--Deionized and chloride-free. (It is essential that only this type of water be used in this test method.). 6.3 Silver Nitrate, Standard Solution (0.0025 M)--Dis solve 0.4247 g of silver nitrate (AgN03) in water, add 3 mL of concentrated nitric add (HN03, sp gr 1.42); and dilute to 1000 mL. Standardize daily against sodium chloride solu tion, 1 mL of 0.0025 M AgN03 solution is .equivalent to 0.0886 mg of chlorine. ' 6.4 Sodium Chloride, Standard Solution (0.0025 M)-- Dissolve 0.1462 g of sodium chloride (Nad) in water and dilute; to 1000 mL. 6.5 Nitric Acid (1+100)--Dilute 10 mL of concentrated nitric add (HN03, sp gr 1.42) to 1000 mL with water. Store in a glass-stoppered bottle. 6.6 Sodium Hydroxide, Standard Solution (0.1 N)-- Transfer the contents of a standard concentrated volumetric ampoule into a polyethylene bottle and dilute to 1000 mL. 6.7 Acetone. 4 One suitable titrator-recorder is the Radiometer TTT-1 titralor equipped with the Radiometer SBU-1 titration assembly, manufactured by Radiometer America Inc., 811 Sharon Drive, Westlake, OH 44145. s The Thomas-Ogg apparatus manufactured by the Arthur H. Thomas Co., Philadelphia, PA, has been found satisfactory for this purpose. 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." 383 DU P0502 96903 # D 2641 7. Report 7.1 Report the results to the nearest parts per million of cellulose dried at 100 to 105"C. 8. Precision and Bias 8.1 A precision of less than 10 % relative is, found by replicate runs by a single analyst. 8.2 No statement of bias can be made as no suitable reference material exists for determining bias. TOTAL CHLORINE 9. Standardization 9.1 Pipet an aliquot of the 0.0025 MNaCl solution into a titration vessel. Add 5 mL of 0.1 N NaOH solution, evaporate, ancl t;;eat as in 10.7. 9.2 Carry out a blank titration by igniting a black paper wrapper, omitting the specimen. Subtract this titration from those obtained for specimens. 10. Procedure 10.1 Cut a suitable air dry test portion of the sample into 0.5-in. (13-mm) squares and weigh to the nearest 0.001 g on a black paper specimen wrapper. For samples containing 5 to 100 ppm chlorine, 1-g air dry test portions are burnt in a 5-L flask; for samples coiitaining OLOO to 1000 ppm chlorine, 0.3-g air dry test portions are burnt in a l-L flask. 10.2 Place the test portion wrapped in the black paper in the platinum basket 10.3 Add 5.0 mL of 0.1 iV NaOH solution to the combustion flask. !ntroduce**the specimen ih the flask :and allow a stream of oxygen to pass through the flask until the air is completely displaced. Then, stopper the flask with a pinch clamp. 10.4 Turn on the igniter and focus the infrared light beam on the black paper fuse on the wrapper until ignition occurs. This operation should be carried out behind a protective shield. 10.5 After the specimen has burned Completely, allow the flask to cool until all vapors are absorbed by the NaOH solution. Transfer the solution to a titration vessel and rinse the flask with deionized water (approximately 50 mL), adding the rinsings to the solution. 10.6 Evaporate the solution to approximately 5 mL on an asbestos-covered hot plate. Then evaporate to dryness under an infrared lamp, and allow to cool. 10.7 Add 4 mL of HN03 (1+100) and swirl to dissolve any residue on the walls of the vessel. Add 25 mL ofacetone, titrate with 0.0025 M AgN03 solution, and record the titration curve. 11. Calculation 11.1 Calculate the chlorine content, C, in parts per million as follows: C-- (AB/W) x 1 000 000 (1) where: A = 0.0025 M AgN03 solution required for titration of the specimen, corrected for the blank, mL, B = ehlorine equivalent of the 0.0025 M AgN03 solution, g/'mL, and W = specimens used, g. WATE^-INSOLUBLE CHLORINE 12. Procedure 12.1 Using clean scissors, cut and. place 4.0 0.01 g of air dry sample in a paper thimble, place in a Soxhlet extractor and extract in accordance with Test Method D 1794, using water instead of alcohol-benzene. 12.2 Remove a 2-g portion of the sample from the thimble. Dry this portiop at for 1 h., pejtertnine the chlorine" in accordance with Section ,9. 12.3 Calculate the chlorine content ja accordance with Section 11. ALCOHOL-BENZENE INSOLUBLE CHLORINE 13. Procedure f' 13.1 Replace the thimble with the remaining pulp in the extractor, and extract in accordance with Test Method D1794. 13.2 Dry the extracted pulp at 60C for 1 h. Determine the chlorine in accordance with Section 9. 13.3 Calculate the chlorine content in accordance with Section 11. LIGNIN-BOUND CHLORINE 14. Calculation 14.1 The Lignin-Bound Chlorine discussed by Howard and Histed17 1is numerically identical to the Alcohol-Benzene Insoluble Chlorine as determined in Section 13. : RESIN-BOUND CHLORINE 15. Calculation 15.1 Calculate the Resin-Bound Chlorine, CM, as follows: 8 = A -- B ~ (2) where: A = water-insoluble chlorine and ; B = alcohol benzene insoluble chlorine. WATER-SOLUBLE ; CHLORINE, 16. Calculation : 16.1 Calculate the Water-Soluble Chlorine, Cws, as fol lows: Cws -- A -- B ' ' (3) where: A = total chlorine and B = water-insoluble chlorine. 7See Howard, E. J., and Histed, J. A., TAPPf, Vol 47, November 1964, PP655-662, and Histed, J. A,, TAPPI, Voi 47, November 1964, pp. 669-673. 384 DUP050296904 # D 2641 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 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 eitherforrevision ofthisstandard 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, ISIS Race St., Philadelphia, PA 1S103. 385 DUP050296905 Designation: D 2689 - 88 Standard Practices for Testing Aikyd Resins1 This standard is Issued Under the fixed designation D 2689; thb number immediately following the designation indicates the year of original adoption or, in the chse ofrevision, the year oflast revision. A numbetTn parentheses indicates theyear of last reapproval. A superscript epsilon () indicates an editorial change sincii the last revision or reapproval. 1. Scope 1.1 These practices cover test methods for testing aikyd resins as listed in Table 1. They are the test methods most often used to characterize alkyds. All of the analytical test methods were subjected to interlaboratory testing using oil-modified alkyds. Their adaptability to other types of alkyds has not been studied. Although each test method specifies a recommended amount of specimen for starting a separate analysis, several ofthe procedures can be conducted on the same starting specimen, if desired. For example, the tests for unsaponifiable matter, fatty acid content, oil identi fication, and phthalic acid content could all be run on a consecutive basis, if all were required. 2. Referenced Documents 2.1 ASTM Standards: D93 Test Methods for Flash Point by Pensky-Martens Closed Tester12 D563 Test Method for Phthalic Anhydride Content of Aikyd Resins and ResimSolutions3 D 1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale)4 D 1259 Test Methods for Nonvolatile Content of Resin Solutions3 D 1306 Test Method for Phthalic Anhydride Content of Aikyd Resins and Esters Containing Other Dibasic Acids (Gravimetric)3 D1397 Test Method for Unsaponifiable Matter in Aikyd Resins and Resin Solutions3 D1398 Test Method for Fatty Acid Content of Aikyd Resins and Aikyd Resin Solutions3 D 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products5 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)6 D 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method6 D 1639 Test Method for Acid Value of Organic Coating Materials5 D 2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids7 D 2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints2 D 2455 Test Method for Identification of Carboxylic Acids in Aikyd Resins3 D2690 Test Method for Isophthalic Acid in Aikyd and Polyester Resins3 D2998 Test Method for Polyhydric Alcohols inAikyd Resins3 D3278 Test Methods for Flash Point ofLiquids by Setaflash Closed-Cup Apparatus2 | j | ! | J 1 f 3. Significance and Use i 3.1 These practices should be used as a reference for any aikyd resin analyst who wants general information about classifying aikyd resins. In each case, the significance and use of the specific classification item will be found in the referenced test method. J | | | | 4. Nonvolatile Content 4.1 A unique test method for determining nonvolatile matter in solutions of aikyd resins in volatile organic solvents provides for the drying of very thin films of resin quickly, thus minimizing chances for volatiles to be trapped or drying oils to oxidize. Test Method A ofTest Methods D 1259, was thoroughly tested with aikyd resins with outstanding repeat ability of 0.1 % and reproducibility of0.2 %: This procedure, sometimes referred to as the "foil" test method, should be considered the "referee" test method for all aikyd analyses requiring maximum precision. 5. Add Value 5.1 Acid value of an aikyd resin is expressed as the number of milligrams of potassium hydroxide required to neutralize the free addity of 1 g of nonvolatile material under the conditions of the test. Test Method D 1639, was especially prepared for this purpose. 1 These practices are under the jurisdiction of ASTM Committee D-l 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 approved May 27, 1988. Published October 1988. Originally published as D 2689 - 68. last previous edition D 2689 - 80. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 6. Unsaponifiable Matter 6.1 The unsaponifiable matter in aikyd resins is the ethyl ether-soluble, water-insoluble portion that remains after a relatively large specimen has been subjected to an aqueousalcoholic saponification. The yield is normally low and is an 7 Annual Book ofASTM Standards, Vols 06.02 and 06.03. 386 DUP050296906 ft**-------------------------------- f! #. D 2689 TABLE 1 ... Test Methods for Testing Alkyd Resins PS--------------- -------------:------------------- - test Method Section ASTM Designation Nonvolatile content ...Addvalue * 'Unsaponifiable matter ! Fatty acid content it Identification of oils and acids .... . Phthalic anhydride content " Isophthalic add content 4 .. 5 6 7 `8 9 10 D1259 D1639 . D1397 D1398 ` D2245. 0 563. D 1306 02690 5, , Polyhydric alcohol content Identification of carboxylic acids Flash point Color [ ' Density [' Viscosity {.a- Clarity t 11 D2S98. 12 D2455 . 13 D 93 D 3278 14 01209 D, 1544 15 6,1475 16 ' ' D1545 17- D2090 ' Method D2245, and the sample may be obtained as described therein or from material remaining from the fatty acid determination of Section 7. 9. Phthalic Anhydride Content 9.1 Alkyd resins that are known to contain phthalic anhydride as the only dicarboxylic acid and are not modified with resins such as phenolics, urea- or melamine-formal dehyde tnay .be analyzed in accordance,with Test Method D 563. Styrene does not interfere, so that styrenated alkyds may be tested by the same, test method.. 9.2 Deteiininatiqn of"phthalic anhydride in alkyd resins that contain isomers of phthalic acid or other dibasic acids such as maleic, fumade, etc., must be made in accordance with Test Method E> 1306, in which the phthalic anhydride is determined gravimetrically as the lead salt. Indication of purity insofar as the presence of modifying as will affect the result. Certain other resins can interfere Sue to variations in degree ofsaponification and solubility in bther. The test method is therefore not applicable to alkyds containing such other resins as styrene, rosin, phenols, and [formaldehyde condensates. The unsaponifiable matter is ietermined gravimetrically in accordance with Test Method jjD 1397 and maybe calculated on the nonvolatile or solution basis according to prior agreement. {7. Fatty Acid Content : 7.1 The total fatty acids in alkyd resins can be measured jgravimetrically on a separate specimen in accordance with Test Method D 1398. This test method provides for the 'isolation of fatty acids after saponification under anhydrous :conditions, removal of the salts of the dicarboxylic acid by `filtration, removal of the unsaponifiable matter and original i solvents by benzene extraction of the filtrate, and finally I ether extraction of the acidified aqueous layer that remains. The test method was prepared for use with orthophthalic ; alkyds and, if isophthalic add is present, a considerable amount will appear in the extracted oil acids where it is readily detected as white crystals. Interference from iso; phthalic acid can be avoided by redissolving the oil acids in ! benzene, filtering into a weighed beaker and drying as before. iSome modifying agents such as urea, melamine, phenols, rosin, and styrene will contaminate the isolated fatty acids in varying degrees and Test Method D 1398 is considered inapplicable in the presence of such other resins. If the fatty acids isolated by Test Method D 1398 are to be examined further for identification (Section 8), a small, weighed crystal of hydroquinone to serve as an antioxidant, should be added8 prior to the evaporation of the ether. 8. Identification of Oils and Oil Adds 8.1 The oils and oil acids contained in oil-modified alkyd resins can be identified by gas chromatographic separation of their methyl esters that are formed in the presence of margaric acid added as an internal standard. The test method is not applicable to fatty acids that have polymerized or oxidized to such an extent that no characteristic monomeric fatty acids remain. The test is conducted in accordance with 10. Isophthalic Acid Content 10.1 A rapid and simple procedure for the gravimetric determination of isophthalic acid in alkyd resins is provided in Test Method D 2690. There is no interference in this test method from styrene monomer of polymer or from other dicarboxylic acids except terephthalic acid, which is recov ered quantitatively. 11. Polyhydric Alcohol Content 11.1 The polyhydric alcohols in alkyds can be determined qualitatively and quantitatively in accordance with the procedure in Test Method D 2998. The resin to be analyzed is dried, subjected to aminolysis, and treated to form trimethylsilyl ether derivatives of the alcohols which are separated by gas-liquid chromatography. An internal standard is used for quantitative purposes. Flame-ionization detectors cannot be used with Test Method D 2998. 12. Identification of Carboxylic Adds 12.1 Method D 2455 describes a procedure for the quali tative determination of all the carboxylic _acids in alkyd resins, including resin-modified alkyds. This procedure makes use of gas chromatographic separation of the methyl esters of the respective acids that are formed by direct transesterification of the resin with lithium methoxide. The acids, including the fatty adds, are identified by their relative retention time which is given for 23 adds and others may be added if desired. Since maleic and fumaric acids react differently than the other adds encountered, an alternative procedure is supplied for their differentiation. It is sometimes possible to identify the drying oils in the alkyd from the fatty acid esters that appear in this procedure, but it is not as reliable for oil identification as Method D 2245 (Section 8). 13. Flash Point 13.1 In the Setaflash closed tester, a small specimen is injected by means of a syringe and its flash temperature is determined visually, as described in Test Method B of Test Method D 3278. This procedure is faster, more convenient, and somewhat more precise than the Pensky-Martens proce dure described in Test Method B of Test Method D 93; 387 DUP050296907 # D 2689 however, results obtained by either test method are accept able. 14. Color 14.1 The Gardner color method, Test Method D 1544, compares a specimen to glass filters by means of a compar ator, while Test Method D1209 compares the specimen to calibrated liquids in Nessler tubes. It is recommended that Test Method D 1544 (Gardner Color Scales) be used for the color specification where practical. Where particularly light color is required. Test Method D 1209 (platinum-cobalt scale), may be used when agreed upon between the producer and the user. There is no reliable correlation between the two test methods. In general. Test Method D 1209 is to be preferred for light-colored liquids while Test Method D 1544 is generally used for darker liquids, such as drying oils, varnishes, and coating resins. 15. Density 15.1 Test Method D 1475 describes the determination of density by either the pycnometer or weight cup test methods. Either test method is acceptable for alkyd resins. 16. Viscosity 16.1 The viscosity of resin solutions may be determined by the bubble-time test method, in accordance with Test Method D 1545. Viscosity is measured at 77'F (25C) by comparing the time for a bubble to traverse a standard tube containing the resin, to the time for standard oils under identical conditions. The bubble seconds are approximately equal to stokes and may be converted to poises by dividing by density. 17. Clarity 17.1 Clarity may be determined in accordance with Test Method D 2090, wherein a specimen is placed in a bubble viscosity tube and rated subjectively for seven factors relating to clarity. The American Society for Testing andMaterials takes no position respecting the validity ofanypatentrights 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 orwithdrawn. YourcommentsareInvited either for revision 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. Ifyou feel that your comments have not received a fair hearing you should make your views known to ths ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. P 388 DUP050296908 p Designation: D 2690 - 89 Standard Test Method for Isophthalic Acid in Alkyd and Polyester Resins1 This standard is issued under the fixed designation D 2690; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A numberin parentheses indicates the year oflast reapproval. A superscript epsilon () indicate) an editorial change since the last revision or reapproval. , . Scope 1.1 TMS test'method covers the gravimetric dietienrimation f the isophthalic acid content cif alkyd resins and polyesters, 'here is no interference from styrene monomer or polymer f,from other cficarboxylic acids except terephthalic acid. " 1.2 This standard may involve hazardous materials, oyer-, iiorn, and equipment. This standard-does not purport to mress all ofthe safety problems,associated with its use. It is he responsibility of the user of this standard to establish ippropriate safety and health practices and determine the ipplicability of regulatory limitations prior to , use. For a ipecific hazard statement, see section 7. [Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water12 Summary of Test .Method . 3.1 The resin is saponified with alcoholic potassium hy- oxide and benzene to precipitate entirely the potassium salt of the phthalic acid isomer. Since the salt contains mtrained impurities, it is dissolved In water and diluted to volume. An aliquot portion is acidified under conditions that release the insoluble add in filterable form. It is then isolated, weighed, and corrected for its slight solubility in oyater.i 41 Significance and Use 4.1 This test method is used to determine,the, amount of isophthalic add contained in alkyd and polyester resins. Use of this test method provides a means whereby the relative applicability of the alkyd or polyester resin to the particular end use may be estimated by the buyer and the seller. 5. Apparatus 5.1 Flask and Condenser--A 250-mL Erlenmeyer flask fitted with an air-cooled glass reflux condenser 30 in. (760 mm) in length. The connection between the flask and condenser should be a standard-taper 24/40 ground joint. 5.2 Heat Source: ' '. ' ' ' 5.2.1 Combination Hot Plate and Magnetic Stirrer, or 51 T.h2i.s2tesHt meeathtiondgisMunadnerttlheeajunrisddMictaiognnoefAtiScTSMtiCrroemrmBittaeseeDa-1nodn BPaainr.t amnitdt5eR.e3eDlBa0tue1d.c3h3CnooaentirPngoFslyuamnnednrseMal,antdefrrRiiatetlsseinadsn. dglias sthse, dmireecdt iruesmponpsoibriolitysiotyf,Su1b5co0m- mCLucrraenptaecditityio.n approved April 28, 1989. Published June 1989. Originally published as D 2690 - 68. Last previous edition D 2690 - 80. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5.4 Volumetric Flask, lOQ-mL volume. 5.5 Fritted-Glass Filter Crucible, medium porosity, 30mL 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 first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination. 6.2 Purity of Water-r--Unless otherwise indicated, refer ences tp water, shall be understood to mean reagent water as defined by Type II of Specification D 1193. ,6,3 Alcphol-Benzene Wash Solution (2+3)--Mix absolute ethyl alcohol (Note 1) with benzene in lie proportion of 2 volumes of alcohol to 3 volumes of benzene. l--The alcohol may be denatured Formula 2-B, but must be anhydrous. 6.4 AlcOhplic Potassium: Hydroxide Solution (0.5 N)--Dissolve 33 g of KOH in 1 L of absolute ethyl alcohol (Note 1) by reflux or by standing overnight. Protect against carbon dioxide absorption. Filter jiist before use. 6.5 Benzene (anhydrous). 6.6 Ether (anhydrous). 6t7- Hydrochloric Acid (sp.gr 1.19)--Concentrated hydro chloric add (HCl). .. 6.8 Methyl Purple Indicator Solution. 7. 'Hazards - 7.1 The reagents and samples used in this test method may, .under some conditions, be hazardous. Refer to the manufacturer's material safety data sheets for specific han dling and safety precautions. Safe laboratory handling proce dures and all applicable OSHA regulations are to be fol lowed. 8. Procedure 8.1 Weigh a portion of resin containing about 400 mg of isophthalic acid (usually i to 3 g of vehicle) into a 250-mL Erlenmeyer flask and dissolve in 10 mL ofbenzene. Add 100 mL of freshly filtered 0.5 N alcoholic KOH solution and insert a magnet stirrer bar. Attach the air condenser and 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. 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." 389 DUP050296909 # D 2690 reflux for 1 Vi h with constant stirring by means of a heating mantle or combination stirrer-hot plate. 8.2 Remove from the source of heat, remove the con denser, and fill the flask to the neck with benzene. Cool the solution to room temperature with stirring, allow to settle a few minutes, then filter with suction through a 150-mL fritted glass Buchner funnel of medium porosity. Transfer and wash to bulk of the precipitate with alcohol (2+3). Rinse the flask with about 25 mL of ethyl ether and add to the funnel, draining thoroughly with suction. 8.3 Dry the funnel and flask in a 105C oven for about 30 min. Dissolve the dipotassium salts in small portions of water by first adding them to the dried flask to remove all traces of the precipitated salts, and then to the funnel collecting them in a clean suction flask. Transfer the filtrate with water to a 100 mL volumetric flask and dilute to the mark. 8.4 Mix the solution thoroughly and withdraw a 50-mL aliquot by means of a pipet and transfer to a 125-mL Erienmeyer flask. If it is necessary to use. smaller aliquots, make the volume up to 50 mL with water. Add a magnetic stirrer bar and about 2 drops of methyl purple indicator solution and while stirring acidify the solution by adding HCI (sp gr 1.19) dropwise until the color changes, then add 7 drops in excess. 8.5 Continue the stirring for about 5 min and collect the precipitated isophthalic, acid in a weighed fritted-glass filter crucible of medium porosity, Po not wash or add any water at this time; instead, collect the filtrate in a clean flask and use it in five 10-mL portions to transfer the precipitate quantitatively to the crucible.'The filtrate may be reused if necessary. Now wash the collected solution in the crucible twice with 3-mL portions of distilled water added from a pipet and directed against the sides of the crucible while rotating so as to effect maximum washing with the two small measured volumes of water. Dry the crucible in an oven at 105C for 1 h, cool in a desiccator, and weigh. If the collected isophthalic sample exceeds 200 mg, withdraw a smaller aliquot from the remaining solution, dilute to 50 mL with water and repeat the precipitation procedure. If less than 50 mg are collected, repeat from the beginning with a larger resin specimen. 9. Calculation 9.1 Calculate the percent of isophthalic, acid / as follows: ,, (P + 0.005) x 100 x 100 SWA where: P -- weight of precipitate, g, S = weight of resin specimen, g, W = nonvolatile content expressed as a decimal, and A = size of aliquot, mL (usually 50). 10. Precision 10.1 On the basis of an interlaboratory study in which one operator in each of six laboratories made duplicate determi nations at each of six laboratories on two samples of different manufacture, the within and between laboratory standard deviatibns were found to be: Isophthalic Add Content, % Standard Deviation, % Within Between Laboratory Laboratory 30 0.025 . 0.18 50 0.083 0.44 Based on these standard deviations, the following criteria should be used for judging the acceptability: of 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 the following: Isophthalic Acid 'Content, % ' Differences, % 30 U15 50 0.50 10.1.2 Reproducibility--Two results, each the mean of duplicate measurements, obtained by operators in different laboratories should be suspect ifthey differ by more than the following: Isophthalic Add Content, % 1 30 " 50 : .... . Differences, % 0.6" . 1.5 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned iri this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and thefisk 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 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 yod feel that your commenta have not received a fair hearing you should make, your viewa known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 390 DUP050296910 Last ASTM Designation: D 2742 - 79 \ Standard Methods for I; Chemical Analysis of Tribasic Lead Phosphbsilicate : These methods cover the chemical analysis'-of the pigment commercially known as tribasic lead phosphosilicate: I; Formerly under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials, these methods were discontinued in 1990. \t % 1* 391 DUP050296911 Last ASTM Designation: D 2744 - 68 (Reapproved 1979)*1 Standard Specification for Trihasic Lead Phosphosilscate This specification covers file material known commercially as tribasic lead phosphosilicate. > Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this specification discontinued in 1088. 392 DUP050296912  Designation: D 2745 - 89 Standard Test Method for Relative Tinting Strength of White Pigments by Reflectance Measurements1 This standard is issued under the fixed designation D 2745; the number immediately Mowing 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. H. Scope LI This test method describes the procedure for deter mining the relative tinting strength of white pigments by reflectance measurements of black tints. 1.2 This test method is applicable only for comparing the test pigment with a reference standard of the same type and grade. 1--Test Method D 332 describes a procedure for visual (assessment of blue tinted samples. 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: D332 Test Method for Relative Tinting Strength of White Pigments by Visual Observation2 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry3 3. Summary of Test Method 3.1 Pigment is dispersed in a vehicle and let down with additional vehicle that has been tinted. Dispersion and let-down are accomplished with a mechanical muller. Both the test and standard pigments are treated identically. Opaque drawdowns are made of the paint and the Y tristimulus values (green-filter reflectance) of the wet films are measured. The relative tinting strength of the test pigment is calculated directly frointhe reflectance values. 4. Significance and Use 4.1 Tinting strength is one of the most important proper ties ofa white pigment. This test method provides a means of testing this property for quality control. 4.2 This test method is a referee method, and the vehicle for preparing the dispersion and the black for tinting are suggested but others may be used provided both the pur- 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 2745 - 68 T. Last previous edition D 2745 - 80. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 14.02. chaser and the seller agree to the changes. 4.3 The results obtained.with a muller do not necessarily agree with industrial situations where different dispersing conditions exist. However, dispersing with a muller is a fast, relatively inexpensive way of testing tinting strength for routine quality control. 5. Apparatus and Materials 5.1 Muller, automatic,4 equipped with a weight that exerts a permanent 50-lbf (220-N) and an additional weight ex erting a 50-lbf making a total of 100-lbf (445-N). The two glass plates shall be kept sharp by removing from the machine and grinding them face-to-face with No. 303 optical emery or equivalent, and water. 5.2 Spatula--A flexible spatula having a chromium- plated or plastic blade 3 to 6 in. (75 to 150 mm) long and another with a 3-in. tapered blade. 5.3 Balances--(1) A balance sensitive to 20 mg and (2) an analytical balance sensitive to 0.4 mg. 5.4 Vehicle--Because the choice of vehicle may affect results, a solvent-free vehicle (excluding refined or low bodied linseed oil)5 should be agreed upon by the purchaser and the seller. 5.5 Tinting Black--A. lamp black predispersed in a ve hicle similar in nature to the test vehicle.6 5.6 Chart--Either gray or white lacquered charts7 cut to a~ convenient size. 5.7 Colorimeter--A filter colorimeter meeting the re- ~ quirements of Test Method E 97. .......... , 5.8 Film Applicator--2 or 3 in. (50 or 75 mm).wide with a clearance of 6 mils-(150 pm) to produce wet films about 3 mils (75 pm) thick. This applicator when used as suggested in the test method will produce an R,, film.8 6. Standard 6.1 A standard white pigment of the same type as the 4 A satisfactory muller is supplied by the Hoover Color Corp., 13 Cordier St, Irvington, NJ 07111. 5 Suggested vehicles include a 50-50 mixture of Aroplaz 1271 and 1278 (Spencer Kellogg Division of Textron, Inc., P.O. Box 807, Buffalo, MV 14240), No. 3 Litbo Varnish (Inmont Corp., Printing Ink Div., Germantown Ave. and New Market St, Philadelphia, PA 19123), and Castor Oil AA, USP (NL Industries, NL Chemicals Div., P.O. Box 700, Hightstown, NJ 08520). 4 Tinting black should be agreed upon between the purchaser and the seller. Suggested materials include Lampblack PF 4340 (Daniel Products Co., 400 Claremont Ave., Jersey City, NJ 07304) and Lampblack 5-24-A-710 (The Hilton-Davis Chemical Co., 2235 Langdon Farm Road, Cincinnati, OH 45237). 7 Suitable charts are available from The Leneta Co, P.O. Box 86, Ho-Ho-Kus, NJ 07423. e A Bird Film Applicator, available from Bird and Sons, Walpole, MA 02081, has been found suitable for this purpose. 393 DUP050296913 # D 2745 TABLE 1 Examples of Preparation of Black Letdown Vehicles Pigment Type Approximate Pigment Density Pigment, g Clear Vehicle, g Black Letdown Vehicle, g Approximate PVC of Final Paint, % Titanium cloxide: rutile anatase Lithopone Zinc oxide, leaded Zinc oxide White lead 4.1 3.8 4.3 5.9 : 5.6 6.8 . 3.000 3.000 5.000 5.000 5.000 3.000 - 2.000 2.250 1.220 2.460 2.660 0.810 1.000 1.000 1.000 1.000 1.000 1.000 2020 35 20 20 20 * Daniel Products Co. Lampblack F is used for this example. 8 A 50-50 (by weight) composite vehicle. Aropiaz 1271 and 1278, is the "vehicle" used tor this example. Predispersed Black.* g Clear Vehicle.8 g 6.80 93.20 2.25 250.00 sample to be tested, as agreed upon by the purchaser and the seller. 7. Procedure 7.1 Place two concentric circles under the base plate of the muller so that they can be clearly seen through the plate. The circles can be drawn on a paper and inserted under the plate, or they can be drawn directly on the underside'ofthe bottom plate. The inner Circle should be 2Vi in. (63 mm) in diameter and the outer circle 4Vi in. (11,4 mm) in diameter. 7.2 Make a preliminary test by dispersing standard white pigment in a dear vehicle at the pigment volume concentra tion (PVC) given in Table l' and adding tinting black to determine the amount of black required to provide a reflectivity of 0.42 0.03. Prepare a "black letdown vehicle" by adding tinting black to clear vehicle so that 1.000 g of the black letdown vehicle will contain the same amount of black that provided this reflectivity.' Three examples are given in Table 1. ' 7.3 Weigh the pigment to the nearest g with the analytical balance in accordance with Table 1 and transfer to the lower plate of the muller. Add clear vehicle to the pigment in accordance with Table 1 (Note 2). Mix with a spatula until a paste is obtained. "Pick up" the paste with the spaiiila arid spread it withiii the area between the two concentric'circles on the plate. Close the muller, mull 25 times, and Collect the paste. Thoroughly mix the black letdown vehicle in its container. Add 1.000 g of black letdown vehicle sis specified in Table 1 to the white paste arid mix in thoroughly with a spatula. Again spread the paste within the two concentric circles, mull 25 times, pickup the paste, spread within, die area, and mull a final 25 times more. Prepare a reference standard with each series erf" test pigments by this same procedure. --An analytical balance is specified for referee-type oftesting for routine work, weighing to 20 mg has been found satisfactory as an alternative procedure. Among the methods of accurately weighing vehicles (either the clear or black letdown vehicles) are these two alternatives: (i) Place a small beaker of vehicle on the weighing pan of the balance. Remove and transfer vehicle employing the spatula ultimately intended for preparing a paste on the muller. Use the weigh-by-difference method. (2) Add the vehicle to a tared metal or plastic plate till the correct weight is reached; transfer to the muller by scraping off the plate with the spatula. If the vehicle tends to run, weigh both pigment and Vehicle on the plate making a crater in the pile of pigment to contain the vehicle. 7.4 Standardize the colorimeter for measurement of the green filter reflectance (that is, T-value) with, if necessary, a wet-film adapter in place. Adjust the colorimeter to the approximate expected reading. Draw down the sample paint on the-chart (lacquered side) with the applicator blade (5.8V Place the film immediately on the reading port, cover-theback of the chart with a flat, black panel (for example, black structural glass) to keep the chart flat and prevent exterior light from entering the colorimeter, and read the reflectance immediately (Note 3), recording the value, dean the port of the colorimeter thoroughly with a rag. Draw down the standard paint and read immediately as before (Note 4). Nora 3--Flooding will cause drifting in the reflectance leading, of some films. When the colorimeter is already adjusted to the expected reading, an experienced operator can read the'reflectance with' high precision in a very short interval. Consequently the tithe lapse between draw-down and reflectance Trading should be as short as posable. --Although the, method is primarily intended. as a rapid method, it obviously can be adapted to measuring the tinting strength in a dry film of paint. For this an appropriate amount of cobalt drier is added to the black letdown vehicle during its preparation (see 7.2), and the films are allowed to dry as needed before making the reflectance measurements. It should, be cautioned that tinting-strength values measured on dry films may differ from those pleasured on wet films. 8. Calculation of Tinting Strength ` 8.1 Calculate the tinting strength as follows: TS = [(1 - -RJ2u/[( *)2/2iRJ. (T) where: TS = tinting strength-of test pigment,R,, = measured reflectant factor (as a decimal),. T = assigned tinting strength of standard, Usually 100 %, ' and .subscripts "u" and "s" refer fo the test and standard pigments, respectively. 9. Report -' 9.1 Report the following information: . ,, , 9.1.1 Tinting strength rounded to three significant figures, 9.1.2 Identification of the pigment, the.reference stand ard, and the arbitrary assigned value, T, of, the tinting strength for the reference standard. (Also identify the vehicle and colorant employed.), and 9.1.3 Name and model number of the colorimeter em ployed. 10. Precision 10.1 On the basis of an interlaboratory test of this test method in which seven laboratories tested , four materials covering a broad range in tinting strength using five types of colorimeters, the standard deviation was found to be 1.16 within laboratories and 1.72 among laboratories. Based on this, the following criteria should be used for judging the acceptability of results at the 95% confidence level-when the 394 DUP050296914 # D 2745 ||andard is assigned a value of 100: 5 10.1.1 Repeatability--Two results obtained by the same iperator on the same pigment should be considered suspect Jf they differ by more than 3.3 units. 10.1.2 Reproducibility--Two reported results, obtained by operators in different laboratories, should be considered suspect if they differ by more than 4.9 units. 5* 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 fights, 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 commentsare Invitedeither forrevision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Ydur comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. Ifyu tenttflat your comrnents have not received.a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Phtiadelphia, PA 19103. 395 DUP050296915 Designation: D 2929 - 89 Standard Test Method for Sulfur Content of Cellulosic Materials by X-ray Fluorescense1 This standard is issued under tbe fixed designation D 2929; 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 test method covers determination of sulfur con tent of cellulosic materials by X-ray fluorescence. 1.2 Using appropriate standards, the range of the proce dure is from approximately 10 ppm to 20 % sulfur. 1.3 This test method is proposed specifically as an alter native to Methods D 871, Sections 29 to 33, and Methods D817, Sections 39 to 43. As applied to cellulose esters it measures the combined sulfur and sulfur in the accompa nying inorganic salts. 1.4 To determine combined sulfur, the sample, when soluble, must first be reprecipitated into dilute acid to remove the noncombined sulfur compounds. 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 Note 3. 2. Referenced Documents 2.1 ASTM Standards: D817 Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate*2 D871 Methods of Testing Cellulose Acetate2 3. Summary of Test Method 3.1 The sulfur content of cellulose, cellulose modification, or cellulose derivative is determined by measuring the intensity of the secondary sulfur Ka X rays emitted on irradiation of the sample with primary X rays of higher energy from an X-ray tube with a target of tungsten or chromium. The sulfur Ka radiation is diffracted with a suitable analyzing crystal and detected with a flow propor tional counter. The entire path of the secondary radiation is purged with hydrogen or helium, or evacuated to a pressure of 0.5 mm Hg or less. The intensity of the sulfur Ka rays, as established by a standard counting period and corrected for background radiation, is then converted to percent sulfur from calibration data.3 4 4. Significance and Use 4.1 This procedure provides a. method for determining sulfur content in cellulosic materials by nondestructive means. Sulfur may be in the form of sulfate esters that may contribute to thermal instability. Sulfur can also be present as salts that can cause haze in solutions. 5. Apparatus 5.1 Wiley Mill, equipped with 60-mesh screen. 5.2 Sample Mold--Chrome steel die of a size depending on the sample holder to be used. 5.3 Laboratory Press, capable ofexerting at least 5000 psi. 5.4 X-Ray Spectrograph, with following equipment: tung sten or chromium target X-ray tube; hydrogen or helium purging system or vacuum system to reach 0.5 mm Hg (or less, if desired); 20-mil Soller slits; flow proportional counter with 90 % argon-10 % methane gas mixture; and NaCl, ethylenediamine dextro tartrate (EDT), or pentaerythritol (PET) analyzing crystal. 1--Radiation from a chromium target tube appears to he more effective than radiation from a tungsten target tube.for exciting sulfur Ka. This may be because a larger part of the "white" radiation of the chromium tube is at the longer wavelength region of tbe spectrum, or because ofthe use ofthinner windows in the chromium tube. However, either the chromium or the tungsten target tube is suitable for sulfur analysis. If a pulse height analyzer is available as a part of the X-ray instrumentation, its use is very helpful in reducing background radiation. Use of a pulse height analyzer is mandatory for the determination ofsulfur below 100 to 200 ppm level. 6. Reagents -_ 6.1 EthylCellulose Phthalate.* 6.2 Microcrystalline Cellulose.5 6.3 Cystine, NIST primary standard No. 143B. 6 jifi if I i 7. Procedure 7.1 Instrument Standardization Pellet--Intimately mix ethyl cellulose phthalate, microcrystalline cellulose, or other selected matrix with finely divided cystine in a weight ratio of approximately 4:1. Press a portion into a pellet' in the sample 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 DOi.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2929 - 70. Last previous edition D 2929 - 70(1985)*'. 2 Annual Book ofASTM Standards, Vol 06.02. 3 This test method is compiled from four techniques, by incorporating certain features of each, as follows: "Sulfur in Cellulose Esters by X-ray Emission Spectroscopy," Eastman Kodak Co.; "Sulfur in Cellulose Acetate by X-ray Fluorescence," Tennessee Eastman Co.; "X-ray Fluorescence Analysis of Modified Cottons" by Tripp, Piccolo, Mitcbam and O'Connor. Textile Research Journal Vol 34, 1964, p. 773, and FMC Corp., American Viscose Div. information furnished by L. H. Phifer and W. B. Swann. 4 Ethyl cellulose phthalate is available from Distillation Products Industries, Rochester, NY 146S0, as Eastman Organic Chemical No. 7484. 5 Microcrystalline cellulose is available from FMC Corp., American Viscose Div., Avicel Sales, Marcus Hook, PA 19061, as Avicel PH-101. 6 Available from National Institute of Standards and Technology, Washington, DC 20899. Eastman White Label or similar grade, available from Eastman Kodak Co., 343 State St, Rochester, NY 14650, is generally sufficiently pure and may be substituted for the NIST material. DUP050296916 D 2929 BfBld for 30 s using a pressure of 5000 lb on the mold. The Sickness of the sample pellet should.be Vn in. or greater. f.2 Standardization ofInstrument: |, 2--Basic standardization techniques and operating parameters Hpy from instrument to instrument. The manufacturer's literature and H analyst's , knowledge of die performance characteristics of the IpKi'i*pm' ent s- hould he' used as a guide in performing this,1function., 3r 7.2.1 Place a standardization pellet in the sample holder Mind center it so that it covers the entire window of the Balder. Evacuate the X-ray path to a pressure of 0.5 mm Hg mm less, ifdesired) or flush the path with hydrogen or helium, raft the gas: flow of the proportional couhter'as suggested'by Ipe manufacturer. ' B 3: Precaution--X rays are very hazardous. The equipment Htould not be turned on until the instruction manual has been read and Understood. B 7.2.2 Set the goniometer-of the X-ray spectrograph at the (appropriate sulfur Ka angle. Turn the X-ray tube on, using mibe manufacturer's recommended voltage and current Selec tion of the operating voltage and currerifof thb Xfydy tube,,is Governed by the type of tube used. Take care not to exceed the rated power output (ip, watts) of the X-ray tube. Make a Blot ofthe sulfurX-ray intensity versus applied voltage to the detector. The voltage chosen should be approximately ijmidway on the plateau. p 7.2.3 If a pulse height analyzer is being used, a common Biway to arrive at the proper settings is to set the gain of the ijjlinear amplifier at approximately half of its maximum. Select the detector voltage about midway on the plateau. Set the minimum pulse rejection voltage at about 5 V and the & at about 10 V. Observe the intensityjvithout the pulse height analyzer on. With the pulse height analyzer on, change either nhe amplifier gain control or the detector voltage until as linear as possible the same intensity as without the analyzer is I obtained. Then increase or decrease the AE control just until ||a maximum intensity is reached. It 7.3 Calibration for Measurement ofSulfur: If 7.3.1 Select five or more representative cellulosic samples i whose sulfur contents, as determined by chemical analysis jjaecording to Methods D 817 or D 871, completely cover the ^required range. Since X-ray fluorescence intensities are lifunctions of concentrations per unit volume, prepare standifiards used to establish the calibration curve in a matrix as linearly identical to that of the sample as possible. The 1 sulfur-containing component should be distributed very | uniformly in the matrix. The physical form of the matrix 1 (powder, flake, pellet, or sheet) is a significant variable. For | accurate work it may be necessary to have separate calibraI tions for each form of sample. I 7.3.1.1 As a calibration standard for cellulose, micro| crystalline cellulose containing intimately mixed known I amounts of cystine may be used. A chemical analysis of the I standards is generally not necessary. I| 7.3.2 Prepare the samples for analysis according to 7.4 and 7.5. | 7.3.3 Measure the intensities of the sulfur Ka X rays of I the standard samples according to 7.6. I 7.3.4 Prepare a calibration curve relating sulfur Ka X-ray if intensity expressed as net counts per second to percent | sulfur. ? 7.4 Treatment ofSample Prior to Analysis: 7.4.1 To analyze for total sulfur content, no treatment is required prior to analysis. If the sample has a high absorbing coating (for example, saran, PVC, etc.) these should be removed or a standard containing a matrix ofthose materials in equivalent concentrations must be prepared. 7.4.2 When analyzing for combined sulfur content, as in a cellulose ester, remove the uncombined sulfur as follows: 7.4.2.1 Dissolve 25 g of sample in approximately 300 mL of acetone, depending on the viscosity. If the sample is of too high acetyl content to be directly soluble in acetone, cool in a dry ice cabinet dvemight, then allow to come to room temperature while tumbling or stirring. 7.4.2.2 Filter the solution, if necessary, through felt or a coarse sintered-glass crucible. 7.4.2.3 Precipitate with rapid stirring into a beaker or pail containing 2 to 3 L of acetic acid-water (1:49).. 7.4.2.4 Filter through a cloth bag or a Buchner funnel and give two 15-min washes with water using mechanical agita tion. A little Na2C03 may be added to the last wash to stabilize samples of high sulfur content. 7.4.2.5 Filter and dry overnight at 60C. 7.5 Preparation ofSpecimen for Analysis: 7.5.1 Grind the sample in a Wiley Mill to pass a 60-mesh screen. Mold a quantify, of the sample for 30 s with a gage pressure to 5000 lb on the mold. Use sufficient sample to obtain a disk at least `/i6 in. thick. 7.5.2 Film specimens can be run directly (without grinding) by using a multiplicity of sheet thicknesses pro vided that the specimen contains no air trapped between the successive layers. If film specimens are coated with a high absorbing coating (for example, saran, PVC, or aluminum), these must be removed if the specimens are to be analyzed as multiple thicknesses. Similarly, a closely wrapped specimen of continuous filament yarn can also be tested directly. 7.6 Measurement ofIntensity ofSulfur Ka X rays: 7.6.1 Place the specimen in the sample holder of the X-ray spectrograph and center so that it covers the entire- sample-holder window. 7.6.2 Evacuate the X-ray path to a pressure of 0.5 mm Hg or less or flush the path with hydrogen or helium. 7.6.3 Record the X-ray count for a standard time period at the sulfur Ka angle. 7.6.4 Repeat the count on the opposite side of the specimen pellet if homogeneity is questioned. - 7.6.5 If a sulfur-free specimen is available, record the background count. This is unnecessary if the standard's matrixes are identical to the samples. 4--A background count is desirable at all concentration levels. It is mandatory for measurement of sulfur concentrations under 100 ppm. 5--An indication of the precision of this test method is given by the standard counting error, which is: sc = + v 7V where: sc m standard counting error of JVX -- WB, ,VT = counts accumulated at sulfur Ka angle during counting interval dr, and ,VB = counts accumulated at background during same counting interval dr. This error level calculation should be used as a guide to counting time. 8. Calculation 8.1 Convert the standard time count values of the spec- DUP050296917 # D2929 imen and the background to counts per second. 8.2 If the background is measured subtract the back ground count rate from the count rate of the specimen pellet to obtain the net count rate of the specimen. 8.3 Convert the net count rate of the specimen to percent sulfur by using the calibration curve. 9. Precision and Bias 9.1 The precision of measurement, or standard deviation, <r, is calculated by normal statistical methods as follows. /2 (x - xf where: x = measured value, x = mean value of n measurements, and n = number of measurements.. 9.1.1 The practical significance of a is that 68 % of all1 results should be within l<r of the mean, 95 % with 2<r and 99.7 % within 3o. 9.1.2 Since random processes are involved in x-ray anal ysis, precision can also be determined from the fact that standard deviation is equal to the square root of the number of counts, N, collected. <rA'= ViV '9.1.3 It may be .more relevant to express precision in terms of the coefficient of variation, . which is the standard deviation as a percent of the number of countsas follows: Viv .. E = -- X 100 = T7= N ViV .. 9.2 Bias has not been evaluated for this test method. I The American Society lor 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 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 itnot revised, eitherreapproved or withdrawn. Your comments are Invitedeitherforrevision olthis 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 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. 398 DUP050296918 Designation: D 2998 - 89 Standard Test Method for Polyhydric Alcohols in Alkyd Resins1 This standard is issued under the fixed designation D 2998; 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 reapprovat. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. |jl. Scope t 1.1 This test method covers the qualitative and quantita tive determination of the polyols in alkyl resins, including jresin- and polymer-modified alkyds. Quantities as low as [0.5 % may be detected and measured, j' 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 japplicability of regulatory limitations prior to use. For a specific hazard statement, see Section 7. >r - ' - 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water2 [ E 260 Practice for Packed Column Gas Chromatography3 S3. Summary of Test Method [ 3.1 The resin sample is dried, subjected to aminolysis to [`release the polyols, treated directly-to form the trimethylsilyl, (TMS) ether derivatives of the polyhydric alcohols which are [separated by gas-liquid chromatography. An internal standard is used for quantitative purposes. The description of apparatus and the recommended operatihg conditions are presented as a guide to a satisfactory analysis as all suitable variations in temperatures, column lengths, substrates, liquid [phases, programming rates, etc., have not been determined. 4. Significance and Use f 4.1 This test method is designed to identify polyhydric i alcohols and to quantify amounts of polyols contained in alkyl iiesins. Polyols are significant ingredients in alkyl resins and impact on such important physical parameters of alkyd [ paints as weatherability, flexibility,-'moisture resistance, and adhesion. Use of this test method will provide a means whereby the relative applicability of the alkyd resin to the particular end use may be estimated by the buyer and the seller. 5. Apparatus 5.1 Linear Programmed Temperature Gas. Chromato graph--Any instrument with a thermal conductivity de- 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 1.33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally published asD2998-71. Last previous edition D2998 - 71 (1981)1. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 14.01. lector and with programming features should be suitable if adaptable to the following recommended-operating condi tions: . Detector cell temperature, "C Detector cell current, mA 300 160 Injection port temperature, 'C Helium flow at exit, cm5/nun Programmed temperature details: Approximate column hearing rate, 'C/min Starting column temperature,-"C Finishing column temperature, "C 300 80 6 100. 300 1--Flame ionization detectors are not recommended for this test as the reaction medium can contaminate the flame jet. 5.2 Column--A. 16-fit (4.9-m) length of `A-in. (6.4-mm) outside diameter copper tubing packed with 20 weight percent of silicone grease4 on 60 to 80-mesh flux-calcined diatomaceous earth,3 and conditioned at 315C until "bleeding" reaches a minimum. 5.3 Column and Instrument Performance--Note the sep aration of closely adjacent polyol peaks and express as peak resolution R as follows: R = 2Y/(A + B) where: Y = distance between maxima of closely adjacent peaks, A = base width of first peak A, and B = base width of peak B. 2--If the peak resolution is equal to or greater than 1.0, the column and instrument are in satisfactory condition. 5.4 Syringe, having a fixed needle, 50-pL capacity. 5.5 Erlenmeyer Flask, 125-mL, with standard joint and water-cooled condenser to fit. 5.6 Micro Test Tube or screw cap vial. 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 4 DC-11 manufactured by Dow-Coming, Midland, MI 48686, or GE SE-30 manufactured by General Electric Silicon Products Div., Waterford, NY 12188, has been found satisfactory for this purpose. 5 Chromosorb W available from Manville Sales Coip., Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108, has been found satisfactory for this purpose. 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." DUP050296919 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 II of Specification D 1193. 6.3 Bis(trimethylsilyl)trifluoroacetamide.7 6.4 1,4-Butanediol. 6.5 n-Butylamine. 6.6 Hexamethyldisilazane (HMDS). 6.7 Methylene Chloride. 6.8 Mixed TMS Reagent--Mix. 20 parts by volume of the bis(trimethylsilyl)trifluoroacetamide with 80 parts of the hexamethyldisilazane and protect from moisture. If stored at 60C in an oven, the reagent remains active and stable. 7. Hazards 7.1 The reagents and samples used in this test method may, under some conditions, be hazardous. Refer to the manufacturer's Material Safety Data Sheets for specific handling and safety precautions. Safe laboratory handling procedures and all applicable OSHA regulations are to be followed. * 8. Procedure 8.1 Weigh a specimen of resin containing approximately 2 g of nonvolatile material into the 125-mL flask. Add 3 mL of methylene chloride, mix, and evaporate, the solvents'jin a 60"C bath with a current of air: Repeat the drying twice, dissolving the resin each time in 3 mL of methylene chlbride. Check for odor of residual solvent and, if necessary, dissolve and dry a fourth time. . 8.2 Weigh accurately about 200 mg of 1,4-butanediQl (Note 3). as standard into the flask followed by 10 mL of butylamine added from a pipet. Reflux under the. water condenser for 2 h, add 0.5 mL of water to the flask through the condenser, and continue refluxing for 2 additional hours. 3--Other polyhydric. alcohols may be substituted for the 1,4-butanediol standard if sufficiently pure. 8.3 Place 5 drops ofthe amjnolysis mixture in a micro test tube, add 0.5 mL of the mixed TMS reagent,, and mix by shaking. Heat for 30 min at 60C in an oven. Inject 40 pL onto the silicone grease column of the chromatograph and follow the operating conditions recommended in 5.1. Hold the temperature at 300C at the completion of the program until all the volatile components have emerged as shown by the chromatogram. 9. Identification 9.1 The peaks on the chromatogram for the polyols can be identified by their relative retention times given in Table 1, if the recommended operating conditions are followed. Cali bration is always recommended and can be made by 7'Bis(trimethylsilyI)trifluoroacetamide is available from the Regis Chemical Co., 1101 N. Franklin St, Chicago, IL 60610, catalog number RC-1 and Pierce Chemical Co., Box 117, Rockford, IL6U0S. TABLE 1 Relative Retention Time of Trlmethylsilyl Ethers Polyol Retention Time Relative to 1,4-Butanediot Ethylene glycol . P/opylene glycql: 2.3-Butanediol 1,3-Butanedlol Neopentyl glycol 1,4-Butanedlol Diethylene glycol ...... Glycerol Trimethylol ethane Trlmethylol propane Triethylene glycol Pentaerythritol ` 0.58 0,63 0.73 0.83 0-86 1.00 1.19 1.29 1.46 1.63 1.83 1.88 ' applying the procedure to a synthetic mixture of polyols. 10. Calculation 10.1 Relate the height of each polyol peak to the height of the known amount of internal standard. Establish correction factors by dissolving known amounts (0.1 to 0.5 g) of the various polyols and internal standard in butylamine by wanning, and proceeding as in 8.3 for'derivative formation and chromatographing. For additional information on cali bration and standardization, see Section 9. of Practice E 260. 10.2 Calculate the percent polyol C as follows: C-(A x Fx P)I(Ix Sx N) where: A = height of polyol peak, mm, F = correction factor, : P = weight of internal standard, g x 100, I == height of standard peak, ,mm, iS. = weight of resm specimen, g, and , N = nonvolatile fraction. 4-r-Tbe nonvolatile fraction N may be. omitted from the calculation ifthe determination is preferred on a solution basis. 11. Precision _ ! '11.1 On the basis of an interlaboratory test of this test method in which one operator in six laboratories analyzed two alkyd resins containing 14.0 and 11.1 % glycerol, 6.8 and 7.2% pentaerythritol, and 4,2 %-ethylene.glycol,.the within- hnd, between-Iaboratory1 standard deviations were found to be as given in Table 2. Based' on these standard deviations, the following criteria should be used forjudging the acceptability of results at a 95 % confidence level': MAX Repeatability--Results obtained by the same analyst in two successive determinations should be considered suspect if they differ by more than the values given in Table 2. j .j { J j | j j ! TABLE 2 Precision of Test Method Polyol Repeatability Degrees of Freedom Standard Deviation Least Significant Difference ReproductoiSty Standard Deviation ~ 'Least Significant Difference Ethylene glycol Glycerol Pentaerythritol' 6 12 12 0.125 0.212 0.137 0.44 0.65 0.42 0.472 0.731 0.298 1.63 2.25 0.92 400 DUP050296920 | # D 2998 1.1.2 Reproducibility--iTwo results, each the mean of laboratories should be considered suspect if they differ by ilicate measurements, obtained by analysts in different more than the values given in the Table 2. TheAmerican 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 ofthe validity ofany such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision &any time by the responsible technical committee and must ba 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. i i I 401 DUP050296921 Designation: D 3021 - 82 (Reapproved 1987)*1 sudiimih:..' Standard Specification for Phthalocyanine Green Pigments1 This standard is issued under the fixed designation D 3021; the number immediately following the designation indicates-the year of original adoption or, ii^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. . "Note--Paragraph 4.1 was editorially changed in May-1987. "v* 1. Scope 1.1 This specification covers chlorinated and chlorinatedbrominated copper phthalocyanine green pigments in dry powder form, for use in paints, printing inks, and related products. A variety of commercial types are available to meet the requirements of different end uses. 2. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments12 D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out2 D 387 Test Method for Color and Strength of Color Pig ments with a Mechanical Muller2 D1135 Test Methods for Chemical Analysis of Blue Pig ments2 3. Composition and Properties 3.1 The pigments shall consist of the product known com mercially as phthalocyanine green, with or without phthalocyanine blue or other ingredients incorporated during man ufacture to improve or alter the properties of the pigment, but free of any other coloring matter either organic or inor ganic. The pigment shall conform to the following require ments: Moisture and other volatile matter, max, % Coloring matter other than phthalocyanines 3.0 none 3.2 Mass Color and Character of Tint--The mass color, and the character ofthe tint formed by mixture with a white pigment, and the strength, shall be within mutually agreedupon limits of a standard acceptable to both the purchaser and the seller. 3.3 Oil Absorption--The oil absorption shall be between 90 and 110 % of that of a reference sample mutually agreed upon between the purchaser and the seller. 3.4 Reaction in Identification Tests--The pigment shall show the same reaction in identification tests (5.5 to 5.8) as a reference sample mutually agreed upon between the pur chaser and the seller. 1 This specification 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 1.31 on Pigment Specifications. Current edition approved June 25, 1982. Published August 1982. Originally published as D 302 i - 72. Last previous edition D 3021 - 72 (1976). 2 Annual Book ofASTM Standards, Vol 06.02. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of |j production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken S from different packages in the ratio of two samples for each 5 tons (inch-pound or SI), except that for shipments of less than 1000 lb, two samples shall be taken. At the option ofthe purchaser, each sample may be tested or samples from the same production may be blended in equal quantities to form j a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures not cov ered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.2 Moisture and Other Volatile Matter--Method A of Test Methods D 280. 5.3 Mass Color and Tinting Strength--Test Method D 387. 5.4 Oil Absorption--Test Method D 281. 5.5 Identification: 5.5.1 To about 50 mg of the sample in a 50-mL-beaker, add 30 mL of H2S04 (sp gr 1.84). Stir occasionally for 15, min, heating if necessary. A dark greenish yellow to a dark reddish color forms, depending on the- degree of bromination. Pour the solution into-250 mL.of water and stir. Hie phthalocyanine green will immediately precipitate as a flocculent mass. 5.5.2 Filter off the precipitate, washing once or twice with water. Scrape a small amount of the precipitate off the filter, place on a clean platinum wire moistened vvith HQ, and subject it to the low flame of a bunsen burner. As the precipitate burns, a light blue-green flame should be clearly evident, indicating organically combined copper. --Characteristic spectrophotometric absorption spectra in the near infrared range (700 to 900 nm) are exhibited by dilute solutions of copper phthalocyanine pigments (2 to 50 mg/L) in H2S04 (sp gr 1.84). The absorption maxima are so sharp and well defined that they may be used for positive qualitative identification ofthe various phthalocyanine pigments. Phthalocyanine green has maxima at approximately 820 and 860 nm for bromine-free types; for the chlorinated-brominated types, the maxima appear at approximately 830 to 840 nm, and 875 to 885 nm. 5.6 Basic Dye Derivatives--Test Method D 1135. 5.7 Other Organic Coloring Matter--Test Method D 1135. 5.8 Chrome Green and Iron Blue--Test Method D 1135. 402 DUP050296922 # D 3021 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'ls subject to revision at arijr time 6y the responsible technical Committee and must be revlbwed every five ydars and Ifnot revised, either raapprovad orwithdrawn. Your comments are Invited either forrevision ofthisstandard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ol (ha 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, DUP050296923 Designation: D 3022 - 84 (Reapproved 1989)' Standard Test Method for Color and Strength of Color Pigments by Use of a Miniature Sandmiil1 This standard is issued under the fixed designation D 3022; 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. Editorial changes were made throughout in March 1989. 1. Scope 1.1 This test method covers the determination, through the use of a miniature sandmiil, of the color and strength of dry color pigments. 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 Section 6. 2. Referenced Documents 2.1 ASTM Standards: C 778 Specification for S tandard Sand12 D 235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)3 D523 Test Method Tor Specular Gloss4 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry5 E 308 Test Method for Computing the Colors of Objects by Using the CIE System6 7 2.2 Federal Specifications:1 TT-R-266 Resin, Alkyd; Solutions 3. Significance and Use 3.1 This test method is a way of testing the color and strength of pigments by use of a miniature sandmiil. It correlates well with industrial practice and is used for routine i quality control. ! i 4. Apparatus 4.1 Balance, sensitive to 10 mg with a capacity in excess of 300 g. ! 4.2 Miniature Sandmiil--A laboratory disperser equipped ! with a l5/8-in. (41-mm) diameter fiber rotaiy disk impeller rotating at a constant 8000 r/min under varying load : conditions. The shaft upon which the impeller is mounted i shall be sufficiently balanced so no whip of the shaft is j observed between 0 and 10 000 r/min.8 8 9 10 11 4.3 Cylinder, 100-mL graduated. ; 4.4 Beakers, 200-mL tail-form, stainless steel, or polyeth- j ylene (approximately 60-mm inside diameter). } 4.5 Strainers, paper cone, disposable, about 40 mesh. j 4.6 Fiber Disks, ls/s-in. (41-mm) diameter phenolic lam- "s'j inated, Vi in. (6 mm) thick.9 j 4.7 Paper Charts, smooth, surface-coated, the surface of ) which should be impervious to paint liquids.10 \ 4.8 Film Applicator, with an 8-mil (200-pm) clearance at j least 3 in. (75 mm) wide. _j 4.9 Color-Measuring Instruments, as defined in Method . E 97 or Practice E 308. 5. Materials --, 5.1 Samples of standard reference pigments as agreed between the purchaser and the seller. 5.2 Standard Sand--Regular 20 to 30mesh (850 to 600-jim) cement testing sand conforming to Specification C 778. The sand shall be screened to remove allsub 30-mesh particles. Twenty to thirty-mesh glass beads may be used instead of sand.11 j j I ; 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 April 27, 1984. Published July 1984. Originally published as D 3022 - 72. Last previous edition D 3022 - 72 (1978). 2 Annual Book ofASTM Standards, Vol 04.01. 3 Annual Book ofASTM Standards, Vol 06.03. * Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 6 Annual Book ofASTM Standards, Vol 14.02. 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-S094. 8 The Sherwin-Williams miniature sandmiil has been found satisfactory for this purpose. Drawings are available from ASTM Headquarters. Order PCN 12430-220-14. 9 Suitable disks are available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. 10 White and black charts available from The Leneta Co., P. O. Box 576, Ho-Ho-Kus, NX 07423 have been found satisfactory for this purpose. Equivalent charts maybe used. 11 Sand is available from Agsco Division, American Graded Sand Co., 189 E. 7th St., Patterson, NX 07524. Glass beads are available from Quackenbusch Co., P. O. Box 607, Palatine, 1L 60067. 404 DUP050296924 # D 3022 20 30 4Q, 50 60 70 80 . FIG. 1 ' (SI Absorption Spatula Procedure 90 15.3 Grinding Vehicle--A long oil alkyd12 meeting U.S. Fed. Spec. TT-R-266 Tjgpe 1-A reduced to 47 % solids with mineral Spirits conforming to Specification D 23_5 (2 parts ill^yd and .1 part mineral spirits by weight). ' ' 5.4 White Tinting Palm?--A flat white tinting paint com- |fetible with the dispersion vehicle meeting'ihe following requirements. ' < 5.4.1 Gloss (60) less than 4, as determined by Test Method D 523. . 5.4.2 Contrast Ratio (2-mil (51-pm) dry film): 99.2 min. 5.5 Drier Blend--One part 6 % manganese naphthenate, 2 parts 6 % cobalt naphthenate, and 4 parts 24% lead i naphthenate by weight. 6. Hazards 6.1 While operating the mill, keep hands well away from the shaft and disk and be sure that no article of clothing (for I example, necktie or long hair) will catch on moving parts. This precaution applies to all cases where the mill is in ;; operation. ; 12 A long oil soya or safflower alkyd at 70 % solids with the following characteristics: Nonvolatile 70 1 %, phthalic anhydride 23 % min, fatty acids 60 tto 65 %, dihydric alcohol 4 % max, acid number 5 to 10, specific gravity : 0.950-0.970, Gardner color 10. 7. Procedure for Mass Color til Weigh to the nearest 10 mg an appropriate amount of pigment to. be tested into, a 200-mL tail-form beaker. (The qm^unt of pigment needed can be,calculated jrom the graph shown ins Fig., 1.; or obtained froni the table on the graph.) To the pigment in the beaker carefully weigh in 55-00 0.01 g of the Jong oil alkyd grindirig vehicle (Note 1). Then add 60 mL of 20 to 30-mesh sand from a graduated cylinder and 1.00 0.01 g of the drier blend: Stir the sand, vehicle,, and pigment with a spatula until the pigment is completely wetted. . ': --For routine control, grinding vehicle, drier blend, and white tint paint can be placed in the type ofdispensers used in stores to tint custom colors. The following amounts are recommended: 2 fluid oz each of vehicle and of white paint, Vi oz-drier. The dispenser shall be reproducible to 2 parts per thousand when dispensing 1-oz charges. - 7.2 Carefully clamp the beaker on the miniature sandmill and adjust the height of the disk so that it is between % and 1 in. (20 to 25 mm) above the bottom ofthe beaker. Turn on the mill and disperse for exactly 10 min, unless otherwise agreed upon, at a shaft speed of 8000 r/min, accurately timing the length of dispersion with a stopwatch or other suitable timing device. [ 405 DUP050296925 #) D 3022 2--For norma! control procedure, a 10-min dispersion interval will be sufficient. For ultimate color development use the procedure in ' Annex Al. 7.3 Shut off the mill and raise the impeller until it is just clear of the liquid, in the beaker and turn the mill on again for a few seconds to remove excess mill base from the impeller. 7.4 Remove the material from the mill and filter into a suitable container through a cone strainer or equivalent 40-mesh (420-pm) disposable screen. 7.5 Repeat the foregoing procedure with the standard reference pigment. 7.6 Draw the test and standard dispersions down simulta neously on a paper chart over a vacuum drawdown plate or other suitable plane surface using the applicator bar specified in 4.8. Compare the color visually while still wet and then set aside in a dust-free area to dry. If desired, evaluate the color difference instrumentally by Method D 2244. Report color, difference in units agreed upon between- purchaser and seller.: 8. Procedure for Tint Color 8.1 From the receiving-container used in 7.4, weigh 5.000 0.010 g of the strained mill base into a 200-mL beaker and add 100.00 0.05 g of white tinting paint. 8.2 Place the beaker on the mill (without sand) and mix at 8000 r/min for 5 min. 3--Some' mill bases require vigorous agitation when-being dispersed into the paint. Normal agitation on a paint shaker is not satisfactory. '. . 8.3 Repeat the above procedure with the standard refer- , ence material and then-proceed as directed in 7.6. 8.4 To determine the relative tinting strength of the test material as compared to the standard at the wavelength of maximum absorbance, or at a wavelength agreed upon be tween purchaser and seller, employ the following procedure. 8.4.1 If the spectrophotometric curves cross or otherwise deviate from a relationship characteristic of effectively iden tical materials, the method is inapplicable (that is, the method is not applicable to metameric specimens). 8.4.2 When spectrophotometers or abridged spectropho tometers are used as color-measuring instruments, determine the lowest reflectance reading between 420 and 680 mm, or at the agreed band of wavelengths, and use it in the calculation. Read and record the reflectance to at least the nearest 0.001 reflectance unit. 8.4.3 With color-measuring instruments that employ broad wavelength filters, use the lowest reflectance obtained, or the reflectance from the agreed filter, in the calculations. Read and record the reflectance to at least the nearest 0.001 reflectance unit. !"# 4--The calculation is based on theory that, strictly interpreted, requires for the types of material being tested, use of a spectrophotom eter or abridged spectrophotometer. However, many users of this test method obtain satisfactory results using color-measuring instruments equipped with broad wavelength fibers. i 8.4.4 Calculate the tinting strength, of color pigments as follows: T,, T[(\ - RJ2/2 RJU [(I - R,,)2/2 +$s where: TS = tinting strength, R = measured reflectance and subscript means reflec tance of material under test (that is, unknown) and "s" means reflectance of standard reference material, and T -- assigned TS of the standard reference material, fre quently assigned, at "100" so that TS is in percent of standard. 9. Precision 9.1 On the basis of an interlaboratory study of this test ; method in which two operators in five laboratories tested five 5 pigments on each of two days, the precision was found to be I as shown. ;j 9.2 Mass Color--The within-laboratory standard devia- j tion was found to be 0.97 MacAdam color-difference units ] and the between-laboratory standard deviation 1.14 units. ! Based on these standard deviations the following criteria j should be used for judging the acceptability of results at the '4 95 % confidence level: 9.2.1 Repeatability--Two results obtained in the same laboratory should be considered suspect if they differ by more than 2.7 MacAdam units. 9.2.2 Reproducibility--Two results obtained by operators in different laboratories should be considered suspect if they differ by more than 3.2 MacAdam units. 1 9.3 Tint Strength--The within-laboratoiy standard devia tion was found to be 2.74 % and the between-laboratory standard deviation 3.46 %. Based on these-standard'devia tions, the following criteria should be used for judging the acceptability of results at the 95 % confidence level. j 9.3.1 Repeatability--Two results obtained in the same j laboratory should be considered suspect if they differ by j more than 7.7 %. 9.3.2 Reproducibility--Two results obtained by operators j in different laboratories should be considered suspect if they differ by more than 9.7 %. ANNEX (Mandatory Information) Al. DETERMINATION OF MAXIMUM COLOR A 1.1 In some cases it may be desirable to determine the maximum color obtainable by this procedure. In this case Section 7 may be modified as follows: A 1.1.1 Carefully determine the total weight of the dispersion mixture and container. Place on the mill and disperse for 10 min. After spinning the impeller free of excess mate- 406 DUP050296926 D 3022 reweigh the container and bring back to the original pight with solvent. Carefully mix the added solvent back |o the dispersion and extract 2 g of sandfree base, reduce 50 g of white paint, and prepare a drawdown. Repeat above process at 10-min intervals until no further inlease in tint strength occurs. Note the time at which maxi mum tinting strength occurs and record for future reference. A 1.1.2 Subsequent samples of this pigment can then be run for the optimum length of dispersion time. However, solvent lost during dispersing must be replaced periodically so that viscosity variations will not affect the rate of disper sion. The American Society tor Testing end Materials takes 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 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 ASTMHeadquarters. 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 1S103. p- 407 DUP050296927 Designation: D 3132 - 84 (Reapproved 1990)e1 Standard Test Method for Solubility Range of Resins and Polymers1 This standard is issued under the fixed designation D 3132; 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. % &'()*Section 10 was added editorially in May 1990. 1. Scope 1.1 This test method covers determination of the solu bility of resins and polymers in terms of the region of solubility parameter and hydrogen bonding of solvents in which complete solution occurs. In some cases dipole moment of the solvents may also be required to delineate more exactly the boundaries of solubility. 1.2 This test method is applicable only if the test solutions are of sufficient clarity and freedom from color to allow accurate visual judgement of complete solubility and of low enough viscosity for solution to take place. 1.3 This standard does not purport to address all of the safetyproblems 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 in 6.2. 2. Terminology 2.1 Definitions: 2.1.1 The solubility parameter 5 of a substance is defined as the square root ofthe "cohesive energy density," or energy of vaporization per unit volume: 8 = (A/ Vjh where: AE = energy of vaporization, and F = molar volume. The value of 5 for a volatile liquid can be calculated accurately from the latent heat of vaporization, or approxi mately from its boiling point. Solubility parameter values for large number of solvents are available in Table 1. 2.1.2 Solvents are also' classified according to their hy drogen bonding power, 7. Numerical values for 7 may be derived from spectroscopic analysis. In one method,12 7 is defined as one-tenth the wavenumber shift observed by Gordy's technique,3 and values range from 0 to about 25. 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 D01.33 on Polymers and Resins. Current edition approved Aug. 31, 1984. Published January 1985. Originally published as D 3132 - 72. Last previous edition D 3132 - 72 (1984). 1 Crowley, J. D.,et at, "A Three Dimensional Approach to Solubility," Journal ofPaini Technology, JPIRA, Vol 38, No. 496, 1966, p. 269; Vo) 39, No. 504,1967, p. 19. 3 Gordy, W., "Spectroscopic Evidence of Hydrogen Bonds," Journal of Chem ical Physics, JCPSA, February 1939, February 1940, March, 1941. Another method,4 which limits values of7 to the range of 2.2 ij to 10, defines 7 by the following equation: !| 7 = (0.0359 x Ax) + 2.2 j| where v is the wavenumber shift as determined by GordyVi method. Hydrocarbons, halogenated hydrocarbons andf nitro-hydrocarbons have low values of 7; esters, ethers, I ether-alcohols, and ketones are intermediate; and alcohols, | amines, and acids have high values. I 2.1.3 The solubility parameter Sm, of a mixture of solvents j having parameters, S2, etc., is a function of the molar I fraction and molar volume of the components: 1 (8txIVl + 82X2^2)Kxi F + x2 F2) I in which Xj and Vh x2 and V2, etc., are the corresponding 1 molar fractions and volumes, respectively. Ifthe components I have the same molar volumes (F, = Vfi, I 8m -- + *282 I Thus, in a mixture of two components. A and B having the j same molar volumes and solubility parameter values of SA | and SB ,,| _ (volume percent A x iA) + (volume percent B x $B) ~ 100 2.1.4 Similarly, the hydrogen bonding value, ym, of a mixture is determined by: _ (volume percent A x 7A) + (volume percent B x yB) ~ 100-- .- and dipole moment by: _ (volume percent A x nA) + (volume percent B x |xB) lL'n~ 100 3. Summary of Test Method 3.1 Solubility of resinous and polymeric materials is dependent upon the solubility parameter, hydrogen bonding, and dipole moment of the solvents. Solubility parameter is the most important property of the three, followed by hydrogen bonding. Consequently, the solubility of most materials is sufficiently defined by the area af solubility parameter and hydrogen bonding oftrue solvents. A material is insoluble or incompletely soluble in a solvent if its solubility parameter and hydrogen bonding properties fall 4 E. I. du Pont de Nemours & Co., Bulletin PA 12-770, "Solvent Formulating Maps for Elvacite Acrylic Resins, Serial A-70562, July 1970. 408 DUP050296928 # D 3132 Ifairfe this region. '3.2 In this test method, the material is tested separately in blvents that cover the entire solubility diagram so that iundaries of complete solubility can be determined. 4. Significance and Use 4.1 This test method is useful for an emperical determina- tion of the solvents) in which a resin or polymer may be dissolved. This test method is also applicable to estimate the TABLE 1 Solvent or Solvent Mixtures Solvent or Solvent Mixture (Mixture Soiubifity Hydrogen Bonding Dipole NO. Given in Volume Percent) Parameter, 8 tA ya Mornent,0 p r Diisopropyl ether 2 n-Pentane 3* n-Heptane 4 SO % Diisobutyl ketone SO % Diisopropyl ether S' Diethyl ether 6' 50 % n-Heptane 50 % Dlisobuty! ketone 7 25 % n-Heptane 75 % Diisobutyl ketone 8 Methyl cyclohexane 9 66.7 % n-Heptane 33.3 % n-Butyl Acetate 10* Diisobutyl ketone 11* 57 % Diethyl ether 43 % n-Butyt acetate 12 66.7 % Diethyl ether 33.3 % 2-Ethylhexanol 13* Cyclohexane 14 40 % n-Heptane 60 % n-Butyl acetate IS 71 % Cyclohexane 29 % Toluene 16* n-Butyl acetate 17* 40 % Cyclohexane 60 %Toluene 18 50 % Cyclohexane 50 % Benzene 19 50 X'n-Butyl acetate 50 % Toluene 20 50 % EGMBE (See No. 23) 50 % n-Butyl acetate 21* 33.3 % Diethyl ether 66.7 % 2-Ethylhexanol 22* Toluene 23 2-Butoxyethanol 24* Benzene 25 Propylene oxide 26 56 % EGMBE 44 % 2-Ethylhexanol 27 50 % Methylene chloride 50 % Toluene 28* 50 % Toluene 50 % Dioxane 29* 2-Ethylhexanol 30 Methyl acetate 31* Methylene chloride 32 66.7 % Methylene chloride 33.3 % Dioxane 33 50 % Dioxane 50 % Methylene chloride 34* Dioxane 35 Cyclohexanone 36* 2-Ethoxyethanol 37 75 % EGMEE 25 % Methyl Isobutyl carblnol 38* Carbon disulfide 39 30 % EGMEE 70 % Methyl Isobutyl carblnol 40 Methyl isobutyl carblnol 41 66.7 % Methylene chloride 33.3 % Nitroethane 42 66.7 % Dioxane 33.3 % Nitroethane 43* 50 % Toluene 50 % Acetonitrile 44* 50 % EGMEE 6.9 11.7 6.6 1.3 7.0 0 2.2 0 7.3 0 2.2 0 7.4 10.1 5.9 2.0 7.4 13.0 6.9 12 7.6 4.2 3.7 1.4 7.7 6.3 4.5 2.0 7.8 0 2.2 0 7.8 2.9 3.3 0.6 7.8 8.4 5.2 2.7 7.9 11.2 6.3 1.5 8.1 14.9 7.6 1.4 8.2 0 2.2 0 8.2 5.3 4.1 1.1 8.4 1.3 2.7 0.1 8.5 8.8 5.4 1.9 8.6 2.7 3.2 0.2 8.7 0 22. 0 8.7 6.7 4.6 1.2 8.7 10.9 62 1.8 8.8 16.8 8.2 1.5 8.9 AS 3.8 0.4 8.9 13.0' 8.9 1.6 9.2 0 22 0 9.2 10.0 5.8 1.8 9.2 15.5 7.8 1.8 .9.3 3.0 3.3 1.0 9.4 7.1 4.8 0.4 9.5 18.7 8.9 17 9.6 8.4 5.2 1.7 9.7 1.5 2.7 1.5 9.8 4.2 3.7 1.1 9.8 5:6 4.2 1.0 9.9 9.7 5.7 0.49.9 11.7 6.4 2.7 9.9 13.0 6.9 1.6 9.9 14.4 7.4 1.6 10.0 0 2.2 0 10.0 17.0 8.2 1.7 10.0 18.7 8.8 1.7 10.2 1.8 2.8 22 10.3 7.3 4.8 1.5 10.4 5.4 4.2 2.2 10.4 15.9 7.9 1.7 m DU P0502 96929 No. 45' 46 47 48 49 50 51 52 53 54 55* 56 57* 58' 59 BO* . .61* 62 63* 64 65 66 67 68* 69 70 71* 72 73 . 74 75 76* 77* 78* 79* 80 81* 82 83 D 3132 TABLE 1 Solvent or Solvent Mixture (Mixture Given In Volume.Percent) 50 % n-Amyl alcohol ! 2-Ethylbutanol 33.3 x Methylene chloride 66.7 X Nitroethane . 75.x Nltroethane ............................... . 25 x Dioxane 75 x-Dioxane 25 % Propylene carbonate Dimethylacetamide 80 % EGMEE 20 X Methanol 33.3 % EGMEE 66.7 X n-Butano! n-Amyl alcohol (pentanol) 48 % Benzene 52 .x Nitromethane 50 x Dioxane 50 x.Dimethylformamlde Nitroethane 25X n-Butyl acetate 75 X Acetonitrile n-Butanol .. 50 X Nitroethane 50 X Acetonitrile 65 X EGMEE 35 % Methanol 66.7 X n-Butano! 33.3 X Dimethylformamide 50 x Dioxane 50 X Dimethyl sulfoxide 50 X Nitroethane 50 X Nitromethane ! Acetonltrle 30 X n-Butanol 70 X Dimethylformamide n-Propanol * 70 X"Acetonitrile 30. X Dimethylformamide 68 X Dimethylformamide 32 X Acetonitrile Dimethylformamide 50 X n-Propanol 50 X Ethanol ., 60 X Nitromethane 40 % Acetonitrile 50 X Ethanol 50 x Dimethylformamide 23 X Dioxane 77 x Propylene carbonate 40 X Dimethylformamide 60' X Dimethyl sulfoxide 70 X Ethanol 30.x; Dimethylformamide 80* X Dimethylformamide 20 x Methanol Nitromethane Ethanol 72 X Dimethyl sulfoxide 28 X Ethanol Dimethyl sulfoxide 46 X Methanol 54 X Dimethylformamide Propylene carbonate 60 x Dimethyl sulfoxide 20 X Methanol 70 X Dimethylformamide 30 x Monomethylformamide Continued Solubilitv Parameter, 5 Hydrogen Bonding . y . t y 10.5 18.7 10.6 2.2 10.8 4.3 10.8 8.5 10.8 12.3 10.8 14.1 10.9. ,, ' 18.8 10.9 11.ft 11.0 . 18.7 1.3 , 10.7 11.1 11.1. . 2.6 8,9 11.4 18.7 11.5 4-4 11.5,. 15.0 11.6 16.4 11.7 . 8,7 11.9 . 2.5 11.9 . ' 6.3 n.9 ., _ 13.8 11.9 12.0 " ' 18.7 8.0 12.0 . 10.0 12.1 11.7 12.3 18.7 12.4 ; 4;o 12.4 12,5 ... , t ' 1v52 6.9 12.6-- , , 9.3 12.6 , 16,6 12.6 . 13.1 12.7 2.5 12.8 18.7 12.9 10.8 13.0 ' 7.7 13.2 14.9 13.3 13.3 4.9 9.9 13.3 11.8 8.9 3.0 3.8 5.3 6.6 7.3 8.2 8.9 2.7 5.6 3.1 4.5 8.9 3.8 7.6 8.2 5.4 3.1 4.5 7.2 8.9.... 5.1 56 6.4 8.9 3.7 7.7 . __ 4.4 5.6 8.2 6.9 3.1 8.9 6.1 5.0 7.6 4.0 5.8 7.0 Dipole Moment,0 p 1.7 2.9 2.8 1.6 3.8 1.6 1.7 1.7 1.8 2.1 3.6 3.4 1.7 3.8 1.6 2.4 2.2 3.5 3.9 36 1.7 3.9 3.8 3.8 1.7 3!5 2.6 3.9 3.9 , ,, 2.3 3.4 3.4 1.7 3.4 4.0 2.8 5.0 .... .3.5 3.8 410 DUP050296930 No. Solvent or Solvent Mixture (Mixture Given in Volume Percent) Solubility Parameter, 5 Hydrogen Bonding yA yB Dipole Moment, '84 85* 86* 87* .88' 89 90 50 % Ethanol SO % Methanol 65.7 % Methanol 33.3 % Dirnelhylforrnamide 57 % Methanol 43 X Dimethyl sulfoxide' ' Methanol.,' Propylene glycol 63 % Methanol 37 % Mdnomethylformamide Ethyleneglycol > 13.6 13.7 13.9 i- 14.5 16.0 15.1 17.1 18.7 16.4. 14.0 18.7 20.6 16.2 20.6 8.9 1.7 8.1 2.4 7.8 2.7 8,9 1.7 9.4 2.2 8.8 2.5 9.6 2.3 A Crowley, Ji D., ef al, "A Three Dimensional Approach to Solubility," Journal of Paint Technology, VOI38, No. 496,1966, p 269; Vol39, No. 504,1967, p. 19. B E. I. du Pont de Nemours & Co., Bulletin PA 12-770, "Solvent Formulating Maps for Elvaclte Acrylic Resins," Serial A-70562, July 1970. 0 McLellan, A. L.,,Tables ot Bxperimental Dipole Moments, VI..H. Freeman & Co., San Francisco, 1963. ^solvents that may be useful for further dilution of a polymer Sr , resin solution without formation of haze or without polymer or resin precipitation. f|r. Apparatus 5.1 Glass Vials, with screw caps, capacity 5 to 20 mL. 5.2 Mixing Rolls, Tumblers, or Other Rotary Mixing f,Machine. ! 6. Reagents and Materials 6.1 Solvents and solvent mixtures used in this test method are listed in Table 1, in order of increasing solubility piparameter. Those with an asterisk, can be used in a prelimijnary survey to establish the general areas of solubility and I honsolubility. Intermediate solvents'are then used to define toore closely the solubility limits of a resin. 6.2 Quality of Solvents--Each solvent should be a good P technical or commercial grade containing not less than 95 %, but preferably 99 %, of the specified compound and should |be essentially anhydrous (<0.3 percent water). ,-./ Warning--Diethyl ether, diisopropyl ether, and dioxane may IJfonn explosive peroxides on long storage, particularly if kept in glass pottles exposed to light. 6.3 Solvent mixtures, which are in volume percent, should be made by adding solvent from burets that have been washed with diethyl ether, dried at 65C and rinsed | twice with solvent before filling. Bottles containing mixtures j should be tightly capped to prevent evaporation. Condensate f above the liquid level should be well mixed in before using 7.Procedure 7.1 Preparation ofSolutions: ' 7.1.1 The ratio of solute to solvent should correspond as much as possible to the intended use of the material but should be chosen to avoid difficulty in effecting solution because the viscosity must be low enough for mixing to take place. For most film-formers the concentration range is from 40 % for low molecular weight resins to 10 % for polymers that give viscous solutions. 7.1.2 The precision of weighing the solute and solvent should ensure a maximum deviation of 5 % in the desired concentration in each series of tests. Report the test concen tration with the results since the solubility parameter range is somewhat dependent upon concentration. 7.1.3 Dry the clean vials at 65C and label or mark them. Select vials that are sufficiently large to promote flow of viscous solutions. A 15-mL vial containing 5 g of solution has been found satisfactory; 7.1.4 Reduce'large lumps of aggregates in tile resin or polymer to a convenient size by means that do not introduce contamination but not to a fine powder that may lead to packing or oxidation. With resins that give solutions of low viscosity, the solvent may be added to the solute or vice versa. The former is usually more convenient as the material can first be weighed into all the vials followed by the selected solvents. With high molecular weight resins that tend to gel, the order of addition markedly affects the time required to dissolve the resin and eliminate gel particles. Consequently, the solvent should be weighed into the vial and then the specimen ip small portions. 7.1.5 In either procedure, after adding the correct amounts of solute and solvent, cap the vial tightly and mix the contents by shaking or swirling. Tumble or rotate the vials end-over-end for 24 h. One method is to place the vials in a quart or gallon can with their long axes perpendicular to the long axis ofthe can and rotate the can at a slow speed On mixing rolls. The rate of rotation should not be so fast as to prevent back and forth flow in the vials. One to five revolutions per minute are suitable speeds.. _ _ 7.2 Interpretation ofResults: 7.2.1 At the encTof 24 h line up the vials for observation. Allow to stand for a few minutes and then classify the appearance of the contents according to the" following ratings: 7.2.1.1 Complete Solution--A single, clear liquid phase with no distinct solid or gel particles. 7.2.1.2 Borderline Solution--Cloudy or turbid but without distinct phase separation. 7.2.1.3 InsohMe--Two phases: either a liquid with sepa rate gel or solid phase or two separate liquids. 1.2.2 Maintain borderline samples at 20 to 27C for 7 days and observe again to determine if the classification has changed. 7.2.3 Plot the solubility results on a graph using solubility parameter as abscissa, hydrogen bonding as ordinate, and symbols to distinguish the three solubility classes. 7.2.4 Identify areas of complete solubility and insolubility and select additional solvents from Table 1 to define more closely the solubility limits of the resin. Repeat the test with these solvents and also with any that produced anomalous 411 DUP050296931 D 3132 results, for example, borderline or insoluble between two complete solutions. 7.2.5 Plot the additional test results and draw in the limits ofsolubility. If anomalies are still present it may be necessary to plot solubility parameter versus dipole moment at eight levels of hydrogen bonding and draw in solubility limits (contour lines) for each level. 7.2.6 The solubility classification in 7.2.1 uses the simpli fied approach that there are no differences within the soluble and insoluble regions. Actually, it is possible to distinguish degrees of solubility and insolubility. The latter ranges from settling of an apparent or borderline solution, through various levels ofgelling and wetting, to complete insolubility when the resin is absolutely unaffected by the solvent Similarly in the soluble region, not all solutions are identical. With resins that are high in molecular weight or have a wide range in molecular weight distribution, there may be only a few solvents that produce perfectly clear solutions. The other solutions may vary from being slightly cloudy to fairly turbid. Viscosity measurements on the solution, allowing for solvent viscosity, might be used to determine the area ofbest solubility. Contour lines of degrees of solubility could be drawn if sufficient solvents were tested. 7.2.7 Because there is this gradation from complete, solu bility to total insolubility, where the borderline is placed may be a matter ofpersonal choice or the end-use of the polymer. High clarity may be required for an unpigmented solution while some turbidity might be acceptable if the material wifi be pigmented in use. 8. Report 8.1 Results ofthis test are preferably presented in the form of a graph showing the region of solubility for the material under test. For written reports, state the minimum and maximum solubility parameter, fi, and hydrogen bonding, y, at which solution took place. If desired, the solubility parameter limits at several levels ofhydrogen bonding can be given. 8.2 Report the concentration of resin used in the tests. 9. Precision 9.1 No statement of precision is at present available for this test method. 10. Keywords 10.1 dilution ratio; resin solubility; solubility parameters of resins The American Society (or 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 ol the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This steindard is subject to revision at any time by the responsible techhical 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 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 ABTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. MSt is 412 DUP050296932 I)) Designation: D 3256 - 86 (Reapproved 1991)41 Standard Test Methods for Chemical Analysis of Phthalocyanine Blue and Green Pigments1 This standard is issued under the fixed designation D 3256; 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. 0 1234--Keywords were added editorially in January 1991. ' ft. Scope 1.1 These test methods cover procedures for the qualitaive chemical analysis of pigments known commercially as :opper phthalocyanine blue and green. 1.2 The procedures appear in the following order: Section Identification............................................................................................... 5 Moisture and Other Volatile Matter................ ................................ 6 Detection of Basic Dye Derivatives..................................................... 7 Detection of Other Organic Coloring Matter............................................ 8 tection of Ultramarine Blue.................................................................... 9 tection of Iron Blue or Chrome Green.......... ................................. 10 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe [uhseearlthopfrtahcitsicestsaannddarddetteor-meisnteabthlieshapapplpicraobpirliiatyteofsraefgetuylaatonrdy limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments2l D1193 Specification for Reagent Water3 3. Significance and Use . 3.1 These test methods are suitable for determining if impurities are present and establishing that the required pigments are present. These test methods may be used for manufacturing and purchasing quality control. 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- I leal Society, where such specifications are available.4 Other l(% 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 j Subcommittee D 01.21 on Chemical Analysis of Paints and Paint Materials. 1 Current edition approved March 27, 1986. Published May 1986. Originally I published as D 3256 - 73. Last previous edition D 3256 - 73. I 2 Annual Book ofASTM Standards, Vol 06.02. j 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 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," by | Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 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. 4.2 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. 5. Identification 5.1 To about 0.05 g of the sample in a 50-mL beaker, add 30 mL of sulfuric acid (H2S04, sp gr 1.84). Stir occasionally for 15 min, heating if necessary to accelerate the solution of the pigment Formation of a dark greenish yellow solution indicates phthalocyanine blue and a dark reddish color indicates bronfinated green pigment, Pour the solution into 250 mL of water and stir. The phthalocyanine pigment should immediately precipitate as a flocculent mass. 5.2 Filter off the precipitate, washing once or twice with water. Scrape a small amount of the precipitate off the filter, place on a clean platinum wire moistened with hydrochloric acid (HC1), and subject it to the low flame ofa bunsen burner. As the precipitate bums, a light blue-green flame should be clearly evident. This indicates organically combined copper. 5678 9:Characteristic spectrophotometric-absorption spectra in the near infrared range (700 to 900 nm) are exhibited by dilute solutions of copper phthalocyanine pigments (2 to 50 mg/L) in H2S04 (sp gr 1.84). The absorption maxima, being sharp and well-defined, may-be used for positive qualitative identification of phthalocyanine pigments. Phthalo cyanine green has maxima at approximately 820 nm and 860 nm for bromine-free types; for the chiorinated-brominated types, the maxima appear at approximately 830 to 840 nm and 875 to 885 nm. 6. Moisture and Other Volatile Matter 6.1 Determine moisture in accordance with Method A of Test Methods D 280. 7. Detection of Basic Dye Derivatives 7.1 Add to 1 g of the sample, 50 mL of a mixture of equal parts of ammonium hydroxide NH4OH (sp gr 0.90) and denatured ethyl alcohol (95 %). Warm gently and filter. Neu tralize the filtrate with tartaric acid solution (200 g/L) until slightly acid to litmus. If the solution is colorless, discounting a slight yellow tinge, no basic dye is present. 7.2 If the solution is colored beyond a slight yellow tinge, add about 5 mL of 0.1 N titanium trichloride (TiCl3) solution (Note 2). If a basic dye is present, the color will lighten significantly. If no basic dye is present, no significant color change will occur. 413 DUP0502 96933 D 3256 ;<=> 2--Titanium trichloride is marketed as a 16% solution in HC1. Mix 7 mL of this solution with 90 mL of HC1 (1 + 12) to obtain a reagent approximately 0.1 N. Protect from oxidation. 8. Detection of Other Organic Coloring Matter 8.1 Procedure--Weigh about 0.05 g of the sample into each of two 50-mL beakers. Add 25 mL (at room tempera ture) of denatured ethyl alcohol (95 %) to one beaker and about 25 mL of acetone to the other. Stir each thoroughly for a few minutes and let stand for about 2 h. Filter through two thicknesses of medium-texture, qualitative filter paper. The presence of more than an extremely slight pink, yellow, or blue tint in either filtrate indicates other organic coloring matter is in the pigment. Organic colors resistant to the above reagents are not likely to be in phthalocyanine pigments but, if desired, procedures given- in standard references can be followed to establish if they are present. 9. Detection of Ultramarine Blue 9.1 Procedure--Warm gently about 1 g of the sample with about 5 mL of HQ (1+1). Decomposition of the ultramarine blue takes place with evolution of H2S. This may be detected by either its odor or a brown coloration appearing on a strip of moistened lead acetate paper. 10. Detection of Iron Blue and Chrome Green 10.1 Procedure: 10.1.1 To 1 g of the sample in a 100-mL beaker, add 25 mL of NaOH solution (50 g/L). Boil for about 1 min. Dilute to approximately 40 mL and filter. 10.1.2 Add HC1 (1+1) to the filtrate until faintly acid to litmus. Add 2 mL of a ferric iron solution [ferric sulfate or ferric alum (20 g/L)]. The development of a blue color reveals the presence of ferrocyanide, and hence iron blue or chrome green in the original pigment. For amounts around 0.05 % iron blue, the color may take 2 to 3 h to develop. 11. Precision and Bias 11.1 No precision or bias information are available for these tests. 12. Keywords 12.1 chrome green, detection of; iron blue, detection of; phthalocyanine blue, analysis of; phthalocyanine green, anal ysis of; pigment; ultramarine blue, detection of 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 the 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 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 tair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 414 DUP050296934 Designation: D 3280 - 85 (Reapproved 1990)k'l Standard Test Methods for Analysts of White Zinc Pigments1 This standard is issued under the fixed designation D 3280; 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 me by agencies of the Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year qfissue which, has been adopted by the Department ofDefense. ?@ ABCDESection 24 was added editorially in May 1990. Scope 1.1 These test methods cover procedures for the analysis white zinc pigments. 1.2 The analytical procedures appear in the following rden ' Section reparation of Sample 6 Zinc Oxide lotal Zinc, Using Diphenylamine as Internal Indicator Jptal Zinc, Using Uranyl Acetate as External Indicator Total Impurities total Sulfur doisture and Other Volatile Matter 7 8 9 10 n Leaded Zinc Oxide 'otal Lead Total Zinc i|Fbta] Sulfur Total Impurities Moisture and Other Volatile Matter Water-Soluble Salts v 12 13 14 13 16 17 Zinc Sulfide J zinc Oxide Zinc Sulfide IjjWater-Soluble Salts doisture and Other Volatile Matter Barium Sulfate Titanium Dioxide 18 19 20 21 22 23 1.3 This standard does not purport to address , the safety Iproblems associated with its use. It is the responsibility ofthe Iuser of this standard to establish appropriate safety and ihpalth practices and determine the applicability ofregulatory limitations prior to use. : 2. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments12 D1193 Specification for Reagent Water3 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 23, 1985. Published December 1985. Originally j published as D 3280 - 73. Last previous edition D 3280 - 73 (1979)<2. 2 Annual Book ofASTM Standards, Vo] 06.02. 3 Annua/ Book ofASTM Standards. Vols 06.03 and 11.01: D1394 Test Methods for Chemical Analysis of y/hite Titanium Pigments2 E 11 Specification for Wire-Cloth Sieves for Testing Purposes4 3. Summary of Test Methods 3.1 Zinc Oxide: 3.1.1 Total Zinc--Determined using diphenylamine as an internal indicator and also using uranyl acetate as an external indicator. Total impurities are calculated. 3.1.2 Total Sulfur--Determined as BaS04 and calculated to sulfur. 3.1.3 Moisture and Volatile Matter--Determined in ac cordance with Method A of Test Methods D 280. 3.2 Leaded Zinc Oxide: 3.2.1 Total Lead--Determined as PbS04 and calculated to percent PbO. 3.2.2 Total Zinc--Determined on the filtrate from proce dure in 13,1.1 in accordance with methods in Sections 8 or 9. 3.2.3 Total Sulfur--Determined as BaS04 and calculated to percent S03. 3.2.4 Total Impurities---Calculated from compositional, data. 3.2.5 Moisture and Other Volatile Matter--Determined in accordance with Method A of Test Methods .D 28Q. 3.2.6 Water Soluble Salts--Determine&gravimetrically, 3.3 Zinc Sulfide 3.3.1 Toted Zinc--Determined using uranyl acetate ex ternal indicator in accordance with Section 9. 3.3.2 Zinc Sulfide--Determined in accordance with Sec tions 8 or 9 and calculating ZnO to ZnS. 3.3.3 Water Soluble Salts--Determined in accordance with Section 18. 3.3.4 Moisture--Determined in accordance with Method A of Test Methods D 280. 3.3.5 Barium Sulfate--The sample is treated with N2S04 and Na2C03 and the residue of BaC03 is dissolved in NCI and (NH4)2S04 added to precipitate BaS04, which is weighed. 3.3.6 Titanium Dioxide--Determined in accordance with Test Methods D 1394. 4. Significance and Use 4.1 White zinc pigments find considerable use in white 3 Annual Book ofASTM Standards, Vol 14.02. 415 DUP050296935 paints, and as such it is useful to fonnulators and users to be able to monitor the amounts of these pigments in whole paints. It is also of interest to raw material suppliers and paint producers to check the specifications of each pigment. 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.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. 5.2 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. 5.3 Concentration ofReagents: 5.3.1 Concentrated Acids and Ammonium Hydroxide-- When acids and ammonium hydroxide are specific by name or chemical formula only it should be understood that concentrated reagents of the following specific gravities or concentrations are intended: Acetic acid, HC2H302 Hydrochloric acid, HC1 Hydrofluoric acid, HF Nitric acid, HN03 Sulfuric acid, H2S04 Ammonium hydroxide, NH40H 99.5 % sp gr 1.19 48 % sp gr 1.42 sp gr 1.84 sp gr 0.90 The desired specific gravities or concentrations of all other concentrated acids are stated whenever they are specified. 5,3.2 Diluted Acid^ and'Ammonium Hydroxide--Con centrations of diluted acids and ammonium hydroxide, except when standardized, are specified as a ratio stating the number of volumes of the concentrated reagents to be diluted with a given number of volumes of water, as in the following example: HC1 (1+99) means 1 volume of concen trated HC1 (sp gr 1.19) diluted with 99 volumes of water. 6. Preparation of Sample 6.1 Grind dry pigments, if lumpy or not finely ground, to a fine powder for analysis. Large, samples may be thoroughly mixed and a representative portion taken and powdered if lumpy or not finely ground. Mix the sample in all cases thoroughly before taking specimens for analysis. 6.2 Separate pigments from paints or pastes, grind to a fine powder, passthrough a 180-pm (No. 80) sieve (Note 1) to remove any skins, thoroughly mix, and oven dry at 105aC. Moisten such pigments after weighing with a little alcohol before adding reagents for analysis. FGHI J--Detailed requirements for this sieve are given in Specifica tion E 11. 6.3 Preserve all samples in stoppered bottles or containers. 5"Reagent Chemicals, American Chemical Society Specifications," American Chemical Society, 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." ZINC OXIDE 7. Total Zinc, Using Diphenylamine as Internal Indicator 7.1 Reagents: 7.1.1 Diphenylamine Indicator Solution (10 g/L)--Dis solve 1 g of diphenylamine in 100 mL of H2S04. 7.1.2 Potassium Ferrocyanide (1 mL = .0.008 g Zn)--. Dissolve 35 g ofK4Fe(CN)6 3H20 in water and dilute to 1 L and add 0.3 g ofpotassium ferricyanide (K3Fe(CN)5). Stand ardize the solution by titrating against zinc (320 to 340 mg), followingfile procedure described in 6.2. Calculate the grams of zinc equivalent to 1.00 mL of the solution. 7.2 Procedure--Weighto 0.1 mg about 0.4 g ofthe sample into a tall form 400-mL beaker. Moisten with about 20 mL of water, and dissolve in 15 mL of HQ. Neutralize with NH4OH, using litmus as the indicator. Add an excess of 15 mL of H2S04 (1+2) and dilute to 200 mL. Heat to approxi mately 60C, add 2 drops of diphenylamine indicator solu tion and while stirring vigorously* titrate with K4Fe(CN)6 so lution to the color change from purple to a persistent yellowish green. KLMN O--The true end point is a sharp, persistent change from a purple to a yellowish green. At the beginning ofthe titration, a deep blue color is developed after addition of a few millilitres of K^FefCN^ solution. About 0.5 to 1.0 mL before the true end point is reached, the solution changes from a blue to a purple color. After the purple color is developed, the titration should be continued dropwise to the persistent yellowish green end point. 7.3 Calculation--Calculate the percent total zinc as ZnO, A, as follows: rV2Zx 1.245-1 LA x 100 5, J (1) where: V2 - K4pe(CN)6 solution required for titration of the specimen, mL, Z = zinc equivalent of the IL,Fe(CN)6 solution, g/m-L, S'] .= specimen weight, and 1.245 = molecular weight ZnO(81.38)/molecular weight Zn(65.38). 8. Total Zinc, .Using Uranyl Acetate as External Indicator 8.1 Reagents: 8.1.1 Uranyl Acetate Indicator Solution-(50 g/L)--Dis solve 5 g of U02(C2Hs 02)2 2H20 in 100 mL of water and make slightly add with acetic add. 8.1.2 Potassium Ferrocyanide, Standard Solution (1 mL = 0.008 g Zn)--Prepare and standardize as in 7.1.2. Run a blank titration with the same amounts of reagents and water. Calculate the zinc equivalent of the solution as follows: Z=WiV-B) (2) where: ... . Z = zinc equivalent of the K4Fe(CN)6 solution, g/mL, W -- zinc used, V = K^FefCN^ solution required for titration of the zinc, mL, and B = K4Fe(CN)6 solution required for titration ofthe blank, mL. 8.2 Procedure: 8.2.1 Weigh to 0.1 mg about 0.4 g of the sample into a tail-form 400-mL beaker. Moisten with about 20 mL of 416 DUP050296936 er and dissolve by adding 10 mL of HCl. Add NH4OH til slightly alkaline to litmus paper. Add HCl until just i, and then add 3 mL in excess. Dilute to about 250 mL th hot water and heat nearly to boiling. Titrate with ce(CN)6 solution, stirring constantly, until a drop of _yl acetate indicator tested in a white porcelain spot plate ows a brown tinge after standing 1 min. 8.2.2 Blank--Run a blank titration with the same amounts reagents and water. i 8.3 Calculation--Calculate the percent total zinc as ZnO, . as follows: '((V-B)Zx. 1.245)1 X 100 (3) itiere: = K4Fe(CN)6 solution required for titration of the sample, mL, | = sample used, g, and 1,245 - molecular weight ZnO (81.38)/molecular weight Zn (65.38). . 9. Total Impurities | 9.1 Calculation--Calculate the percent total impurities, A, as follows: A = 100 -r (L + Zj + S,) (4) where: L = total lead as PbO, %, iZi -- total zinc as ZnO, %, and S$ = total sulfur as S03, %. 10. Total Sulfur 10.1 Reagents: 10.1.1 Bromine Water {saturated). 10.1.2 Aluminum--Reagent grade granular aluminum. 10.1.3 Barium Chloride Solution (100 g BaCl2 L)--Dis solve 117 g BaCl2<2H20 in water and dilute to 1 L. 10.2 Procedure: 10.2.1 Weigh to 0.1 g about 10 g ofthe sample into a 400mL beaker. Add 50 mL ofsaturated bromine water, 100 mL of water, and 35 mL of'HCl. Boil until all the bromine has been expelled, cool, and add 3 to 5 g of granular aluminum. Heat to boiling, filter, and wash well with hot water. 10.2.2 Dilute the filtrate to 300 mt with water, neutralize with NH4OH, and add 6 drops of HCl. Heat to boiling and add 25 mL of hot BaCl2 solution dropwise, with constant stirring. Allow to stand in a warm place for at least 2 h. 10.2.3 Filter, using a weighed Gooch crucible, or a fine textured filter paper and wash well with hot water. Diy and ignite in a muffle furnace for 30 min. Cool, and weigh as BaS04. 10.3 Calculation--Calculate the percent sulfur. A, as fol lows: where: P = BaS04 precipitate, g, S2 = specimen weight, g, and 0.1374 == molecular weight of sulfur (32.064)/molecular weight BaS04 (233.43). 11. Moisture and Other Volatile Matter 11.1 Procedure--Determine moisture and other volatile matter in accordance with Method A of Test Methods D 280. LEADED ZINC OXIDE 12. Total Lead 12.1 Procedure: 12.1.1 Weigh to the nearest 0.1 mg about 0.5 g of the sample into a 400-mL beaker. Dissolve in 250 mL of water and 20 mL of HNOs (Note 2). Add 5 mL of H2S04 and evaporate to dense white fumes. Cool, add 50 mL of 95 % alcohol and 200 mL of water, and let stand cold 1 to 2 h. Filter, using a weighed Gooch crucible. Wash the precipitate with H2S04 (1+99) and combine the filtrate and washings. If the zinc content of the sample is known to be 40 % or over, reserve the filtrate and washings for the determination of total zinc (Section 13). PQRS 3--Ifthe sample contains calcium or barium, the lead and zinc should be separated by precipitation with H2S after solution in HO, making alkaline with NH40H and then acid with acetic acid Dissolve the FbS and ZnS in dilute HNOj and determine the lead and zinc as above. 12.1.2 Ignite the precipitate in the crucible at dull red heat (550 50C) for 20 min, cool, and weigh. 12.2 Calculation--Calculate the percent total lead as PbO, A, as follows: r(P, x 0.736)-, A x 100 (6) where: Px = PbS04 precipitate, g, 3 = sample used, g, and 0.736 = molecular weight PbO (223.2l)/molecular weight PbS04 (303.28). 13. Total. Zinc 13.1 Reagents--See 7.1 or 8,1, whichever is applicable. 13.2 Procedure: 13.2.1 If the zinc content of the sample is known-to be 40 % or over, determine zinc on the filtrate obtained in 12.1.I. If the zinc content is known to be under 40 %, weigh to the nearest 0.1 mg about 1 g of the sample, precipitate and filter off the lead as PbS04 as described in 12.1.1, and determine zinc on the filtrate. 13.2.2 Evaporate the appropriate filtrate to dryness and determine zinc as directed in Sections 7 or 8. 14. Total Sulfur 14.1 Reagents--See 10.1.3. 14.2 Procedure: 14.2; l Weigh to the nearest 0.1 mg about 1 g ofthe sample, into a 400-mL beaker. Add 10 mL of water, 3 g of NH4C1, and 5 mL of HCl saturated with bromine. Heat on a steam bath for about 15 min. Add 50 mL of water, neutralize with dry Na2C03 in excess. Boil 10 to 15 min. Allow to settle, dilute to 250 mL with hot water, filter, and wash with hot water. 14.2.2 Redissolve the residue in HQ, reprecipitate as be fore, and wash with hot water. Acidify the combined filtrates with HCl, adding 5 mL in excess. Boil 10 to 15 min. Neu- 417 DUP050296937 # D 3280 tralize with NH4OH and add 6 drops excess HCl. Heat to boiling and add 25 mL of hot BaCl2 solution dropwise, with constant stirring. Allow to stand in a warm place for at least 2 h. 14.2.3 Filter, using a weighed Gooch crucible or a fine textured filter paper, and wash well with hot water. Dry and ignite in a muffle furnace for 30 min. Cool and weigh. 14.3 Calculation--Calculate the percent sulfur as S03, A, as follows: (P2 x 0.343): A = x 100. (7) volumetric flask. Dilute to the mark mid filter through a dry, fine paper. TUV18.2.2 Transfer 400 mL of the clear filtrate to a 600-mL beaker. Add 20 mL of HCl and neutralize With NH4 using litmus paper. Add HCl until just acid and then add 3 mL in exdess. Heat nearly to boiling and titrate with K4Fe(CN)6 solution as described in 8.2. 18.3 Calculation--Calculate the percent zinc oxide, A, as follows: d(v3 -- B3) Z X 1.245)-] x 100 (10) where: P2 54 0.343 BaSQ4 precipitate, g, specimen weight, g, and molecular weight S03 (80.07)/molecular weight BaS04 (233.43). 15. Total Impurities 15.1 Calculation--Calculate the percent of total impuni ties, A, as follows: A = 100 -(L + Zt + S5) (8) where: L - total lead as PhO, %, Z, = total zinc as ZnO, %, and Ss = total sulfur as S03, %. 16. Moisture and Other Volatile Matter 16.1 Procedure--Determine moisture and other volatile matter in accordance with Method A of Test Methods D 280. 17. Water-Soluble Salts 17.1 Procedure: 17.1.1 Weigh to the nearest 1 mg about 5 g of the sample into a 500-mL graduated flask. Add 250 mL of water at room temperature and shake for 10 min. Dilute the solution to the mark with water,; mix by shaking,, and filter through a dry, fine paper. 17.1.2 Transfer 400 mL of the clear filtrate to a weighed platinum dish and evaporate to dryness at 105 2C, cool in a desiccator, and weigh rapidly. 17.1.3 Blank--Make a blank! determination at the same time in a similar manner. 17.2 Calculation--Calculate - the percent water-soluble salts, IF, as follows: - JW = jR-B2h X 100 . (9) where: R = dry salts obtained from the sample, g, Bz = water-soluble salts obtained from the blank, g, and S5 = sample represented in the aliquot used, g. ZINC SULFIDE where: V3 = K4Fe(CN)6 solution required for titration of the specimen, mL, B3 = K4Fe'(CN)6 solution required for titration of the blank, mL, Z = zinc equivalent of the iQFefCNle solution, g/piL, S6 = sample represented in the aliquot used, g, and 1.245 = molecular weight ZnO (81.38)/moleCular weight Zn (65.38). 19. Zinc Sulfide 19.1 Reagents--See Section 7 of 8, whichever is appli cable. 19.2 Procedure--Weigh to the nearest 0.1 mg a portion of the sample into a tail-form 400-mL beaker. Moisten with water, add 10 mL of H2S04 (1+1), and evaporate to dryness. Cool, and proceed as directed in 7.2 or 8.2. 19.3 Calculation--Calculate the percent zinc sulfide, C, as follows: WK(F4-B4)Z 1.491h C = x 100- 1.20A '(11) where: V4 = IQFefCN^ solution .-required for titration of the specimen, mL, . B4 = K4Fe(CN)6 solution required for titration of the blank, mL, Z = zinc equivalent of the K4Fe(CN)6 solution, g/mL, S7 =* sample Used, g, , A = percent of zinc oxide (Section 17), ~ L20 = factor for conversion of percentage of ZnO to the ZnS equivalent, and , 1.491 - molecular weight ZnS (97.44)/molecular weight Zn (65.38). ., ., 20. Water-Soluble Salts 20.1 Procedure--Determine water-soluble salts as. di rected in Section 17. 21. Moisture 21.1 Procedure--Determine moisture and other volatile matter in accordance with Method A of Test Methods D280. 18. Zinc Oxide 18.1 Reagents--See 8.1. 18.2 Procedure: 18.2.1 Weigh to 1 mg about 5 g of the sample into a 500mL Erlenmeyer flask and add 200 mL of acetic acid (3+97). Shake continuously for 20 min and transfer to a 500-mL 22. Barium Sulfate 22.1 Reagents: 22.1.1 Ammonium Sulfate Solution (30 g/L)--Dissolve 30 g of (NH4)2S04 in water and dilute to 1 L. 22.1.2 Methyl Orange Indicator Solution--Dissolve 0.1 g of methyl orange in 100 mL of water. Filter if necessary. 418 DUP050296938 D 3280 22.1.3 Sodium Carbonate Solution (2 g/L)--Dissolve 2 g f Na2C03 in water and dilute to 1 L. 22.2 Procedure: 22.2.1 Weigh to the nearest 1 mg about l g of the sample ato a 400-mL beaker. Moisten with water;: arid add 100 mL fH2S04 (1+1), and evaporate to dryness. Cool, add 200 mL i water, and carefully break up the residue. Boil for 15 min. :er, and wash with water. 12.2.2 Transfer the residue and paper to a platinum crule and bum off the paper. Cool, add 6 g 0f Na2CO3, and crucible or a fine textured filter paper, and wash with hot water until free of chlorides. Dry, ignite in a muffle furnace for 30 min, cool, and weigh. 22.3 Calculation--Calculate the percent barium sulfate (BaSOJ, A, as follows: A = x 100 where: P3 - BaS04 precipitate, g, and Ss - sample used, g. (12) 23. Titanium Dioxide 23.1 Procedure--Determine titanium dioxide in accord i ance with Sections 9 to 13 of Test Methods D 1394. If the pigment being analyzed is relatively low in Ti02, the use ofa larger spedmen than that specified in Test Methods D.1394 should give more accurate results. 24. Keywords . 24.1 analysis;,barium sulfate; lead; sulfur, uranyl acetate; white zinc pigment; tfinc 4. Cover with 2 g of Na2C03, and fuse for 40 min over a ker burner. CToheoAl maenrdicalneSaecehleth/ feorfTuessitoinng awnditMha2te0ri0alsmtakLesonfohpoostition respecting the validity ofany patent rights asserted in connection ter in ition. a 400pwa-ittmhenaLtnrybigeihtetasm,keamnre,dnFtthioienltreeidsrkinaotfnhiindsfrsiwntaganesdmaherdnw.t oUitfshseurhschoofrtitghNhistass,2taaCrned0ea3nrdtiraerley expressly their own advised, that determination responsibility. of the validity of any such 12.2.3 Disso1 lvTehisthsteanBdaardCIS0s3ubwjeictthtohreovtisiHonCa1ta(n1y+tim4e),bcypaitecrheisnpgonsible technical committee end must be reviewed every five years and filtrate inifaP6it0re0vi-smedL, ebitheearkreearp.pWrovaesdhortwhitehdpraawpne. Yrowuricthomwmaentetsra,re invited either forrevision pfthis siantfard or for additional standards utralize w:itahndNshHou4ldO`bHe ,adudsreinssgedmtoe/t^hSyTMl oHreaandgquearatesrst.hYeouinr cdoimcma-ents wilt receive careful consideration at a meeting of the responsible . Add HC1tveuiecnwhnstiicklanjulocwsonmt tmaoidtthtedeeA,aSwnThdMicthChyoeomunmmiatatedyedaotnt6enSddta.rnoIdfpaysrodusin,fe1e9el1xth6caeRtsaysco,euSr cto, mPhmileandteslphhaiave, not received PA 19103. a fair hearing you should make your ute to 400 mL, heat to boiling, and add 25 mL of hot H4)2S04 solution slowly, while stirring. Allow to stand in a in place for at least 4 h. 12.2.4 Filter off the predpitate, using a weighed Gooch s 419 DUP050296939 <1 Designation: D 3360 - 80 (Reapproved 1989) ________ ______________ L - .- i._ Standard Test Method for Particle Size Distribution by Hydrometer of the Common White Extender Pigments1 This standard is issued under the fixed designation D 3360; the number immediately following the designation indicates the year of original adoption or, is 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 1.1 This test method covers the determination of the particle-size distribution in the sub-sieve size range of the common extender pigments such as aluminum silicate (kaolin clay), magnesium silicate (talc), calcium carbonate (calcite or dolomite or precipitated calcium carbonate), and mica pigments, and may also be extended to the denser prime pigments such as die white titanium pigments (rutile or anatase) and similar mineral pigments when and if such information is of concern. Particle-size distribution has significance in the evaluation of rheological and pigmentary properties of pigments in paint and also may sometimes be used to characterize the identity or grade of pigments. 1.2 Sedimentation methods having as their basis Stoke's law have found general acceptance for this purpose. Results, are expressed in terms of equivalent spherical diameter (e.s.d.), the diameter of a sphere having the same specific gravity as the particle in question and which settles at the same rate. Most mineral pigment particles are more or less asymmetrical, but despite differences in the relationship between equivalent spherical diameter and actual dimen sions, the results ofa sedimentation particle-size analysis can be correlated readily with many pigment properties. 1.3 Procedures limited to gravitational sedimentation12'33,44,5 5are relatively inaccurate for pigment particles smaller than about 1 pm e.s.d., and centrifugal procedures may be required for the much finer ranges. Nevertheless, the data obtained above the 1 pm limitation provide useful information. This test method is particularly applicable to pigments if a major fraction of the particles fall in the range from about 15 to 1.5 pm, but have a total particle-size range of at least two decades. 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 1 This test method is under the jurisdiction of ASTM Committee D-t on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Sept. 2, 1980. Published November 1980. Originally published as D 3360 - 74. Last previous edition D 3360 - 74. 2 Norton, F. H., and Speil, S., Journal of the American Ceramic Society, Vol 21, 1938, p. 89. 3 Casagrande, A., "Hydrometer Method for Determination of Fineness Distri bution of Soils," Julius Springer, Berlin, 1934. 4 Andreasen, A. H. M., "The Evaluation of Ground Materials," Kalloid Biehefte, Vol 27, 1928, p. 349. 5 Lane, Marvin K. "Improved Method for Measuring Particle Size Distribu tions by Gravity Sedimentation with a Hydrometer," A Work Manual by Lane, M. K., 4147 West Byron St., Chicago, IL 60641. appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments6 .. D 422 Method for Particle-Size Analysis of Soils7 D1193 Specification for Reagent Water8 E 100 Specification for ASTM Hydrometers9 E 300 Practice for Sampling Industrial Chemicals10 1 | l 1 i; 3. Summary of Test Method 3.1 For the determination of particle-size distribution by l the application of Stokes' law to the sedimentation of ; particulate material out of an initially homogeneous suspen- 1 sion, any systematic spt of measurements which permit the I determination of the suspension density (that is, the "percent solids") at some defined distance beneath the surface of the - j suspension at some appropriately selected series of sedimen- | tation time durations can be converted to a particle-size distribution. In this procedure, the suspension density is estimated at the effective distance beneath the suspension surface of the center of gravity of a floating hydrometer observed at a series of convenient time intervals selected to increase roughly exponentially. '\ XYZ[ \--Any alternative system that provides-an equivalent set of measurements (for example, the Andreasen Pipet Method,'* or any ofthe optical sampling methods based on change in turbidity, light scattering, and light or' Xtfay absorption, etc.) will also yield a particfe-size distribution. Methods based on optica] measurements, however, are much less generally applicable because of certain technological limita tions too complex to be dealt with here. 4. Apparatus 4.1 Stirring Apparatus, commonly known as a "malted milk mixer," with a vertical high-speed shaft (approximately 10 000 r/min) tipped with a 25-mm diameter sine-wave impeller. The preferred mixing cup is a stainless steel cup about 180 mm deep and slightly tapered from an outside diameter at the top of about 100 mm to about 70 mm at the bottom. Some very fine particle pigments may require additional shear for complete dispersion. In some circum- 6 Annual Book ofASTM Standards, Vol 06.02. 7 Annual Book ofASTM Standards, Vol 04.08. *Annual Book ofASTM Standards, Vois 06.03 and 11.01. 9 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 10 Annual Book ofASTM Standards, Vote 06.03 and 15.05. 420 DUP050296940 # D 3360 NOMOGRAPHIC CHART FOR SOLUTiOH OF STOKES' LAW n - Vis c o s it y or Imh o ft $mc cm1 s - Spectrrc Gewrr cr MAffts A JO9 ' ttc/nc OaAnrr or UawR * if - veioctrr & cn per sec D - Duntreff or c a m m *tm t - Tc hf zkat vhc *) H - H&6HT m m 7 -Jf*t 0 ,steo*tFs H 0 9 to It rs a ft 15 to t$ f- r 35 \3 >0 i its 70 i --so 00 Hi. 15 50 -JO 111 IIs els N 24 25 26 27 28 29 3.0 3/ 32 5 Ss *) esrmreo Avur-etrugs wse rue reeao /Wf m soar or ne resr re m me me/i Htumenr nu*n9 /$ ruae. St o k e s ' La w D - Va ~o A 1800 n =f KEY 0 * FIG. 1 Casagrande Nomographic Chart jo 2$ - otstcn Of (KrJJCAU 20 is -j 16 Hcmr Hgtwice coeaesiwss ntvnt. vr(6 TO HtAOinS Rr OeTEJtHUtCi* H** H,+i'(k- Ttt't4t*rAt*) 5" .X. t <1 5- tie Rr tf t o ee BETeenuiro ne ewcneMT muss or Rr. cpwespotsms wues *r frrore ptornp crt jftstrr stp* or(nod'Satie we conYfmctiT svewvistetis twee. roe son susrenstotts m mtea **r /trojconem neAstrvttf pt/wnes ocrmttt 0 SfS OOP 1040 KIT* 4ft eeeueeer or 9.009a nor at u s s p- svooesrepi ceuaoATtoft at so*c /ft oenstr/es. Srueon utte avia, nee ft, 14 *0 t4 or h */ n tren nut nemos enter t mah Mirer rue {a )-reuses mar ee conn/rca rw {3} aw (/) scuff. AffiY omr ro moenstofts iff w a u r . fsttf flit. Anti **1 W- m. / stances, dispersion in a blender cup at maximum r/min may be considered instead of preparation with a "malted-milk mixer." (See 7.3.) 4.2 Hydrometer, certified with a minimum of 3 points of certification, graduated in units of specific, gravity, and having a' range from 0.995 to .1.038. The approximate dimensions are as follows: bulb length, 139 mm, bulb diameter 31 mm, and overall length 280 mm. Such a hydrometer is identified as a "Soil Hydrometer"5 in Specifi cation E 100, and is also described in Method D 422. 4.3 Sedimentation Cylinders, glass, (two or more), having ap inside diameter of about 65 mm and an overall height of 450 min with a calibration mark to hold 1205 mL.5 4.4 Thermometer, accurate to 0.1 *C over a range from 1*5 to 35'C. 4.5 Water Bath, large enough to accommodate two or more of the sedimentation cylinders immersed to slightly above the 1205-mL graduation mark, and having circulating water and means for keeping its temperature throughout the bath to within 0.IC over a range from 18 to 30C. ]^_` 2--In place of the water bath, the procedure may be carried out in a constant-temperature room controlled to the same precision as noted above. 4.6 Time--A stopwatch, or the equivalent, and an ordi nary watch or clock. 4.7 Balance, sensitive to 0.01 g. 4.8 Drying Oven, with accurate thermostatic control to 2C at 110C. 4.9 Wash Bottle, containing reagent water. 4.10 Casagrande Nomographic Chart (see pig. 1). 5.1 Purity of Water--Unless otherwise indicated refer ences to water shall be understood to mean Type II reagent water conforming to Specification D 1193. 5.2 Dispersing Agents--The different pigments, depend ing on their specific surface properties, mayjequire differing dispersant system^ to effect optimum stable -dispersions. Among the various' common dispersing agents which have been found useful are: 5.2.1 Tetrasodium Pyrophosphate, TSPP (Na4P207)--A freshly prepared 5 % solution of TSPP in water. 5.2.2 Sodium Hexametaphosphate (NaP03)6. 5.2.3 Calgon T.n 5.2.4 Daxad 30 (25 % active dispersant).1121 5.2.5 Dispex N-40 (40 % active dispersant).13 , 5.3 Antifoaming Agent--Pine oil, or capryl alcohol, or the equivalent. 6. Test Specimens and Sample 6.1 Sampling procedures should conform to the general practice outlined in Practice E 300. 6.2 Specimen Size--At least 50 g of well-pulverized 11 Calgon T, Calgon Corp., P. O. Box 1346, Pittsburgh, PA 15230. 12 Daxad 30, W. R. Grace, 3 Hanover Square, New York, NY 10004. 13 Dispex N-40. Allied Colloids Inc., 1 Robinson Lane, Ridgewood, NJ. 421 DUP050296941 D 3360 TABLE 1 Pigment Aluminum silicate Aluminum silicate (Predispersed) Magnesium silicate Calcium carbonate Mica pigment TI02 Pigment (Rutte, Anatase) Examples of Recommended Dispersants and Suggested Dispersant Concentrations Specific Gravity Recommended Dispersant Concentration, or Amount per 30-g Sample 2.58 2.58 2.85 2.71 2.82 4.00 TSPP (NaPOa)e TSPP TSPP Daxad 30 CalgonT Calgon T Calgon T TSPP 6 mL of 5 % solution 0.15 to 0.25 g 3 mL of 5 % solution 6 mL of 5 % solution 0.5 to 0.8 % `active" dispersant based on weight of dry pigment as above as above as above 4 mL of 5 % solution/20 g sample " pigment is required for each particle-size distribution deter mination. 7. Procedure 7.1 Determine the moisture content of the pigment by drying a 10-g sample to constant weight at 110C essentially as described in Test Methods D 280. 7.2 Weigh out the equivalent of 30 0.05 g of dry (moisture-free) pigment. (In the special case of predispersed aluminum silicate pigments, weigh out 30.10 0.05 g ofdry sample. For denser pigments such as Ti02 (sp gr 4.0), the sample size should be reduced to about 20 g.) 7.3 Preparation of the Pigment Dispersion--Place 150 to 200 mL of distilled water in the mixing cup, start the mixer, add the pigment sample, and stir for 5 min. Then add the amount and type of dispersant (see Note 3) as suggested in Table 1, and mix for an additional 5 min. Loose agglomer ates or floes must be broken up into individual particles, but it is equally important to avoid mechanical attrition of the particles, especially in coarser pigments. For most common pigments, a 10-mm mixing period is sufficient. 7.4 Transfer the suspension into one of the graduated sedimentation cylinders, rinse out the mixing cup several times to ensure complete transfer of the sample, and finally dilute to the 1205-mL mark with distilled water adjusted to the same temperature as the water bath. If needed (but only if needed) add a drop of the anti-foaming agent. Close the mouth ofthe cylinder with a rubber stopper to fit (No. 13) or with the palm of the hand, and mix the suspension in the cylinder by inverting several times with shaking. Place the cylinder in the constant temperature bath (see Note 4) and stir the suspension occasionally with a glass rod to prevent sedimentation. Make a reference (blank) solution by filling the second cylinder to the mark with distilled water con taining the same amount and type of dispersant as used with the pigment sample, and place along side in the bath. When both cylinders have attained the temperature of the bath, remove the cylinder with the suspension and remix by inversion and shaking as before. abcd e3 The accuracy of the test depends entirely on obtaining complete and stable deflocculation of the pigment so that each of its particles settles individually. The quantity and type of dispersing agent noted in Table 1 is usually satisfactory for the pigments listed when received in the usual form. Flocculation may occur due to attractive charges between the particles at which time the individual particles cease to fall independently. The pigment particles may come together to a variable degree to form floes which descend as loosely associated groups or clusters of particles. When this occurs the apparent test results are much too "coarse." Signs of flocculation prior to or during the sedimentation test may be any or all ofthe following; (a) Large clusters or pigment floes suddenly become visibly apparent in the sedimenting suspension. J(b) An ill-defined, loosely mobile bed of sediment floes may form at the bottom of thecylinder. Ifthe pigment has been properly and stably | dispersed, the sediment bed will be dense, solidly and tightly packed, | well defined, and may appear to be graded in size if the particle size is | Jwidely distributed. Such a dispersed sediment bed is extremely difficult to resuspend by simple shaking and mixing. m (c) A very clear layer of solution may suddenly appear at the top of jl the cylinder, and this clear layer gradually descend with a definite j] demarcation between clear solution and "flocculated" sediment. If the a pigment has been properly and stably dispersed, there will always be a ll slight residual turbidity extending to the surface ofthe suspension due to f ultra-fine particles which remain in stable suspension even to the end of the test. t (d) Slight or partial flocculation (that is, when only a few floes form 1 intermittently during the settling period) is more difficult to detect. Evidence for this occurrence is also the clear zone of solution at the t surface of the suspension as well as a qualitatively "looser" sediment 1 bed. Slight or partial flocculation is particularly difficult to detect when tf the size distribution of the pigment is very narrow. (e) One may be sure with confidence that flocculation is not a source g of error in the test results by running a series of sedimentation tests on j the same pigment sample using different dispersing agents over an | appropriate range of dispersant concentrations. That sedimentation test ! that yields the finest distribution is the one least likely to contain floes rj arid most likely to represent the "actual" size-distribution. Dispersion requirements so determined then become "standard for that particular .. | fghi jkpigment type." J The bath may he held at any constant temperature between J 18 and 30"C, preferably only a few degrees above the normal maximum temperature of the laboratory. 7.5 Immediately after this final mixing, replace the sample cylinder in the bath, insert the hydrometer into it, and simultaneously start the timer. Immerse the hydrometer only slightly beyond the point where it floats freely. 7.6 Take hydrometer readings at such- intervals that the total accumulative elapsed times form an approximate geometrical progression. A convenient series of time inter vals is 1, 2, 2, 5, 10, 10, and 30 min and 1,2, 3, 7, and .10 h, which together yield an elapsed time series of 1, 3, 5, 10, 20, and 30 miri and 1,2,4,7,14, and 24 h. Read the hydrometer at the top of the meniscus, to the nearest estimated 0.001 units of specific gravity. After the first two or three time intervals, it is good practice to remove the hydrometer from the suspension, rinse it off, and float it in the reference (blank) solution. Great care must be taken to minimise any disturbance of the suspension by inserting and removing the hydrometer veiy slowly and evenly. 7.7 For each reading, record the elapsed sedimentation time, the temperature of the pigment suspension (or water bath) and the hydrometer readings for both the pigment suspension and the reference (blank) solution. See Table 2, which provides an example of a convenient data and computing form. j j j 8. Calculation 8.1 Percent ofPigment in Suspension--Calculate for each 422 DUP050296942 F Date # D 3360 TABLE 2 Particle Size Distribution-Hydrometer Method--Calculation and Data Sheet Sample No:::---------------Operator: --------------------------- -A x 103 Temperature-----------------------------Density Time Time Interval Total Time *R" "D" V D(ii) (R - d) x 10s % Finer ------ R"--Hydrometer reading on suspension. "D*--Hydrometer reading on blank. D(u)--Equivalent spherical diameter in micrometres Use Casagrande Nomographic Chart to Determine 1. A x 10a from temperature and density. 2. V from "Ft* and time. 3. D(ji), from V and A x 103 leading the percent of dry pigment remaining in suspension it the level which the hydrometer measures the density ofthe suspension by the following equation: P = (100 000/C) X [G/((? - S)] x [(/t - B)/r] svhere: jP = % pigment remaining in suspension, C = original concentration of suspension in grams of pig ment per litre, (for a sample of 30 g dry weight in 1205 mL of suspension, C = 24.9 g/L), Rr = hydrometer reading in the pigment suspension, B = hydrometer reading in the blank solution, and G = specific gravity of pigment particles. (For'example, in the absence of an actual determination of the specific t gravity, a value, of 2.6 may be taken for aluminum silicate pigment.) 8.1.1 Take the value of (Rr - B) for the initial 1-min sedimentation reading to be a measure of the starting (concentration. The percent remaining in suspension for each subsequent reading then becomes simply the ratio of its (Rr -- B) value to the initial (Rr -- B) value multiplied by 100. lmno 5--In the case of pigments reasonably free from coarse particles (larger than about 15 jim), the above calculations for the initial hydrometer readings should give values of 100 % for the percent remaining in suspension. Variation from this figure may be due to ' inaccurate measurements of the test specimen or volume of the lmno; suspension. 6--Readings taken during the first few minutes of sedimenta tion are more subject to possible error from several causes than are subsequent readings. These causes include settling of coarse particles on the hydrometer bulb, failure to attain complete temperature equilib rium, and the possible presence of entrained air in the suspension. Of these, the last named is perhaps the most frequent source of error. Treatment of the suspension before mixing with a small amount of an antifoam agent helps to prevent this, 8.2 Equivalent Spherical Diameter ofthe Particles: 8.2.1 Calculate the equivalent spherical particle diameter corresponding to the percent indicated by each hydrometer reading in accordance with Stokes' law. A particle of this equivalent spherical diameter is assumed to be at the surface of the suspension at the beginning of sedimentation and to settle during the accumulated time to the level at which the hydrometer measures the suspension density. 8.2.2 Casagrande's nomographic solution of Stokes' law2,5 shown in, Fig. 1 offers a convenient means for calcu lating equivalent spherical diameter. Its use requires calibra tion of the hydrometer in terms of the actual depth of its center of gravity below the surface of the suspension (Hr) for each hydrometer reading, Rr. The formula for calibration of hydrometers graduated in specific gravity units is shown in the upper right-hand corner ofthe chart. Calculated values of Hr for convenient intervals ofRr must be plotted on the Hr Rr scale for each individual hydrometer. Note that the hydrometer is calibrated for actual depth below the surface of the liquid, but that hydrometer readings of the density of the pigment suspension are made at the top of the meniscus, which is slightly raised above the surface of the suspension. For this reason a meniscus correction must be made. With the recommended hydrometer, it has been found that the. addition of 0.0003 to-the specific gravity reading made at the top of the meniscus gives values which correspond closely to the specific gravity reading at the surface level. 8.2.3 The use of the chart is explained in the key. A line through the value of S, the specific gravity ofthe sedimenting pigment particles and /, the temperature, gives the value for A x 103, which is constant for a given temperature (of the bath or constant temperature room). A line through H, and T, the accumulated time, gives a value for v, the sedimenta tion velocity in centimetres per second; and finally, a line through A x 103 and v gives the corresponding value for the equivalent spherical diameters, D, in millimetres. 9. Report 9.1 The report shall consist of a graph made by plotting for each hydrometer reading the percent remaining in sus pension ("percent finer than") against the equivalent spher ical diameter, using semilogarithmic graph paper with the particle size values on the logarithmic scale (see Fig. 2). A 423 DUP050296943 # D 3360 value for the percent finer than 2 pm may be read from the graph and reported separately. 9.2 Although the. entire cumulative particle size distribu tion curve may be of general interest, the particle size distribution criteria customarily used for extender pigments is either the weight percent less than 2 pm e.s.d., the weight median particle size, that is, the "50 % finer than" point on the distribution curve, or both. At either extreme of the particle size distribution curve, that is, the largest 10 % and the smallest 10 %, the test precision and accuracy tend to be considerably less than in the remaining 80 % mid-range of the distribution. 10. Precision 10.1 Based on interlaboratory studies of this test method in which operators in 6 laboratories measured the particie size distribution of three extender pigments: aluminum silicate (kaolin), magnesium silicate (talc), and calcium carbonate, the following criteria should'be used for judging the acceptability of results at the 95"% confidence level. 10.1.1 Repeatability--Duplicate results by the same oper ator should be considered suspect ifthey differ by more than 1 pm at the weight median ("50 % finer than") point, or 3 % at the percent less than 2 pm point on the cumulative, distribution curve. 10.1.2 Reproducibility--Two results, each the mean of duplicate measurements obtained by operators in different laboratories, should not be considered suspect unless they differ by more than 2 pm at the weight median ("50 % finer than") point, or 5 % at the percent less than 2 pm point on the cumulative distribution curve. 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 ifnotrevised, either reapproved or withdrawn. Your comments are invited either for revision oi 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. 424 DUP050296944 Designation: D 3432 - 89 Standard Test Method for Unreacted Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography1 This standard is issued under the fixed designation D 3432; 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 (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 Standards for the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the determination of free toluene diisocyanates in urethane prepolymers and unpigmented coating solutions. pqrs 1--This test method may also he useful for the determination of free isocyanate monomers of other types upon taking precautions to confirm suitability. 1.2 There is no reason to believe this test method would not work for pigmented coatings. 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 8. 2. Referenced Documents 2.1 ASTM Standards: D2372 Practice for Separation of Vehicle from Solvent- Reducible Paints2 D 2698 Test Method for Determination of Pigment Con tent of Solvent-Reducible Paints by High-Speed Centri fuging2 E 260 Practice for Packed Column Gas Chromatography3 3. Summary of Test Method 3.1 A standard solution of the diisocyanate is analyzed by gas chromatography using an internal standard techniqueThe unknown specimen is then chromatographed, again using an internal standard, and a response factor is calcu lated from the standard solution. The unreacted diisocyanate content of the unknown is calculated from the chromatogram of the specimen. 4. Significance and Use 4.1 This test method provides a measurement of the unreacted diisocyanate content of urethane prepolymers and coating solutions. This measurement is of basic importance to the health of the users. 5. Interferences 5.1 Under the test conditions described in this test method, other diisocyanates or impurities having identical or nearly identical elution times may interfere. It is generally necessary to know the identity of the diisocyanate being used in the specimen being tested, either by knowledge of the composition or by a separate analysis. 5.2 The temperature specifications for the injection port and column oven must be strictly followed to prevent thermal decomposition of the specimen. Decomposition can be detected by the failure ofthe recorder pen to return to the baseline after elution of the diisocyanate monomer. 5.3 Since resin solution specimens leave a nonvolatile residue in the injection port, the use of glass injection port liners is recommended. The glass liner should .be changed daily or after each group of 10 specimens that are analyzed. 5.4 Since diisocyanates are highly reactive with water, a suitable drying cartridge should be used in the carrier gas line. 6. Apparatus 6.1 Gas Chromatograph equipped with flame ionization detector (FID) and capable of linear temperature program- . ming to 300C. .......... 6.2 Chromatographic Column, 6.6 ft (2~m) by 0.125-in... (3.2-mm) outside diameter, 0.085-in. (2.1-mm) inside diam eter stainless steel (or glass, 2-mm inside diameter), packed with a 10 % methyl vinyl silicone4 on 80/100 mesh flux- calcined diatomaceous earth.5 The packing is prepared by dissolving 1.0 g of the methyl vinyl silicone in 50 mL of methylene chloride. This solution is placed in an evaporating dish and 9 g of the diatomaceous earth is added with gentle stirring. The evaporating dish may be gently heated on a steam bath or evaporated at room temperature. The packing should be gently stirred, periodically, until dry and free- flowing. A newly packed column should be conditioned overnight at 200C with a flow of dry carrier gas. ptuv 2--Any other column, either packed or capillary, may be substituted if the required separation is obtained. 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 mittee D01.33 on Polymers and Resins. Current edition approved April 28, 1989. Published July 1989. Originally published as D 3432 - 80. Last previous edition D 3432 - 80. 2 Annual Book ofASTM Standards, Vol 06.01, 5 Annual Book ofASTM Standards, Vo! 14.01. 4 UC-W-98, licensed by Union Carbide Corp., 39 Olde Ridgebury Rd., Danbury, CT 06817-0001, has been found satisfactory for this purpose and is available from most suppliers ofgas chromatographic accessories. 5 Chromosorb W-HP, manufactured by Manviile Sales Corp., Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108, has been found satisfactory for this purpose and is available from most suppliers of gas chromatographic accessories. 425 DUP050296945 # D 3432 wxyz 3--Other methods of packing preparation may be used, provided a free-flowing, uniformly coated packing results. 6.3 Chromatographic Syringe, {| j j }~ 6.4 Analytical Balance, accurate to 0.1 mg. 6.5 Glassware--All glassware used should be oven-dried to eliminate moisture. 6.6 Recorder, Recording Integrator or Computer with appropriate software. 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. 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 Ethyl Acetate (99+ %), urethane grade, dried over a Type 5A molecular sieve. 7.3 Standard Solution A--Weigh about 5.0 g <?f 1,2,4trichlorobenzene (TCB) to 0.1 g and dilute to 500 mL with ethyl acetate (1 mL = 10 mg TCB). 7.4 Standard Solution B--Weigh about 0.25 g of the diisocyanate to 1 mg into a dried 100 mL volumetric flask and add 10 mL of Standard Solution A by pipet. Dilute to 100 mL with ethyl acetate and mix well. This solution has a shelf life of one day. 7.4.1 If the unreacted diisocyanate content of the prepo lymer or coating solution exceeds 1 %, then Standard Solution B should be made by diluting 0.25 g of the diisocyanate monomer, weighed to 1 mg, with Standard Solution A to 10 mL in a dried 10-mL volumetric flask. No additional solvent is added in this case. 7.5 Toluene Diisocyanate (TDI), 99.5+ % assay, mixture of 80 % 2,4- and 20 % 2,6-isomers. 7.6 1,2,4-Trichlorobenzene (TCB). 8. Hazards 8.1 Diisocyanates can be toxic when inhaled or adsorbed through the skin. Provide adequate ventilation and wear impermeable gloves (for example, rubber, polyethylene, etc.) when handling these materials. Consult the manufacturer's Material Safety Data Sheet (MSDS) before handling any of these materials. 9. Procedure 9.1, Prepare the gas chromatograph (refer to Practice E 266) as follows: 9.1.1 Injection Port Temperature--lSO'C. When first using the method, it may be desirable to experiment with slightly higher and lower temperatures to determine if the injection port temperature is high enough for complete volatilization of the monomer, but low enough to avoid decomposition of the polymer (see 5.2).6 6 "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." 9.1.2 Oven Temperature--150C (for TDI). For other isocyanates, isothermal or temperature programmed analysis may be necessary. 9.1.3 Detector Temperature--300C. 9.1.4 Carrier Gas-^-Dry helium or nitrogen (see 5.4), flow rate adjusted to obtain proper elution time (3.7 min) of the internal standard (30 mL/min nominal). 9.2 Separation may be required for products containing pigments. Pigments may be removed using procedures given in Methods D 2372 or D 2698. Report the values for unreacted diisocyanate in the product on a pigment-free basis. 9.3 Calibrate by injecting a 1 pL aliquot of Standard Solution B (7.4) and obtain a chromatogram. 9.4 Specimens Having 0.1 to 1.0 % Unreacted Diisocya nate: 9.4.1 Weigh a 5-g specimen (0.01 g) into a tared 25-tnL (7-dram) vial. Pipet 1 mL of Standard Solution A into the vial. Add 10 mL of ethyl acetate and mix thoroughly. , w 4--Additional solvent may be added if required to reduce viscosity of the specimen. Increase the specimen size to be injected proportionally. 9.4.2 Inject a 1 pL aliquot of the test solution (Note 5); Obtain a chromatogram, internally or by temperature pro gramming as required. w 5--One-inicrblitre syringes tend to "freeze" during use With polymer solutions; therefore, a 10 pL syringe is recommended. Employ the proper technique to inject the-desired specimen size. 9.5 Specimens Having 1 to 10 % Unreacted Diisocyanate: 9.5.1 Weigh a 5-g specimen (0.01 g) into a tafed 25 mL (7-dram) vial. Pipet 10 mL of Standard Solution A into the vial and mix thoroughly. No additional solvent is added in this case. 9.5.2 Inject a 1 pL aliquot of the test solution (Note 5). 9.6 The order of elution (see Fig. 1) is: . Compound Retention Time, min ___ Ethyl acetate TCB TDI 0.4 1.9 3.7 ,, 9.7 Construct baselines under the internal standard and isocyanate peaks by drawing a straight fine from valley to valley under the respective peaks. With the standard solu tion, the isocyanate peak may return to the baseline more promptly than with sample solutions that contain polymeric species. However, it is important that the tail of the diisocyanate peak returns to the baseline. Failure to do so indicates thermal breakdown that will result in high values. Illustrations of peak shapes are shown in Fig. 1. Due to the nonsymmetrical shape of the peaks, measure peak areas by electronic integrator or planimeter. 10. Calculation 10.1 Calculate the response factor (RF) as follows (see 9.3): RF = (W, X /! )/(J+ X A0 where: Wl = weight of diisocyanate in Standard Solution B, W-t c b -- weight of TCB in Standard Solution B, A, = area of diisocyanate peak(s) (see 9.6 for measure ment), and 426 DUP050296946 FIG. 1 TDI Adduct Sample jU^CB = area of TCB peak (see 9.6). , ? 10.2 Calculate the weight percent unreacted diisocyanate, ;Z>, as follows: 10:2.1 For specimens having 0.1 to 1.0% unreacted diisocyanate: D = (Ai x RFX WrCB X W0)/(ArCB X W) where: Ax = area of diisocyanate pealc(s), ArCB = area of TCB peak, . ,W -- specimen weight, g, ! Wt CB = weight of TCB per millilitre in Standard Solution A, g, and RF = response factor from 10.1. 10.2.2 For specimens having 1 to 1.0 % unreacted `diisocyanate: ., P = (1,XRFX IVTCB x 100)/(xlTCB x W)11 11. Report i 1.1 Report the results to two decimal places, expressed as weight percent unreacted diisocyanate in the solution (ex ample: 0.45 % unreacted TDI). 12. Precision and Bias 12.1 On the basis of an interlaboratory test of this test method in which one operator in each of six different laboratories tested three unpigmented materials coveriiig a range of three levels of TDI in urethane coating solutions,- the within-Iaboratory standard deviation was found to be 0,016 % and the between-laboratory standard deviation was. found to be 0.085 %. Based on these standard deviations, the following criteria should be used for judging ihe precision of results at the 95 % confidence level: < 12.2 Repeatability:--Duplicate results by a single operator should be considered suspect if they differ by more than 0.06 % absolute. 12.3 Reproducibility--Two results, each the mean of. duplicate measurements obtained by operators in different laboratories, should be considered suspect if they dilfer by more than 0.31 % absolute. Ths American Society for Testing and Materials takes 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 live years and ifnot revised, either reapproved orwithdrawn. 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, whlcti 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. 427 DUP050296947 Designation: D 3516 - 89 An American National Standard Standard Test Methods for Ashing Cellulose1 This standard is issued under the fixed designation D 3516; 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 four ashing methods for cellulose. These are intended for use on unbleached and bleached cellulose in sheeted or bulk fiber form. Each one of the test methods has advantages, so that preference applica tions exist for all four. 1.2 The test methods appear as follows: Sections Test Method A--Ash in Cellulose at 57SC Test Method B--Sulfated Ash in Cellulose at 575"C Test Method C--Ashing Cellulose by Schoniger Oxidation Test Method D--Wet Ashing of Cellulose for Inorganics 6 to 11 12 to 17 18 to 22 23 to 29 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 Note 12. 2. Referenced Docnments 2.1 ASTM Standards: D1193 Specification for Reagent Water2* D1348 Test Methods for Moisture in Cellulose3 3. Summary of Test Methods 3.1 Test Method A, Ash in Cellulose at 575C --This test method measures the ash content of cellulose, which is defined for this test as the residue remaining after ignition at 575 25C until all carbon has been burned off. It is the simplest ofthe four test methods for the determination of ash content only, and it should not be considered as a standard preparative procedure for elemental analysis. --The ash content at this ignition temperature is a reasonable measure of the mineral salts and inorganic foreign matter in the cellulose. The weight of ash obtained varies with the temperature of ignition. Higher temperatures (850"C) will convert calcium carbonate and other carbonates to the oxides and thus give lower values for ash. The composition of ash may vary with the pulping process employed for manufacture, which limits the significance of the ash determination in absolute terms. 3.2 Test Method B, Sulfated Ash in Cellulose at J75C -- In this ashing procedure the metal salts are converted to sulfates by treatment with sulfuric acid and ignition at 575 ' 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 1.36 on Cellulosics. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 3516 - 76. Last previous edition D 3516-76 (1985). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.02. 25C to overcome limitations of Test Method A. It should not be considered as a standard preparative test method for elemental analysis. 2--Conventional dry ashing at high temperature (over 850"C) results in loss of carbon dioxide from metal carbonates, decomposition of magnesium sulfate, and loss of sodium salts. Ashing at lower temperatures (575C) gives a better estimate of the inorganic impurities, but has the disadvantage of requiring a long ignition time and also the heat produced by the burning pulp can raise the temperature for above 575C for a short period of time, converting calcium carbonate to the oxide in varying amounts. The sulfated ash method overcomes these objectionable features and has additional advantages. It is relatively insensitive to ignition time. Ash weight remains constant during weighing, and because the ash does not melt it will not attack the crucible. 3.3 Test Method C, Ashing Cellulose by Schoniger Oxida tion--This test method is generally applicable to ashing cellulose for subsequent analysis of inorganic constituents. The procedure utilizes the Schoniger technique in which the cellulose is burned in a combustion flask and all combustion products are dissolved in an aqueous medium, thus avoiding the possibility of physical loss of sample such as can occur in dry ashing (Test Methods A and B). A limitation is the relatively small sample of 1 g, which ran be ashed without excessively large apparatus in which to carry out the oxida tion step. Small specimens may not be adequately represen tative where a particulate contaminate is involved. 3.4 Test Method D, Wet Ashing of Cellulose for Inor ganics--This test method is recommended for ashing cellu lose for subsequent analysis of inorganic constituents. The procedure employs saturation of the-cellulose with a concen trated solution of hydrogen peroxide followed by incre mental addition to a small volume of concentrated sulfuric acid. It has the advantage over Test Method C of not requiring special apparatus and can be readily applied to samples of 5 to 10 g. The test method becomes tedious and less convenient for use where larger specimens such as 50 or 100 g are required. Specimens this large, although not generally required, may be necessary for the determination of trace levels of constituents such as manganese or silica. Smaller samples may not be adequately representative where a particulate contaminate is involved. 4. Significance and Use 4.1 Ash content gives an estimation of the inorganic content of cellulose samples. The presence of high levels of ash can be expected to be detrimental to the process of making cellulose derivatives. It also provides a rough esti mate of silica content which can have a significant effect on the performance of filters in cellulose derivative manufac turing facilities. 428 DUP050296948 # D 3516 fe Purity of Reagents J pj.l Reagent grade chemicals shall be used in all tests, itless otherwise indicated, it is intended that all reagents Wall conform to the specifications of the Committee on jjialytical Reagents of the American Chemical Society, pftere such specifications are available.4 Other grades may be led, provided it is first ascertained that the reagent is of TABLE 1 Ash, 55 Over 0.5 0.20 to 0.5 o.i2 to oa 0.08 to 0.12 0.04 to 0.08 Less than 0.04 Suggested Sample Sizes Moisture-Free Cellulose, g 5 10 20 30 40 50 fffficiently high purity to permit its use without lessening the curacy of the determination. |; 5.2 Purity of Water--Unless otherwise indicated, refer|jces to water shall be understood to mean reagent water as 5ned in Specification D 1193. and dried at 105C for a moisture determination. 5--Test Methods D 1348, Method B is suitable. However, accuracy ofthe moisture test is hot critical for the ash determination and any method capable of obtaining the percent oven dry within 0.5 % of TEST METHOD A--ASH IN CELLULOSE AT 575C the true value is adequate. 8.2 Heat the platinum dish in the muffle furnace at 575C Apparatus5 6.1 Balance, with an accuracy to 0.05 g is required for jjtyeighing cellulose samples. '*'6.2 Analytical Balance, with a sensitivity of 0.1 mg is Inquired. It should be checked with Class S weights. 6.3 Drying Oven, with the capability of maintaining a fcmperature of 105 2C. r 6.4 Desiccator, such as silica gel, indicating drierite, or |magnesium perchlorate are suitable. 6.5 Muffle Furnace, electric, capable of maintaining a ({temperature of 575 25C, is recommended. for 15 min, cool arid weigh to the nearest 0.1 riig. Place the weighed cellulose in the platinum dish and place the dish on the open door of the muffle furnace, previously set and allowed to reach equilibrium at 575C. Allow the cellulose to char without flame by gradually moving the dish into the muffle, and continue ashing with the door closed for 1 h. ' 6--With some pulps, the character ofthe ash inhibits complete carbon removal and gray or black specks persist after 3 h ofignition. The addition of a few drops ofdistilled water to the ash after 8.3 followed by drying and reignition at 575'C for 1 h or more may be required. Extreme cases may require a second treatment with water. 7--If the sample is too large, either separate ashings are 3--Back to front temperatures in muffle furnaces frequently lexceed the 2SC range, so that operating limits should be established jfor a given furnace. required or successive additions ofcellulose are made with extreme care so as not to disturb the ash. 8.2 is then repeated between each addition. 8.3 Remove the dish from the muffle furnace and allow to 6.6 Dish, platinum, 100-mL capacity or larger. Porcelain {{crucibles are not recommended. 6.7 Tongs, approximately 20 "in. (0.5 m) long, with Priickel-chromium or platinum tips. J |: 7. Test Specimen cool somewhat. Place it in the desiccator and allow it to cool to room temperature. 8--Care must be taken at all times to keep drafts away from the light, fluffy ash. 8.4 Weigh the dish and ash to the nearest 0.1 mg. Reignite for a 15-min period and reweigh. Repeat as required to 7.1 The amount of cellulose selected fbr each ash determi- obtain constant weight. JJnation depends on the aril content of the test specimen and Sshould be varied so that the weight of the ash will be not less 9. Calculation Jthan 10 mg and preferably over 20 mg. Table 1 gives 9.1 Calculate the ash percent of moisture-free cellulose, E, t suggested sample sizes. as follows: __ ; J 7.2 Selection of the specimen shall be in such a manner as | tb be representative of the lot being tested. 4--No set , sampling procedure has been established to be applicable to all samples. It will suffice to specify that the specimen shall where: --_ (C-Bt 100X100) E~ (A (D) ` ... (1) be representative of the lot bang sampled. A = weight of specimen as is, g, 8. Procedure B = weight of dish, g, C = weight of dish plus ash, g, and 8.1 Weigh out, to the nearest 0.05 g, sufficient cellulose to D = oven dry cellulose in specimen, % ip give the correct range of aSh weight (see Table 1). At the 10. Report same time, a separate specimen (3 to 5 g) should be weighed* 1 10.1 Report the results to the nearest 0.01 %. Duplicate determinations should check within approximately 5 %. * "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 Resin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 1 Suitable apparatus is available from A. H. Thomas Co., Vine St. at 3rd, P. O. Box 779, Philadelphia, PA 19105. 11. Precision and Bias 11.1 A precision of 8 % relative at the 95 % confidence level is found for specimens at the 0.05 % ash level. 11.2 No statement of bias can be made as no suitable reference material exists for determining bias. 429 DUP050296949 D 3516 TEST METHOD B--SULFATED ASH IN CELLULOSE AT 575C 12. Apparatus and Reagent 12.1 Hot Plate. 12.2 Additional apparatus shall be in accordance with Section 6. 12.3 Sulfuric Acid--Concentrated H2S04. and true weight was determined, and carrying through 14.# to 14.8 as they apply. 15. Calculation 15.1 Calculate the sulfated ash, S, as percent of moisturefree cellulose, as follows: o _ (C-B~m00Kl00) S (A) <D) ' 13. Test Specimen 13.1 The: amount of cellulose selected for each ash deter mination-,depends upon the sulfstted ash content of the test specimen and should be varied so that the weight of the ash will be not less than 10 mg and preferably over 20 mg. Table 1 gives suggested specimen .sizes for Test Method A. The table is applicable to sulfated ash also, providing the percent ash column is taken as percent sulfated ash. --The sulfated ash values will be higher than the ash obtained by ignition of the cellulose without addition of the sulfurie 'acid. The magnitude .of the difference will depend upon the .proportions of different inorganic salts present, but based on the following conversion factors for the kits commonly present, will generally be about twice the regular ash: MgSO, MgO CaSO, ' CaO MgSQ4 2.43; MgCQ3 1.43 (2) Na,SQ4 CaSO, = 1.36; Na2C02 = 1.34 (3) 13.2 Selection of the specimen shall be in such a manner as to be representative of the lot being tested (see Note 4). 14. Procedure 14.1 Weigh out to the nearest 0.05 g sufficient cellulose to give the correct range of ash weight (see Table 1). At the sam time, weigh a separate specimen (3 to 5 g) and dry to constant weight at 105 2C for a moisture determination (see Note 5). 14.2 See 8.2. 14.3 Remove the dish and allow it to ,0001 to room temperature (see Notes 7 and 8). 14.4 Moisten the ash with 1 to 2 mL of concentrated H2S04 and heat on a hot plate until all the dense white fumes of sulfur trioxide (S03) are liberated. 14.5 Place in the muffle furnace and ignite at 575C for 1 h. If carbon persists repeat I4.3? 14.4, and 14.5. 14.6 After the last trace of carbon has disappeared, ignite in the muffle furnace for 1 h at 575C. 14.7 Remove the dish and allow it to cool somewhat before placing it in desiccator and cooling to room tempera ture. 14.8 Weigh the dish and sulfated ash to the nearest 0.1 mg. Reignite for a 15-min period and reweigh. Repeat as required to obtain constant weight --To remove the ash from the dish, clean with boiling hydrochlo1r1ic--aOcind. igniting sulfated ash at 575C, there should be no fusion with the dishes, even when ashing cellulose that gives an alkaline ash. 14.9 Prepare a reagent blank for the H2S04 corresponding to the number of millilitres of H2S04 used in 14.4 and 14.5, by the addition of the acid to a platinum dish after ignition where: A ~ weight of specimen, g, B = weight of dish, g, C -- weight of dish plus sulfated ash, g, R - weight of H2S04 reagent blank residue, g, and D = oven-dry cellulose in specimen, %. 16. Report 16.1 Report the results to the nearest 0.01 %. Duplicate determinations should check within approximately 5 %. 17. Precision and Bias 17.1 A precision of 15 % relative is found for specimens in the 0.1 to 0.3 % ash range. 17.2 No statement of bias can be made as no suitable reference material exists for determining bias. TEST METHOD C--ASHING CELLULOSE BY SCHONIGER OXIDATION 18. Apparatus 18.1 Combustion Flasks, 5000 mL, round bottom, borosilicate glass, with 65/40 bail andjoint stopper. The.flasks are equipped with perforated platinum specimen carriers sealed into the extended stem of the flask stopper. 18.2 Igniter, suitable for igniting the specimen in the flask. An infrared igniter is preferred. 18.3 Specimen Wrappers, black paper. . ~ 18.4 Pipet, 5 mL. 18.5 Volumetric Flask, 50 mL. ___ 19. Reagents ~- 19.1 Deionized Water, high-purity, with- a conductivity <1.0 (unho/cm at 25C. 19.2 Absorption Solution--0.2 N H2S04 prepared from concentrated H2S04. 20. Procedure 20.1 By hand, tear a 2- to 3-g air-dried test portion of the sample into 1 to 1.5-cm pieces arid store in closed airtight, glass or polyethylene bottles. 20.2 Weigh a 1-g portion of the prepared sample to 1 mg, and wrap in a square of black ignition paper. ,, 20.3 Weigh a second portion of sample, approximately 1 g to 1 mg, and determine the moisture content in accordance with Test Methods D 1348. This test method determines the weight loss on a 1-g specimen placed in a gravity convection oven at 105C for 4 h. 20.4 Add by pipet, 10 mL of 0.2 N H2S04 as an absorption solution to the combustion flask. 20.5 Place the specimen contained in the wrapper into the platinum carrier and insert into the flask. 430 DUP050296950 D 3516 ,,,6 Allow a stream of oxygen from a low-pressure, alated supply (2 to 3 lb./in.2 (14 to 21 kPa)) to flow into flask for a period of 30 s to displace the air. Secure the pper in the flask with the pinch damp and place the ansion balloon on the side tube. "OTE 12: Precaution--It is required that laboratory goggles be worn -ring 20.6, 20.7, and 20.8 as a safety measure. 120.7 Place the flask behind a safety shield or in a hood th a protective door. 60.8 Turn oil the igniter and focus the infrared light beam the fuse strip of the black paper wrapper until ignition urs. Allow the specimen to burn completely and cool the k for 1 h so that, all vapors are absorbed in the solution. 0.9 Transfer the solution tp a 150-mL beaker and rinse flask with two 15-mL portions of deionized water and d to the absorption solution in the beaker, 20.10 Transfer the contents of the beaker to a 50-mL oiumetric flask and rinse with 2 to 4-mL portions of eionized water. Add water to bring to 50-mL volume. dentify as Schoniger ash solution. l! .20.11 Ash a black wrapper identical in weight to one used ' or wrapping the specimen by following 20.4 to 20.10, Identify as wrapper andAbsorption solution blank. f $21. Calculation 21.1 Calculate the concentration equivalent for oven-dry . (cellulose, C, in Schoniger ash solution, as follows (Note 13): f- (Am (50)000) (5) 30-g specimen to solution in a form suitable for aliquoting for metals analysis is about 2 h. 24. Apparatus 24.1 Balance, sensitivity to 0.01 g. 24.2 Beakers, Berzelius, 300-mL. 24.3 Beakers, 150-mL. 24.4 Cylinder, graduated-pharmaceutical, 50-mL. 24.5 Forceps, 20-cm stainless steel, TFE-fluorocarbon tipped. 24.6 Hot Plate, sensitive temperature control, ceramic-top surface or alternative suitable for use with platinum ware. Metal surfaces are not suitable. 24.7 Pipet, 10-mL. 24.8 Rubber Bulb, foT filling pipet. 25. Reagents 25.1 Hydrogen Peroxide, 50 % H202. 15--The actual concentration is not critical, but the absolute minimum is 30 % below which the test fail?. One should be aware that hydrogen peroxide solution tends to lose strength upon standing. 25.2 Sulfuric Add, concentrated H2S04. 26. Hazards 26.1 The procedure specifies many repetitive manual additions of a strong oxidant and organic material to conceptrated, acid. It is imperative that the analyst wears protective equipment for the eyes and hands, and works in a fume hood free of distraction during the steps in Section 28. where: * A = weight of cellulose spedmen, and B = oven-dry cellulose in specimen, % 13--Use of the solution for subsequent analysis assumes . parallel treatment of both the Schoniger ash solution and the wrapper ;i absorption solution blank to provide for the analytical blank correction, if 14--The purpose in specifying the calculation of equivalent oven-dry cellulose in grams per millilitre is to provide for convenient use rof aliquots for subsequent elemental analyses. I 22. Precision and Bias 22.1 A precision of20 % relative is found for specimens at the 0.2 % ash content level. The operator's technique is very important in keeping the precision at a high level. 22.2 No statement on bias can be made as no suitable reference material exists for determining bias. TEST METHOD D- -WET ASHING OF CELLULOSE FOR INORGANICS 23. Summary of Test Method 23.1 A test specimen of pulp is torn into small pieces approximately 1 cm across, saturated with a solution of hydrogen peroxide, and added one piece at a time to a small volume of concentrated sulfuric acid. 23.2 The cellulose is oxidized to carbon dioxide and water. The water is volatilized by the heat of the reactions involved. 23.3 An analyst experienced with the technique can ash 30 g of pulp into an initial volume of only 10 mL of sulfuric acid in about 30 min. Total procedural time for converting a '27. Sampling .` 27.1 Select an appropriate sized sample as specified in the methods for inorganic elements to be determined, with an allowance for a moisture determination. 27.2 Tear the pulp by hand into small pieces approxi mately 1 cm across. 27.3 Weigh the selected weight of the spedmen to 0.01 g. 27.4 Determine the moisture content on a separate spec imen in accordance with Test Methods D 1348. 27.5 Correct the spedmen weight (27.3) to -the oven^dry basis for subsequent calculations. 28. Procedure 28.1 Pipet 10 mL of H2S04 to a 300-mL tall form Ber zelius beaker. 28.2 Place approximately 10 g of the weighed pulp spec imen into a 150-mL beaker. 28.3 Pour approximately 50 mL of H2Oz into a 50-mL graduated cylinder. 28.4 Distribute approximately 30 mL of the measured portion of H202 over the 10 g of spedmen allowing the pulp to saturate with it. 28.5 Add 2 to 3 mL of H202 to the 10 mL of H2S04 by allowing it to run down the side ofthe beaker. Carefully swirl to mix, resulting in gas evolution. If mild boiling is not evident, heat gently on hot plate to induce it, then remove the beaker from the hot plate. 28.6 With stainless tongs, add the pulp saturated with H202 one piece at a time allowing for almost complete destruction between each addition. 431 DUP050296951 D 3516 16--A porcelain spatula has been used in place of stainless tongs to transfer the pulp to the acid apd may be preferable for spec imens in powdered state. Pulps vary in their behavior to the ashing step. Thirty grams of some pulps have been ashed with only 2 or 3 additions of H202 separate from the pulp. These are required whenever the acid retains a brown or black residue after destruction of a pulp addition. With other pulps, ten or more 1 to 2 mL additions ofhydrogen peroxide may be required. 28.7 After the initial 10-g portion of pulp has been ashed, repeat 28.2 to 28.6 on a second 10-g portion of the weighed specimen. 28.8 Repeat 28.7 until the total specimen is ashed. 28.9 Rinse the sides of the beaker containing ashed spec imen with distilled water from a wash bottle. Use the minimum amount required. 28.10 Swirl the beaker to mix the rinse water with the acid. 28.11 Place the beaker on the hot plate and heat to the point that dense fumes of H2S04 evolVe. 17--If the arid discolors^ remove the beaker from the hot plate, allow it to cool, and add 2 to 3 mL offi202 to the beaker. Return the beaker to the hot plate and continue heating. Repeat this step as required to attain a colorless solution! 28.12 Continue heating to remove the excess acid. 18--The final volume ofacid is selected relative to subsequent analyses, however 2 to 3 mL has been satisfactory fpr most applications. 28.13 Remove the beaker from the hot plate, allow it to cool, and with extreme care add distilled water, allowing it to flow down the side of the beaker to the required dilution. Transfer it to a 25-mL volumetric flask; and adjust to volume. 19--Ifan ash-determination is desired, transfer the solution to a preweighed platinum dish, take to dryness, and ignite at approximately 400"C prior to weighing. The residue may then be taken up in distilled water for elemental analysis. Some sulfates may be difficult to solubilize, particularly ferric sulfate, requiring subsequent beating. 28.14 Prepare a reagent blank corresponding to the 10 mL of H2S04 and the volume of H2Oz used by slow addition.of increments of the peroxide to the acid followed by gentle heating to remove the oxygen' and water. Complete the blank in accordance with 28.12 and 28.13. ' " / 28.15 The solutions from 28.13 and 28.14 are now suitable for subsequent elemental analysis. 29. Precision and Bias 29.1 A precision of 20 % relative is found for specimens at the 0.5 % ash content level. 29.2 No statement of bias can be made as no suitable reference material exists for determining bias. i j I The American Society tor Testing and Materials takes noposition 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 die risk of Infringement ofsuch rights, ere entirely their own responsibility. This standard Is subjeetto revision et 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 Invitedeither for revision otthis 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, 9/hlch you may attend. If you feel that'your comments have not received a fair hearing you should make your views knownto the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. '^ 432 DUP050296952 Designation: D 3619 - 77 (Reapproved 1989) An American National Standard Standard Specification for Aluminum Silicate Pigments (Anhydrous)1 This standard is issued under the fixed designation D 3619; 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. Scope 1.1 This specification covers the white pigments that ~nsist substantially of anhydrous (calcined) natural aluinum silicates12 (ofthe 1+1 layer type) and are restricted to ose minerals which conform to the chemical compositional i prescribed herein and which can be suitably, processed i what is known as paint pigment quality. |, Referenced Documents P 2.1 ASTM Standards: D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out3 D718 Test Methods for Analysis of Aluminum Silicate Pigment3 D1203 Test Methods for Volatile Loss from Plastics Using Activated Carbon Methods4 D1483 Test Method for Oil Absorption of Pigments by Gardner-Coleman Method3 D2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment3 D 3360 Test Method for Particle Size Distribution by Hydrometer of the Common White Extender Pigments3 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode5 3. Composition and Properties | 3.1 Preparation--The pigment shall be made by grinding, {(milling, washing, purifying, or otherwise processing, natural hydrous aluminum silicates followed by heat treatment (calcination) sufficient to reduce the residual percent loss on [ignition to a maximum of 0.5 % and otherwise conforming to the composition requirements (weight percent) given in Table 1. 3.2 pH--The pH of a water slurry of the pigment shall be within a range from 4.5 to 5.5 unless otherwise agreed upon between the purchaser and the seller. 3.3 Water-Soluble Matter--The water-soluble matter shall be not more than 0.60 %. 3.4 Wet-Sieve Residue--The pigment shall contain no more than 0.02 % wet-sieve residue retained on a 45 pm (No. 325) sieve (grit or coarse particles) except as may be 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 D0I.31 on Pigment Specification. Current edition approved Nov. 10, 1977. Published January 1978. 2 Synonymous terms are kaolinite and china clay. 3 Annual Book ofASTM Standards-, Voi 06.02. * Annual Book ofASTM Standards, Vol 08.01. 3 Annual Book ofASTM Standards, Vdl 15.05. agreed upon between the purchaser and the seller. 3.5 Brightness (Color)--The brightness (color reflectance) shall conform to the following requirements: 3.5.1 The brightness shall be not less than 9&% nor more than 92 % expressed as percent reflectance of standard illuminant C at 457 am compared to a freshly smoked magnesium oxide surface by means of an accepted inte grating sphere reflectance spectrophotometer6 or a mono chromatic reflectance meter,6 or 3.5.2 The color may be specified by actual determination of dominant wavelength, hue, and spectral efficiency as can be calculated from the tristimulus integration of the reflec tance, curve, or 3.5'3 The color shall be equal, within agreed upon toler ances, to that of a reference standard agreed upon between the purchaser and the seller. 3.6 Oil Absorption--The oil absorption shall be within the range from 40 to 60 g/100 g as determined by the spatula rub-out test (Test Method D 281) or within a range from 60 to 80 g/100 g as determined by the Gardner-Coleman test method (Test Method D 1483) (see 5.1.4). It may be noted that reproducible test results using the spatula rub-out test method (Test Method D 281) are found to be very difficult to obtain because of a very high electrostatic charge imparted to the anhydrous pigment during the rub-out procedure. Al though a spatula rub-out test result can be obtained, it has been found by experience that much more reproducibleresults can be obtained by use of the Gardner-Coleman test method. 3.7 Particle Size--Anhydrous aluminum silicate pig ments may be furnished in several types w grades whose properties are dependent in part on the average particle size or particle size distribution about the average, or both; characteristic particle shape is as thin, flat, and laminated plates. The particle size or size distribution, or both, shall be within agreed upon tolerances to that of a standard agreed upon between the purchaser and the seller, but in general, the average particle size should be close to 2 pm. 4. Sampling 4.1 Two samples shall be taken at random from different packages of each lot, batch, day's pack, or other unit of production in the shipment. When no markings distin guishing between units of production appear, samples shall be taken from different packages in the ratio of two samples for each 10 000 lb, except that for shipments of less than 10 000 lb, two samples shall he taken. At the option of the 6 The General Electric Reflectance Spectrophotometer (Diano Corp-)> the General Electric Reflectance Meter, and the ElRefo Blue Reflectance Meter have all been found suitable for this purpose. 433 DUP050296953 1 3619 TABLE 1 Pigment Composition Requirements {Percent by Weight) The major constituents shown In the analysis are combined as complex aluminum silicate and do not exist as free oxides. ideal Typical Range, Max Aluminum oxide, 7 s03, % Silicon dioxide, SiOj, % iron oxide. Fe203, % Titanium dioxide, Ti02, % Calcium oxide, CaO, % Sodium oxide, Na^O, % Potassium oxide, KsO, X Other oxides, % Free moisture (105*0), X, Loss on ignition (1000C), % Free silica (either amorphous or as crystaliirte quartz), X" 45.91 44.4 54.09 52.3 .. 0.1 . 2.0 ... . . "... <0.5 . <0.5 4349* 56-50 . d. . : 2.5 0.1 ... 0.1 0.1 - V 0.T V. 0.5 0.5 1.0 Permitting Op to about 5 % excess AI2O3, for example, as allophane. '' Permitting up to about 5 % excess SIO* for example, but no more than 1 x of free slca (SCy either amorphous-,or as crystalipe quartz. purchaser, the samples may be tested separately or after blending the samples from the'same production unit in equal quantities to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ATM;test methods. where applicable. Test procedures not covered by" ASTM test methods shall be agreed upon between the purchaser and. the seller, except as follows: .' i 5.1.1 Hydrogen ion Concentration (pH)--Prepare a sample having 20 % solids, but otherwise in accordance with Test Methods D1203. Determine the pH in accordance with Test Method E 70, except maintain sufficient agitation ofthe slurry srich that ail particles are in suspension Ut the time of nteasuremeiit.' ' r ' 5.1.2 Waler-Soluble Matter-Test Method D2448. 5.1.3 Coarse Particles--Test Methods D 718. ' 5.1.4 Oil'Absorption--Test Methods D 281 6i D1483. 5.1.5 Particle Size Distribution--*test Method D3360. 5.1.6 Chemical Analysis--Test Methods D 7,18. . 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 of any such patent rights, arid the risk of Infringement ofhitch 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 reapprovedor withdrawn. Yourcomments are invited either for revision of this standard erfor additional standards *' and should be addressed to'ASTM Headquarters. Your comptents will receive careful consideration at a meeting of the responsible' -. technical committee, which you may attend. Ifyoli feet that your eommants have not received a fair hearing you should make your views known to the ASTM Cofnmlttee on Standards, 1916 Race St, Philadelphia, PA 1S103. s 1, .< -.if....- ? i.: ' . .Hi. '. .. i ** ; 1; u- i 434 DUP050296954 Designation: D 3680 - 89 An American National Standard Standard Test Method for Residual Vinyl Chloride Monomer Content of Poly(Vinyl Chloride) Resins, Compounds, and Copolymers by Solution Injection Technique1 This standard is issued under the fixed designation D 3680; 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. Scope rl.l This test method can be used to determine small * ounts of residual vinyl chloride monomer (VCM) in ly(vinyl chloride) (PVC) resins. It may be possible to use it pt other resins or compounds containing'vinyl chloride Ibvided there are no other volatile components present with same retention rime as vinyl chloride monomer. <2 This standard may involve hazardous materials, oper|dons, and equipment. This standard does not purport, to iddress.all ofthe safety problems associated with its use. It is %e 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 9.. ' l. Referenced Documents. 2.1 ASTM Standards: E 260 Practice for Packed Column Gas Chromatography2* E 355 Practice' for Gas Chromatography Terms and 1 Relationships2 . Terminology 3.1 Abbreviations 3.1.1 VCM--vinyl chloride monomer. ' 3.1.2 PVC--poly(vinyl;chloride) resin. , 3.1.3 RVCM--residual vinyl chloride monomer. 3.1.4 DMAC--dimethyl acetamide: 3.1.5 THF--tetrahydrofuran. 4. Summary of Test Method 4.1 The resin, compound,., or copolymer, specimen is dissolved in a suitable solvent and is then' aitijlyzed by conventional gai chromatographic (GC) techniques. Anal ysis time can be decreased by utilizing, a bfickflush mode to eliminate the solvent. 5. Significance and Use 1 5.1 Poly(vinyl chloride) resins must contain a minimum possible amount of unreacied, or free vinyl chloride j mbnomer.' 5.2 Under optimutn conditions approximately 1 ppm * 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint j and Related Coatings and Materials and is the direct responsibility- of Subcom, mittee D0L33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally ! published as D3680 - 78. Last previous edition D 3680 - 78. 2 Annual Book ofASTM Standards, VoL 14.01. VCM can be detected in PVC resins. 6. Interferences 6.1 Any material that elutes at approximately the same retention time as VCM will cause erroneously high RVCM results. 6.2 Special care mnst be exercised in interpreting the RVCM results obtained from the analyses of PVC copoly mers or compounds. Many ingredients are added to PVC resins to obtain compounds with desired properties for each particular end use. These additives, or components in them, could possibly have the same retention time as VCM. In general, if a PVC compound apparently has a much larger VCM content than the starting resin, then the presence of some interfering component can be suspected'as the prob able cause of the larger than expected amount in the compound. 'l jr . .r , 7. Apparatus 7.1 Gas Chromatograph, with dual flame ionization de tector, and heated injection port with removable glass inserts. 7.2 Recorder, 0 to 1-mV full scale. No t e 1--Electronic integrators, or computer systems dan be used to obtain peak areas and make the required calculations. J -'17.V .'i v s!',. >f<\ ':* 7.3 Analytical Balance, capable of weighing to 0.0001 g. 7.4 Soap Film Flowmeter. 7.5 Stopwatch. --- 7.6 Pressure Regulators, for all the required gas cylinders. 7.7 Filter Dryer Assemblies, For each of the GC gas cylinders. 7.8 Vials, 6-dram, with polyethylene-lined screw caps.3 N 2--Caps with .wax liners, .should npt be used for sample dissolution. No t e 3--Vials and daps should be used only once and discarded. ' 7.9 Serum Bottles, 60-mL, and Stoppers.4 u. 7.10 Liquid Sampling Syringes, 10 and 50-pL. GC Liquid Sampling`Syringes, 10 and 50-ftL. 7.11 Qas Syringes, 0.1 and 1-mL,5 equipped with, valve s Vials #609S7-L, available from Kimble Glass Co., Div. Owens Coming, Inc., One Sea Gate, Toledo, OH 43666, or equivalent, has been found satisfactory for this purpose. ' 4 Fisher No. 3-220C bottles and'3-225 stoppers, available from Fisher Scientific Co.l 711 Forbes Ave., Pittsburgh, PA 15219, or equivalent, have been found, satisfactory for this purpose. 5 Series A-2 syringes, available from Precision Sampling Corporation, 16 Tech Circle, Natick, MA 07160, orequivalent, have been found satisfactory for this purpose. 435 DUP050296955 Tec Carrier Gas Source Auxiliary Plow Controller Ball Valve Injection Port Short Column A Tee Long Column c. Detector FIG. 1 Schematic of Backflushing Method locks. 7.12 Ball Valve, two-way, stainless steel.6 7 8 7.13 Flow Controller.1 7.14 Screw Cap, 6-dram, with Needle Seal Septa.9 7.15 Reciprocating or Wrist-Action-Type Shaker. 7.16 Column and Packings--Any ofdie following may be used: .7.16.1 Vs in. outside diameter by 1 ft plus '/* in. outside diameter by 6 ft stainless steel packed with 80/100 mesh Poropak S or Poropak Q-S.9 7.16.2 Vs in. outside diameter by 20 ft stainless steel packed with' 20 % Tergitol E-3510 11on 60/80-mesh Chromosorb W-AW," 7.16.3 Vs in. outside diameter by 3 ft plus Vs in. outside diameter by 6 ft with 0.2 % Carbowax 150012 1o3n Carbopak 7.16.4 Vs in. outside diameter by 20 ft packed with 20 % Apiezon L14 on 60/80-mesh Gas-Chrom Q.15 No t e A--The above-mentioned column lengths and packing have been used successfully for this analysis. However, any column that will elute VCM in reasonable lengths of time (1 to 4 min) can be used provided any interfering components are hot eluted at the same time as VCM. "Catalog No. 4152-A-316, available from Whitey Co., 318 Bishop Rd, Highland Heights, OH 44143, or equivalent, has been found satisfactory for this purpose. 7 Model 8744A, Brooks Instrument Co., Div. Emerson Electric Co., 407 W. Vine St., Hatfield, PA 19440, or equivalent, has been found satisfactory for this purpose. 8 Precision Sampling Corp. Catalog No. 614063 and No. 644350, or equivalent, has been satisfactory for this purpose. 8 Poropak is a trademark for porous polymer beads developed by the Dow Chemical Co., 2020 Dow Center, Midland, MI 48674, and marketed for gas chromatographic use by Waters Associates, Inc. 10 "Tergitol E-35," a trademark of the Union Carbide Corp., 39 Old Ridgebury Rd, Danbury, CT 0681741001, or equivalent, has been found satisfactory for this purpose. 11 "Chromosorb W-AW," a trademark of Manville Products Corp., 717 17th St., P.O. Boa 5108, Denver, CO 80217, or equivalent, has been found satisfactory for this purpose. 12 "Carbowax 1500," a trademark of Union Carbide Corp.. or equivalent has been found satisfactory for this purpose. 13 Carbopak, a trademark ofSupelco Inc., Supelco Park, Bellefonte, PA 16823, or equivalent, has been found satisfactory for this purpose. 14 "Apiezon," a trademark ofthe James F. Biddle Co., 510 Township Line Rd., Blue Bell, PA 19422, or equivalent, has been found satisfactory for this purpose. 15 "Gas-Chrom Q," a trademark of Applied Science Laboratories, 111 Bullard, Parkway Suite 208, P.O. Box 16118, Tampa, FL 33687, or equivalent, has been found satisfhctory. 7.17 Jars, 2-oz (60-mL), with aluminum or polyethylerie-s lined screw caps. 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,16 where such specifications are available. 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 Air, breathing or water-pumped. 8.3 N.N-Dimethyl Acetamide (DMAC) (Note 5). No t e 5--Either: solvent (DMAC or THF) may be used. However,' they must be free ofany contaminants that have the same retention time as VCM or any internal standard that may be Used. To determine this, inject 10 jiL ofsolvent and obtain a chromatogram under the conditions of Section 11. 8.4 Hydrogen, prepurified or zero gas. 8.5 Nitrogen, oxygen-free. - __ No t e 6--Helium may also be used as the carrier gas. 8.6 Pentane, at least 99 %. 8.7 Teirahydrofuran (THF) (Note 5). .. 8.8 Vinyl Chloride Monomer, polymerization grade. 9. Hazards 9.1 In addition to other precautions, conduct all opera tions including the preparation of standards, transfer of solvents, and column backflushing (if the technique de scribed in 11.1 is used) in a properly functioning fume hood. 10. Sampling and Storage 10.1 Keep all resin samples in tightly sealed jars. Samples should be analyzed within 24 h. If 24 h are exceeded, report the age of the sample. Use 2-oz (60-mL) bottles with aluminum or polyethylene-lined screw caps, completely filled, and seal with electrical tape. ""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." 436 DUP050296956 # D 3680 , ,. 10.2 Compound samples can be kept in the same type jars. The remaining precautions are not required as long as ithe jar is tightly sealed. * 11. Preparation of Chromatograph '11.1 Install the chromatographic column and condition at feast overnight at the temperature limit for the packing being used. Do not connect the exit end of the column to the detector while conditioning. Turn offhydrogen and air to the detector while the column is disconnected. One method of Schieving the backflushing of the solvent is shown schemat ically in Fig. 1. The two columns are separated by a "Tee" fitting. Connect the short column between the injection port and One end of the "Ted." Connect the longer column between the other end of the "Tee" and the detector. Connect a line from the outlet of the ball valve to the center inlet of the "Tee." This auxiliary line may be filled with a 1 suitable column packing if desired to act as a pressure buffer when switching to the backfhish mode. Insert "Tee" into the ! carrier gas supply line to supply the auxiliary flow controller. ! 11.2 Adjust the carrier gas flow as follows (Note 7): 1'1.2.1 Close off the auxiliary flow with the ball valve. 11.2.2 Set flow at 30 mL/min with the chromatograph flow control valve. 11.2.3 Remove the septum from the injection port. 11.2.4 Open the ball valve. 11.2.5 Again adjust the flow to 30 mL/min with the auxiliary flow control valve. 11.2.6 Close the auxiliary flqw with the ball valve. 11.2.7 Replace the septum on the injection port. 11.2.8 The system is now ready for an analysis. No t e 7--If posable with the chromatograph being used, adjust the earner' flow at the analysis temperature. ; 11.3 Set detector air and hydrogen flows and pressures at the optimum conditions for the make and model of chro matograph being used. 11.4 Set temperatures as follows: 11.4.1 Optimize oven (chromatograph column) tempera ture to elute VCM between 1 and 4 min after injection. 11.4.2 Injection Port--200C. 11.4.3 Detector--Ax least 20C above maximum column temperature. Nora 8--Other systems of backflushing have been evaluated. How ever, none ofthem have been very successful. This is probably due to the fact that a small amount ofsolvent seems to remain in the column and injection port This small amount of solvent is always detected at the extreme detector sensitivity required for this analysis. It may then take as long as 30 to 40 min to return to a stable baseline. Two alternative methods of flushing solvent from the column are described in Annex Al. _ ' No t e 9--A trial-and-error method is used to determine the optimum time to remove and replace the septum holder for backflushing the solvent. The objective is to wait as long as possible to be sure that the VCM has passed through the short column but still to retain ail, or most, of the solvent in the short column before removing the septum to backflush it, then to replace the septum after the solvent has backflushed out through the injection port. 12. Calibration by External Standard 12.1 Prepare solution mixtures of varying amounts of VCM in solvent to cover the expected parts per million range of concentration. These can be prepared as described for the internal standard method in 13.2 and 13.3 without adding the internal standards. Obtain a gas chromatogram for each calibration standard using the parameters listed in Section 11. Prepare a chart plotting the peak height (or area) from the chromatograms versus the known concentration ofVCM in each calibration standard to establish a detector response curve. 13. Calibration with an Internal Standard 13.1 Prepare a polymer solvent solution containing a known amount of internal standard as follows: 13.1.1 Partially fill a 1-L Volumetric flask with solvent. 13.1.2 Into a separate beaker or flask containing a tared weight of solvent, add, by means of a syringe, approximately 0.0150 g of pentane. Reweigh the container immediately and determine the exact amount of pentane added to the nearest 0.1 mg. . 13.1.3 Immediately upon reweighing, quantitatively add the contents of the container to the 1-L volumetric flask. Do so by rinsing the container with aliquot portions of the solvent. Bring to the mark with fresh solvent. Mix thor oughly and calculate the grams of pentane , per 20 mL of solution as follows: Grams pentane/20 ml = weight:of pentane/50 13.1.4 Store the internal standard solution, thus prepared, in an amberized bottle. Label the bottle Solution A. 13.2 Weigh 50.00 0.01 g of the solvent into a tared, serum bottle to the nearest 0.1 mg. Immediately seal the vial. Record the weight of the solvent. 13.3 Using a 0.1-mL Pressure-Lok17 syringe add about 0.025 mL. of liquid vinyl chloride monomer to the sealed bottle. Reweigh to the nearest 0.1 mg. Determine the weight of vinyl chloride added and the total weight of the solution. Calculate the grams of vinyl chloride per gram of solution. Identify this as Solution B. .grams VCM Grams VCM/gram Solution B = gfams VCM + grams solvent 13.4 Pipet 20.0 mL of Solution A into a'rial equipped with a screw cap and a TFE-fliiorocarbon. "Minin&rt"18- valve. Immediately cap, weigh, and record the weight of the solution and the sealed container. .._ 13.5 Using the UmL syringe, inject approximately 1 mL of; Solution B into the contents of the vial. Reweigh and determine the weight of Solution B that was added to Solution A. Once prepared, this standard is not to be opened. Prepare a new standard each time a fresh Solution A is prepared. 13.5.1 Calculate the amount of vinyl chloride in the prepared standard as follows: weight of VCM = weight of Solution B x grams VCM/grams of Solution B (from 13.3) 13.6 Using the operating conditions described in Section 17 Pressure-Lok syringes, manufactured by Precision Sampling Corp., are made specifically to maintain liquids and gases under pressure within the syringe. 18 Mininert valves and caps are manufactured by the Precision Sampling Corp. The caps are designed so that the contents of the vial can be removed with a syringe without removing the cap. The valves attach to the lever fitting ofa syringe to permit sampling or storage under pressure. 437 DUP050296957 # D 3680 11 and the procedure described in Section 14, inject 10 JJ.L of this standard solution containing known amounts of pentane and VCM into the chromatographic system. Determine- a Response Factor (RF) as outlined below from the ratio of peak areas of the vinyl chloride and pentane and their known weights: weight of pentane x peak area VCM ^ ~ weight of VCM X peak area pentane 13.6.1 Example: Pentane VCM Weight 0.0002940 0.0005190 .Area 6471 8921 0,0002940 x 8921 = 0.781 0.0005190 X 6471 No t e 10--For highly accurate determinations of the response factor, it is advisable to run the calibration standards a minimum of five times. The average of these runs is then used. The stability of the response factor must be verified at least once per week. 14. Sample Analysis Procedure 14.1 Sample Preparation: 14.1.1 Mix the sample to be analyzed completely so that the portion selected will be as representative as possible. Weigh 1 g of the sample to ,be analyzed into a tared 6-dram vial and recap the vial and contents and determine the specimen weight to the nearest 0.1 mg. 14.1.2 By means of a pipet, add 20.0 mL of solvent or Solution A (see Section 13) containing the solvent and internal standard to the specimen vial. - No t e 11--Twenty millilitres of solvent yields a 5 weight-% solution. Ten millilitres of solvent will yield a 10 weight % solution. 14.1.3 Place the vial on a shaker until the spedmen is completely dissolved. Once it is visually in solution, the specimen must be shaken for at least'one additional hour. Leave all specimens on the shaker until they are analyzed. 14.2 Inject 10 jiL of the prepared specimen. , No t e 12--A larger volume of prepared specimen (greater than 10 pL) may be utilized when analyzing for very low levels ofvinyl chloride. Care must be taken, however, to back flush the extra solvent from the system before injecting subsequent specimens. Also With latger injetfion volumes (20 to 40 pL) there is sometimes a possibility that some of the solvent does not volatilize. For cases in which backflush capability does not exist, the use of a smaller specimen size and another solvent, for example, acetone, has been found to be acceptable. No t e 13--The syringe used to inject specimens into the chromato graphic system must be rinsed with solvent between each specimen injection. No t e 14--The glass insert in the injection port will catch and retain the solid particles from the specimen that would gradually foul the column. Loosely pack the Va in. at the outlet end of the glass tube with glass wool. Change this trap after every specimen. Change the septum at the beginning of each shift. Do not force the septum tightly against the glass tubing as this will restrict flow to the column. 14.3 At the predetermined time (see Note 9) remove the septum and actuate the ball valve to backflush the solvent. 14.4 At the end of the predetermined time (see Note 9) first actuate the ball valve to stop the backflush flow, then replace the septum on the injection port. 14.5 Allow at least 2 min for the baseline to equilibrate. Allow the equipment to sii longer if necessary until there is minimal baseline drift at the attenuation to be used for the analysis. No t e f5--After running the last specimen prior to a break in the analysis routine (of a limited time span) leave the system in the backflushing mode. An example of this would be a lunch break. When the down time will be ofa longer nature, suchas an entire shift, perform the normal backflushing operation after the last specimen and.then leave the equipment with earner flow in the forward position. 15. Calculation--External Standard Method 15.1 Determine the monomer content of the specimen from the calibration dhart (see section 12). Compare the peak height (or area) ofthe VCM peak ofthe chromatogram to the calibration curve and read the corresponding concentration in parts per million (ppm). No t e ;16--The use of the external standard technique is extremely dependent on specimen size. Amount of specimen injected must be as much the same as it is possible to obtain for each injection. No t e 17--The concentration value obtained from the calibration curve is the total VCM in solution. In order to convert the VCM concentration to a specimen weight basis, if a 10 Weight % spedmen solution was prepared, the- chart value must be multiplied by a factor of 10. If a 5 weight % specimen solution was made, then the multiplying factor is 20. r . 16. Calculation--Internal Standard Method 16.1 Calculate weight percent VCM as follows: ~ area VCM x weight pentane in sample x 100 Weight % VCM = area p'enfanFx sample Weiihtx RF-----> 16.2 Calculate parts per million VCM as follows: area VCM X-weight pentane in sample x 106 ppm VCM -- area pentane x sample weight X RF No t e 18--See 13.6 for calibration instructions for determining the Response Factor (RF). 16.3 Example: Weight pentane in specimen . = 20 ml X 0.0000147 g/ml = 0.0002940 g RF - 0.781 Specimen weight = 0.9385 g Area VCM ' '' = 1 211 Area pentane = 11 868 --- ... ,, ~ 1211 X 0.0002940 X, 100 Weight % VCM - n 868xo.9385 xO.781 ppm VCM = 0.0041 % VCM, and = 0.004 (x 10 000) - 4 ppm VCM. . ___ , ... 17. Precision and Bias 17.1 Precision--The following values were determined for the coefficients of variation of this test method, using an internal standard, on the basis of an interlaboratory test program (1976) involving twelve laboratories reporting aver ages of duplicate analyses. 17.1.1 Precision for Resin Samples: Intralaboratojy 8.3 % Interlaboratory 24.8 % 17.1.2 Precision for Compounds: " At 2 ppm At 30 ppm Intralaboratory Interfaboratory 5.8 % ` 28,8 % 5.8 % 10.3 % 17.2 Bias--Since no absolute method is available for comparison, no statement of accuracy can be presented for this test method. 438 DUP050296958 w D 3680 Hii * ANNEX ' (Mandatory Information) Al. POLYMER SOLVENT REMOVAL BY ALTERNATIVE CARRIER GAS FLOW SYSTEMS Ai.l Alternative carrier gas flow systems for removing the lymer solvent from the column system are shown schetically in Figs. A1.1 through Al .4 on the following pages. ve actuating times, both to eliminate the solvent and to return to baseline equilibrium conditions must be determined experimentally for each individual column system being used, X' FIG. At.2 Backflush Schematic of Flow System Utilizing an 8-Port Sliding ' Plate Valve with Two Columns FIG. A1.1 BACKFLUSH Schematic of Row System Utilizing an 8-Port Sliding Plate Valve with a Single Column 439 DUP050296959 3680 i PRECO] IBBCI POSITION 710311 1,05X11011 No t e--At a predetermined time, after the monomer peak has passed through the precolumn, the valve is activated to flush the solvent out the injection port and short precolumn. . FIG.A14 Schematic of Flow System Utilizing a 4-Port Rotary Valve with Two Columns 31 ii jf p o s it io n s miser j; FIG. A1.3 Schematic Of Flow System Utilizing a 6-Port Rotary Valve with Two Columns The American Sdblety 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 time by the responsible technical committee and must be reviewed every five years, and Ii it not revised, either reipproved or withdrawn. Your comments are invitedeither forrevision 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 .| vlews knofon to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. J j 440 DUP050296960 Designation: D 3720 - 90 Standard Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments by X-ray Diffraction1 This standard is issued under the fixed designation D 3720; 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 ebange since the last revision or reapprovaL . Scope 1.1 This test method covers the determination of the ratio anatase to rutile in titanium dioxide pigments. The ethod is also applicable to pigment mixtures and pigented coatings containing titanium dioxide. 1.2 This standard does not purport to address the safety oblerns associated with its use. It is the responsibility ofthe er of this standard to establish appropriate safety and alth practices and determine the applicability ofregulatory citations prior to use. Referenced Documents 2.1 ASTM Standards: D215 Test Method for Chemical Analysis of White Linseed Oil Paints12 D2371 Test Method for Pigment Content of Solvent- Reducible Paints2 D2698 Test Method for Determination of the Pigment Content of Solvent-Reducible Paints by High Speed Centrifuging2 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 3. Summary of Test Method 3.1 The X-ray diffraction pattern obtained from a mate|Mal is characteristic of that material. The intensity of a diffraction peak entirely due to one component of a mixture is dependent upon the amount of that substance in the {mixture. To a minor extent the peak intensity of the r. Component is also dependent on the mass absorption coeffi cient of other materials present. Since the test method utilizes the ratio ofthe intensities of diffraction peaks of two Sehemically similar materials, it is expected that the effects of ||other constituents will be the same for both materials. 3.2 The intensity of the diffraction maxima for anatase and rutile is measured by X-ray diffractometry. The intensity ofthe anatase peak is converted to anatase content relative to ^ rutile and the rutile content is determined by difference. 3.3 The X-ray diffraction measurement is made on single pigments, pigment mixtures, films of pigmented coatings, and films prepared from liquid coatings, if interfering materials are not present. When interfering materials are 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint l and Related Coatings and Materials and is the direct responsibility of Subcom1? mittee DO! .21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990. Originally ) published as D 3720 - 78. Last previous edition D 3720 - 84. 2 Annual Book ofASTM Standards, Vol 06.01. present, the pigment is separated from the redissolved (or ignited film, or from the liquid coating and treated to isolate the titanium dioxide. 4. Significance and Use 4.1 This test method is used by titanium dioxide pigment manufacturers and users for process control and product acceptance. 5. Interferences 5.1 Calcium sulfate interferes, but its effect is eliminated by chemical removal (see,Test Method D 215). It is desirable to assure by analysis that any residual CaS04 is considerably less than the level of anatase being sought. The insoluble residue after removal of calcium sulfate should be ignited above 700C. Chrome yellow and the valentinite form of antimony trioxide also interfere if not removed. High amounts of iron render analysis difficult due to increased background (see Note 1). Additives, such as antimony and zinc, and impurities, such as niobium and zirconium, are generally- present in solid solution and thus would not have interfering diffraction peaks. Surface treatments such as silica and alumina do not interfere. Extreme differences in particle size between the anatase and rutile portions affect the results. No t e 1 --Background scatter due to high iron levels in a sample may be reduced by use of a cobalt or molybdenum target tube in place ofthe copper target tube. The background may be eliminated for all practical' purposes by use of a curved crystal monochromator equipped with a graphite crystal in conjunction with a copper target tube. 5.2 In the calculation of converting the ratio to percent it. is implicitly assumed that the sum of anatase and rutile is 100 %, an assumption normally made in Ti02 pigment systems. Other materials present would interfere to the extent that they dilute the sample. The third polymorphic form of Ti02, brookite, would have such an effect However, it reportedly does not occur in commercial titanium dioxide pigments. 6. Apparatus 6.1 X-Ray Diffractometer--The principle components of . this instrument are: (a) X-ray generator, (b) copper target X-ray tube, (c) goniometer, (d) detector, (<?) electronic circuit panel, (f) computer (if used), and (g) strip chart recorder or printer. 6.2 Operating Conditions--The X-ray tube voltage and filament current and other settings are selected to record X-ray diffraction peaks of weak intensities. 6.2.1 Nickel Filter, to remove Cu K beta radiation if a monochromator is not used. Cu K beta radiation will produce a diffraction line from the rutile phase of Ti02 that 441 DUP050296961 # D 3720 appears at the same 26 angle as the anatase analytical line. 6.3 Typical Apparatus Conditions: 6.3.1 High-Voltage Power Supply-- Select X-ray tube voltage, filament current, and other settings so that 0.1 % anatase generates a signal with intensity at least four times the noise level. 6.3.2 Detector--Scintillation detector operating at op timum voltage. 6.3.3 Pulse Height Analyzer--Settings will depend on instrumentation used. 6.3.4 Slits--Receiving slit, 0.15; others, 1. 6.3.5 Chan Speed, l/z in. (12.5 ram)/min. 6.3.6 Goniometer Speed, lA/min, scanning or 0.02 steps with 4.8 s per step. 6.3.7 Time Constant, 5. 6.3.8 Scanning Range, 26 = 28 to 24. . 6.3.9 Scale Factors--For samples of low anatase content a scale factor of 100 counts full scale is normally used for the 26 = 26 to 24 range (anatase diffraction maximum), and a scale factor of 5000 counts full scale is normally used for the 26 = 28 to 26 range (rutile diffraction maximum). The scale factors may be changed depending on the level of anatase expected in the sample. 7. Reagents 7.1 Purity of Reagents--Untreated rutile and anatase grades of titanium dioxide pigments are used to make synthetic standards for calibration. The crystalline structures of the reagents must be 100 % rutile and 100 % anatase as determined by examining these materials by X-ray diffrac tion to assure this purity. 7.2 Mixing Reagents--A" series of rutile standards of varying rutile content are prepared to cover the range of interest by thoroughly mixing known amounts of 100 % rutile and 100 % anatase together. The pigments are dis persed in. a solvent such as isopropyl alcohol and then mixed, followed by air drying. This dry cake is ground up using a mortar and pestle to ensure homogeneity.8 8. Hazards 9. Specimen Preparation i t.t: + i 9.1 Powder Samples: 9.1.1 Packing the specimen in the specimen holder tc obtain a planar surface is one of the most important phases :$! in X-ray analysis. Ripples or indentures in the specimen surface cause variations in the test because of an error of. eccentricity and a change in the intensities of the peaks. The chance of preferred orientation of pigmentary TiOz is remote because of its small particle size. 9.1.2 Pack the specimen in a die suitably constructed to accommodate the specimen holder for the goniometer. T| Apply constant pressure with a hydraulic press (see Note 2); Alternatively, place the specimen holder on a flat, smooth '?a firm surface and pack the specimen into the opening by f applying constant and firm pressure with a flat blade. The possibility of variations among different bags of the same lot should be considered. No t e 2--Use of a set procedure with a hydraulic press will improve specimen preparation uniformity compared to hand-packed specimens. This js particularly true where more than one person is involved in ii!l specimen preparation. 9.2 Coatings on Metal Panels: 9.2.1 Cut the coated panel into the proper shape and size to fit an adjustable specimen holder and analyze without further preparation. This assumes that interferences are not present (see Section 5). 9.3 Liquid Coating Samples: 9.3.1 Liquid coating samples without interfering materials present (see Section 5) are analyzed as cast films of the total paint on aluminum or other suitable substrate. A 1 to 2-mil (25 to 50-p.m) dry film thickness is adequate. 9.3.2 Liquid paint samples with interfering materials present (see Section 4) must not be analyzed until the interfering components are removed. This can be accom plished by centrifuging (Methods D2371 or D2698) to separate the total pigment. The separated pigment is treated according to 19.2.1 of Method D 215 to obtain interferencefree Ti02. Quantitative results are not required for either separation procedure. 8.1 X-ray producing equipment can be dangerous to both the operator and persons -in the immediate vicinity unless safety precautions are strictly observed. Refer to the manu facturer's instruction manual. Exposure to excessive quanti ties of'X-radiation may be injurious to health. Therefore, users should avoid exposing any parts of their bodies, not only to the direct beam, but also to secondary or scattered radiation that occurs when an X-ray beam strikes or has passed through any material. It is strongly recommended that users check the degree of exposure by film carried on them of by the use of dosimeters and that blood counts be made periodically. Before utilizing the equipment, all per sons designated or authorized to operate X-ray instrumenta tion or supervise its operation, should have a full under standing of its nature and should also become familiar with established safe exposure factors by a careful study of the National Bureau of Standards Handbook "X-Ray Recom mendations of the International Roentgen Ray Committee on X-Ray Protection" and other standard publications on the subject. Inquiries should be made of state agencies as to existing requirements. 10. Procedure - 10.1 Record the X-ray diffraction maxima of the anatase and of the rutile peak by scanning the range between 26 = 26 to 24 and 26 - 28 to 26, respectively. Scan each range twice, 10.2 Draw the baseline between the lowest points of the trace on each side of the peak. Measure the peak height above the baseline expressed in chart units, centimetres, counts per second, or other convenient units for the anatase arid rutile peaks. Average the net peak -heights of the duplicate funs. 10.3 Since only ratios are used, the peak heights need pnly be corrected for differences, if any, in the scale factors used for the two peaks. Any consistent units can be used, not just counts per second. 10.4 Prior to and after analyzing the unknown sample, analyze one of the standards to verify instrument stability. 11. Calculations 11.1 Determine the value of the constant, K, as follows K={IJIS)KWJWV) 442 DUP050296962 r( D 3720 & vhere: fa = net intensity of the anatase diffraction peak, l = net intensity of the rutile diffraction peak, Ra = weight of anatase, and r = weight of rutile. ! 11.1.1 AT is equal to the slope of a calibration plot ch ained when the intensity ratio IJIt is plotted as a iunction qf yjW,, using data derived from a series of standards that Span the concentration range of interest. Routine calibration jrocedures are followed.3-4 1 No t e--The value of K is influenced by the instrument conditions selected in Section 3. Data for standards and test samples must be collected using the same conditions. | 11. .palculate the anatase leve} relative to rutile from the leak intensities above background as follows: I !' - 5! Percent anatase =-------- 100 it ; .. t , L + ffi ;!*:. - '. ' .Y, : . 12. Precision 12.1 On the basis of an interlaboratory test of this test method in which four operators in four laboratories tested two materials withcomposition approaching 100 or 0% anatase of rutile, the within-laboratory standard deviation was found to be 0.06 % for a single determination. The between-laboratdries standard deviation was found to be 0.0.7 % absolute for results each the mean of two determina tions. Based on these standard deviations, the following criteria should be used for judging the precision of results at the"95 % confidence level. 12.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.18 % absolute for materials approaching !00 or 0 %. 12.1.2, 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 0.22 % absolute for materials approaching 100 or 0 %. 13 Keywords 3 Myers, H. and Spnrr, R., Analytical Chemistry, Vol 29, 1957, p. 760. * Zingaro, P. W,, Norelco Reporter, Vol 5, No. 5-6. 13.1 anatase pigment analysis; rutile; titanium oxide anal ysis; X-ray diffraction. *'3 The American Society tor 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 9/such rights, are entirely their own responsibility. This.standard is subject to revision at any time by thg responsible technical committee and must be reviewed every five years and ' ' Ifnot revised, eitherreapproved dr withdrawn. Yourcomments are invited either for revision ofthls standard or for additionalstandards a. end sliould be addressed to ASTM'Headquarters. Your comments will receive careful consideration at a meeting of the responsible ; > technical committee, whichyou.may attend, If you feel ihat your comments have not received a fair hearing you should make your views known to the ASTM Gbmrgittee on Standards, 1916Rsce St., Philadelphia, PA 19103. : i! 443 DUP050296963 i Designation: D 3721 - 83 (Reapproved 1991)1 Standard Specification for Synthetic Red iron Oxide Pigment1 This standard is issued under the fixed designation D 3721; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, theyear of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<6 indicates an editorial change since the last revision or reapproval. ei No t e--Keywords were added editorially in July 1991. 1. Scope 1.1 This specification covers synthetic red iron oxide for use in paints and coatings manufactured by any of the following: ; 1.1.1 Calcination of iron salts. 1.1.2 Precipitation from iron salts. 1.1.3 Calcination of synthetic iron oxide. 1.1.4 Product of organic reduction. 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 ,, D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 3. Composition and Properties 3.1 The pigment shall conform to the following require ments: Fe^, mid, % Moisture and other volatile matter, mat, % Organic coloring matter Total sulfates expressed as S03, max, % Coarse particles (total residue retained on a 45-g.m (No. 32S) sieve) max, % 93.0 1.0 none 2.0 1.0 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials, and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved March 25,1983. Published July 1983. Originally published as D 3721 - 78. Last previous edition D 3721 - 78. 2 Annua/ Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vois 06.01 and 06.02. Matter soluble in water, max, % pH value, min 0.2 5.0 3.2 Inasmuch gs.iron oxide.pigments are available in a range of colors, lie mass color and, if desired by the pur chaser, the character of the tint formed by mixture with a white pigment shall be within mutually agreed upon limits of a reference sample mutually agreed upon between the seller and the purchaser. This sample should be tested in accor dance with Test Method D 387. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day'$, pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear samples shall be taken from different packages in the ratio of two samples for each ,10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, or after blinding iri equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Total Iron Oxide, Sulfur, and Organic Coloring Matter--Methods D 50. 5.1.2 Moisture and Other Volatile Matter--Test Methods D 280, Method A. 5.1.3 Matter Solublp in Water--Test Methods D 1208. 5.1.4 Coarse Particles in Dry Pigments--Test Methods D 185. 5.1.5 pH Minimum--Test Methods D 1208. 5.1.6 Mass Color and Tinting Strength--Test Method D 387. 6. Keywords 6.1 iron oxide; manganese; pigments 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 (A/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 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. 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 Pace St., Philadelphia, PA 19103. 444 DUP050296964 Designation: D 3722 - 82 (Reapproved 1991Jet Standard Specification for Natural Red and Brown Iron Oxide Pigments1 This standard is issued under the fixed designation D 3722; 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 revision or reapproval. 11 Nora--Keywords were added editorially in July 1991. jScope . 1 This specification covers dry and wet ground naturally curring iron oxide, dry and wet ground calcined naturally purring iron oxide, and mixtures of these with synthetic |n oxides. These pigments are suitable for use in paints or eatings. Referenced Documents 2.1 ASTM Standards: I 50 Test Methods for Chemical Analysis of Yellow, |l Orange, Red, and Brown Pigments Containing Iron and Manganese12 1:0185 Test Methods for Coarse Particles in Pigments, p . Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain , Pigments2 pi Composition and Properties , 3.1 The pigments shall conform to the following require- Total iron as Fe203, min, % Bloxsture and'other volatile matter, max, % ^Organic coloring matter JjjTotal sulfates expressed as S03 C Matter soluble in water, max, % 70.0 1.0 none 2.0 2.0 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint I and Related Coatings and Materials and is the direct responsibility of Subcom mittee P01.31 on Specifications for Pigments. Current edition approved Oct 29,1982. Published January 1983. Originally published as D 3722 - 78. Last previous edition D 3722 - 78. 2AnmialBook ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM, Vois 06.01 and 06.02. Matter soluble in water, max, % (primer pigments) Coarse particles (total residue retained on a No. 325 (45-jj.m) sieve) max, % 1 JO 2.0 3.2 Inasmuch as iron oxide pigments are available in a range of colors, the mass color and, if desired by 'the purchaser, the character of the tint and the tinting strength shall be within mutually agreed upon limits of a reference sample acceptable to both the seller and the purchaser when tested in accordance with Test Method D 387. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately, or after blending in equal quantities the . samples from the same production unit to form a composite sample. ^ 5. Test Methods 5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods. Test procedures not-cov-ered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Total Iron Oxide, Sulfur, and Organic Coloring Matter--Methods D 50. 5.1.2 Moisture cmd Other Volatile Matter-Test Method D 280, Method A. 5.1.3 Matter Soluble in Water--Test Method D 1208. 5.1.4 Coarse Particles in Dry Pigments--Test Method D185. 6. Keywords 6.1 iron oxide; natural brown; pigments 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 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 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 tair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 445 DUP050296965 Designation: D 3724 - 82 (Reapproved 1987)e1 Standard Specification for Synthetic Brown iron Oxide Pigment1 This standard is issued under the fixed designation D 3724; 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. il No t e--Paragraph 4.1 was editorially changed in May 1987. 1. Scope 1.1 This specification covers the pigments commercially known as synthetic pure brown iron oxides and blends. These pigments are suitable for use in paints and coatings. Methods of manufacture are: 1.1.1 Precipitation of iron Salts. 1.1.2 Calcination of precipitated iron oxides. 1.1.3 Blends of synthetic red, yellow, and black iron oxides, 1.1.4 Blends of synthetic red, yellow, and black iron oxides plus the addition of carbon black to a maximum of 5.0 %. Small amounts of carbon black are added to obtain tinting colors not obtainable when synthetic brown iron oxide or carbon black are used singly. blend. It shall be a soft dry finely pulverized pigment and shall conform to the following requirements: FeO Fe203 Carbon black, max, % Moisture and other volatile matter, max, % Organic coloring matter Total sulfates expressed as S03, max, % Coarse particles (total residue retained on No. 325 (45-um) mesh sieve, max, % Matter soluble in water, max, % o to 10 % 83 to 98 % 5.0 % 1.0% none 2.0 % 1.0 % 0.5 % 3.2 Inasmuch as synthetic brown iron oxides are available in a wide range of shades. The mass color and character of the tint and the tinting strength formed by a mixture with a white pigment shall be within mutually agreed upon limits of a standard acceptable to both the purchaser and the seller when tested by Test Method D-387. 2. Referenced Documents 2.1 ASTM Standards: D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese12 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D1208 Test Methods for Common Properties of Certain Pigments2 D 3872 Test Method for Ferrous Iron.in Iron Oxides2 E 350 Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and Wrought Iron4 E 351 Test Methods for Chemical Analysis of Cast Iron-- All Types4 3. Composition and Properties 3.1 The pigment shall be a manufactured iron oxide or a 1 This specification is under the jurisdiction ofASTM Committee D-i on Paint . and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Oct. 29,1982. Published January 1983. Originally published as D 3724 - 78. Last previous edition D 3724 - 78. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 4 Annual Book ofASTM Standards, Vol 03.05. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each ldt, batch, day's pack, or other unit of production in a shipment When no markings distinguishing between units of production appear, samples shall be taken from different packages in the ratio oftwo samples for each 5 tons (inch-pound or SI), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from' the same production unitto form a composite sample. 5. Test Methods .5.1 Tests shall be conducted in accordance with the appropriate ASTM test methods: Test procedures not cov ered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.1.1 Total Iron Oxide, Sulfur and Organic Coloring Matter--Methods D 50, 5.1.2 Ferrous Iron Content--Test Method D 3872.. 5.1.3 Moisttfre and Other Volatile Matter--Test Method D280--Use Method A for pigments containing less than 8 % ferrous iron oxide. Use Method B for pigments con taining more than 8 % ferrous iron oxide. 5.1.4 Matter Soluble in Water--Test Method D 1208. 5.1.5 Coarse Particles in Dry Pigment--Test Method D 185. 5.1.6 Carbon Black Content--Test Methods E350 or E351. 446 DUP050296966 D 3724 The American Society for Testing end 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 mm responsibility. This standardis subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and ifnot 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 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. 447 DUP050296967 Designation: D 3733 - 78 (Reapproved 1984)41 Standard Test Method for Silicon Content of Silicone Polymers and Silicone-Modified Alkyds by Atomic Absorption1 This standard is issued under the fixed designation D 3733; the number immediately following the1 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 (t) indicates an editorial change since the last revision or reapproval. 61 No t e--Editorial changes were made throughout in August 1984. 1. Scope 1.1 This test method covers the determination of the silicon content of silicone polymers and silicone modified alkyds when present in the nonvolatile portion of polymers, resins, or liquid coatings to the extent of 1 % or more. 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 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: D1153 Specification for Methyl Isobutyl Ketone21 D1193 Specification for Reagent Water3 D2372 Practice for Separation of Vehicle from Solvent- Reducible Paints4 D2698 Test Method for Determination of the Pigment Content of Solvent-Reducible Paints by High Speed Centrifuging4 D2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings4 3. Significance and Use 3.1 The silicon content of silicone modified alkyds has a direct relationship to the cost and performance characteris tics, especially heat resistance of coatings prepared from them. 4. Summary of Method 4.1 The polymer solution or separated coating vehicle is diluted with methyl isobutyl ketone, and the silicon content is determined by atomic absorption spectroscopy. 5. Apparatus 5.3 Atomic Absorption Spectrophotometer, consisting of an atomizer and a single-slot burner; gas pressure-regulating and -metering devices for nitrous oxide (N20) and acetylene; a silicon hollow-cathode lamp with a regulated constant current supply; a monochromator and associated optics; a photosen- m sitive detector connected to an electronic amplifier; and a -m read-out device. m 5.2 Centrifuge. || 5.3 Pipets, 5, 10, 15, and 20-mL capacity. H 5.4 Volumetric Flasks, 25, 50, 100, and 1000-mL. 6. Reagents 1 6.1 Purity ofReagents---Reagent grade chemicals shall be jl used in all tests. Unless otherwise indicated, it is intended j that all reagents shall conform to the specifications of the 1 Committee on Analytical Reagents of the American Chem- j ical Society, where such specifications are available.5 Other J| grades may be used, provided it is first ascertained that the M reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 1 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. J 6.3 Octaphenylcyclotetrasiloxane.6 " f 6.4 MethylIsobutyl Ketone (MIBK), complying with Spec- | ification D 1153. J 6.5 Silicon, Standard Stock Solution (100 pg/rriL)--Weigh r exactly 0.709 g of octaphenylcyclotetrasiloxane and quanti- . k tatively transfer to a 1-L flask. Dilute to volume with MIBK. \ 7. Calibration and Standardization __ J 7.1 Prepare the following standard solutions from the 100 J pg/mL silicon standard stock solution, diluting to the ; . indicated volumes with MIBK: Stock Solution, mL Dilute to, mL Concentration, - pg/mL 20 25 80 15 25 60 10 25 40 5 25 20 5 50 10 5 100 5 7,2 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the 1This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Material and is the direct responsibility of Subcommittee D01.33 on Varnish and Resins, Including Shellac. Current edition approved Oct. 27, 1978. Published December 1978. 3 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.01. 1 "Reagent Chemicals, American Chemical Society Specifications,1' Am. Chem ical Sou, 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." 6 Available as Standard Reference Material No. 1066a from Office of Standard Reference Materials, Room B-314, Chemistry Building, National Bureau of Standards, Washington, DC 20234. 448 DUP050296968 D 3733 Banufacturer's literature for establishing optimum condi5ns for the specific instrument used. i7.3 Turn the instrument on and set the wavelength to the gl.6-nm silicon line. Apply the recommended current to ie silicon hollow-cathode lamp. Allow the instrument to jarm up for about 15 min and set the slit width. Adjust the jitrous oxide and acetylene pressures and ignite the burner U accordance with instructions. ft No t e 1 --An acetylene pressure of 7 psi (48 kPa) and a nitrous oxide jlessure of 30 psi (207 kPa) have been found to be satisfactory for most Ijistruments. 1 7.4 While aspirating MIBK, carefully adjust fuel and oxi- [ant flow rates as well as aspiration rate, until a clean, steady ,,kme is obtained and no detectable carbonization occurs on |je burner head. Aspirate the 5 jxg/mL standard solution and ike any necessary readjustments in instrument parameters obtain maximum absorption. Record optimized fuel and Jbxidant flow rates for future reference and use for calibration id sample analyses. 7.5 Aspirate MIBK. When the recorder, meter, or other lead-out device reaches a constant value, adjust it to zero Immediately. 7.6 Aspirate each of the appropriate standard solutions in ascending silicon concentrations, ending with the 100 pg/mL standard. Record the corresponding instrument readings. Aspirate MIBK between each standard, and after the last standard. : 7.7 Construct a calibration curve on linear graph paper by plotting the absorbance versus concentration (micrograms per millilitre) for each standard solution. No t e 2--Complete calibration and-standardization (7.3 to 7.7) immediately prior to sample analysis. 8. Procedure 8.1 If the sample is a pigmented coating, remove all traces sr1 of pigment by centrifuging in accordance with Methods D 2372 or D 2698. Determine the nonvolatile content of the vehicle or polymer solution in accordance with Guide D 2832. 8.2 Prepare at least two replicate specimens by weighing by difference from a dropping bottle or syringe, a quantity of the vehicle or polymer solution equivalent to 60 to 240 mg (see Note 3) of solids directly into 100-mL volumetric flasks. Dilute to volume with MIBK and mix thoroughly. No t e 3--If the approximate silicon content is known, use the following specimen weights to optimize analytical results: Expected Silicon Content, % Optimum Weight of Solids, mg 70 150 300 600 8.3 Aspirate each specimen solution and determine the absorbance in the same manner in which the instrument was calibrated. Determine the concentration of silicon in micro grams per millilitre from the calibration curve. If the absorb- ance is above the range covered by the calibration curve, dilute an aliquot ofthe sample solution to a suitable volume with MIBK. If the absorbance is below the range covered by the calibration curve, repeat the analysis using a larger spec imen size. No t e --The method ofstandard 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. 9. Calculation 9.1 Calculate the mean concentration of silicon in the nonvolatile portion of the material under test as follows: CxF Silicon, % in nonvolatile = }vKxS where: C ** concentration ofsilicon in the aspirated test solution, M-g/mL. F = dilution factor from 8.3 (volume diluted to volume of aliquot), NV = percent nonvolatile of material under test, and S - specimen weight, g. 9.2 To calculate the equivalent amount of silicon dioxide in the sample, multiply the percent silicon found by 2.139. 9.3 If the type of silicone polymer present in a varnish or coating vehicle is known, separate analysis of the silicone polymer allows the determination of a conversion factor that may then be used to calculate the percent of silicone polymer present in the vehicle. 10. Report 10.1 Report the percent of silicon, silicon dioxide equiva lent, or silicone polymer present in the nonvolatile content of the material under test. 11. Precision87 11.1 In an interlaboratory study of the method, the withinlaboratory coefficient of variation was found to be 4.11 % relative at 21 degrees of freedom and between laboratoriescoefficient of variation was 5.27 % relative at 6 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--Two results, each the mean of du plicate determinations, obtained by the same operator on different days, should be considered suspect ifthey differ by more than 12.1 % 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 18.2 % relative. 7 Supporting data are available on loan from ASTM Headquarters. Request RR:D01 - 1009. 449 DUP050296969 # D 3733 The American Society for Testing and Materials takes no position respecting the validity ofany 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 standerd Is subject to revision et any time by the responsible technical committee and must bp reviewed every five years and ifnotrevised, either reapprovad or withdrawn. Your comments are Invited either forrevision ofthis sthndardorforadditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a Meeting of die responsible ' technical committee, which you may attend. If you faal that your comments have not received a fair hearing you,should make yourviews known to-the ASTM Opmmittee on Standards, 1916 Race St., Philadelphia, PA 19103. '- y ; - , (bj. -r*: 450 DUP050296970 Designation: D 3872 - 86 (Reapproved 1991)* Standard Test Method for Ferrous Iron in Iron Oxides1'12 This standard is issued under the fixed designation D 3872; 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 reapptoval. el No t e--Keywords were added editorially in 1991 jjf. Scope f 1.1 This test method covers the quantitative determination Offerrous oxide (FeO) by oxidation offerrous iron (Fe++) in in acid solution to the ferric state (Fe+++) and titration with potassium dichromate using diphenylamine as the indicator. 1.2 This test method is applicable to synthetic black iron Joxide, natural black iron oxide, magnetite or brown iron oxide where part ofthe iron content is present in the ferrous state (Note 1). It is applicable to iron oxides where the ( ferrous iron content ranges.from. 50 to. 0.20 %. No t e 1--Natural iron oxides and magdetife may contain tiaces of-i metallic iron that will be combined with and analyzed as FeO. 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 Imitations prior to use. ! 2. Referenced Documents : 2.1 ASTM Standards: ' """ D5Q Test Methods for Chemical Analysis of -Yellow,.. Orange, Red, and Brown Pigments Containing Iron and Man- gan<$e3 !; i, Matter Vol|iti4lJpdei:,.the,jest Conditions) in Pigments* D769 Specification for Black Synthetic Iron Oxide3. r< D1193 Specification for Reagent Water4 D 3722 Specification for "Natural Red and' Brown Iron Oxide Pigments3 D3724 Specification for Synthetic'Brown Iron Oxide . Pigment? t i:i ' 3. SiSgnifti^mce'and lise .. ( 3.i;].fhii'l^fcmeth9d may be used for production,quality contfol or spdbificatidh adcdpiance. tion ofthe inert gas and vent for gas and digestion fumes. 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.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently Jbih 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 Type II of Specification D 1193. 5.3 Diphenylamine Indicator--Dissolve 1 g of diphenyla- mine in. 100 mL of concentrated (H2SO^) (sp gr 1.84). 5.4 Hydrochloric Acid (1+1)--Dilute concentrated hydro chloric acid (HC1, sp gr 1.19) with an equal volume ofreagent water. 5.5 Iron Ore, Standardf Mesabi No. 27-D.6 5.6 Potassium Dichromate, Standard Solution (0.1 N)-- Dissolve14.904 g of K2Cr207 in water and dilute to 1 L. Standardize against National Bureau of Standards standard sample No. 27-D of Mesabi iron ore. Calculate the Fe factor in grams per millilitre for the solution as: .r ' . Fe-W (li. where: _ , ' ' ,' , W - weight ofFe inthe standard iron ore (not the splutipn, .. as there is none), and' , ... ' . Vt - K2Cr207 required for titration of standard', mL. . 5.7 Sulfuric-Phosphoric Acid Solution--Prepare by care-' fully adding 600 mL of concentrated sulfuric acid (H2S04) (sp gr 1.84) tb 8,00 mL of water while stirring, thenadd 600 mL ofphosphoric acid (85 tb 87 fa) mixing thoroughly. Cooi and store. 4. Apparatus 4.1 The digestion apparatus consists of a standard 500-mL Erjenmeyer flask fitted with a two-hole rubber stopper and glass tubing, as shown in Fig. 1, to provide for the introduc 6. Preparation of Sample (Note 2) ,, 6.1 Mix the sample thoroughly and take a representative portion for the analysis. Exercise care at all times to prevent oxidation ofthe Fe++ iron to the Fe+++ state (Note 2). Grind 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 SubcommitteeD01,21 on Chemical Analysis of Pajnts and Paint Materials, Current edition approved April 25, 1986. Published June 1986. Originally published as D 3872 - 79. Last previous edition D 3872 - 79. 2 This method is equivalent to Method 7161 of U.S. Federal Test Method Standard 141. 3 Annual Book ofASTM Standards, Vo! 06.02. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. ' 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washiiigtoo.DG. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Vap NostiandCo, Inc., New York, NY, and the "United States Pharmacopeia." 6 May be secured from National Bureau of Standards, Department of Com merce, Washington, DC 20234. Other recognized'primary iron standard may be substituted. 451 DUP050296971 Rubber # D 3872 natural iron oxides or natural magnetites to 100 % minus 100 mesh. 6.2 Finely divided synthetic black iron oxides if not carefully dried can oxidize so that part of the Fe++ iron is. converted to Fe+++. For this reason moisture should be deter mined on a separate specimen or by Test Methods D 280, Part B. Vacuum drying at temperatures not exceeding 65C is recommended. No t e 2--Coarsely ground natural iron oxides and magnetite are very slow to dissolve. Exercise-care in grinding oxides containing ferrous iron to avoid generating heat, as additional grinding could oxidize ferrous.to feme iron; ` No t e 3--;Synthetic black iron oxides may contain small amounts of carbon black to increase tint strength. Carbon black will not dissolve during the digestion step and should not be confused with the Soluble iron oxide.' ! 7.4 Remove the flask from the hot plate and.add 30 mL of sulfuric-phosphoric add solution. Add 60: mL of water and cool in the water bath for 5 min. 7.5 Remove the C02 apparatus and add 5 drops of the diphenylamine indicator. Titrate with the standardpotassium dichromate solution. The end point is sharp with a color change from green to purple. Avoid goihg pSst the end point. 7. Procedure 7.1 Weigh 0.5 g of oxide to 1 mg and transfer to the 500-mL Eflenmeyer flask. Wash down the sides of the flask with 15 mL of water. 7.2 Attach the stopper With funnel and the gas delivery tube to the flask. Open the C02 valve until a gentle stream of gas flows through the flask. Nitrogen may be substituted. 7.3 Add 15 mL of 1+1 HC1 (1+1). Digest on an asbestos pad on the hot plate at just below boiling temperature until completely dissolved or there is no further reaction (Note 3). Finely divided synthetic black or brown oxides usually require 5 to 10 min but natural oxides or magnetites may require considerably longer. 8. Calculations 8.1 The percent FeO or Fe++ in the unknown sample are calculated by using Eq 2 or 3. - where: W = weight of Fe in standard solution, g, and P = potassium dichromate solution, mL. %Fe0.jl^xU865.x 100 (2) where: F -- Fe value, and S - specimen weight, g. 452 DUP050296972 # 0 3872 V x F x 100 Fe++ = .-- weight of FeO _ 71.85 1.2865 molecular weight of Fe ~ 55.847 8.2 Report results to 6.1 %. (3) Precision and Bias 9.1 The precision statements are based on an interlabora ry study of the method in which operators in seven Jjoratories analyzed in duplicate on two days two commer- synthetic black iron oxides containing 20 and 23 % rrous iron oxide. The within-laboratory standard deviation i found to be 0.235 for the first material and 0.05 for the eond, each with 7df. The between-laboratory standard aviations were 0.061 and 0.058, respectively, each with 6 df. Based on the pooled standard deviations, the following criteria should be used forjudging 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 riiore than 0.5 % Absolute at FeO Contents of 20 to 25 %. 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 0.8 % absolute at FeO contents of 20 to 25 %. 9.2 Bias--Bias 1ms not been determined. 10. Keywords 10.1 ferrous iron content; iron oxides, ferrous iron con tent; pigment, iron oxides The American 'Society for Testing and Materials takes noposition respecting the validity of any patent- rightsrasserted 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 reapprovedor withdrawn. YOiir comments are Invited eitherforrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wlll recSive careful consideration at a meeting of the. responsible technical committee, which you may attend, ifydu tee! 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. 453 DUP050296973 HJiln Designation: D 3876 - 79 (Reapproved 1989)1 Standard Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography1 This standard is issued under the fixed designation D 3876; 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. l No t e--Editorial changes were made throughout in October 1989. 1. Scope 1.1 This test method is applicable to the determination of methoxyl and hydroxypropyl substitution content in cellu lose ether products by a Zeisel-gas chromatographic tech nique. 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 of regulatory limitations prior to use. For specific hazard statements, see Section 5 and Notes 2 and 3. 2. Referenced Documents 2.1 ASTM Standards: D1347 Test Methods for Methylcellulose12 D 2363 Test Methods for Hydroxypropyl Methylcellulose2 3. Apparatus 3.1 Gas Chromatograph,3 with thermal conductivity de tector and heated injection port. 3.2 Electronic Integrator4 3.3 Glass Tubing,5 *6.4 mm in outside diameter, 4 mm in inside diameter, and 1829 mm long, packed with reagent (4.8). Two are required. 3.4 Syringes, 10 and 100 jiL. 3.5 Reaction Vials, Caps, and Heating Blockf 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- 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 1.36 on Cellulosics. Current edition approved Dec. 28, 1979. Published February 1980. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Hewlett-Packard Model 5700, available from Hewlett-Packard, Route 41, Starr Rd, P.O. Box 900, Avondale, PA 19311, has been found satisfactory for this purpose. 4 Hewlett-Packard Model 3380 has been found satisfactory for this purpose. 5 Tubing from Alltec Associates, P.O. Box 117, Rockford, IL 61105 has been found satisfactory for this purpose. * Reacti-therm Heating module, Reacti-Block Reacti-vials and Mininert valve tops from Pierce Chemical Co., Box 117, Rockford, 1L 61105 have been found satisfactory for this purpose. 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 i lessening the accuracy of the determination. 1 4.2 Adipic Acid, M.P. 151to 153C. i 4.3 o-Xylene, ACS. j 4.4 Toluene, ACS. 2 4.5 lodomethane, 99% min. 4.6 2-Iodopropane, 97% min. .4 4.7 Hydriodic Acid (sp. gr:1.69 to 1.70), 57%. 4.8 Acetone. i 4.9 10 % Methyl Silicone Oil,* UCW 982 on 100/120 mesh solid support. 5. Hazards 5.1 Safety precautions must be taken , for handling of hydriodic acid. . 1 5.2 During the reaction, the glass vialsare under pressure. Exercise caution in handling the hot vials. 6. Summary of Test Method9 6.1 When methyl cellulose or hydroxypropyl methyl cel- lulose is reacted with hydriodic acid in the presence of adipic acid, 1 mol of methyl iodide and 1 mol of Isopropyl iodide are liberated for each mole of methoxyland hydroxypfopoxyl that is substituted on the cellulose chain. The methyl iodide and isopropyl iodide are extracted in situ with oxylene and quantitated by gas chromatography using an internal stand- ard technique. ' ! i | j 7. Significance 7.1 This test method determines the methoxyl and hydroxypropoxyl content of cellulose ethers by a Zeisel-gas chromatographic technique. 7 "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." 8 Chromosorb WHP brand packing from Applied Science Laboratories, Box 440, State College, PA 16801, has been found satisfactory for this purpose. 9 Reference for methoxyl and hydroxylpropoxyl content are in Dow Method No. MC-36 "Determination of Methoxyl and Hydroxyl-propoxyl Substitution in Cellulose Ether Products by a Zeisel Gas Chromatographic Technique." 454 DUP050296974 # D 3876 ^Sampling 8.1 A specific sampling method is currently under study f the subcommittee. it Apparatus Preparation and Conditioning 1:94 Column10--Pack the two pieces of glass tubing (3.3) fth a reagent (4.9) under vacuum and mechanical vibration ijng silanized glass wool to contain the packing. Install each the gas chromatograph to facilitate on-column injection lad allow it to come to equilibrium over a 12-h period under fie following conditions: Oven temperature Injection port temperature Detector temperature Deteetor current Attenuation. Carrier gas Column A Column B 100"C isothermal 2OO'C 200C 170 mA 1 helium 20 mL/min 20 mt/rain I' No t e 1--The conditions used here were determined to be optimum $r the column used. Optimum conditions should be determined for Ipch column on an individual basis. 9.2 Integrator. 9.2.1 Settings'0 Attenuation 1 Start delay 0.5 Chart auto Chart speed 0150 cm/in. Area reject off Slope sensitivity must be determined 1.2.2 Approximate component retention times Minutes 3.00 5.00 7.00 13.00 Component _ methyl iodide * isopropyl iodide toluene (internal standard) 0-xylene | 10. Preparation of Standard Solutions I 10.1 Internal Standard Solution (25 mg toluene/ml xylene): 10.1.1 Weigh a 100-mL volumetric flask containing 10 mL of o-xylene to the nearest 0.01 g. 10.1.2 Add 2.50 0.01 g of toluene. 10.1.3 Dilute with o-xylene to 100 mL. 10.2 Calibration Standard Solution: 10.2.1 Weigh 130 to 140 04 mg of adipic acid into a 3-dram vial. 10.2.2 Add 4.0 mL of 57 % hydriodic acid. 10.2.3 Pipet 4.0 mL of the internal standard solution into the vial and cap with a serum stopper or septum top.11 10.2.4 Weigh vial and contents to nearest 04 mg. 10.2.5 Add 30 pL of isopropyl iodide to the vial through the septum top with a syringe. Weigh and record the amount of isopropyl iodide added to nearest 04 mg. 10.2.6 Add 90 pL of methyl iodide to the vial with a syringe. Weigh and record the amount added to nearest 0.1 mg. 10.2.7 Mix the contents well. 10 These settings were used with the Hewlett-Packard Model 3380 Integrator. Other units may require different settings. 11 Mininert valve tops from Pierce Chemical Co., Box 117, Rockford, IL 61105 have been found satisfactory for this purpose. 10.2.8 Convert the alkyl iodides into their respective alkoxyl equivalents using the following equations: /31 x 1000\ mg methoxyl = g methyl iodide x l 11-42 / (I) mg hydroxy propoxyl = g propyliodide X W mg toluene = internal standard solution concentrated X 4 ml (3) 11. Calibration of Electronic Integrator12 11.1 Inject 2 pL of the upper layer of the prepared standard solution (10.2) into the gas chromatograph and start the electronic integrator. 11.1.1 Calibrate in accordance with the manufacturer's instructions. . 11.2 In the event an electronic integrator is not available the peak areas can be measured manually and a factor determined for each component can be obtained using the following equation: F = Ax B Cxi) (4) where: A = weight ofthe component in the standard solution, mg, B = peak area of the internal standard solution, toluene from the standard run, C = peak area of the component from the standard nm, D = weight of the internal standard solution, mg, and F = component response factor. 12. Procedure 12.1 Sample Preparation: 12.14 Dry the sample at 105C (221F) for 30 min and store in a desiccator. 12.1.2 Weigh 60 to 70 04 mg into a clean 5-mL reactor-vial. -- 124.3 Weigh into the reactor vial an amount of adipic add equal to the spedmen weight. (See Note 4). 12.1.4 Add 2.00 0.01 mL of internal standard solution (10.1). 124.5 Add 2.00- 0.05 mL of 57 % hydriodic add. No t e 2: Warning--Use a hood, goggles, and other appropriate safety equipment. Hydriodic acid can cause systemic damage. 12.1.6 Immediately cap tightly and weigh the vial. The cap should be tightened firmly to prevent leakage. 124.7 Shake the spedmen for approximately 30 s. 124.8 Place the reactor-vial into a 150C (302F) heated block for 1 h, with removal for shaking after 20 min. Replace the spedmen for the duration of the heating time. No t e 3: Warning--A possible safety hazard exists because the vials contain a hot corrosive acid under pressure. 124.9 After 1 h heating time, remove the specimen and place in the hood to cool for about 45 min. The specimen will separate into two layers. 12.140 Reweigh to determine any loss due to leakage. If 12 The Hewlett-Packard 3380 has been found satisfactory for this purpose. Other electronic integrators may require a different calibration technique. 455 DUP050296975 D 3876 loss is greater than 0.0100 g the specimen should be discarded. No t e 4--The weight ratio of adipic add to the spedmen can range from 0.9 to 2.0. Excessive adipic acid may cause low methoxyl values. 13. Analysis 13.1 Enter into the integrator the milligrams of specimen and toluene internal standard used in the preparation of the specimen. 13.1.1 This can be calculated from the concentration of the internal standard solution. 13.2 Inject 2 pL of the upper layer of the specimen into the gas. chromatograph and immediately start the integrator. 14. Calculation 14.1 The integrator printout records the methoxyl or hydroxypropoxyl substitution, or both, in weight percent. 1'4.2 If an electronic integrator is not available the peak areas can be measured manually and the alkoxyl substitution may be calculated using the following equation: CxfxgxlQO lx J (5) where: G ~ peak area of the component from the specimen run, F = component response factor obtained in 11.2, 1 H - weight of the toluehe internal standard in the spec imen, mg, * / m peak area of the internal standard from the specimen run, and / = specimen weight, mg. 15. Precision 13.1 The data using an electronic integrator show an average relative precision of 1.7% for methoxyl substitution (26% level) and 3.4% for hydroxypropyl substitution (0.3 to 10% level) at the 95% confidence limit 2c. 15.2 Interlaboratory Test Data.13 15 15 Available from ASTM Headquarters. Request RR:D23-1000. The American Society (or 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 Ifnot 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, 1916 Race St., Philadelphia, PA 19103. 456 DU P050296976 Designation: D 3926 - 80 (Reapproved 1991)61 Standard Test Method for Percent Solids in Titanium Dioxide Slurries1 This standard is issued under the fixed designation D 3926; 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 No t e--Keywords were added editorially in July 1991.: 'J. Scope 1.1 This test method covers the determination of the weight percent of solids in aqueous slurries of titanium diox ide pigments. 1.2 This test standard does notpurport to address all ofthe ,safety problems, if any, associated with its use. It is the Responsibility ofthe user ofthis standard to establish appro priate sqfety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water21 3. Summary of Test Method 3.1 Slurry is weighed by difference into a tared aluminum foil dish, dried at 105C in an oven for I h,' cooled in a f desiccator, and weighed. | Significance and Use 4.1 This test method is intended as a quick and reliable procedure for measuring the titanium dioxide pigment Con tent of aqueous slurries, included with the pigment content in the percent solids are the various nonvolatile additives used in preparing a stable slurry. Because the oxide modifiers on some titanium dioxide pigments may change somewhat with prolonged drying, in this method the solids of the slurry are considered dry after heating at 105C for 60 to 65 min. S. Apparatus 5.1 Oven--Laboratory oven capable ofmaintaining a tem perature of 105 2C (Note 1). The oven may be a gravityconvection type or an oven with a low velocity, forced draft. An oven with a high-velocity, forced-draft air change, com monly used for baking finishes, is not suitable. No t e 1--The temperature in the oven must be constantly moni tored. Many older ovens will no longer maintain 2C\ some will maintain this tolerance for a while but occasionally the thermostat will "stick" and the temperature will vary considerably. 5.2 Balance--Laboratory analytical balance, accurate to 0.1 mg, with 1-g optical readout range for fast weighing. 1 This test method is under Ihe 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 Sept 2, 1980. Published November 1980. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. No t e 2--Periodically check the accuracy of the i-g optical scale of the balance by use ofa known 1-g, weight; adjust the balance if needed. The zero adjustment of the optical scale needs to be checked at least every hour routinely and immediately ifthere is any possibility ofa spill having occurred on the balance. 5.3 Desiccator--Standard laboratory desiccator utilizing an indicating drying medium. 6. Reagents and Materials 6.1 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. 6.2 Aluminum Foil Dish--Disposable aluminum foil dishes, approximately 60-mm diameter by 18 mm high, 1 to 2 g in weight. 6.3 Disposable Syringe or Dropper--Disposable 2 or 3mL syringes or 2 to 5-mL droppers. 7. Procedure 7.1 Weigh two new, empty aluminum dishes each to 0.1 mg. For each dish, this is Wt. With a syringe add 2 mL of water io each dish. , 7.2 Shake or stir the slurry sample until it is homogeneous and free Df any settled material. If the container is trans parent or translucent, the absence of settled material sticking to the bottom of the container can be ascertained visually. Otherwise insert a spatula or the like to make sure there is no settled material. 7.3 Immediatelyjwithdraw 0.4 to 0.8 g of slurry in a new, empty disposable syringe or dropper. The specified amount can be estimated by a prior trial in another syringe or dropper. Wipe off the slurry from the outside ofthe syringe or dropper with a dean, absorbent paper. Cover the sample bottle. Weigh the syringe or dropper and slurry to 0.1 mg. This is W2. 7.4 Transfer the contents of the dropper into one of the weighed aluminum dishes. Add the slurry dropwise, gently shaking the dish to disperse the test spedmen in the water. When no additional slurry can be transferred from the dropper, reweigh to 0.1 mg the dropper with any residual material inside. This is W3. 7.5 Shake the sample of slurry briefly and withdraw a second 0.4 to 0.8 g of slurry in another new dropper. Weigh and transfer contents as in 6.3 and 6.4 to the second weighed aluminum dish. 7.6 Place the two dishes and contents directly onto the metal shelfin the oven at 105 2C for 60 to 65 min. Do not dry in the oven longer than the spedfied 65 min. 7.7 Remove the dishes from the oven, cool in the desic cator for 10 to 60 min, remove one dish at a time, and weigh 457 DUP050296977 #) D 3926 immediately to the nearest 0.1 mg. This is WA for each dish. ments to two decimal places. jIMljil Do not cool longer than 60 min since there is a slight possibility of an equilibrium moisture exchange between the drying medium and some dried titanium dioxide pigments. 9. Report 9.1 Round the' calculated mean value to the nearest 0.1 % and report as pertsent solids. This rounded mean value is considered to be one result. Example: solids = 62.2 % ^ 8. Calculation 10. Precision 8.1 For each of the duplicate measurements calculate the percent solids to two decimal places as follows: (w4- tr,)ioo % Solids = W2-WK where. = weight of empty aluminum dish, g, W2 = weight of dropper plus slurry, g, W3 = weight of dropper after discharging slurry into dish, andg, : W4 = weight of dish and slurry after drying, g. Example. * W, = 1.4431 W2 = 2.0894 Hf, = 14905 = 1.8158 ' . % solids .. .= (1.8158 - 1.4431)100 2.0894 --. 1,4905 = 62.23 ,^ ;, 8.2 Calculate the mean value of the duplicate measure- 10.1 On the basis of an interlaboratory test of this method in which 17 operators in 15 laboratories analyzed 8 materials with solids contents at different levels, the wiihin-laboratory standard deviation was found to be 0.12 % and the between- laboratory standard deviation was found to be 0.23 %. Based ' i | on these standard deviations, the following criteria should be ' used for judging the acceptability of . results at .the 95 % {| confidence level: -S - 10.1.1 Two.results, each the mean ofduplicate determina- Jj tions, obtained by the same operator at different times f should be considered suspect if they differ by more than | 0,34 % absolute^ , , v.. . ' 10.1.2 Two results, each the mean ofduplicate determina- 3 tions, obtained by operators in different laboratories should :j be considered suspect if they differ by more than 0;65 % j absolute. < ' < t i 11. Keywords > ; 11.1 slurries, nonvolatile content; solids in titanium pig- 1 ment slurries; titanium dioxide slurries V The American Society for Testing and Materials takes noposition respecting thevalidity of anypatent rights assattedin connection with any item mentioned in this standard. Usorb`61 this standard are expressly advised that determination of the valldky of any such . patent rights, and the risk of infringement of such ripbts, are entirely their own responsibility. ' , d . . this standard is subject to revision at any time by the responsible technical committee and must be reviewed every five yearsand * ifnot revised, eitherreapprovedor withdrawn. Your conimehts are Invited either for revision ofthis standard orfor addjtional standards and should be addressed to ASTM Headquarters. Ydur comments will receive carpful consideration at a meeting of the, responsible. technical committee, which you.may ,attend; It ygu feel that your com/tienls have hot rec&lved a fair hearing you should maim ydir , views known to. the ASTMporrmijitse on Standgrps,, ISIQRace St., Philadelphia,'PA 13103. ' '. : C ;; r<" R! j.';" f: i : :u ' ;r. , 458 ' If * . : < c..n e. V-* DUP050296978 Designation: D 3971 - 89 Standard Test Method tor Dichloramethane-Soltable Matter in Cellulose1 TJis standard is issued unde? ,:he Bxed designation D 3971; the number immediately following tb.e designation indicates the year of original adoption or, in therrase of revision, the year oflast revision. A numberih'parenibe^ indicates the year oflastisipproval. A superscript epsilon (e) indicates an editcriol change^ince the last revision or reapproval. 2. Scope ' 1.1 This test method covers the determination of, di-. ihloromethane-sOluble. matter in bpiiulo'sp and is applicable, b dissolving-type cellulose pulps prepared from, cotton or vood. I 1.2 This standard may involve hazardous-materials, oper-^ ktions, and eqtiipfhenf.' This standard 'does not purpprt to pddress all ofiytcfegy problems associated with its iise. it is me responsibility of the user of this standard-to establish IAppropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 12, Referenced Document I 2.1 ASTM Standard: D1348 Test Methods for Moisture in Cellulosei2 3. Summary of Test Method 3.1 A sample is extracted with, dichloromethane in a Soxhlet apparatus as a measure of the waxes, fats, resins, and oils present. 4. Significance and Use 4.1 Dichloromethane-soluble materials are typically re ferred to as extractives. These extractives are comprised of organic materials that originated in the wood or cotton. The ^measure is an indication of the efficiency of removal ofthese substances during pulping and bleaching. The extractive level is of concern to dissolving pulp users since the presence Of large amounts of extractives could inhibit the processing of cellulose into the desired derivative. 5. Apparatus 5.1 Extraction Apparatus3, Soxhlet, (Coming 3840 or 13880)--consisting of a 250-mL flask (Coming 4100), an ! extractor tube with standard taper 45/50 top joint (Coming 3740), and a Allihn standard taper 45/50 (Coming 3840), or Friedrichs standard taper 45/50 (Coming 3880) type con; denser. 5.2 Extraction Thimble, either (/) standard thickness paper, 43 by 123 mm, (2) Alundum4, 34 by 100 mm, i 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 Subccm- . mittee DO 1.36 on Cellulosics. j, Current edition approved Oct. 27, 1989. Published December 1989. Originally j published as D 3971 - 80. Last previous edition D 3971 - 80 <1985). 2 Annual Book ofASTM Standards, Vol 06.02. i 3 Available from the Coming Glass Works, Coming, NY 14832. } 4 Alundum is a registered trademark of Norton Co., P.O. Box 350, Akron, OH 44309, and can be obtained from any laboratory supply house. mtedium pbfosity, or (3) glaiSs ivfth cdt(se^bnisi^''ftittdd- glass disk, 45 by 130 mm. 5.3 Heating Pev/pe-^Steam bathpj-j^ljing mantle. ...:: 5A 'Pyen, Xiph^]^^% lQ^ i 4 4 .*' 5.5 Dish, evaporating, disposable, light aluminum, 63 -. mm in diameter-by I7v5 mm.deep.? . . 5c6 Desiccator with efficient desiccant. 6; ReagtinU. \ 6.1 Dichloromethane, ACS, 99 % CH2C12, having a res idue after evaporation of less than 0.002 %. 7. Procedure 7.1 Weigh 8 to 12 g of loose pulp, to the nearest 0,01 g, into an extractor thimble that has previously been extracted with dichloromethane. For sheet pulp, cut a sample into strips about 10 mm wide and 70 mm long, and weigh about 20 g into a thimble. Weigh a separate portion for a moisture determination in accordance with Test Methods D 1348. 7.2 Place the extraction thimble with sample in the extractor and connect the flask. Pour 250 mL of the dichloromethane into the body of the extractor. Connect the assembled extractor to the condenser and place the flask in the heating device. Turn on the cooling water to the con denser and adjust the heating rate to cause siphoning 6 to 8 times per hour. Continue the extraction for 5 h. 7.3 Heat the evaporating dish in the oven at 105C for 30 min, cool in a desiccator, and weigh to the nearest 0.1 mg. ~ 7.4 When the extraction is complete, disconnect the flask . at a time when most of the solvent has collected in the extractor. Partially evaporate the solvent in the' extraction flask to a volume of 15 to 20 mL. Transfer the extract to thd tared weighing dish"by washing with three 5-mL portions of fresh solvent. 7.5 Place the dish on a steam hot plate and evaporate just to dryness. Then place the dish in the oven at 105C for 1 h, cool in a desiccator, and weigh to the nearest 0.1 mg. No t e: Caution--Care must be taken to keep the steam hot plate surface clean in order to prevent contamination of the bottom of the aluminum dish and a subsequent unmeasured increase in tare weight 7.6 Run a blank determination with the solvent used in the test. Evaporate 250 mL of the solvent to dryness and weigh the residue to the nearest 0.1 mg. Correct the weight of the dried extract by the weight of residue found. 8. Calculation 8.1 Calculate the percent of dichloromethane-soluble 5 Fisher Scientific Catalog No. 08-732-5C available from the Fisher Scientific Co., 711 Forbes Ave., Pittsburgh. PA 15219 has been found satisfactory for this purpose. 459 DUP050296979 D 3971 matter, D, on the dry basis as follows: D = (we- wb)/wj[m 7 /100 x 100 where: We = oven-dry weight of extract, g, Wb - oven-dry weight of solvent blank determined in 7.6, g, Ws = weight of sample, g, and M = moisture in sample, % (Test Methods D 1348). 9. Report 9.1 Report the diphloromethane-soluble matter to the nearest 0.01 %. 10. Precision and Bias 10.1 Results of a round robin study by five laboratories showed that for a content of 0.20 % extractives the relative standard deviation was 10 %. For samples at the <0.15 % level the relative standard deviation was <7 %. 10.2 No statement of bias can be made as no suitable reference material exists for determining bias. The American Society for Testing endMaterials takes no position respecting Ota validity ofanypatent rights asserted in connection with anyTtem 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 lights, 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 invitedeither forrevision ofthis standard or foraddiUona!standards and should be addressed to ASTM Headquarters. Your comments wlli receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel Mat your comments have not received a fair hearing you Should make your views known to the ASTM Committee on Standards, 1S16 Race $t., Philadelphia, PA 19103. j I ) t 460 DUP050296980 Designation: D 4085 - 81 {Reapproved 1987) Standard Test Method for Metals in Cellulose by Atomic Absorption Spectrophotometry1 This standard is issued under the fixed designation D 4085; 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, 1. Scope ! 1.1 This method covers the determination of the iron, copper, manganese, and calcium content of cellulose pulp from wood or cotton. 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: D1193 Specification for Reagent Water21 D 1348 Test Methods for Moisture in Cellulose3 D 3516 Practices for Ashing Cellulose3 E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods4 E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method5 3. Summary of Method 3.1 The sample is ashed in accordance with Practices D 3516. 3.2 This method is dependent on the fact that metallic elements in the ground state will absorb light of the same wavelength they emit when excited. When radiation from a given excited element is passed through a flame containing ground-state atoms of that element, the intensity of the transmitted radiation will decrease in proportion to the amount of the ground-state element in the flame. A hollow cathode lamp whose cathode is made of the element to be determined provides the radiation. The metal atoms to be measured are placed in the beam of radiation by aspirating the specimen into an oxidant-fuel flame. A monochromator isolates the characteristic radiation from the hollow cathode lamp and a photosensitive device measures the attenuated transmitted radiation. 4. Significance and Use 4.1 Manganese in pulp acts as a catalyst in oxidizing cellulose. 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 1.36 on Cellulosics. Current edition approved Dec. 28, 1981. Published February 1982. 2 Annual Book ofASTM Standards, Vote 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.02. * Annual Book ofASTM Standards, Vol 14.02. 5 Annual Book ofASTM Standards, Vote 06.03 and 14.02. 4.2 Iron in pulp can cause yellowness in rayon fibers and influence cellulose acetate plastics color. Iron also causes problems in photographic and blueprint papers. 4.3 Copper in puip can act as a retardant in oxidizing cellulose and can affect viscose'ripening. Copper interferes with the dye level of rayon fibers , and influences cellulose acetate plastics color. 4.4 Calcium in pulps can cause problems in processing into acetate, rayon, cellophane, etc. Calcium ,can create undesirable deposits in viscose spinning and film casting operation. Calcium can influence viscosity control during cellulose acetate manufacture. 5. Apparatus 5.1 Atomic Absorption Spectrophotometer, consisting of an atomizer and burner, suitable pressure-regulating devices capable of maintaining constant oxidant and fuel pressure for the duration of the test, a hollow cathode lamp for each metal to be tested, an optical system capable of isolating the desired line of radiation, an adjustable slit, a photomultiplier tube or other photosensitive device, and a read-out mecha nism for indicating the amount of absorbed radiation. 5.2 Oxidant--Air, which has been cleaned and dried through a suitable filter to remove oil, water, and other foreign substances, is the usual oxidant. 5.3 Fuel--Acetylene, commercially available, is the usual_ fuel. Acetone, always present in acetylene cylinders, can be prevented from entering and damaging the burner head by replacing a cylinder that has a gage pressure of only 3 .5 kPa (50 psi) remaining.'. 5.4 Volumetric Flasks, 25, 100, and 1000-mL. No t e 1--In listing the apparatus for this method, the items required for the ashing step are not listed. For these items refer to Practices D3516. 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. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water should be understood to mean reagent water conforming to the requirements in Specification D 1193, Type I. 6.3 Hydrochloric Acid (1+1)--Add 50 mL of concen trated hydrochloric acid (HC1, sp gr 1.19) to 50 tnL of water. 6.4 Hydrochloric Acid (1+99)--Dilute 10 mL of concen trated hydrochloric add (HC1, sp gr 1.19) to 1000 mL with water. 461 DUP050296981 me. D 4085 6.5 Nitric Acid (l+ 1)--Add 50 mL of concentrated nitric acid (HN03l sp gr 1.42) to 50 mL of water. 6.6 Sulfuric Add (1+1)--Add 50 mL of concentrated sulfuric add (H2S04) sp gr 1.84) to 50 mL of water. 6.7 Standard Solutions--the solutions that follow with HC1 (1+99) to prepare the standards to be used for calibration. Store all solutions in polyethylene bottles. 6.7.1 Iron (l mL = 1.0 mg Fe)--Dissolve 1.000 g of pure iron in 100 mL of H2S04 (1 + 1) with the aid of heat. Cool and dilute to 1 L. 6.7.2 Copper (1 mL = 1.0 mg Cu)--Dissolve 1.000 g of electrolytic copper contained in a 250-mL beaker in 30 mL of nitric acid (1+1). Slowly add 4 mL of H2SQ4 (1+1) and heat until SOs fumes evolve. Cool and dilute to 1 L. 6.7.3 Manganese (1 mL = 1.0 mg Mn)--Dissolve 3.076 g of manganous sulfate monohydrate (MnS04 H20) in a mixture of 10 mL of HC1 and 100 mL of water. Dilute to 1 L. 6.7.4 Calcium (1 mL = 1.0 mg Ca)--Weigh 2.497 g of calcium carbonate (CaC03) and transfer it to a 500-mL Erlenmeyer flask. Add 10 mL of water. Pour 10 mL of HC1 slowly down the side ofthe flask. Add an additional 200 mL of water and heat until solution is complete. Cool and dilute to 1 L. No t e 2--Acceptable standard solutions are available commercially from any laboratory supply bouse. 6.8 Lanthanum Solution (50 g/L)--Wet 58.65 g of lanthanum oxide. (La203) with water. Add slowly 250 mL of HC1 to the mixture. When dissolved dilute to 1L with water. 7. Preparation of the Sample 7.1 Select a representative sample in the amount of 30 g, 5 g for the determination of moisture and 25 g for the determination of the metals. 8. Procedure 8.1 Weigh about 25 g of pulp to the nearest 0.01 g. At the same time weigh out a separate sample for oven-dry cellulose determination. Ash the sample by Method D in Recom mended Practices D3516. Determine moisture content in accordance with Method D 1348. No t e 3--Method D in Recommended Practices D 3516 has been listed as the preferred one because it minimizes opportunity for sample loss during ashing, especially for the iron determination. However for calcium, or manganese greater than 1 mg/kg, low results may occur from sulfate interferences and Method A in Recommended Practices D 3516 may be preferred. 8.2 Calibration and Standardization ofAtomic Absorption Spectrophotometer. 8.2.1 The method of operation varies with different models of atomic absorption spectrophotometers. Therefore, no attempt is made here to describe in detail the steps for placing an instrument into operation. 8.2.2 Prepare working standard solutions daily from those described in 6.7. Make the final calcium dilutions to contain 1 % lanthanum. 8.2.3 Atomize the standards and calibrate the spectropho tometer for the element of interest. 8.3 Analyze the sample solutions prepared from 24.13 and 24.14 of Method D in Recommended Practices D 3516 in accordance with 8.2. Iron, copper, and manganese nor- TABLE 1 Precisian Data from Interlaboratory Testing Program Using Dry Ashing Metal Average, mg/kg 2S. mg/kg 23 D2S. mg/kg HR). mg/kg Iron Copper Manganese Calcium 4.0 0.22 2.0 201 1.7 0.25 0.7 42 41 2.4 28 110 0.34 0.45 34 1.0 1.3 21 59 59 mally can be run without further dilutions. Dilutions for calcium should be made 1 % in lanthanum. No t e --If Method A in Recommended Practices D 3516 was used, digest,the ash from 7A with 5 mL HQ (1+1) on a steam bath, cool and dilute in a 25-mL volumetric flask to volume with water. Further dilutions for calcium should be made 1 % in lanthanum. 8.3.1 A reagent blank should be used to zero the atomic absorption spectrophotometer before taking sample readings, 9. Calculations 9.1 Calculate the concentration of the metallic ion, in milligrams per litre, using the calibration determined in 8.2.3. ! ' j j f J j|; | | t f where: M -- metal content, mg/kg, C -- amount of material determined in sample solution, mg/L, V -- final dilution volume of sample, mL, and W= weight of oven-dry cellulose, g. 10. Precision and Bias ^ 10.1 Precision--An interlaboratory test of this procedure was conducted using a single cellulose pulp. Four laborato ries conducted tests using both dry ashing and wet ashing procedures; one additional participating laboratory used wet ashing only. The results of this study are presented in Table 1 (dry ashing) and Table 2 (wet ashing). 10.1.1 Data in the tables include the overairaverage value, two-sigma limits (2S), two-sigma limits in-percent'{2S %) and difference-two-sigma limits (D2S) as defined in Recom mended Practice E 177. An estimate of the reproducibility interval, I(R) as defined in Practice E 691, is included. These statistics apply only to testing carried out.in a manner similar to the study on which they are based and should be considered as guidelines rather than exact mathematical quantities. 10.1.2 The within-laboratory, single operator, same-day, single-machine precision ofthis method is represented by the two-sigma limits (2S) in the tables. The corresponding relative precision, two-sigma limits in percent (2S %), is also | j: I f j TABLE 2 Precision Data from Interlaboratory Testing Program Using Wet Ashing Metal Average, mg/kg 2S, mg/kg 2S % D2S, mg/kg HR). mg/kg Iron ' 5.9 2.9 49 4.1 6.3 Copper 0.91 1.02 112 1.4 1.7 Manganese 1.9 0.7 24 1.0 1.6 Calcium 193 23 12 34 34 462 DUP050296982 D 4085 ven. It is not likely that all sources of error in this Procedure are directly proportional to the test level. Therere, the indexes in percent may not apply at levels far inoved from those in the tables. 110.1.3 In most experiences less than 5 % of all random airs of measurements will not differ in absolute value by ore than the difference two-sigma liririts (D2S) shown in Le tables. This is also equivalent to the repeatability interval, ftr), as defined in Practice E 691. 10.1.4 On the basis of test error alone (including both 'thin- and between-laboratoiry components) the difference, in absolute value, of two test results obtained in different laboratories on the same material will be expected to exceed the reproducibility interval, I(R), only about 5 % of the time. This index is only a guideline, as noted in Practice E 691, and may change'at test levels appreciably different from those used in the interlaboratory test. 10.2 Bias--In the absence of a suitable reference material, no accuracy determination is possible. It should be noted, however, that dry ashing methods are subject to loss of some metals during ignition, yielding lower results than wet ashing procedures. This may have been the case for the iron and copper results in the interlaboratory test. 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 oflany 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 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 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. 463 DUP050296983 Designation: D 4139 - 82 (Reapproved 1991)ei Standard Guide for Determining Volatile and Nonvolatile Content of Pigments1 ; This standard is issued under the fixed designation b 4139; 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'reapprbval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ' el No t e--Keywords were added editorially in july (991. i M i i ii 1'I if 1. Scope 1.1 This guide is intended to aid in the selection of the proper ASTM test method for determining the volatile and nonvolatile content of pigments. No t e--Test methods for determining the composition of the volatile fraction are not covered by this guide. '. ' 1.2 The standards included are as follows: Standard Section ASTM Designation Inert or low hiding pigments White pigments Black pigments Aluminum and zinc pigments Blue pigments Green pigments Yellow, orange, brown pigments Red pigments Miscellaneous 4.1 D 280 4.2 D280 4.3 D280 D 1509 4.4 D 280 D480 4.5 D280 D 1135 4.6 D280 4.7 D280 D3724 D763 4.8 D280 4.9 2. Referenced Documents 2.1 ASTM Standards: D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments12 D480 Test Methods for Sampling and Testing of Flaked Aluminum Powders and Pastes2 D763 Specification for Raw and Burnt Umber Pigments2 D1135 Test Methods for Chemical Analysis of Blue Pigments2 D1509 Test Method for Carbon Black--Heating Loss D3724 Specification for Synthetic Brown Iron Oxide Pigment2 3. Significance and Use 3.1 The nonvolatile content of raw materials may be used to determine the total nonvolatile content (solids) of paint and related coatings. Such information may be usefbl to coatings producers and users for the determination of the total solids available for film formation and for the estima tion of the volatile organic content. 1 This guide is under the jurisdiction of ASTM Committee D-l on Point 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 25, 1982. Published August 1982. 2 Annual Book ofASTM Standards, Vol 06.02. 4. Procedure 4.1 Inert or Low Hiding Pigments." 4.1.1 Test Methods D 280 Contain Method A for pig ments that do not decompose at 110C and uses a time of 2 h at 105, to 110*C. Method B is for pigments (hat decompose at 110C and use* a vacuum to remove the volatile material. 4,1.'1.1 Test Methods D 280 are applicable to anhydrous and hydrous aluminum silicate, calcium carbonate, magne sium silicate, pumice, and wet ground mica pigments for determination of hygroscopic moisture and other matter volatile under the test conditions. 4.2 White Pigments--Test Methods D 280 are applicable to titanium dioxide and zinc sulfide pigments. 4.3 Black Pigments: 4.3.1 Test Methods D280 are applicable to synthetic black iron oxide pigment. 4.3.2 Test Method D 1509 is used to determine heating loss in carbon black pigment. 4.4 Aluminum and Zinc Pigments: 4.4.1 Test Methods D480 cover the determination of nonvolatile matter in aluminum paste. 4.4.2 Test Methods D 280 are applicable to zinc dust (metallic zinc powder). 4.5 Blue Pigments: . 4.5.1 Test Methods D280 are . applicable to copper phthalocyanine blue and ultramarine blue pigments. ` 4.5.2 Test Methods D 1135 cover the determination of moisture in iron blue pigments by the Brabender moisture tester and bytoluene distillation. 4.6 Green Pigments--Test Methods D 280 are applicable to pure chrome green, chrome oxide green, and phthal ocyanine green pigments. 4.7 Yellow, Orange, Brown Pigments: 4.7.1 Test Methods D280 are applicable to zinc yellow (zinc chromate), chrome yellow, chrome orange, cuprous oxide, natural red and brown iron oxide, molybdate orange, ocher, raw and burnt sienna, and raw and burnt umber pigments. 4.7.2 Specification D 3724 specifies methods for the deter mination of moisture and other volatile matter in synthetic brown iron oxide pigment, requiring use of Test Methods D 280, Method A for pigments containing less than 8 % iron and Method B for pigments containing more than 8 % iron. 4.7.3 Specification D 763 specifies 105C for determina tion of moisture and other volatile matter in raw and burnt umber. Additional loss at temperatures above 110C is considered to be ignition loss. 4.8 Red Pigments--Test Methods D 280 are applicable to 464 DUP050296984 atural red and brown iron oxide, synthetic red iron oxide, ure para red toner, red lead, and pure toluidine red toner igments. 4.9 Miscellaneous--No recommended methods are avail able for pigments not specifically listed in 4.1 through 4.8. Procedures to be used for determination of volatile and nonvolatile content of pigments not specified in 4.1 through 4.8 should be agreed upon between the producer and user. 5. Precision 5.1 None of the references standards contain precision statements. 6. Keywords 6.1 nonvolatile content of pigments; volatile content of pigments 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 tie reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invltedelther for revision of this standard or for additionalstandards 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 commants have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 465 DUP050296985 Designation: D 4142 - 89 Standard Guide for Testing Epoxy Resins1 < This standard is issued under the fixed designation D4I42; the number immediately following thi deagnatfrin indicates the year of `' original adoption or, in the .case ofrevision, the yearoflast revision. A numbecin parenthesesindicates the year of lasteap[Stfoval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovaL 1. Scope . - ... : 1.1 This guide covers methods for testing epoxy resins as listed in Table 1. M of.tlig i^tex^ib- oratory participation in aceordance-with usual.ASTM guide lines. Each method specifies'a ; recommended amount of ; sample for starting & separate IrialySis,''buf^evejal cif.tBie.'"' procedures can be conducted on the same starting material if so desired. For example, viscosity, color, and density could be run on the same specimen. 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: D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)12 D 1209 Test Method for Color of Clear Liquids (Platinum. Cobalt Scale)3 D 1259 Test Methods for Nonvolatile Content of Resin Solutions4 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products5 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method6 D1639 Test Method for Acid Value of Organic Coating Materials5 D 1652 Test Methods for Epoxy Content of Epoxy Resins4 D1726 Test Method for Hydrolyzable Chlorine Content of Liquid Epoxy Resins4 D1847 Test Methods for Total Chlorine Content of Epoxy Resins4 3. Significance and Use 3.1 This guide directs the user to test methods which 1 This guide is under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally published as D 4142 - 82. Last previous edition D 4142 - 82{1. 2 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4Annual Book ofASTM Standards, Vol 06.02. 1 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. determine properties generally accepted' as standard test items'fof clasification of epoxy resins. 4.;EpoxyCqntent . ..... . ,, 4:L The epoxy content of epoxy resins is' determined by "reacting asblution of the resin with a standard solution of fryarogen bromide in glacial acetic acid. The quantity of add consumed is a measure of the epoxy content Test Methods D 1652 was found to have a repeatability of 2 % of the epoxy content and a reprodudbility of 6 % of the epoxy content. 5. Hydrolyzable Chlorine 5.1 Test Method D 1726 covers the determination of the easily hydrolyzable chlorine content of liquid epoxy resins in concentrations below 1 weight %. The specimen is refluxed with a known amount of a standard alcoholic potassium hydroxide solution. The amount of hydroxide consumed is measured by titration and corresponds to the hydrolyzable chlorine content of the resin. By interlaboratory testing, the repeatability was found to be 0.02 %, and the reprodudbility was found to be 0.05 %, both absolute. 6. Total Chlorine 6.1 Organic and inorganic chlorine compounds are determined in epoxy resins in accordance with Test Methods D 1847. The resin specimen is oxidized by combustion in a bomb containing oxygen under pressure. The chlorides formed are dissolved in a sodium carbonate solution and then dther titrated or determined graVimetrically. The abso lute repeatability and reproducibility for the titration method are 0.02 and 0.05 weight %, respectively. For the gravimetric method, the .repeatability and reproducibility are both re ported to be 0.05 weight %, absolute. 7. Viscosity 7.1 Kinematic viscosity is determined by measuring the time for a volume of liquid to flow under gravity through a calibrated glass capillary viscometer in accordance with Test Method D 445. The dynamic viscosity can be obtained by multiplying the measured kinematic viscosity by the density of the liquid. The limits of precision at the three sigma level of-confidence were found to be 0.35 % relative within one laboratory and 0.70 % relative between laboratories: 7.2 It is also possible to measure viscosity by the bubble time method described in Test Method D 1545. The rise time of a bubble in the resin contained in an ASTM viscosity tube is measured. The rise time in seconds is approximately equal to the viscosity in stokes. In the range from 4.5 to 440 St, duplicate runs by one operator should be considered suspect if they differ by more than 4.9 % relative. Two results, each the mean of duplicates obtained by different { li I 1 : i ? 466 DU P0502 96986 Index of ASTM Standards, Section 6 Chalk Chalk See Calcium carbonate Chalking white/lightly tinted exterior paint films, practice, A 0 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 D1360 (06.01) Checking exterior paints, test, A D 660 (06.01) Chemical analysis--paints/related coatings/materials calcium borosilicate, test, D 4487 (06.02) C4-C13 alcohols, cheraical/physical analysis (selection/use of test procedures), E 852 (06.03) chemical analysis of yeUow/orange/red/brown pigments . containing iron/maganese, test, D.50 (06.02) ethyl methyl pentanol content/purity 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, D 4450 (06J)2) Chemical-resistant linings inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) Chemical-resistant materials/products clear/pigmented organic coatings, test, D1308 (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 (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) dear/pigmented organic coatings, test, D1308 (06.01) dipropylene glycol monomethyl ether, spec., D4836 (06.03) propylene glycol monomethyl ether acetate, spec., D4835 (06.03) propylene glycol monomethyl ether, spec., D 4837 (06.03) China clay See Aluminum silicate (hydrous) Chinese blue See 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/materiais ethylcellufose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D1347 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, D1439 (06.02) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, lest, D 5194 (06.03) Chlorinated hydrocarbons dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) Chlorinated phenol preservative content wood products, qualitative test for, D 2921 (06.01) Chlorine content cellulose, test, D 2641 (06.02) epoxy resins/compounds, test, D 4301 (06.02) hydrolyzable chlorine content of liquid epoxy resins, test, D1726 (06.02) total chlorine content of liquid epoxy resins, test, D1847 (06.02) Chloroform-insolubles content chloroform insoluble matter in oiticia oil, test, D1958 (06.03) Chromate coatings formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) Chromatkity See Color (headings) Chromatic pigments zinc yellow (zinc chromate) pigments, spec., D478 (06.02) Chromatography--gas (detergents) methoxyl/hydroxypropyl substitution (of cellulose ether products), by Zeisel technique, test, D 3876 (06.02) Chromatography--gas (paints/related coatings) identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) Chromatography--gas (paints/related coatings/materials) acrylate esters, purity, test, D 3362 (06.03) alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06.03) analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06.03) analysis of purities/impurities of styrene, test,' t> 3962 (06.03) analysis ofp-xylene, method, D 3798 (06.03) analysis of styrene by capillary gas chromatography, test, D 5135 (06.03) aromatics (ethylbenzene and eight-carbon (Cg/heavier) in mineral spirits, test, D 3257 (06.03) benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, D 4534 (06.03) chemical analysis of benzene, by gas chromatography, test, D 4492 (06.03) _ dichloromethane/1,1,1 -trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457(063)1) ethoxyl substitution in cellulose ether products, by gas chromatography, test, D4794 (06.02) ethyl methyl pentanol content/purity value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.03) fatty acid composition, by gas-liquid chromatography of methyl esters, test, D1983 (06.03) identification of carboxylic acids in alkyd resins D 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) monopentaerythritol in commercial pentaerythritol, test, D 2195 (06.03) phenol content (of tar acid mixtures), by gas liquid chromatog raphy, test, D 3626 (06.03) pinene composition (of wood/gum/sulfate turpentine), test, D 3009 (06.03) purity analysis of isopropylbenzene (cumene), test, D 3760 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, D3054 (06.03) 570 DUP050297087 Index of ASTM Standards, Section 6 Coatings ty of methyl (amyl ketone/isoamyl ketone), test, D 3893 (06.03) Kty of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) nty of methyl isobutyl ketone, by gas chromatography, test, 0 3329(06.03) ity of propylene glycol monomethyl ether/dipropylene glycol * monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) galitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, _: practice, D 3168 (06.01) pdual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) ilvent composition analysis (ofsolvent-type paints), direct-injection technique, practice, D 3271 (06.01) iophene content of refined benzene, with flame photometric detection, test, D 4735 (06.03) otai non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, test, D 2360 (06.03) Sjniformity (of traffic paint vehicle solids), practice, D 2743 (06.01) ,,jacted monomer content of latexes, test, D4747 (06.02) Jhreacted monomer content of latexes using capillary column * gas chromatography, test, D 4827 (06.02) icted toluene diisocyanate content of urethane prepoly mers/coatings, test, D3432 (06.02) Volatile resin acids in tall oil/gum/wood rosin, by gas V. chromatography, test, D 3008 (06.03) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) fxylene isomer analysis, by gas chromatography, test, D 2306 (06.03) xylene, purity of ortAo-xylene, test, D 3797 (06.03) omatography--gas (solvents) ! benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) solvent composition analysis (of solvent-type paints), direct-injection technique, practice, D 3271 (06.01) 'hromatography--paper cellulose (chemically refined), composition by chromatographic analysis, method, D1915 (06.02) irome green Sa Pigments (general properties) {) chemical analysis of pbthalocyanine blue/greet 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, D 126 (06.02) Chrome yellow and orange chrome yellow/orange pigment, spec., D 211 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Chromium content--paints/related coatings chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, 0 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 yellow) 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 greeu/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 system 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, D 2090 (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, D185 (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 of coating-films to metallic substrates, by tape test, D3359 (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 D 4257 (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/laoquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D3717 (06.01) 571 DUP050297088 ig-- ..... .. i _ - D 4143 ||olids. Test Method D 1475 is a general method for deterjjjnining the density of fluid formulated coatings and compo- Aients thereof and is therefore equally applicable for determiIpation of the density of lattices. Jj& Viscosity ; F 8.1 Lattices are non-Newtonian materials having Rheological properties that can be characterized by apparent. fviscosity measurements made using rotational-type viscomIjeters. Test Methods D2196 describes techniques using a (Brookfield viscometer by which apparent viscosity can be Itneasured and relative shear rate and time dependence of (apparent viscosity can be assessed. |9. Consistency g, 9.1 Consistency of formulated fluid paints, lacquers, varnishes, and their, mdividuaf fluid components, including | high-viscosity lattices, are frequently measured using the Stormer viscometer. Test Method D 562 describes operation of the Stormer viscometer for measuring the consistency of such materials either with or without a stroboscopic timer. 10. Water Content' 10.1 Although the major component of the volatile mate[ rial in a latex is usually water, other volatile components may be present. Test Method D3792 was developed for deter[ mining the water content of liquid latex coatings1 by direct TABLE 1 Methods tor Testing Latex Vehicles Test Method Section ASTM Designation Latex sampling methods Nonvolatile content Minimum film formalion temperature (MFTy. '< ' 'i' Qualitative polymeric analysis Density Viscosity Consistency Water content pH Surface tension . 3 , D 3925 4 Method under development 5 - D2354 6 D31S8 7 D1475 8 D2196 9 D562 10 D3792;D4017 11 E 70 12 D'1417 injection into a gas chromatograph. This method is equally suitable for determining water content of lattices. Test Method D4017 is based on the Karl 'Fischer method and is also applicable for determining the water content of lattices. 11. pH 11.1 -The pH of a latex can be measured by the general procedure described for aqueous solutions in Test. Method E 70. 12. Surface Tension 12:1 The surface tension of latex may be determined by the technique given in Test. Method D 1417. It is useful as a quality control/assurance test, and as an indicator of the wetting characteristics. '' The American Society for TestingandMaterials takds rid 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 crtthe 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 notrevised, either raapproyed 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 af a meeting of the responsible technics 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. DUP050296989 Designation: D 4209 - 82 (Reapproved 1991 )e1 Standard Practice for Determining Volatile and Nonvolatile Content of Cellulosics, Emulsions, Resin Solutions, Shellac, and Varnishes1 This standard is issued under the fixed designation D 4-209; 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 No t e--Keywords were added editorially in July 1991. 1. Scope 1.1 This practice is intended to serve as a guide to the selection of the proper ASTM test method for determining the volatile and nonvolatile content of cellulosics, emulsions, resin solutions, shellac, and varnishes. Unless otherwise specified, the test methods referenced appear in Volume 06.02 of the Annual Book ofASTM Standards. No t e--Standards for determining the composition of the volatile fraction are not covered by this practice. 1.2 The standards referenced in the practice are as follows: Classification Cellulosics Emulsions Resin Solutions Shellac Varnishes " Section 5.1 5.2 5.3 ' . 5.4 5.5 ASTM Standard D871 D914 D 1347 D2369 ' D 1259 D 1490 D29 ' D 1650 D 115 D 1644 2. Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products12 D29 Test Methods for Sampling and Testing Lac Resins3 D115 Test Methods for Varnishes Used for Electrical Insulation4 D360 Specification for Shellac Varnishes3 D871 Methods of Testing Cellulose Acetate3 D914 Test Methods For Ethylcellulose3 D 1259 Test Methods for Nonvolatile Content of Resin Solutions3 D1347 Test Methods for Methylcellulose3 D1490 Test Method for Nonvolatile Content of Urea- Formaldehyde Resin Solutions3 D1644 Test Methods for Nonvolatile Content of Varnishes6 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paint and Paint Materials. CurTent edition approved Nov. 26. 1982. Published January 1983. 2 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 10.01. 5 Annual Book ofASTM Standards, Vol 15.06. 6 Annual Book ofASTM Standards, Vol 06.01. D 1650 Test Methods for Sampling and Testing Shellac Varnish3. D 2369 Test Method for Volatile Cbntent of Coatings6 D4758 Test Method for Nonvolatile Content of Latexes5 3. Terminology (see Terminology D16) 3.1 Definitions: 3.1.1 cellulose esters--derivatives of cellulose in which one or more of the hydroxyl hydrogens have been replaced by acyl groups. 3.1.2 cellulose ethers--derivatives of cellulose in which one or more of the hydroxyl hydrogens have been replaced by alkyl groups! 3.1.3 cellulose nitrates (nitrocellulose)--derivatives of cel lulose in which one or more of the hydroxyl hydrogens have been replaced by nitrate groups. 3.1.4 emulsion vehicle--an emulsion of binder in water. The binder may be oil, oleoresinous varnish, resin, or other emulsifiable liquids ^ 3.1.5 latex--a stable aqueous dispersion of synthetic resin, produced by emulsion polymerization, as the principal constituent of the binder. 3.1.6 shellac varnish--a solution or "cut" of a speeified type and grade of dry lac resin in a suitable alcohol. 3.1.7 varnish--a liquid composition that is converted by oxidation or thermal cross-linking to a transparent or trans lucent solid film after application as a Thin layer. - 4. Significance and Use 4.1 The nonvolatile content of raw materials may be used to determine the total nonvolatile content (solids) of paint and related coatings. Such information may be useful to coatings producers and users for the determination of the total solids available for film formation and for the estima tion of the volatile organic content 5. Procedure 5.1 Cellulosics: - 5.1.1 Test Methods D 1644, Method A, should be used for determining the amount of alcohol present in nitrocellu lose shipments. This method may also be used for other cellulose derivatives if mutually agreed upon by producer and user. 5.1.2 Moisture in three different cellulose derivatives may be determined using test methods given in the following standards: 470 DUP050296990 # 0 4209 Cellulose Derivative ASTM Standard Section Cellulose acetate Ethylccllulose Methylcellulose D 871 D 914 D 1347 3-4 4-6 3-4 | 5.2 Emulsions and Latices: jf 5.2.1 Test Method D 2369, Procedure B may be used to [determine the nonvolatile and volatile content of most [emulsions. Important considerations are the presence of [volatile plasticizers and surfactants and the presence of | oxidizable components in oleoresinous vehicles and drying [oil modified alkyds. | 5.2.2 Test Method D 4758 should be used to determine the nonvolatile and volatile content of synthetic latex sam ples. 5.3 Resin Solutions: 5.3.1 Test Methods D 1259, Method A is recommended for solutions of non-heat reactive resins that remain stable and release solvents under the test conditions. Examples include alkyds and rosin esters. 5.3.2 Test Methods D 1259, Method B is recommended for solutions of heat reactive resins that undergo condensai tion or other reactions or both under the influence of heat. Examples include the formaldehyde reaction products of urea, melamine, and phenols. Method B is also recom mended for resin solutions that release solvent slowly, for example, epoxy resin and vinyl resin solutions when these contain high boiling solvents. 5.3.3 Method A and Method B of Test Methods D 1259 differ primarily in the longer drying time specified; for Method B (2 h versus 30 min). In both methods, a weighed specimen of resin solution is spread under pressure between two weighed sheets of aluminum foil, which are then sepa rated and dried at 105C. The method is unique in that it provides for drying of very thin films of resin, minimizing chances for volatiles to be trapped. 5.4 Shellac: 5.4.1 Sections 14 and 15 of Test Methods D29 describe two methods for the determination of volatile matter (mois ture) in lac resins. Method A (Section 14) is recommended for orange shellac, button lac, garnet lac, and dry bleached lac. Method B (Section 15) is recommended for bleached lac in the form of hanks, bars, and crushed fresh ground. 5.4.2 Sections 14 to 16 of Methods D 1650 are recom mended for the determination of the nonvolatile and volatile content of shellac varnishes. 5.5 Varnishes: 5.5.1 Test Methods D 1644 describes two methods for the determination of the nonvolatile and volatile content of var nishes. Method A requires heating a 1.2 g specimen at 105C for 3 h in an oven, while Method B requires heating a smaller specimen at 149C for 10 min on a hotplate. Method A may give high results due either to incomplete elimination of vol atile matter or to absorption of oxygen by oxidizing-type varnishes. 5.5.2 Sections 18 to 22 of Methods D 115 is applicable to the following classifications of varnishes used for electrical insulation: alcohol-soluble varnishes, oxidizing air-drying varnishes, thermosetting varnishes, oxidizing baking var nishes, air-drying asphaltic varnishes, silicone varnishes, and thermosetting laminating varnishes. Determine nonvolatile matter in electrical insulating varnishes intended for elec trical equipment operating at 180"C and above in accordance with Methods D 115 except that the temperature used shall be 275 5.5F (135 3C) or at a temperature agreed upon between the producer and user. 6. Precision 6.1 Some of the referenced ASTM standards have preci sion limits. Reference to the individual standards for preci sion statements is recommended. 7. Keywords 7.1 nonvolatile content of cellulosics, emulsions; volatile content of cellulosics, emulsions TheAmerican Society for Testing anti 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 every five years and ifnotrevised, eitherreapproved 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. 471 DUP050296991 # Designation: D 4277 - 83 (Reapproved 1988)'ti Standard Guide for Testing Amino Resins1 This standard is issued under the fixed designation D4277; 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 No t e--Sections 3 and 4 were renumbered in October 1988. 1. Scope 1.1 This guide covers test methods suitable for testing heat-reactive nitrogen resins, particularly urea-formaldehyde and melamine-formaldehyde resins. The test methods used are listed in Table 1. 2. Referenced Documents 2.1 ASTM Standards: D883 Definitions of Terms Relating to Plastics12 D1013 Test Method for Determining Total Nitrogen in Resins and Plastics3 D 1198 Test Method for Solvent Tolerance of Amine Resins3 D1209 Test Method for Color ofClear Liquids (Platinum- Cobalt Scale)4 D1259 Test Methods for Nonvolatile Content of Resin Solutions3 D 1475 Test Method for Density of Paint, Varnish, Lao . quer, and Related Products3 D 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method6 D 1639 Test Method for Add Value of Organic Coating Materials5 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus7 3. Terminology 3.1 Definition--The following definition is taken from Definitions D 883: 3.1.1 amino resin--a resin made by polycondensation of a compound containing amino groups such as urea or melamine with an aldehyde, such as formaldehyde, or an aldehyde-yielding material. 4. Significance and Use 4.1 This guide summarizes the currently available ASTM test methods useful for testing amino resins. These test methods may be used by producers and users to characterize 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 1.33 on Polymers and Resins. Current edition approved Aug. 26, 1983. Published October 1983. 2 Annual Book ofASTM Standards, Vol 08.01. 5 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Bode ofASTM Standards, Vols 06.01 and 06.03. s Annual Book ofASTMStandards, Vol 06.01. 6 Annual Book ofASTM Standards, Vols 06.01, 06.02 and 06.03. 7 Annual Book qfASTM Standards, Vol 06.03. TABLE 1 Methods for Testing Nitrogen Resins Test Method Section ASTM Designation Total nitrogen In resins end plashes Solvent tolerance of amino resins Color of dear liquids Nonvolatile content resin solutions Density Viscosity Acid value Rash point S 6 7 8 9 10 11 12 D1013 D1198 D1209 D1259 D1475 D1545 D1639 D3278 a variety of properties of nitrogen resins related to their quality and safe use. 5. Total Nitrogen 5.1 Test Method D1013 is a standard Kjeldahl procedure for nitrogen determination, directly applicable to amino resins and solutions thereof. 6. Solvent Tolerance 6.1 The amount of hydrocarbon that an amino resin tolerates is measured in accordance with Test . Method D1198. The end point of this titration, a defined degree of turbidity, is sensitive to both the alkylation and degree of polymerization of the amino resin. 7. Color 7.1 The color of solutions of amino resins can be mea sured using.Jhe platinum-cobalt scale according to the procedure in Test Method D 1209. 8, Nonvolatile Content 8.1 The nonvolatile content of amino resins is measured using Test Methods D 1259, Method B, which applies to heat reactive resin solutions and requires a longer drying time. A very thin film, created by pressing a resin specimen between sheets of aluminum foil, is dried for 2 h and weighed. There may be some reaction of amino resins during the drying procedure, but the repeatability (0.7 % absolute) and repro ducibility (1.7 % absolute) are acceptable. 9. Density 9.1 Test Method D 1475 is a general-purpose test method for determination of density using a pycnometer or cup. It is fully applicable to amino resins. 10. Viscosity 10.1 Viscosity of amino resins is determined in bubble seconds, approximately equal to stokes, using standard 472 DUP050296992 # D4277 1. Acid Value 11.1 Test Method D 1639, which describes titration of a sin specimen with standard potassium hydroxide, is suitble for determining the acid value of amino resins. 12. Flash Point 12.1 Test Methods D 3278 provide for either a flash/no flash or finite flash point determination using the Setaflash closed tester. It is applicable only when the material to be tested has a flash point between 0 and 110C and a viscosity lower than 150 St at 25eC. TheAmerican Society tor 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 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 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. 473 DU P050296993 i Designation: D 4288 - 83 (Reapproved 1989)1 StandardSpecifieaSion for O^lcium^QrosilibatePiginents1 This standard is issued under the fixed designation D 4288; the number immediately following the designation indicates the year of original adoptionor, in the case,ofrevision, the year oflast revision. A number in parentheses indicates theyeac oflast reapproval. A superseripVeps%n(<)iridicates,aneditqrialchangesiriC9.the lastrevisionror.reapproval. . > E! No t e--Editorial changes were made throughout in March 1989. 1. Scope 1.1 This specification covers three grades of pigment commercially known as calcium borosilicate composite pig ment. The two types differ in chemical composition while the two classes of Type I differ in oil absorption. 2. Referenced Documents 2.1 ASTM Standards: C 958 Method for Determinatioin of Particle Size Distri bution of Alumina or Quartz by X-Ray Monitoring of Gravity Sedimentation21 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out4 D1366 Practice for Reporting Particle Size Characteristics of Pigments4 D 3360 Test Method for Particle Size Distribution by Hy drometer of the Common White Extender Pigments4 D4487 Test Methods for Analysis of Calcium Borosili cate4 3. Composition and Properties 3.1 All types of pigment shall consist of a complex composite of alkaline earth silicates and borates and shall conform to the requirements of Table 1. 3.2 The mass color of the dry pigment is white. The shade and tinting strength when specified shall be equal to that of a reference sample mutually agreed upon between the pur chaser and the seller. 3.3 Particle Size: 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.31 on Pigment Specifications. Current edition approved Oct. 28, 1983. Published December 1983. 2 Annual Book ofASTM Standards, Vol 15.02. 3 Annual Book ofASTMStandards, Vols 06.01 and 06.02. 4 Annual Book ofASTM Standards, Vol 06.02. . 3.3'. L All types 'are characterized by major, amounts of -. 'particles in the' 1 to 10-fim range, Coarse particles retained on a 45-pm (No. 325) sieve shall be less than 0.3 %. The maximum specific surface diameter (SSD) shall be 2.5. 3.3.2 Where closer control within a grade or type is re- quired, the fineness requirements shall be as agreed upon between the purchaser and the seller. 3 I j I 1 j 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages, in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two samples shall be taken. At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. i , : ; ! 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. ~ 5.2 Chemical Analysis--Test Methods D 4487. 5.3 Ignition Loss--Test Methods D 4487. 5.4 Particle Size--To be determined' by Test Method D 3360 or equivalent instrumental technique.5 5.5 Specific Surface Diameter--Particle Size by Sedimen tation Methods section of Practice D 1366. 5.6 Oil Absorption--Test Method D 281. 5.7 Coarse Particles--The Insoluble Dry Pigments sec tion of Test Methods D 185. 5 The Micromerilics Sedigraph S000D Particle Size Analyzer, manufactured by Micromeritics Instrument Corp-, 568 Goshen. Springs Rd, Norcross, GA 30093, has been found satisfactory for this purpose. See Method C 958 for operating instructions. Other instruments having a similar slurry density measurement function may also be used. 474 DUP050296994 # D 4288 TABLE 1 Requirements for Pigments Weight % it Compositional Requirements Type 1,10% B203 Min- Max jjSjldum oxide {CaO} Hbron oxide (B203) pica (Sicy ' Moisture and other volatile matter Blition loss at 450C P* 41 9 38 2.5 ClassA 46 11 42 0.75 6.0 Class B min max min max BoperVes: P6il absorption (lb/100 lb pigment) ptjjbarse parficies ' i Total residue retained on 45-pffl (No. 325) sieve, % 35 41 .0.3 23 29 0.3 Type 2,17% B203 Min Max 41.5 45.5 15 17.5 32 < 36 0.75 2.5 6.0 37 47 0.3 The American Society for Testing and Materials takes noposition respecting the validity ofany patent rights asserted In connection with any Hem mentioned in this standard. Users of this standard are expressly advised that determination of the validity ofany suchpatent rights, and the risk of tnfrhigefnent of such rights, fire entirely their,own responsibility. This standard Is subject tojpvjflon at any time by the responsible technical committee and rhust 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 will receive careful consideration at a meeting of the responsible technical committee, which yog may attend, it you fee1 that your comments have not received a fair hearing you should make your views known to the ASThl Committee on Standards, ISIS Race St., Philadelphia, PA 19103. m 475 DUP050296995 Designation: D 4301 - 84 (Reapproved 1990)e1 Standard Test Method for Total Chlorine in Epoxy Resins and Compounds1 This standard is issued under the fixed designation D 4301; 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. fl No t e--Section 10 and Note 2 were added editorially in April 1990. 1. Scope 1.1 This test method describes a procedure for the deter mination oftotal chlorine in epoxy resins and glycidyl ethers. 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: D 1193 Specification for Reagent Water2 3. Summary of Test Method 3.1 The material, dissolved in dimethoxyethane (DME) or other suitable inert solvent, is reacted with sodium biphenyl to convert bound organic chlorine to the water soluble chloride. The excess reagent is decomposed with isopropyl alcohol. The chloride ion is then titrated potentiometrically with silver nitrate. 4. Significance and Use 4.1 The presence of residual chlorine in epoxy resins is deleterious to final product properties. This test method has been found to be applicable to resins or ethers with chlorine contents ranging from 50 ppm to 35 % by weight. Other halogen compounds react with the reagent but are distin guished from chlorine by the final potentiometric titration. Epoxy and other functional groups will consume reagent but do not affect the results. 5. Apparatus 5.1 Potentiograpk. 5.2 Beaker, of appropriate size. 5.3 Buret, of appropriate size. 5.4 Stirrer, magnetic or paddle. 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- 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 DO! .33 on Varnish and Resins, Including Shellac. Current edition approved Jan. 5, 1934. Published July 1984. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. ical Society, where such specifications are available.3 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 P 1193. 6.3 Sodium Biphenyl Reagent4 (in ether solution). No t e .1--Store in a refrigerator When not in use to prevent loss of activity. 6.4 Nitric Acid (HN03) (1+1,), aqueous solution. 6.5 1,2-Dimethoxyethane. 6.6 Silver Nitrate (AgNo3), 0.1 and 0.01 N standardized solutions. 6.7 Methyl Red Indicator (0.2 % alcohol solution), dis solve 0.2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol. 6.8 Isopropyl Alcohol. 7. Procedure 7.1 Pipet 5 mL of 1,2-dimethoxyethane into a clean, dry 250-mL beaker. Add a weighed amount of sample. (If the material is anticipated to be low in total chlorine, use 0.40 g of sample. For materials high in chlorine, weigh 0.1 to 0.2 g of sample.) Gently swirl to dissolve. 7.2 Add about 15 mL (one bottle) of sodium biphenyl reagent and mix thoroughly. If the solution loses its dark blue or green color within 5 min, add_another 15 mL of reagent. Allow to react for 5 min. 7.3 Add lOCTmL of isopropanol to decompose the excess reagent and to serve as the titrating medium. Add 3 to 5 drops of methyl red solution and neutralize with HN03 (1+1). Add 5 to 8 drops of add in excess; start the stirrer. 7.4 Titrate the solution potentiometrically using standard AgN03 solution. (For low chlorine content, titrate with 0.01 N AgN03 and for high chlorine content use 0.10 AT AgN03). The scale of the titration curve will depend on the instru ment used but should give a curve of the approximate scale of 0.25 mL/cm and 30 mV/cm. The end point is selected as the middle of the steepest portion of the curve. 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." 4 This reagent is available in small bottles (15-mL) from Southwestern Analytical Chemicals, P. O. Box 485, Austin 63, TX. It may also be prepared as described in Analytical Chemistry, Vol 26, p. 748. 476 DUP050296996 D 4301 o t e 2--It may be preferable to use the first or second derivative to nine the end point providing appropriate equipment is available. .5 Repeat the determination and also run a blank using reagents but omitting the specimen. Calculation $ 8.1 Calculate the weight percent of chlorine, C, as follows: C -- {' V~B)xNx S 3.546 ere: -- titration of specimen, mL, = titration of blank, mL, = normality of AgN03 solution, and = weight of specimen, g. 8.2 Calculate the mean of the two runs. 9. Precision 9.1 On the basis of an interlaboratory study of this test method in which one operator in each of three laboratories analyzed in duplicate on two different days five materials containing 0.1 to 0.3 % total chlorine, for a total of 60 determinations, the within-Iaboratory standard deviation was found to be 5 % relative and the between-laboratories standard deviation 7 % relative. Based on these standard deviations the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 9.2 Repeatability--Two results, each the mean of two runs, obtained by the same operator should be considered suspect if they differ by more than 15 % relative. 9.3 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. 10. Keywords 10. chlorine; glycidyl ethers; liquid epoxy resins The American Society for Testing and Materials takes no position respecting the validity of any paters 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. 477 DU P050296997 Designation: D 4358 - 84 (Reapproved 1990)1 Standard Test Method for Lead and Chromium in Air Particulate Filter Samples of Lead Chromate Type Pigment Dusts by Atomic Absorption Spectroscopy1 This standard is issued under the fixed designation 0 4358; 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 ei NOTE--Section 14 Was added editorially in May 1990. J 1. Scope 1.1 This test method determines amounts of lead and chromium in residues obtained from air sampling of lead chromate and lead silico-chromate type pigment dusts. It is not applicable to all pigment dusts or to paint overspray samples of any kind. 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 Standard: D 1193 Specification for Reagent Water21 3. Summary of Test Method 3 .1 The filter containing the air particulate sample is dis solved with nitric acid followed by treatment with 50 % aqueous ammonium acetate solution. The solution is trans ferred to a volumetric flask and lead and chromium deter mined by atomic absorption. 4. Significance and Use 4.1 This test method covers only the analysis of the pig ment dusts on filters, the results being expressed as micro grams of lead and of chromium. Sampling procedures are not a part of this test method, nor are those calculations that are required to convert the results to concentration of lead and chromium in the sampled air, as required by the U.S. Occupational Safety and Health Act (OSHA). 5. Apparatus 5.1 Atomic Absorption Spectrophotometer, consisting of an atomizer and burner; gas pressure regulating and meter ing devices for air, acetylene, and nitrous oxide; provision for hollow cathode source lamps with regulated constant current supply; a monochromator with associated optics; a photode tector; an amplifier; and digital or analog readout system. 5.2 Lead Hollow Cathode Lamp or electrodeless discharge source lamp. 5.3 Chromium Hollow Cathode Source Lamp. 5.4 Volumetric Flasks, 10-mL. ' * \ I, 6. Reagents and Materials ' . 6,1 Purity ofReagents--Reagent,grade chemicals shall be \ used in all tests. Unless otherwise indicated, it is intended :i that all reagents shall conform to the Committee on Analyt- ' icaL Reagents of the American Chemical Society, where such jj specifications are available.3 Other grades may be used, provided it is first ascertained that, the reagent is of suffi- ciently high purity to permit its use without lessening the | accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer- 1 ences to water shall be understood to mean reagent water " | conforming to Type II of Specification D 1193. 6.3 Ammonium Acetate Solution (50 % W/V aqueous)-- | Dissolve 250 g ofammonium acetate (NH4C2H302) in water | and dilute to 500 mL. \ 6.4 Nitric Acid (sp gr 1.50)--Concentrated nitric acid I (HN03). . 6.5 Nitric Acid, (1+3)--Dilute 1 part concentrated nitric I acid with 3 parts water. ,, . _ t 6.6 Lead, Standard Stock Solution,(1000 |j.g/mL)r-Dis- :{ solve 0.1599 g of lead nitrate (Pb(N03)2) in-50 mL of water | containing 20`mL ofconcentrated HN03 and 10 mL of 50 % ; ammonium acetate solution, and dilute to 100 mL with water. |j 6.7 Chromium, Standard Stock Solution (1000 pg/mL)-- i| Dissolve 0.3734 g ofpotassium chromate (K2Cr04) in 50 mL j water containing 5 mL of concentrated HN03 and dilute to 100 mL with water. 6.8 Filter Blank--Miflipore 0.8-pm pore :size, 37-mm diameter, mixed esters of cellulose. Type AA white, plain, or equivalent. 6.9 Hydrogen Peroxide--30 % (H202). 7. Calibration and Standardization 7.1 Good atomic absorption practice requires that the test 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 D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved April 27, 1984. Published August 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, NY and the "United States Pharmacopeia." 478 DUP050296998 i #. D 4358 solutions being analyzed be aspirated into the flame interjersed between or at least contiguous to aspiration of the ^calibration standards. The formal separation of calibration " nd analysis is for clarity of the methodology only and such Separation should not be made in practice. 7.2 QperationaLinstructions for atomic absorption spec trophotometers vary with different models. Consult the man ufacturer's literature for establishing optimum conditions for (the specific instrument used. 7.3 Insert the lead source lamp into the appropriate holder, rum on the instrument and apply the current recommended by the manufacturer to the source lamp. Allow the lead source Ibunp a lO-min warmup. Adjust the wavelength to 283.3 nm, jset the slit to 0.7-nm bandpass, and maximize the transmitted energy by fine,adjustment of the wavelength. . , 7.4 Prepare fresh standard solutions each day containing 6.5, 1.0,2.0, 5.0, and 10.0 ppm lead by appropriate dilutions of the lOOO .pg/mL stock standard. 20 mL of concentrated HN03 and 2 mL of 50 % ammonium acetate should be added in each case per 100 mL of final dilution. . 7.5 .Adjust the air and .acetylene pressure or flow rates and ignite the burner according to the instruction manual. Adjust the acetylene to give a rich flame. Allow a few minutes to equilibrate. ; 7.6 Aspirate water to rinse the atomizer chamber. Aspirate the 10 ppm standard and make any necessary readjustment in instrument parameters to obtain maximum absorption. 7.7 Aspirate each standard solution and record the corre sponding instrument readings. Aspirate 1+3 HN03, then \vater between each standard. | 7.8 Construct a calibration curve for lead on linear graph ! paper by plotting tihe absorbance versus concentration (miJ crograms per millilitre) for each standard solution. * 7.9 Replace the lead source lamp with the chromium j source lamp, adjust the applied current to that recommended and allow to warm up for 10 min. Adjust the wavelength to 357.9 nm, set the slit to 0.7-nm bandpass, and maximize transmitted energy by fine wavelength adjustment. 7.10 Prepare fresh standard solutions each day containing O.i, 0.2, 0.5, 1.0 and 2.0 ppm chromium by appropriate dilutions of the 1000 pg/mL stock standard. Add 20 mL of concentrated HN03 and 2 mL of 50 % ammonium acetate in-each case per 100 mL of final dilution. 7.11 Turn on air and acetylene, adjust the flow rates and ignite according to the instruction manual. Adjust the acety lene to give a rich flame. Allow a few minutes to equilibrate. (Note 1). No t e I--The National Institute for Occupational Safety and Health (NIOSH) recommends the use of a nitrous oxide-acetylene flame, which reduces iron and nickel interference in the chromium determination. However, chromium sensitivity in the nitrous oxide flame is also much lower, so that air/acetylene is specified here. Iron, aluminum, titanium as well as SOj= interference may be reduced by adding 10 % of W/V KHSO* to both standard and sample solution, employing an air/ acetylene flame. The comparison of the experimental lead to chromium ratio noted can be of some use here. (See Section 11.) 7.12 Aspirate water into the flame. Then aspirate the 2.0 ppm standard and adjust burner position and flame compo sition to give maximum absorption. 7.13 Aspirate all standards into the flame, aspirating water between each standard and the next. Construct a calibration curve for chromium on linear graph paper by plotting the absorbance versus concentration (micrograms per millilitre) for each standard solution. 8. Procedure 8.1 With each batch of samples a filter blank (minimum of 1 filter blank for every 10 filter samples) from the same membrane lot must be analyzed. The filter blank is carried through all steps of the analysis along with the sample(s). 8.2 Carefully open the filter cassette containing the air particulate sample. Remove the filter using forceps and deposit it in a 50-mL beaker. 8.3 Add 6 mL of 1+3 HN03, cover the beaker with a watch glass, and keep just under boiling by placing on a hot water bath. Heat for 10 min. Add 2 mL of 50 % ammonium acetate solution and continue to.-heat, adding water as needed to keep the volume at about 5 to 6 mL. The solution must not be allowed to go to dryness. When analyzing lead silicochromate-type pigment dusts, add 0.5 mL of 30 % hydrogen peroxide (H202) after the 2 mL of 50 % ammo nium acetate solution, and continue heating until cellulose filter completely dissolves. 8.4 Continue heating for 1 h. If the cellulose filter is not dissolved, continue the digestion until the solution is clear. Cool and transfer to a 10.0-mL volumetric flask. Dilute to volume with water and determine lead and chromium. 3.5 Prepare the atomic absorption instrument for lead as noted in 7.3, 7.5, and 7.6. 8.6 Aspirate the test solution into the flame. Record the reading. Aspirate 1+3 HN03, then water between test solu tions. 8.7 Aspirate the appropriate standards, usually one above and below the test solution concentration. Aspirate 1+3 HN03, then water between each standard and the next. Record readings. 8.8 If the absorption of any test solution is greater than that of. the 10 ppm lead standard, make an appropriate dilution (matching the stindard matrix), aspirate and mea sure the absorbance of the diluted solution. It is important that the diluted test solution be aspirated with the flame not beingshut off or altered following aspiration ofthe standards. 8.9 Prepare the atomic absorption fnstrument for chro mium as noted-in-7.9, 7.11, and 7.12. 8.10 Repeat steps 8.6 through 8.8, in this case for chro mium except that, between each standard or sample and the next, aspirate only water. 8.11 from the calibration curves determine.the lead and chromium concentrations in the aspirated solutions. 9. Calculation 9.1 Calculate the micrograms of lead. A, on the filter as follows: A -- (L)( k'jX-F) (1) where: L = lead read from calibration curve (8.11), pg/mL, = final volume of lead solution which is measured (8.8 or if no dilution is necessary, 8.4), and F => [volume to which originally diluted (8.4) divided by millilitres of aliquot of original dilution taken for final dilution). 479 DUP050296999 # D 4358 . 9.2 Calculate the micrograms of chromium, B, on the filter as follows: 3 = (CX*W) (2) where: C = chromium read from calibration curve (8.11), pg/mL, V2 = final volume of chromium solution which is measured (8.10 or if no dilution is necessary, 8.4), and F - [volume to which originally diluted (8.4) divided by millilitres of aliquot of original dilution taken for final dilution]. 10. Lead to Chromium Ratio 10.1 If the workplace dust involves a single, known lead chromate or lead silicochromate type pigment, the deter mined lead to chromium ratio found (9.1 and 9.2) may be compared with the theoretical ratio (or actual ratio) of the bulk pigment as an internal check. 11. Report 11.1 Report the micrograms of lead and the micrograms of chromium present on the filter. 12. Precision for Lead Chromate Type Pigment Dust 12.1 Lead Determination--On the basis of an interlabo ratory study of the test method in which operators in eight laboratories analyzed sixteen air particulate samples contain ing from 16 to 80 jig oflead and from 3 to 15 pg of chromium, the within-laboratory coefficiept of variation of the lead de termination was found to be 9 % relative at 21 df and the between-laboratory coefficient of variation was 15 % relative at 18 df. 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 26 % relative for lead. 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 40.4 % relative for lead. 12.2 Chromium Determination--In the same interlabora tory study of the test method, the within-laboratory coeffi cient of variation of the chromium determination was found to be 11 % relative at 20 df and the between- laboratory coefficient of variation was 19 % relative at 18 df. Based on these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level. 12.2.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator op different days should be considered suspect if they differ by more than 33 % relative for chromium. 12.2.2 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 54 % relative for chromium. 13. Precision for Lead Silicochromate Type Pigment Dust 13.1 Lead Determination--On the basis of an interlabo ratory study of the test method in which operators in five laboratories analyzed sixteen air particulate samples con taining from 37 to 116 pg of lead and 2 to 8 pg ofchromium, the within-laboratory coefficient of variation of the lead determination was found to be 2.7 % relative at 15 df and the between-laboratory coefficient of variation was 9.4 % rela tive at 12 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 determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 8.2 % relative for lead. 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 28.4 % relative for lead. 13.2 Chromium Determination--In the same interlabora tory study of the test method, the within-laboratory coeffi cient of variation of the chromium determination was found to be 2.3 % relative at 12 df and the between-laboratory coefficient of variation was 23.6 % relative, at 9 df. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence leveL. 13.2.1 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 6.8 % relative for chromium. :' * 13.2.2 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 68,8 % relative (Note 2) for chromium. No t e 2--Error appears large due to the low range of chromium studied (2 to S pm per filter) leading to poor reproducibility. 14. Keywords 14.1 air particulates; air sampling; atomic absorption spectroscopy; chromium; lead; pigment dust 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 end 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 Committee on Standards, 19IS Race Si., Philadelphia, PA 19103. 480 DUP050297000 Designation: D 4368 - 89 Standard Guide for Testing PoIy(Vinyl Chloride) Resins1 This standard is issued under the fixed designation D 4368; 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 covers test methods for poly(vinyl chloride) resins and vinyl chloride copolymers for use in coatings applications. The test methods listed in Table 1 were tested by interlaboratory participation in accordance with ASTM guidelines. Also included are methods useful to test the suitability of resins for use in fluid nonaqueous vinyl dispersions. 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 practicep and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1243 Test Method for Dilute Solution Viscosity ofVinyl Chloride Polymers12 D1705 Test Method for Particle Size Analysis of Pow dered Polymers and Copolymers of Vinyl Chloride3 D1755 Specification for Poly(Vinyl Chloride) Resins3 D 1823 Test Method for Apparent Viscosity of Plastisols and Organosols at High Shear Rates by Extrusion Viscometer3 D1824 Test Method for Apparent Viscosity of Plastisols and Organosols at Low Shear Rates by Brookfield Viscometer3 D1895 Test Methods for Apparent Density, Bulk Factor, and Pourability of Plastic Materials3 D1921 Test Method for Particle Size (Sieve Analysis) of Plastic Materials3 D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational (Brookfield) Vis cometer4 D2222 Test Method for Methanol Extract of Vinyl Chloride Resins3 D3030 Test Method for Volatile Matter (Including Water) of Vinyl Chloride Resins3 D 3205 Test Method for Viscosity of Asphalt with Cone and Plate Viscometer5 1 This guide is under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO!.33 on Polymers and Resins. Current edition approved April 28, 1989. Published June 1989. Originally published as D 4368 - 84. Last previous edition D 4368 - 87. 2 Annual Book ofASTM Standards, Vol 08.01. 3 Annual Book ofASTM Standards, Vol 08.02. 4 Annual Book ofASTM Standards. Vol 06.01. s Annual Book ofASTM Standards, Yol 04.03. D 3680 Test Method for Residual Vinyl Chloride Mono mer Content of Poly(Vinyl Chloride) Resins, Com pounds, and Copolymers by Solution Injection Tech nique6 D 3749 Test Method for Residual Vinyl Chloride Mono mer in Poly(Vinyl Chloride) Homopolymer Resins by Gas Chromatographic.Head Space Technique7 D4287 Test Method for High-Shear Viscosity Using the ICI Cone/Plate Viscometer4 E 442 Test Method for Chlorine, Bromine, or Iodine in Organic Compounds by Oxygen Flask Combustion8 3. Significance and Use 3.1 The test methods listed and discussed in this guide are used to determine the purity and physical properties of poly(vinyl chloride) and vinyl chloride copolymers. This information is. useful to polymer producers and coatings manufacturers. 4. Total Chlorine Content 4.1 The determination of the total chlorine in vinyl chloride homopolymers and copolymers is'useful for the compositional analysis of the polymer and also to determine the amount of vinyl resin present in a coating binder, provided no other chlorine-containing ingredients are present. 4.2 Test Method E442 involves the determination of chlorine in organic compounds by the oxygen flash tech nique (Schoeninger technique). 5. Dilute Solution Viscosity __ 5.1 The dilute solution viscosity provides a measure ofthe relative molecular weight of the vinyl resin. In Test Method D 1243, 0.2 g of the sample in 100 mL of cyclohexanone Is employed. The flow time of the solution in a standard ' Ubbeiohde viscometer at 30 0.5C is used to calculate the inherent viscosity (logarithm viscosity number). 5.2 The procedure is applicable to all vinyl chloride homopolymers and copolymers used in coatings. 6. Viscosity Measurement (of Vinyl Dispersions) 6.1 Viscosity behavior is important to the use of fine powder vinyl resins (dispersion resins) in fluid nonaqueous dispersions for coatings applications. These dispersions are. called plastisols when only plasticizers) is(are) employed with the resin, and organosols when volatile diluents or solvents are also present. 6 Annual Book ofASTM Standards, Vol 06.02. 7 Annua! Book ofASTM Standards, Vol 08.03. 8 Annual Book ofASTM Standards. Vol 15.05. 481 DU P050297001 D 4368 TABLE 1 Test Methods for Vinyl Chloride Resins Method Section ASTM Designation Viscosity, dilute solution Particle size (sieve analysis) Pdy(vinyi chloride) resins, specification Viscosity, vinyl dispersions, high shear Viscosity vinyl dispersions, low shear Apparent density Particle size (sieve analysis) Methanol extract Volatile content Residual VC1 monomer-solution technique Residual VC1 monomer-head space technique Viscosity,.high shear, cone and plate Total chlorine content 5 11 6 6 6 10 11 7 8 9 9 6 4 D1243 D1705 D1755 D1823 D1824 D1895 D1921 D2222 D3030 03680 D 3749 D4287 E 442 6.2 The flow behavior of the dispersions at low shear rates, which determines the relative ease of mixing and pumping (transfer) and is also related' to low shear coating applications for example and dip coating, is measured in Test Method D 1824 or Test Method D2I96 with a Brookfield viscometer. The flow at high shear rates, related to high shear application such as in coil coating, is character ized in Test Method D 1823 using an extrusion rheometer. High shear flow can also' be determined using a coneand-plale viscometer, following thegeneral procedure of Test Method D 3205 or with the equivalent Test Method D 4287, 6.3 The preparation and testing of the resin-in a standard vinyl plastisol, which contains 60 parts of di(2-eihylhexyl phthalate) and 100 parts ofthe test vinyl dispersion resin, are described in Specification D 1755. 7. Methanol Extract ; 7.1 The amount of nonvolatile, methanol-soluble mate rial present in the vinyl resin, such as surface active agents, plasticizers, and other alcohol-soluble additives, is obtained in Test Method D 2222 by weighing the material soluble in refluxing methanol: 7.2 This procedure provides a * relative measure of the polymeric purity of the resin. 1 = * **'*' 7.3 With some low molecular weight vinyl copolymer resins with moderate comonomer content, the methanol extraction may also remove the low molecular fraction ofthe polymer. 8. Volatile Content , 8.1 The volatile material present in the vinyl resin is determined from the loss in weight observed on heating a resin specimen to constant weight in an air-circulating oven at 110*C (see Test Method D 3036). 9. Residual Vinyl Chloride Monomer 9.1 Residual vinyl chloride' monomer present in either vinyl chloride homopolymers or copolymers is measured in Test Method D3680 using analysis of a solution of the test resin in tetrahydrofuran injected into a gas chromatograph. 9.2 Gas chromatography using a head space sampling technique is also applicable to poly(vinyl chloride) (Test Method D 3749). 10. Apparent Density : ; 10.1 The apparent or bulk density ofthe solid resin is the weight of the powder per unit volume* that is, grams per cubic centimetre (or pounds per cubic foot). This parameter: is a measure ofthe compactness of the powder, A cylindrical cup of 100 0.5 mL is used in measuring this characteristic in Test Methods D 1895; a small quantity of powdered carbon black is used to dissipate the electrostatic charge present occasionally on vinyl resin powdersor granules. 11. Particle Size 11.1 The ipedian particle size and. particle size distribu tion of the resin sample are determined nsing sieve analysis (Test Method D 1921). A small amount of carbon black is used to dissipate the static charge generated'in the procedure. The lower size limit of the determination-is about 38 pm; for smaller particle sized resins, sedimentation methods are recommended. . .? * 11.2 Test Method D 1705 describes a-wetssieve method that can also be used to determine the particle size and distribution. The American Society for Testing and Msterials takes no position respecting,thevalidlty of any patent rlghts assertedin connection with any Item mentioned in this standard. Users of this standard are expressly advised ihafdetermination 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 Starry time by theresponsible technical committee and mustbe reviewed everyflveyears end ifnot revised, either reapproved or Withdrawn. Yotit comments'are Invited either for revision of this 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. If you feel that your comments have not received a fair hearing you should make yoyr views known to the ASTM Committee on,Standards, 1916 Sacs St., Philadelphia, PA 19103. 482 DUP050297002 <1 Designation: D 4450 - 85 (Reapproved I990)1 Standard Test Method for Analysis of Zinc Hydroxy Phosphite Figment*1 This standard is issued under-the fixed designation D 4450; 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. e* No t e--Section 1S was added editorially in May 1990 1. Scope 1.1 This test method is intended for the determination of zinc oxide and phosphorous acid content of the pigment commercially known as zinc hydroxy phosphite. The zinc content is determined by EDTA titration and calculated as zinc oxide (ZnO), while the phosphorus content is deter mined colorimetrically and calculated as phosphorous acid (H3p o 3 'Y',, 1.2 The analytical procedures appear in the following order: " ' ' Zinc oxide. Phosphorous acid Sections 6 through 8 9 through 14 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 arid mp limitations, prior to use. . 2. Referenced Document 2.1 ASTM Standard: \ D1193 Specification for Reagent Water2 3., Summary of Test Method 3.1 The zinc is determined by dissolving the test sample in nitric acid, adjusting the pH of the solution to 5 to 5.5 and titrating with EDTA. 3.2 The phosphorus1 is determined colon'metrically with the aid of nitric acid, ammonium vanadate^ and ammonium molybdate. The absorbance ofthe test sample is compared to a calibration curve that yields the number of milligrams of phosphorus. 4. Significance and Use i 4.1 This test method may be used to confirm the stated zific oxide and phosphorous acid content of zinc hydroxy phosphite'pignient. 5. Purity of Reagents 5.1 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.3 O* ther 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 ffie determination. 5.2 Unless5 otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. TOTAL ZINC AS ZINC OXIDE 6. Reagents 6.1 Ammonium Hydroxide (sp gr 0.90), concentrated ammonium hydroxide (NH40H). 6.2 Glacial Acetic Acid (min 99.7 %), concentrated glacial acetic acid (CH3COOH). 6.3 Acid Ammonium Acetate Buffer--Mix 400 mL of distilled water and 400 mL of reagent grade ammonium hydroxide (sp gr 0.90). Add 375 mL of reagent grade glacial acetic acid slowly while stirring, -> 6.4 Cupric Sulfate Solution (0.1 M)--Dissolve 25 g of CuS04 5HzO in distilled water and dilute to 1 L. 6.5 Disodium Ethylenediaminetetraacetate Dihydrate (0.05 M) (EDTA''Solution)--Dissolve 18:6 g of the reagent grade salt in distilled water and dilute to 1 L. Standardize the solution as follows: t6. 5.1 Transfer 25 mL of lead standard (6.6)~to a 400-mL beakdr. Add concehtrated ammonium hydroxide'(6.1) dropwise 'untilra- permanent precipitate just Forms. Add 25 mL of acid ammonium acetate (6.3), dilute to 200 mL, heat to boiling, add 4 drops ofcopper EDTA (6.7) and' 12 drops of PAN (6.8), and titrate with EDTA to a dear yellow. 6.5.2 Calculate the molarity ofthe EDTA, M, as follows: AT 25 x 0.0.1036/Lx 0.20721 (1) where L -- EDTA solution, mL. Also 1 mL of primary standard 0.05 M lead nitrate = 0.01036 g of lead and 0.20721 is the milliequivalent weight of lead. 6.6 Primary Standard (0.05 M lead nitrate)--Dissolve 16.5615 g reagent grade lead nitrate in distilled water and dilute to; 1 L (1 mL = 0.01036 g lead). 6.7 Copper-EDTA Solution--Mix equivalent amounts of cupric sulfate solution (6.4) and EDTA solution (6.5) and `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 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Jan. 25, 1985. Published December 1985. 1Anmia! Book ofASTM Standards, Vols 05.03 and 11.01. 3 "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 NostJand Co., Inc., New York, NY, and the "United States Pharmacopeia.** 483 DUP050297003 # D 4450 store in a dropping bottle. The cupric sulfate EDTA equiva lence may be determined as follows: 6.7.1 Pipet 10 ml . ofcupric sulfate into a beaker, and add concentrated ammonium hydroxide (6.1) dropwise until the precipitate that forms just redissolves. Dilute to 200 mL with water, add two Murexide indicator tablets, crush with a stirring rod to dissolve, and titrate immediately with EDTA to purple. 6.8 Pan Indicator [l-(2-pyridylazo)-2-naphthol]--Dis solve 0.1 g in 100 mL of ethanol. 6.9 Murexide Indicator Tablets--Ammonium salt of purpuric acid. 6.10 Nitric acid (sp gr 1.42)--Concentrated nitric acid (HNOj). 7. Procedure 7.1 Weigh accurately 0.2 g of pigment and transfer to a 400-mL beaker. Add 5 mL of nitric acid (6.10) and 50 mL of water and boil gently for 10 min. Cool, and add ammonium hydroxide (6.1) until the pH of the solution is from 5 to 5.5 (as indicated by pH paper). Add 25 mL of acid ammonium acetate (6.3), boil 5 min, dilute to 200 mL with water, heat to boiling, add 4 drops of copper-EDTA (6.7) and 12 drops of PAN (6.8), and titrate while hot with standard EDTA to a clear yellow. I 8. Calculation 8.1 Calculate the percent zinc oxide, A, as follows: A=LxMx 0.08137 X 100/5 where: 1L -- EDTA required for titration,mL, ]M = molarity of EDTA solution, !S - specimen, g, and | 0.8137 = milliequivalent weight of zinc oxide. (2) I TOTAL PHOSPHORUS AS PHOSPHOROUS; ACID jj || 9. Reagents I , 9.1 Standard Phosphorus Solution--Dissolve 0.9156 g of ) secondary sodium phosphate (Na2HP04) in about 200 mL j ofwater. Add 20 mL of nitric acid (sp gr 1.42), dilute to 1 L, j and mix. 1 mL = 0.0002 g P. ! 9.2 Ammonium Vanadate Solution--Dissolve 2.5 g of | ammonium vanadate (NH4V03) in 500 mL of hot water, ! When solution is complete, add 10 mL nitric acid (sp gr 1.42), cool, dilute to 1 L, and mix, P 9.3 Ammonium Molybdate Solution--Dissolve 100 g of f ammonium molybdate (NH4)sMo7024 4HzO in 800 mL. of ! water and dilute to 1 L. Filter before use. 1 9.4 Bromine, reagent grade. > 9.5 Bromine Water, distilled water saturated with bro| mine. f 9.6 Nitric Acid (sp gr 1.42), concentrated nitric acid I (HN03). I 9.7 Nitric Acid (2:3)--Dilute 200 mL of nitric acid (sp gr I 1.42) to 500 mL with water. || 10. Apparatus i 10.1 Photoelectric Colorimeter, either a single- or doubleU beam spectrophotometer with a wavelength capability of 465 1 pm. 10.2 Volumetric Flasks, 100-mL. 10.3 Tubes, 10-mm or 20-mm. 10.4 Filter Paper, medium texture. 11. Calibration Curve 11.1 Transfer from a pipet 0.0, 1.0, 3.0, 7.0, 10.0, 15.0, and 20.0-mL aliquots of standard phosphorus solution (9.1) to a 100-mL volumetric flask. To each flask add 10 mL of nitric add (9.7), 10 mL of ammonium vanadate (9.2), and 10 mL of ammonium molybdate (9.3), dilute to the mark, and mix. Allow solutions to stand 20 min and transfer to a 20-mm tube. Read the absorbance ofthe solution at 465 pm. Construct a calibration curve for phosphorus by plotting the absorbance versus milligrams of phosphorus in 100 mL of solution for each standard solution. 12. Procedure 12.1 Weigh accurately 0.2 g of pigment and transfer to a 150-mL beaker. Add 25 mL of bromine water (9.5), 10 mL nitric add (9.6), and 0.5 mL bromine (9.4), and mix the solution. Allow to stand in a warm place for about Vi h, and then gently boil off the bromine until the solution is clear. 12.2 Cool the solution and transfer to a 100-mL volu metric flask. Make to the mark with water and mix. 12.3 Pipet 10 mL of the solution into a 100-mL volu metric flask and add 10 mL nitric acid (9.7), 10 mL of ammonium vanadate (9.2), and 10 mL of filtered ammo nium molybdate (9.3). 12.4 Dilute the sample td the mark, mix, and allow to stand for 20 min, and transfer to a 20-mm tqhe. 12.5 Read the absorbance of the sample at 465 pm and from the calibration curve, read the numberof milligrams of phosphorus (n the test solution. 12.6 Run a blank with the sample. 13. Calculation 13.1 Calculate the percent phosphorus add, C, as follows: ; C = A -BX 2.646/SX 10 (3) where: --- _ . .... A = phosphorus in test solution, mg, ~ B , = phosphorus in reagent blank, mg, S = specimen in aliquot, g and 2.646 = gravimetric factor to convert phosphorus to phosphorous acid. 14. Precision4 14.1 In an interlaboratory study of this test method, in which two samples containing 18.5 to 19.0 % H3P03 and 77.6 to 78.0 % ZnO were analyzed by one operator in each of four laboratories for H3P03 and five laboratories for ZnO, the within-laboratory and between-laboratories pooled standard deviations, after discarding one day's results from one laboratory for both samples of ZnO (see Table 1). Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 14.1.1 Repeatability--Two results, each the mean of two 4 Supporting data are available from ASTM Headquarters. Request RR:DO1.1048. DU P050297004 i TABLE 1 Standard Deviation Withln-laboratory Between-laboratory _______________Sw__________ DF_____________ Sb__________ OF H3P03 0.196 8 0.515 T" ZnO 0.193 S 0.42 8 D 4450 14.1.2 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 1.78 % absolute for H3P03 and 1.37 % absolute for ZnO at the same contents as in 14.1.1. s, obtained by the same operator should be considered pect ifthey differ by more than 0.65 % absolute at H3P03 ntents of 18 to 20 % and more than 0.63 % absolute at O contents of 75 to 80 %. 15. Keywords 15.1 phosphorus acid; pigment analysis; zinc; zinc hy droxy phosphate; zinc oxide The American Society tor Testing and Materials takes no position respecting the validity ofany patent rights assorted 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, mid 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 ter revision ot this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careiul 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. 485 DUP050297005 Designation: D 4462 - 85 (Reapproved 1989) Standard Specification fdr Zinc Hydroxy Phosphite Pigment1 This standard is issued under the fixed designation D 4462; 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 specification covers a zinc hydroxy phosphite pigment havitig the general formula ZnHP03-[ZnO2Zn(OH)2). 2. Referenced Documents 2.1 ASTM Standards: D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments3 D281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out3 D4450 Test Method for Analysis of Zinc Hydroxy Phosphite Pigment3 3. Composition and Properties 3.1 The pigment shall consist of zinc hydroxy phosphite and shall conform to the requirements in Table 1. 3.2 The mass color of the dry pigment is white. The shade and tinting strength, when specified, shall be within mutually agreed upon limits of a reference sample acceptable by the purchaser and the seller as tested in an agreed test procedure. 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DOI.31 on Pigment Specifications. Current edition approved July 16, 1985. Published October 1985. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. 4. Sampling 4.1 Two samples shall be taken at random from different packages from each lot, batch, day's pack, or other unit of production in a shipment. When no markings distinguishing between units of production appear, samples shall be taken from different packages, in the ratio of two samples for each 10 000 lb (5000 kg), except that for shipments of less than 10 000 lb two sample^ shall be taken: At the option of the purchaser, the samples may be tested separately or after blending in equal quantities the samples from the same production unit to form a composite sample. 5. Test Methods 5.1 Tests shall be conducted in accordance with the following ASTM test methods. Test procedures not covered by ASTM test methods shall be mutually agreed upon between the purchaser and the seller. 5.2 Chemical Analysis--Test Method D 4450. 5.3 Moisture Loss--Determine the hygroscopic moisture loss by Method A of Test Methods D 280. 5.4 Oil Absorption--Test Method D 28L 5.5 Sieve Residue--Determine the residue on a No. 325 sieve in accordance with the Procedure for Insoluble Dry Pigments of Test Methods D 185. TABLE 1 Requirements for Zinc Hydroxy Phosphite Pigment Min Max Zinc (as ZnO), % Phosphorus (as HaPOa), 55 Moisture, % Oil absorption, lb/100 lb pigment, % Residue, No. 325 sieve. 56 74.7 79.7 18.5 20.1 1.25 15 - 22 1.0 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 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 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 will receive carehA 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, 7976 Race St.. Philadelphia, PA 19103. 486 DUP050297006 Designation: D 4487 - 90 Standard Test Methods for Analysis of Calcium Borosilicate1 This standard is issued under the fixed designation D 4487; 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. Scope 1.1 These test methods cover the analysis of the pigment Ifnmereially known as calcium borosilicate. 1.2 The test methods appear in the following order: Test Methods Sections , licon Dioxide (SiOJ........................................... ............... - 6 to 9 $>n Oxide (Fe2Oj)........................................... ................. . 10 to 13 iron Trioxide (B2O2) ................................................. 17 to 20 tlcium Oxide (CaO)...... ....................................... ....................... 21 to 23 Moisture and Volatile Matter............................................................... 24 jVater of Hydration....................................................................... 25 to 26 ^oarse Particles............................................................ 01 Absorption ..........................................i'....................... ........... 28 1.3 Individual specimens may be used for the direct fdeterminations of Si02, fi203^ and CaO. Si02 and Fe203 Ijshould be removed before the determination ofthe B203 and H 1.4 This standard does not purport to address the safety ^problems associated with its use. It is the responsibility ofthe Iuser of this standard to establish appropriate safety and . health practices and determine the applicability ofregulatory I {imitations prior to use. i 2. Referenced Documents 2.1 ASTM Standards: D 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints12 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments3 , D 281 Test Method for Oil Absorption of Pigments by Spatula Rub-Out3 D1193 Specification for. Reagent Water4 3- Significance and Use 3.1 These test , methods compile in one place, recom mended procedures for analysis of the pigment known commercially as calcium borosilicate. This pigment is used extensively in paints and the composition is important to the user and producer.. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be 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 D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990. Originally published as D 4487 - 85. Last previous edition D 4487 - 85- 2 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 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 ate 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 II of Specification D 1193. 4.3 2C7 oncentration ofAdds and Ammonium Hydroxide-- When acids and ammonium hydroxide are specified by name or chemical formula only, it should be understood that concentrated reagents of the following specific gravity are intended: Hydrochloric acid (HQ) Nitric acid, (HNOj) Sulfuric acid (H2SO4) Ammonium hydroxide (NH4OH) 1.19 1.42 1.84 0.90 5. Preparation of Samples 5.1 Thoroughly mix and comminute the sample before taking portions for analysis. > SILICON DIOXIDE ' 6. Apparatus 6.1 Evaporating Casserole, 250-mL capacity. 6.2 HotPlate. 6.3 Porcelain Filtering Cmpible, medium porosity, 30-mL capacity, , ... ..V n ' 6.4 .Drying Oven, maintained at 100 it .5C. 6.5 Muffle Furnace. 7. Reagents 7.1 Hydrochloric Acid {1+1). 7.2 Hydrochloric Acid (1+19). 7.3 Hydrochloric Acid (1+99). 8. Procedure 8.1 Introduce a 1-g specimen, weighed to the nearest 0.1 mg into an evaporating casserole. Add 50 mL of HC1 (1+1) and thoroughly mix. 8.2 Place the casserole on a hot plate and evaporate carefully to dryness, 8.3 Place the casserole in the oven at 100'C for 2 h. Do 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Cbem. Sop., 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." 487 DUP0502970Q7 D 4487 not allow the oven temperature to exceed 105CC at any time. Remove the casserole and allow to cool for 10 min. 8.4 Completely wet the residue with 25 mL of HC1 (1+1) and cover the casserole with a watch glass. Warm just to boiling on a hot plate and maintain for 10 min. 8.5 Add 25 mL of water, free any material from the sides of the casserole with a stirring rod, and immediately filter through a tared porcelain crucible of medium porosity. 8.6 Wash the residue with two 5-mL portions of hot HCl (1+19), one 5-mL portion of hot HCI (1+99), and finally with two 5-mL portions of hot water. Save the combined filtrates for the determination of iron oxide (Sections 10 to 12). 8.7 Place the crucible containing the precipitate in the muffle furnace from 600 to 800C and heat to constant weight (4 mg). Cool in a desiccator and weigh. 9. Calculation 9.1 Calculate the percent of Si02, A, as follows: A = R/Sy (100) where: R = weight of residue, g, and -- weight of original specimen, g. (i) IRON OXIDE 10. Apparatus 10.1 Volumetric Flasks, 250-mL and 1000-mL capacity. 10.2 Buret, 10-mL capacity. 11. Reagents 11.1 Potassium lodate (0.01878 N)--Dry 1.0 g of KI03 at 120C for 2 h in a drying oven. After cooling, weigh 0.6700 g and dissolve it in 100 mL of water. Dilute the solution to 1 L in a volumetric flask. 1 mL = 0.001500 g Fe203. 11.2 Potassium Iodide (KI)--lodate free. 11.3 Starch Indicator Solution--Make a homogeneous paste of 10 g of soluble starch in cold water. Add to this 1 L of boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L) may be added to preserve the indicator. Iflong storage is required, the solution should be kept in a refrigerator,at 4 to 10C. Prepare fresh indicator when the end point of the titration from blue to colorless fails to be sharp. 11.4 Sulfuric acid (H2SO,,) (1+18). 11.5 Sodium Thiosulfate, Standard Solution (0.025 N)-- Dissolve 1.5 g of sodium thiosulfate (Na2S203-5H20) in 50 mL of water and dilute to 250 mL. Standardize as follows: Pipet 10 mL of the KJ03 solution into each of three 150-mL beakers. Dilute each to 100 mL with water, add 2 g ofKI and 5 mL of H2S04 (1+18), and dissolve the KI with stirring. Titrate the liberated iodine with 0.025 N Na2S203 solution until the color of the solution becomes pale yellow. Add 2 mL of starch indicator and continue the titration dropwise until the color changes from blue to colorless. / = 1 mL Na2S203 = 0.01500/ Vl g Fe203 (2) where: I = iron oxide equivalent of Na2S203 solution, K, = Na2S203 required for titrations, mean, mL, and 0.01500 =(10.00 mL KIQ3) x (0.001500 g Fe203/mL 3 12. Procedure 12.1 Dilute the solution obtained from the procedure in 7.6 to 100 mL with water. Add 10 mL of HCl and 5 g K], Dissolve the KI with stirring. 12.2 Titrate with 0.025 N Na2S203 solution until the color becomes a pale yellow. Add 2 mL of starch indicator ! solution and continue the titration until the color changes from blue to colorless. 13. Calculation 13.1 Calculate the percent of iron oxide, D, as follows: D=(lx K2)/5, (100) (3) where: V2 = Na2S203 solution required for titration, mL, and Si = weight of original specimen, g. SOLUTION OF PIGMENT FOR THE DETERMINATION OF BORON TRIOXIDE AND CALCIUM OXIDE 14. Apparatus 14.1 Boiling Flask--300-mL capacity with ground glass connection. 14.2 Buchner Funnel, 56-mm diameter. 14.3 Filter Paper, 55-mm diameter.6 14.4 Filter Flask, 250-mL capacity. 14.5 Hot Plate/Stirrer. 14.6 pH Meter. 14.7 Reflux Condenser, with ground glass connection, water cooled. 14.8 Sintered Glass Crucible, 50-mL capacity, medium porosity. 14.9 Volumetric Flask, 250-mL capacity. 15. Reagents 15.1 Hydrochloric Acid (1+1). 15.2 Hydrochloric Acid {1+25). 15.3 Nitric Acid {1+1). - 15.4 Potassium Hydroxide, pellets.. 15.5 Potassium Hydroxide Solution, 28 g/L. __ 16. Procedure .... 16.1 Introduce 2.5 g of sample, weighed to 0.1 mg, into the 300-mL boiling flask. 16.2 Add 50 mL of HCl (1+1) and 2 drops HN03 (1+1). Place a magnetic stirring bar in the flask, connect the reflux condenser to the flask, and reflux for 1 h on the hotplate with constant stirring. 16.3 Remove the hotplate and place an ice bath under the flask. After the solution has cooled, wash -the condenser down with a small amount of water (10 mL) and remove from the flask. 16.4 Filter the mixture through a Buchner funnel equipped with filter paper6 into a 250-mL filter flask. Wash the boiling flask with several 5-mL portions of hot water to transfer all the material to the filter. 16.5 Cool the filtrate in an ice bath to a temperature of approximately 10C, add 15 g of KOH pellets and swirl to 6 Whatman No. 50 Filter Paper, available from Whatman, Inc., or equivalent, has been found satisfactory for this purpose. 488 DUP050297008 # D 4487 B dissolve them. Using the pH meter, neutralize the solution to If a pH from 6.0 to 7.0, adding first KOH pellets and finally 1 either KOH (28 g/L) or HC1 (1+25). Be careful not to add H' appreciably to the volume of the solution, nor to exceed a pH of 7.0. li 16.6 After neutralizing the solution, warm it gently on a H hot plate to coagulate "the iron precipitate. Filter off the iron jli precipitate with a medium-porosity sintered glass filter into a Bj clean 250-mL filter flask. K 16.7 Replace the sintered glass crucible oh the original E filter flask and add 10 mL of water. Dissolve the iron E precipitate by the dropwise addition of HC1 (1+1) and If constant stirring. Filter with suction and wash the crucible 1 with two 5-mL portions of hot water. Swirl the acidic I solution around in the flask to dissolve any iron precipitate I adhering to the sides of the flask. R 16.8 Repeat the neutralization step (16.5) and filter the I solution through the sintered glass crucible into the flask f containing the first filtrate (16.7). I 16.9 Wash the flask used in the neutralization with two I 5-mL portions of water, and then wash the precipitate in the B crucible. | 16.10 Transfer the filtrate quantitatively to a 250-mL I volumetric flask and dilute to volume. Use this filtrate for I the determination of boron trioxide*(Sections 17 to 19) and I calcium oxide (Sections 20 to 22). I BORON TRIOXIDE 17. Apparatus 17.1 pH Meter.. 17.2 Buret, 25-fnL capacity. 17.3 Volumetric Flasks, 1000-mL and 100-mL capacity. 17.4 Drying Oven, maintained at 105 2C. 18 18. Reagents ; 18.1 Hydrochloric Acid (1+19). 18.2 Mannitol. 18.3 Phenolphthalein Indicator 'Solution--Dissolve 0.10 g phenolphthalein in 50 mL of ethyl alcohol. Dilute to 100 mL with water, 18.4 Thymol Blue Indicator Solution--Dissolve 0.1 g of thymol blue in 50 mL of0.01 N sodium hydroxide:'Dilute to 100 mL with ethyl alcohol. 18.5 Mixed Indicator Solution--Mix 25 mL of thymol blue indicator solution with 75 mL of phenolphthalein indicator solution. Adjust the pH froin 6.0 to 7.0 on a pH meter with either HQ (1+19) or NaOH (0.1 N). 18.6 Potassium Hydrogen Phthalate (KHP)--Acidimetric standard. 18.7 Sodium Hydroxide, Standard Solution (0.1 N)-- Dissolve 4.0 g of NaOH pellets in 100 mL of water and dilute to 1 L in a volumetric flask. Standardize as follows: Dry 2.0 g of KHP for 2 h at 105C in the oven and cool. Weigh 1.6420 g and dissolve in 50 mL of water. Transfer quantita tively to a 100-mL volumetric flask and dilute to volume with water (1 mL = 0.002800 g B203). Pipet 25 mL of the KHP solution into each of three 150-mL beakers. Add 3 drops of phenolphthalein indicator and titrate with 0.1 N NaOH until the color changes from colorless to red. B = I mL NaOH = 0.07000/^ g B203 (4) where: B = B203 equivalent of NaOH solution, V3 = NaOH used in standardization titrations, mean, mL, and 0.07000 = (25.00 mL KHP) x (0.002800 g B203/mL KHP). 19. Procedure 19.1 Pipet 50 mL of the filtrate from the procedure in 16.10, which has been diluted to volume, into each of two 150-mL beakers. 19.2 With the pH meter, adjust the pH of each solution to 6.0 using either HC1 (1+19) or 0.1 N NaOH. Add 10 g of mannitol and dilute to 100 mL with water. 19.3 Add 1 mL of mixed indicator solution and titrate with 0.1 N NaOH. The end point is when the color changes from yellow to dark violet. 20. Calculation 20.1 Calculate the percent ofboron trioxide, E, as follows: E=Bx VJS2 (500) ' (5) where: R, = NaOH used in titrations, mean, mL, and S2 = weight of original specimen, g. CALCIUM OXIDE 21. Apparatus 21.1 Buret, 25-mL capacity. 21.2 Volumetric Flasks, 500-mL and 1000-mL capacity. 21.3 Reagents. 21.4 Ammonium Hydroxide (1+4). 21.5 Buffer Solution--Dissolve 33.75 g of ammonium chloride in 285 mL of NH4OH, add 5 mL of concentrated ammonium sulfide, and dilute to 500 mL with water. 21.6 Calcium Standard--Dry 7 g of calcium carbonate (CaC03) at 105C for 2 h. Weigh 6.2461 g of the dried GaC03 into a 500-mL flask. Slowly add HQ (1+1) until all the CaC03 has dissolved. Add 200 mL of water and boil for a few minutes to expel C02. Cool and adjust the pH from 5 to 6 by adding NH40H (1+4) or HC1 (1+1): Transfer solution to a 1000-mL volumetric flask and dilute to volume. 1 mL = 0.003500 g CaO. - 21.7 Sodium Carbonate (0.2 %) *--Dissolve 2 g Na2C03 in water and dilute to 1 L, " 21.8 Sodium Carbonate (10 g/L)---Dissolve 10 g Na^C^ in water and dilute to 1 L. ' 21.9 Eriochrome Black T Indicator Solution--Dissolve 1.0 g of Eriochrome Black T in 30 mL of 0,2 % sodium carbonate (Na2C03) solution. Dilute to 100 mL with isopropanol. Adjust the pH to 9.0 with Na2C03 solution (10 g/L). Indicator shelf life: 2 months. 21.10 EDTA, Standard Solution (0.17 N)--Weigh 63.3 g of disodium ethyJenediamine tetraacetate (EDTA) and 0.1 g magnesium chloride (MgQ2), and dissolve in 500 mL of NaOH (20 g/L) solution and dilute to 1 L with water. Standardize as follows: Pipet 50 mL of calcium standard into each of three 150-mL beakers. Add 15 mL of buffer solution and 3 to 4 drops of indicator solution to each beaker. Titrate immediately with EDTA solution (0.17 N) until the color changes from red to a definite blue. 489 DUP050297009 D 4487 C = 1 mL EDTA = 0.1750/ K5 g CaO (6) where: C = CaO equivalent of EDTA solution, Vs EDTA required for titrations, mean, mL, and 0.1750 = (50 mL Ca Standard) x (0.003500 g CaO/mL). 22. Procedure 22.1 Pipet 50 mL of the filtrate from the procedure in 15.10 into each of two 150-mL beakers. Add 25 mL ofbuffer and 3 to 4 drops of indicator solution to each beaker. 22.2 Immediately titrate with EDTA until the color changes from red to a definite blue. 23. Calculation 23.1 Calculate the percentof calcium oxide, F, as follows: F = C X V6/S2 (500) (7) where: V6 - EDTA required for titrations, mean, mL, and S2 - weight of original specimen, g. MOISTURE AND OTHER VOLATILE MATTER 24. Procedure 24.1 Determine moisture and other volatile matter in accordance with Method A of Test Methods D 280. WATER OF HYDRATION 25. Apparatus 25.1 Casserole. 25.2 Muffle Furnace, preferably electrically heated main tained at a temperature of 450 10C. 26. Procedure ; 26.1 Place the casserole in the muffle furnace and heat at 450'C for 30 min. Remove to a desiccator, cool, and weigh to the nearest 0.1 mg. 26.2 Remove the weighing bottle containing approxi mately 3 to 5 g of previously dried pigment (Section 24) from the desiccator; Transfer most of the pigment to the casserole and weigh to 0.1 mg. Subtract the weight ofthe dish from the total weight to obtain the specimen weight. 26.3 Place the dish containing the specimen in the muffle furnace heated at a temperature of about 250C and raise the temperature to 450C. Maintain temperature at 45Q"C for 1 h. Remove the dish from the furnace to the desiccator and allow to cool to room temperature. Weigh to the nearest 0.1 mg. Bleat again at 450C for 15 min to check the loss i weight. The two weights should not differ-by more than % mg 26.4 Calculate the percent water of hydration onthe basis of dried pigment to 0.01 %. COARSE PARTICLES 27. Procedure 27.1 Determine the percent of coarse particles in the pigment in accordance with Test Methods D 185. 28. Oil Absorption ! 28.1 Detennine the oil absorption of the pigment in accordance with Test Method D 281. , 29. Precision7 .. 29.1 In an interlaboratory study of this test method in which operators at four locations made single, analyses on two days of two pigments containing 32.9 and 39.3 % Si02, 16.5 . and 10.6 % B2Q3 and 40.7 and 44.1 % CaO, the within-laboratory pooled standard deviations were found to be 0:27 % for Si02, 0.13 % for B203, and 0.31 % for CaO, each, with 8 df, and the equivalent between-laboratories standard deviations 0.346 %, 0.255 % and 0.495 %, with 6 df each. Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 29.1.1 Repeatability--Two results, each single determina tions, obtained by the same operator on different days should be considered suspect if they differ in percent absolute by more than 0.88 % Si02, 0.48 % B2O3, _nnd l.01 % CaO at levels of 32 to 40 % Si02, 10.5:to 16.5 % B203 and 40 to 45% CaO. 29.1.2 Reproducibility--Two results, each single determi nations, obtained by operators in different laboratories should be considered suspect .if. they,.differ in percent absolute by more than 1.20 % ' Si02, 0.88 % .B203, and 1.72 % CaO at the same.leyels as in 29.1.1. 30. Keywords 30.1 boron-trioxide; calcium borosilicate pigment anal ysis; calcium oxide; iron oxide; silicon dioxide; water of hydration 7 Supporting data are available, from ASTM Headquarters. Request RR: D01-1047. 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 Ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthisstandard 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 net received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 490 DUP050297010 Designation: D 4613 - 86 (Reapproved 1990),ei Standard Test Method for Measuring Apparent pH of Water Insoluble Phenol-Formaldehyde Resins1 ^ This standard is issued under the fixed designation' D46I3; 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 reapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. fl No t e--Keywords were added editorially in September 1990. fScope 1.1 This test method covers the measurement of the rent pH of a water extract of an acetone solution of `ter insoluble phenol-formaldehyde resin. f.2 This standard does not purport to address all of the retyproblems associated with its use. It is the responsibility the user ofthis standard to establish appropriate safety and tlth practices and determine the applicability ofregulatory mitations prior to use. . Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water12 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode3 . Summary of Test Method 3.1 Aqueous test solutions are generally used in deterinining pH. In this test method the resin is dissolved in etone, water is added, and the apparent pH is measured dth a pH meter. 44. Significance and Use 4.1 The hydrogen ion concentration (pH) is of critical importance due to its effect on the performance of the end product The pH is widely used in quality control and process control. 5. Apparatus 5.1 pH Meter, complying with Test Method E 70. 5.2 Beaker, 250-mL. 5.3 Balance, accurate to 0,1 g. 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 Water, conforming to Type II of Specification D 1193. 6.3 Acetone, reagent grade. 6.4 pH Standard Solutions--4, 7, 10 for standardization of pH meter. 7. Procedure 7.1 Standardize the pH meter with the 4,7, or 10 standard buffer in the expected testing range. 7.2 Weigh a 10 0.1 g specimen of the resin under test into a 250-mL beaker. 7.3 Add 40 mL of acetone and dissolve the specimen. Add 40 mL of water and stir for 5 min at room temperature. Allow the solution to settle for 1 min. Immerse the electrode^ into the solution (Caution: Keep undissolved resin away from electrode) and record the result. 7.4 Wash the electrode with acetone, followed by, water until clean or until the pH meter retumsjto the standard buffer reading. .. . 8. Report 8.1 Report the pH to 0.1 units. 9. Precision and Bias 9.1 The precision and bias for this test method have not been determined. 10. Keywords 10.1 pH; phenol-formaldehyde resins; water-insoluble 1 This test method is under thejurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.33 on Polymers and Resins. Current edition approved Sept 26, 1986. Published November 1986. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 15.05. 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." 491 DUP050297011 D4613 The American Society lor Testing and Materials takes no position respecting the validity clanypatent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination d the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This stenderd Is subject to revision at any time by the responsible technical committee and must be reviewedevery five years and if not revised, either reapproved or withdrawn. Yourcomments are Invited either for revision ot 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. 492 DUP050297012 t Designation: D 4639 - 86 (Reapproved 1990),'1 Standard Test Method for Volatile Content in Phenolic Resins1 This standard is issued under the fixed designation D 4639; 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.41 41 No t e--Editorial changes were made in August 1990. Scope 1.1 This test method covers the determination of matter i a solid phenolic resin that is volatile at 300F (150Q. 1.2 This standard does not purport to address all of the Isafety problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and Jhedlth practices and determine the applicability ofregulatory ^imitations prior to use. !( ;2. Summary of Test Method 2.1 A specified weight of resin is added to a tared * aluminum dish and weighed. The resin is then heated for 2 h ; in an oven at 300F (150C) and reweighed. 3. Significance and Use 3.1 Volatile material causes problems when phenolic resins and varnishes are heated at temperatures above 300F ( 150*0- Heating a specified weight of resin for 2 h at this temperature indicates the amount of volatile material emitted when molding or curing phenolic resins. 4. Apparatus 4. L Analytical Balance, capable of weighing to 0.1 mg. 4.2 Thermometer, glass, having a range from 1 to 200C and accurate to 1*C. 4.3 Circulating Oven, maintained at 300 3.5F (150 2C). 4.4 Aluminum Drying Dishes, 2V2-in. (63 mm) diameter, 3A-in. (20 mm) depth or equivalent. 4.5 Desiccator. 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 Subcommittee DO 1.33 on Polymers and Resins. Current edition approved Nov. 28, 1986. Published January 1987. 5. Procedure 5.1 Mark two aluminum dishes for identification of each resin being tested and weigh them on the analytical balance to 0.1 mg. Record as w,. 5.2 Weigh a 5-g specimen of resin to 0.1 mg into each aluminum dish. Record total weight as w2. 5.3 Place the dishes in the oven for 2 h at 300*F (150C). 5.4 Remove from oven and immediately place in desic cator until they cool to room temperature. Reweigh imme diately upon removal from the desiccator and record as w3. 6. Calculation 6.1 Calculate the volatile content, V, as follows: V, % = 100 - F*--^ x 100 lw2 - wi where: w, = weight of aluminum dish, g, w2 = weight of aluminum dish and specimen used, g, and w3 = weight of aluminum dish and specimen after 2 h in oven, g. 7. Report 7.1 Report the following information: _.. 7.1.1 Resin identification, time, and temperature. 7.1.2 Percent of volatile matter, or volatile content (av erage of duplicate determinations). 8. Precision and Bias 8.1 The precision and bias for this method have not been determined. (}_ Keywords *. 9.1 phenolic resins; Volatile Content 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 rigtts, 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 cl the responsible technical committee, which you may attend. If you feel (hat 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. 493 DUP050297013 <1 Designation: D 4640 - 86 (Reapproved 1990)1 Standard Test Method for Determining Stroke Cure Time of Thermosetting PhenblFormaldehyde Resins1 This standard is issued under the fixed designation D 4640; 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. " No t e--Keywords were added editorially in September 1990. 1. Scope 1.1 This test method covers the determination of the cure rate at any specified temperature for a thermosetting phenolformaldehyde resin. The time at that temperature required to make a fluid mixture change into a hard immovable mass indicates speed, of cure. 1.2 This standard does not purport to address alt 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. Description of Terms Specific to This Standard 2.1 stroke cure time--the time required for a resin being held at a specified temperature on a hot plate and being stroked with a spatula, to adhere to the hot plate and not to thfe spatula. 3. Summary of Test Method 3.1 This test method employs the use of controlled heat and a thin layer of resin to determine the time in seconds required to change from a fluid stage to a cured immovable stage. 4. Significance and Use ' 4.1 This method is significant as a process control for polymerization time. 4.2 When the cure times are determined at several tem peratures and plotted as time versus temperature, different resins can be compared for curing characteristics. 5. Apparatus 5.1 Electric Hot Cure Plate, with a smooth surface free of 1 This test method is under the jurisdiction of ASTM Committee D-J on Paint and Related Coatings and Materials and is the direct responsibility of Subcoin* mittee DOI.33 on Polymers and Resins. Current edition approved Nov. 28, 1986. Published January 1987. rough spots with adjustable control to hold the temperature within 3.5F,(2G) (Note 1): 5.2 Spatula, 3 by 7/i in. (75 by 10 mm), stainless. 5.3 Stopwatch. ' 5.4 Knife; brass, putty with straight edge. 6. Procedure 6.1 Adjust the hot plate to the desired test temperature. No t e 1--Usual temperatures are 300"F (150"C), 32d`F'(l60`C), and 330*F (165'C). \ 6.2 Place an approximately 0.5-g specimen on the hot plate and spread over an approximately 2-in.2 (130-mm2) area with a clean spatula as quickly as possible. Start the stopwatch immediately upon adding the specimen to the hot plate, then stroke steadily across the specimen in alternating smoothing and patting motions. : 6.3 As the resin approaches the cured stage, it becomes- more viscous and stringy. Stop the stopwatch when the resin on the hot plate and the spatula no longer adhere to each other. Record the elapsed time. 6.4 Remove cured resin from hot plate immediately with the straight edged putty knife. No t e 2--The longer on the hot plate, the harder it is to remove. No t e 3--Test results can be affected by. differences in construction ofhot plates, the stroking and,patting with spatula, and the starting and stopping of the stopwatch. 7. Report___ 7.1 Report the following information: 1 7.1.1 Stroke cure time in seconds; record to the nearest whole number. 7.1.2 Test temperature. 8. Precision and Bias 8.1 No statement is made about either the precision or bias ofthis method for measuring stroke cure since the result merely states whether there is conformance to the criteria for success specified in the procedure. 9. Keywords 9.1 phenol-formaldehyde resins; stroke cure time 494 DUP050297014 # D 4640 The American Society tor Testing and Materials takes no position respecting the validity of any patent 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 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 torrevision ofthis standard or for additional standards andshould 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, 1916flace St., Philadelphia, PA 19103. 495 DUP050297015 <1 Designation: D 4706 - 87 Standard Test Method for Determining Qualitatively Methylol Group in Phenolic Resins1 This standard is issued under the fixed designation D 4706; 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 1.1 This test method covers a procedure to determine qualitatively the presence of methylol group in phenolformaldehyde resins. No t e--The values stated in SI units are to be regarded as standard. 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 This test method of qualitatively determining the presence of methylol groups in a phenol resin uses the reaction of ferric chloride with the methylol group to produce a blue color at room temperature. 3. Significance and Use 3.1 This test method provides a fast and simple method for determining the presence of methylol group for quality control testing. 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 1.33 on Varnish and Resins, Including Shellac. Current edition approved May 29, 1987. Published July 1987. 4. Apparatus 4.1 Test tube, 6 by 1-in. (152 by 25-mm) glass. 4.2 Acetone, reagent grade. 4.3 Ferric chloride, 5 % aqueous solution. 4.4 Balance. 5. Procedure 5.1 Place 0.1 g of the specimen under test in a test tube. 5.2 Add 10 mL of acetone. 5.3 Shake and dissolve specimen. 5.4 Add two drops of 0.5 % ferric chloride solution and swirl. 5.5 Observe color, yellow or blue. 6. Report 6.1 Report the following information: 6.1.1 Yellow equals methylol group absent. 6.1.2 Blue equals methylol group present. 7. Precision and Bias 7.1 Precision and bias do not apply since this is a qualitative test method that is recorded by a color change. 8. Indexing Terms 8.1 This test method is indexed under the following terms: ferric chloride; methylol group content; phenol-formalde hyde (PF) plastics; plastics, general; and resins (subheading phenolic). , 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 validityof 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 tor revision ofthis standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a mooting 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. 496 DUP050297016 Designation: D 4747 - 87 (Reapproved 1991)e1 Standard Test Method for Determining Unreacted Monomer Content of Latexes Using ! Gas-Liquid Chromatography1 : This standard is issued under the fixed designation D 4747; 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 l superscript epsilon () indicates an editorial change since the last revirion or reapproval. i. <l No t e--Keywords were added editorially in July 1991. IH Scope 1.1 This test method covers the determination of free lionomer content of acrylic latexes. Monomers that have fcen successfully determined by this procedure include f-butyl methacrylate, n-butyl acrylate, styrene, and methyl ||ethacrylate. The determination ofother monomers has not :n evaluated, but this test method is believed to be applicable. The established working range ofthis test method p flrom 100 to 1000 pg/g, but there is no reason to believe it prill not work outside ofthis range, provided that appropriate utions and adjustments in specimen size are made. | 1.2 The volatile composition of acrylic latexes is expected change with time and environmental factors. This time lependence of the determination may be seen as an artifi cially large deviation of results, making the method mostly iplicable for in-house quality control, where sampling and Analysis conditions can be better controlled. 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. See Section 7 for `specific hazard statements. |2' Referenced Documents 1 2.1 ASTM Standards: D3980 Practice for Interlaboratory Testing of Paint and Related Materials12 E 260 Practice for Packed Column Gas Chromatography3 J-3. Summary of Test Method 3.1 A suitable aliquot of the latex is internally standard[ ized with isobutyl acrylate, diluted with water, and then i injected into a gas chromatographic column containing a I packing material coated with a stationary phase that separates the internal standard and monomers in question from (each other and from other volatile compounds. 4. Significance and Use 4.1 Excessive amounts of unreacted monomer may cause 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 I.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Nov. 27, 1987. Published January 1988. 1 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 14.01. concerns relating to toxicity and odor. This test method is designed to measure the unreacted monomer content of latexes. The results may be used to monitor the extent of polymerization during manufacture, as well as to establish maximum unreacted monomer content for regulatory pur poses. - 5. Apparatus 5.1 Gas Chromatograph, any gas-liquid chromatographic instrument having a flame ionization detector and linear temperature programming. An injection port using re- placable glass liners to facilitate periodic removal of accumu lated residues is recommended. 5.2 Column, 2 by 2-mm inside diameter glass or 6 ft by Vi-in. outside diameter steel tubing, packed with 10% by weight of a 2-nitroterephthalic acid derivative of Carbowax 20M on 100/120 mesh add washed, silane treated diato- maceous earth.4 A column of equivalent or superior perfor mance may also be used. 5.3 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 level of 0.03 % of full scale (see Practice E 260). ~ 5.4 Liquid Charging Devices, microsyringe, 10-|iL ca- padty or an automatic liquid sampling device. 5.5 Dropper Pipets, glass, disposable. .__ 5.6 Vials, approximately 7-mL capadty, with caps. Open " top screw cap vials fitted with polytetrafluoroethylene/ silicone septa are preferred. 5.7 Autosampler Vials, 2-mL capacity (optional). 5.8 Analytical Balance, accurate to 0.1 mg. 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 Columns prepared from the following stationary phases and supports "have been found suitable for this purpose: Stationary Phases > SP-1000--Supelco, Inc., Beliefoute, PA AT-1000--Ailtech Assoc., Deerfield, IL 0V-351--Ohio Valley Chem. Co., Marietta, OH FFAP--Various manufacturers Supports Chromosorb W-HP--Manville Corp., Denver, CO Gas Chrom QII--Alltech Assoc., Deerfield, IL Supelcoport--Supelco, Inc., Bellefonte, PA Anakrom Q--Analabs, North Haven, CT 497 DUP050297017 # D 4747 TABLE 1 Instrument Conditions Detector Airflow Hydrogen flow Column (suggested) Canter gas, flow rate Temperatures: flame ionization 240 tnL/min 30 mL/min 2 by 2 mm inside diameter glass, packed with 10 % . of-a 2-nitroterphtriallc add denvative of Carbo- wax 20M on 100/120 mesh acid washed, silanetreated diatomaceous earth. Helium, 30 mL/min Injection port Detector block Column 250C 2S0C Initial Hold time Program rate Final " Final hold Injection volume 4 min 2Q0C, or higher as needed (see 8.1) 10 min, or as needed . 2j iL 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. ` 6:2 Carrier Gas, helium of 99.995 % or higher purity. High purity nitrogen may also be tised. * 6.3 Acetone, reagent grade. ''' ' ^ i;. 6.4 Isobutyl Acrylate (intemalstandard), 99+'-%' pure. No t e f--(sobutyL acrylate was, found to be a suitable internal standard, but any other monbiheir' not found in the sample maj be substituted. The internal standard'chosen should yield a clear Chromato graphic separation; and Should be free of interferences. :> 6.5 Monomers ofInterest, 99+ % pure. 7. Hazards < 7.1 Acrylic and methacrylic monomers are Considered hazardous. Precautions shbuld be taken to avoid inhalation and skin or eye contact with these chemicals, All sample preparations should be done in a well-ventilated area; such as a fume hood. .' r 8. Preparation of Apparatus 8, i Cohanri Conditioning--Mach, one end ofthi'b column to the inlet side of the instrument leaving the exit end of the column discotthectejd. This prevents the cdhtaibiiiatiQn of the detector due to column blbed. Set the helium flow rate at 30 mL/min and purge the column at ambient temperature for 30 min. Program the column oven from 50 to 220C at 2C/min and maintain at 220C overnight. In no case should the temperature of the column be allowed to exceed 275*C 8.2 After cbnditionihg, connect the exit end of the column to the detector and establish the operating condi tions required to give the desired separation (see Table 1). Allow sufficient time for the instrument to reach equilibrium as indicated by a stable baseline. Control the detector temperature so that is is constant to within 1C without 5"Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagent? not listed by the American Chemical Society, see "Reagent Chemicals and Standards*?1 by Joseph Rosin, D. Van Nostrand Co.; Inc., New York, NYr and the "United States Pharmacopeia." '. 1 thermostat cycling which causes an uneven baseline. Adjust the carrier gas flow rate to a constant value. 9. Calibration '' " 9.1 Determine the retention ofeadh component expected to be present by injecting small amounts either separately or in known mixtures. Retention times shoUld be determined each day the method is used. ;9.2 Standardization--Determine in duplicate the relative response of the monomers of interest to the isobutyl acrylate internal standard as follows: 9.2.1 Weigh to 0.1 mg about 0.05 g of isobutyl acrylate and each monomer of interest into a vial (5.6). Weigh approximately 5 g of acetone into the vial and mix well. 9.2.2 Weigh approximately 0.05 g of the solution (9.2.1) into another vial, add approximately 5 g qf acetone and ,mix welL ,9.2.3 Inject a 1-jiL aliquot of the solution firom 9.2.2 opto, the, column and recordthechromatogram. The elution order for acetone, and each of the monomers using the conditions given in Table 1 is shown in Fig, 1. 9.2.4 Measure the peak areas, of the .individual compo nents and calculate the relative response factor, RF, for the monomers of interest as follows: , : i. : RF-(W, X AS)/(WSX A,), 1 where: , ; . . itF = relative response factor for each monomer, , Av = peak area produced by the mqnomei; , As =? peak area produced by the intemal standard,, Wt = weight of monomer used for,cafibration (9,2.1), and ," Wz -- weight of internal, standard (9.2,1), 10. Procedure 10. i If the composition of the latex is hot kndwn or if the approximate leiel of mOhomers1 in the latex is not known, a, preliminary analysis must be performed bydiluting'approx-' ' (7 Vej 0.63 t .ri (raVHYL !; -- V , ,Te'! 3. 18 (ISOBUTYL ACRYLATE)' 4.55JW-BUTYJ. ACRYLATE) 5.79 (N-BUTYl METHACRYLATE) 6.S0 (STYRENE) ,v U. .8.103 ' 8.72 STOP i; HP, -RUN AREA Si 26 RT AREA AREA Tc 3.8 0.94 1.36 1.71 "2.$e 3.19 4.S5 5.79 6.50 3.03 i.3.72 .9.50 9.77 4910000 33690 16450 1947000 17190 3542000 2S65000 3780000 3625000 1189 3328 1478 11530 24.005 0. 165 0.030 9.519 . 0.084 17.317 12.548 18.431 17.723 0.005 0.01-5 0.00? 0.056 OIL FACTOR: 1.0000 E+ 0 FIG. 1 Typical Chromatogram 498 DUP050297018 A-D 4747 tely 0.5 g of latex with approximately 5 g of water and -ting a 2-p.L aliquot into the ehromatographicJcolumn. j the same conditions as for standardization, record the aks of all components at attentuation settings that provide rimum peak heights. [Use the relative retendon times to ntify the monomers! present. If the specimen has a aponent ehitihg at the same retention time as isobutyl ylate, choose a different ihternal standard (Note'0. , ` j 10.2 Prepare a dilute solution of the internal standard by eighing to 0.1 mg about 0.05 g of isobutyl acrylate and 5 g `acetone into a septum vial. Take care to minimize losses e to evaporation. Prepare this solution fresh each day the ethod is used. [10.3 Weigh to 0.1 mg an appropriate amount of sample to a septum vial using Table 2 as a guide to specimen size. ) weigh to 0.1 mg 50 mg ofthe dilute solution prepared in .2 into the vial. Add about 3 to 5 g of water or acetone. ke the vials on a wrist action shaker or other suitable "et vice for 15 min. j No t e 2--The viscosity of a number of latexes increases upon the |dition of an organic solvent. If acetone (or another organic solvent) is und to be compatible with the specimen, it should be used as the "uent instead of water. It should be kept in mind that some organic 1vents may interfere with the chromatographic separation. 10.4 Inject 2 pL of the prepared solution (10.3) into the hromatographic column and record the chromatogram Jising the conditions as in 10.1. Measure the peak areas (Note ) of the internal standard and relevant monomers, multilying each area by the appropriate factor to express the peak eas on a common basis. No t e 3--Peak areas may be determined by any method that meets the precision requirements of Section 12. Electronic integration is ommended for best results. 10.5 Repeat procedure in 10.3 through 10.4 and calculate the mean values. 11. Calculations 11.1 The weight of the internal standard present in the diluted specimen (10.3) is calculated as follows: wA = {wsjW6Wi where: TABLE 2 Suggested Dilutions No t e--This table shall be used only as a guide. If the monomer concentrations are outside the range given, appropriate adjustments must be made in terms of specimen size, dilution and amount of internal standard added. Level of Free Monomer Expected, PS/9 250 500 750 1000 Specimen Size, S 2 1 0.7 0.5 Diluent. S 3 4 4.3 4.5 W4 ~ weight of internal standard in diluted specimen in 10.3, . ,W5 - weight ofinternal standard used to prepare solution in 10 2 W6 = weight of acetone plus weight qf internal standard " userfto prepare solution in 10.2, and W-j =;weight ofthe dilute internal standard solution (10.2) `addedtothe specimen ,in 10.3, 11.2 Calculate the concentration, C, of each monomer present in the latex sample from the results obtained from 10.5 as follows: C = [<rf3 xW4x RF}/(tVs x A4)] x 10* where: C = concentration of free monomer, pg/g, A3 = peak area produced by the monomer, A4 = peak area produced by the internal standard, RF = relative response factor for each monomer (9.2.4), W4 -- weight of internal standard (11.1), and fVs = specimen weight (10.3). 12. Precision and Bias6 12.1 Precision--In an interlaboratory study of the method by five laboratories using four samples, the withinlaboratoiy coefficient of variation was found to be 16.8 % relative at 11 degrees of freedom and the between-laboratories coefficient of variation was 18.1 % relative at 8 degrees offreedom. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level (see Practice D 3980 and Note 4). 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 52 % 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 59 % relative. No t e 4--Variation in results may be due to the changing composi- ~ tion of the samples used for the study. This precision statement should be used only as a guide, since it represents only'the.magnitude of variation that is possible, which will vary with time depending on the latex and the particular monomers being determined. 12.2 Bias--Bias cannot be determined for this test method. 13. Keywords 13.1 acrylic latexes chromatography (subheading gas chromatography); gas chromatography, analysis of mono mers; latex paints; latex vehicles; styrene; trace monomers; unreacted monomers in latexes 6 Supporting data are available from ASTM Headquarters. Request RR: D01-1055. 499 DUP050297019 # D 4747 The American Society for 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 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 and must be reviewed every five years arid ifnot revised, eitherreapproyed or withdrawn. Yourcomments are Invitedeither for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wW 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 M \l 500 DUP050297020 Designation: D 4758 - 87 Standard Test Method for Nonvolatile Content of Latexes1 This standard is issued under the fixed designation D 4758; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A niunber in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproyal. , Scope 1.1 This lest method covers a quality control test for ynvolatile content of latex vehicles. The specified timelimperature conditions (180C, 20 min) were selected to How test completion in 1 h or less. For latex vehicles used in fertain air-dry or low-temperature bake coatings, as well as *br those that contain temperature-sensitive materials, the use of a lower temperature and other bake time will more accurately reflect the effective nonvolatile content (Note 1). Alternative time-temperature conditions should be agreed lipon between the producer and user. No t e 1--The test conditions of Test Method D 2369 (tiOC, 60 'min) have been found suitable for use with many latex vehicles. 1.2 This test method is not intended to be employed for Idetermining the volatile organic content (VOC) of formu lated coatings. 1.3 This standard may involve hazardous materials, operations or equipment. This standard does not purport to ` address all ofthe safety problems associated with its use. It is responsibility of the user of 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: D2369 Test Method for Volatile Content of Coatings12 E 145 Specification for Gravity-Convection and Forced- Ventilation Ovens3 E 300 Practice for Sampling Industrial Chemicals4 3. Significance and Use 3.1 This test method is designed to quantify the weight percent of a commercial, synthetic latex product that, when incorporated into a coating product, constitutes the binder content of the applied coating. 4. Sampling 4.1 Procedures described in the Slurry Sampling section of Practice E 300 shall be used for sampling latexes. 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 1.33 on Varnish and Resins, Including Shellac. Current edition approved Nov. 27, 1987. Published January 1988. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 14.02. 4 Annual book ofASTM Standards, Vols 06.03 and 15.OS, 5. Apparatus 5.1 Oven, forced-ventilation Type IIB, as specified in Specification E 145, with closed vent. 5.2 Balance, sensitive to 0.1 mg. 5.3 Desiccator. 5.4 Weighing dish, aluminum, approximately 57 mm in diameter by 18 m deep. 5.5 Syringe, 5-mL disposable. <r. Procedure 6.1 For each latex to be tested, wash two aluminum dishes with a suitable reagent grade solvent (for example, toluene) or heat to constant weight to assure that volatile contami nants are removed. Determine . the tare weight of the aluminum dishes to 0.1 mg. 6.2 Thoroughly mix the sample on a mechanical shaker or can roller to assure homogeneity. 6.3 Draw 3.5 mL ofthe sample into the syringe and weigh to 0.1 mg. 6.4 Transfer 1.5 0.1 mL of the latex into a tared weighing dish and reweigh the syringe to 0.1. mg. Calculate the latex specimen weight, S, as follows: S = w2 where: Wj = initial weight of syringe and latex, g, w2 = weight of syringe and latex remaining after discharging specimen, g. 6.5 Repeat 6.4 for the duplicate determination. 6.6 Transfer the aluminum dishes to an oven operating at 180 4C and heat for 20.0 I min.-(Note 2). Remove from the oven,._cool in a desiccator for 5 min at room temperature and weigh to 0.1 mg. Determine the weight of residue, N, in each dish as follows: N = Wx - W2 where: Wt = weight of dish and residue, g, W2 -- tare weight of aluminum dish, g. NOTE 2--Add distilled water to viscous test specimen prior to baking. 7. Calculation 7.1 Calculate the mean weight percent nonvolatile mate rial (% NVM) where Subscripts 1 and 2 refer to the indi vidual data from the duplicate determinations: % = AV'y/-+ x J00 8. Report 8.1 Report the nonvolatile content to 0.01 weight %. 501 DUP050297021 # D 4758 9. Precision 9.1 An interiaboratory study was conducted on this test method in which one operator in each of five laboratories made duplicate determinations on each of two days on six commercial latices containing 44 and 65 % nonvolatile matter. The latex polymer types were three all-acrylics, a vinyl acetate-acrylic copolymer, and acrylic terpolymer and a vinyl acetate-vinyl chloride-ethylene copolymer. Two labora tories could not run the test on two latexes because they had gelled, and in the statistical analysis all results obtained on one latex were rejected because they differed significantly from the others. The pooled within-laboratory standard deviation was found to be 0.09 % absolute with 20 degrees of freedom and the between-laboratories standard deviation 0.16% absolute with 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: 9.1.1 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 0.27 % absolute. 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 0.48 % absolute. 10. Indexing Terms 10.1 This test method is indexed under the following terms: accelerated testing; air dry coatings; baked coatings; latex paints; latex vehicles; low temperature bake coatings; nonvolatile matter content; and temperature teste (sub heading low). 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. Users of this standard are expressly advised that determination of (he validity ofany such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. \ This standard.^ subject to revision.at arty time by the responsible technical committee and must be reviewed every five years and it netrevised, eitherreapproved or withdrawn. Your comments ere Invited either forrevision 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, ityou feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Place $L, Philadelphia, PA 19103. . 502 DUP050297022 Designation: D 4794 - 88 Standard Test Method for Determination of Ethoxyl Substitution in Cellulose Ether Products by Gas Chromatography*1 This standard is issued under the fixed designation D 4794; 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 1.1 This test method is applicable to the determination of I ethoxyl substitution in cellulose ether products by a Zeisel ! gas chromatographic technique. 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 1 the responsibility of the user of this standard to establish % appropriate safety and health practices and determine the i applicability of regulatory limitations prior to use. For I specific hazard statements, see Section 5 and Note 3. 2. Summary of Test Method 2.1 When ethyl cellulose is allowed to react with hydriodic acid, one mole-of ethyl iodide is liberated for each mole of ethoxyl ether substituted on the cellulose chain. The ethyl iodide is extracted in-situ with o-xylene and quantitated by 8 gas chromatography usiiig an internal standard technique. 3. Apparatus 3.1 Gas Chromatograph with thermal conductivity de tector and heated injection port. 3.2 Electronic Integrator. ... 3.3 Column--<Jlass tubing, two, 6.4-qim outside diam eter, 4-mm inside diameter, 1829 mm in length, packed with the reagent in 4.7, coiled to fit injection system and instrument, or equivalent column and packing as appro priate. 3.4 Syringe, 10 pL. 3.5 Reaction Vials, Caps, and Heating Block.2 3.6 Syringe, 100 pL. 4. Reagents and Materials 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 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 D01.36 on Cellulose and Cellulose Derivatives. Current edition approved Oct 31, 1988, Published December 198S. 1 Reacti-Therm Heating Module, Reacti-Bloek, Reacti-Vials, and Minnert valve tops, trademarks of the Pierce Chemical Company P.O. Box 117, Rockford, IL 61105-9976, have been found satisfactory for this purpose. ical. Society, where such specifications are available.3 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 Iodoethane, 99 % minimum. 4.3 O-xylene. 4.4 Toluene. 4.5 Hydriodic Acid, 57 % (sp gr 1.69 to 1.70). 4.6 Acetone, technical grade. 4.7 DC550, 20 %, on 100/120 mesh Chromosorb PAW. 5. Hazards 5.1 Safety precautions must be taken for, handling of hydriodic acid. 5.2 During the reaction, the glass vials are under pressure. Exercise precaution in handling the hot vials. 6. Apparatus Preparation and Conditioning 6.1 Column (Note 1)--The two pieces of glass tubing are packed with reagent under vacuum and mechanical vibra tion using silanized glass wool to contain the packing. Install each in the gas chromatograph to facilitate on column injection and allow to come to equilibrium over a 12-h period under the cohditions described below: Oven temperature, "C Injection port temperature, *C Detector temperature, 'C Detector current, ma Attenuation Polarity Carrier gas Column A, mL/min Column B, mL/rtriiT" > 100 isothermal 200 200 170 ma 1 A helium 20 20 No t e 1--The conditions used here were determined to be for the column. Optimum conditions should be determined for each column on an individual basis. 6.2 Integrator: 6.2.1 Settings (Note 2): Attenuation Start delay Chart Chart speed, cm/rnin Area reject Slope sensitivity 0.5 auto ' 0.50 off must be determined' for each GC - No t e 2--These settings were used with a Hewlett-Packard 3380 Integrator. Other units may require different settings. '"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." 503 DUP050297023 # D 4794 6.2.2 Approximate Component Retention Times: Minutes Component 1.13 1.80 2.30 3.00 4.45 methyl iodide ethyl iodide isopropyiiodide toluene (internal standard) o-xylene 7. Preparation of Standard Solutions 7.1 Internal Standard Solution (25 mg toluene/mL oxylene): 7.1.1 Weigh a 100-mL volumetric flask containing 10 mL of o-xylene to the nearest 0.01 g. 7.1.2 Add 2.50 0.1 g of toluene. 7.1.3 Dilute with o-xylene to 100 mL. 7.2 Calibration ofStandard Solution: 7.2.1 Pipet 4.0 mL of 57 % hydriodic acid into a 3-dram vial. 7.2.2 Pipet 4.0 mL of the internal standard solution (prepared in 7.1) into the vial and seal with the mininert valve. 7.2.3 Weigh the vial and contents to the nearest 0.1 mg. 7.2.4 Add 90 pL of ethyl iodide to the vial with a syringe. 7.2.5 Weigh and record the amount of ethyl iodide added. 7.2.6 Mix well.. 7.2.7 Calculate the ethoxyl equivalent of the ethyl iodide using the following equation: mg ethoxyl = g ethyl iodide x [(45 X 1000)/156] mg toluene = concentration of int. std. x 4 mL 8. Calibration of Electronic Integrator 8.1 Inject 2 pL of the standard solution prepared in 9.2 into the gas chromatograph and record the chromatogram. 8.1.1 Calibrate the integrator according to the manufac turer's instructions. 8.2 If an integrator is not available peak areas and response factors can be determined manually as follows: F = (A X B)/(C X D) where: F = component response factor, A - weight of ethoxyl equivalent in the calibration standard, mg, B = peak area of internal standard (toluene) from standard run (8.1), C = peak area for component from standard run (see 8.1), and D -- weight of internal standard in the calibration standard, mg. 9. Procedure 9.1 Specimen Preparation: 9.1.1 Dry the specimen at 105C for 30 min and store in a dessicator. 9.1.2 Weigh 60 to 70 mg of the specimen prepared in dry 9.1.1 into a clean, tared 5-mL reaction vial (see 3.5). 9.1.3 Add 2.0 mL of the internal standard solution prepared in 7.1 to the vial. 9.1.4 Add 2.0 mL of hydriodic acid to the vial. 9.1.5 Cap tightly and weigh the vial. 9.1.6 Shake the specimen for 30 s. 9.1.7 Place the vial in a heated block (150C) for 1 h, removing and shaking the, specimen after 20 min. No t e 3: Warning--Vials contain a hot corrosive acid under pres sure. 9.1.8 Remove the specimen and cool in the hood for 45 min. The specimen will separate into two layers. 9.1.9 Reweigh to determine any loss due to leakage. Discard any specimen with loss greater than 25 mg. 9.2 Analysis: 9.2.1 Enter the weight of the toluene (internal standard) , and the weight of the specimen into the integrator if an integrator is being used. 9.2.2 Inject 2 pL of the upper layer of the specimen into the gas chromatograph. 10. Calculation 10.1 The integrator reports the ethoxyl concentration in weight percent. 10*2 If an integrator is not available, calculate the peak areas and concentrations manually using the following equation: E = {GxFxHx 100)/(/'X J) where: E - ethoxyl concentration, weight %, G = peak area of component, F = response factor for component (10.2), H = weight of toluene (mg) in the specimen, mg, I = peak area of toluene, and J -- specimen weight, mg. _ -- ,> - 11. PrecisioiTand Bias4 11.1. Precision--The relative precision was. found to be 0.64 % at the 95 % confidence level. 11.2 Bias--No justifiable statement can be-made on the bias of the procedure in this test method because no suitable reference material for determining the bias exists. 4Supporting data is available from ASTM Headquarters. Request RR: D0f 1058. 504 DUP050297024 # D 4794 The American Society for Testing and Materials takes no position respeoting 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 dt any time by the responsible technical committee andmust be reviewed every five years end Ifnot revised, eitherreapprcrved or withdrawn. Your comments are invited eitherforrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a mealing 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. 505 DUP050297025 Designation: D 4795 - 88 Standard Test Method for r Nitrogen Content of Soluble Nitrocelluiose--rAlternative Method1 - 'Z::., . 11 ' ' {V; " ', This standard is issued under the fixed designation D 4795; 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 Test Methods D 301 for measuring nitrogen content in nitrocellulose by nitrometer are the accepted standard. However, the glassware is specialized and the precision is dependent on the development of a high level of skill by the operator. The ferrous-sulfate titration of nitrate is a classical procedure. By controlling critical variables and automating the actual titration, precision equivalent to the nitrometer can be achieved with nitrocellulose. This test method de scribes such a procedure. 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 safely and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D301 Test Methods for Soluble Cellulose Nitrate12 D 1193 Specification for Reagent Water3 2.2 Military Standards:4 MIL-STD M-244A MIL-STD 286 208.1.3 3. Summary of Test Method 3.1 A weighed specimen of nitrocellulose is dissolved in sulfuric acid and titrated automatically with ferrous sulfate. The nitrogen content of the specimen is calculated using the equivalence factor of the ferrous sulfate. 4. Significance and Use 4.1 This test method provides a simpler means for mea suring the nitrogen content of nitrocellulose than the nitrometer described in Test Method D301. Under con trolled conditions, the procedure described is capable of results equivalent to those obtained by the nitrometer. 5. Interferences 5.1 The presence of moisture (or other volatile compo 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 1.36 on Cellulose and Cellulose Derivatives. Current edition approved Oct. 31, 1988. Published December 1988. 2 Annual Book ofASTM Standards, Vol 06.02. 1 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave,, Philadelphia, PA 19111-5094, Attn: NPODS. nents) in the specimen will affect results. It is recommended that only thoroughly dry specimens be used. 5.2 Temperature rise must be controlled during the titration. The cooling bath provides that control. However, if the rate of titrant addition is too fast, temperature may rise out of control. Results may then be erratic. Adherence to the procedure will avoid temperature excursions. For optimum system efficiency, room temperature should be maintained at 23 2C. 5.3 The strength of the sulfuric acid used to dissolve the specimen is very important. Too low an acid strength slows the rate of solution which, in turn, causes titrations to be abnormally slow. Results then become erratic. 6. Apparatus 6.1 Acid Bottle Safety Dispenser. 6.2 Fisher Titralyzer II Titration System, or equivalent, with 25 mL amber buret: 6.2.1 Electrode, platinum. 6.2.2 Electrode, glass. 6.3 Desiccator, with drying agent. 6.4 Weighing bottles, 12-mL capacity, aluminum (pre ferred) or glass. 6.5 Analytical Balance, accurate to 0.1 mg. 6.6 Ovens--135C, for drying standards, and 1001C, for drying specimens, having unexposed heating elements and the door latch removed. 6.7 Circulating Unit, for chilled water, 5. 2C. 6.8 Blender, with 8-oz blender jar.-- ...... 7. Reagents 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.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. 7.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type III of Specification D 1193. 7.3 Sulfuric Acid (H2S04) 95 to 98 %. 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." 506 DU P050297026 # D 4795 rii 7.4 Ferrous 'Sulfate Solution--Dissolve 350 g of ferrous IJulfate crystals (FeS04) in 1000 mL of distilled water. Add 000 mL of 1+1 H2S04 solution. Makes 2 L. 1 7.5 Potassium Nitrate (KNOf Standard or an equivalent liitrate primary standard. Jj 7.6 Nitrocellulose Standard--A sample with a known Ifutrogen value or other known organic nitrate. T ;8. Hazards | 8.1 Since the sample of nitrocellulose must be dried, it is imperative that care be exercised in storage, handling, and Pdisposal. E>ry nitrocellulose is extremely flammable. Refer to b*jfhe Procedure section for Drying Samples of Methods D 301. & 8.2 Strong sulfuric acid used as the solvent for the | specimen can bum the skin. The ferrous sulfate titrant is also I'Strongly acidic. Take proper precautions to protect the operator and the equipment. 8.3 To prevent bums from acid dripping off the electrodes land dispenser tip, always wipe the electrodes and dispenser |tip with a tissue before reaching under them to retrieve a beaker. I 9. Preparation of Apparatus 9.1 If the system has been down for at least 8 h, purge the system. 10. Calibration and Standardization 10.1 Weigh a sample bottle containing 0.5000 0.05 g of KN03 that has been dried in a 135C oven for a minimum of 4 h and stored in a dessicator. If KN03 has been out of the oven for 4 h or more, redry in a 135C oven for a minimum of 1 h. (Nitrocellulose specimens are dried in a 100"C oven for a minimum of 1 h. If out of the oven more than 2 h, redry for "A h.) Turn on the pump of the chilled water circulator to start water flowing through the cooling bath. 10.2 Place the magnetic stirring bar into a dry 250-mL beaker and fill the beaker with 150 mL of H2S04 (20 2C). 10.3 Place the beaker in the cooling bath on the stirrer unit. Start the stirrer and adjust the speed for a slight vortex. Too vigorous a vortex can cause the nitrocellulose to splash onto the sides of the beaker. 10.4 With the stirrer operating and the electrodes up in the air away from the acid, slowly pour the specimen into the vortex of the swirl. Be careful not to touch the dispensing tip or electrodes with the weighing bottle. Reweigh the weighing bottle to find the weight of the standard by difference. 10.5 Allow most of the KN03 to dissolve. Visually inspect the solution until no more chunks or chips of KN03 remain. The solution may be cloudy. 10.6 Lower the electrodes and the dispensing tip into the H2S04. 10.7 Set the controls to the desired settings. 10.8 As the KN03 dissolves and HN03 is formed by the reaction of H2S04 and the specimen, a millivolt potential change is evident by a rising recorder pen. 10.8.1 When the pen shows a leveling off, it is an indication that the majority of the KN03 is in solution. Visually inspect the solution to verify the fact that chips are no longer present. 10.9 Set the buret control to a rate of about 5 mL/min. Allow 10 0.1 mL to dispense at this rate. 10.10 Stop the buret, switch the dispense-rate switch to automatic, and restart. Allow the titration to proceed auto matically to the end point. 10.11 At the completion of the automatic titration, imme diately record the millilitre reading. Switch the electrode setting to STANDBY. 10.12 Raise the electrodes from the acid and allow most ofthe acid to drip into the titration beaker. Carefully wipe by dabbing the electrodes and dispensing tip with a tissue. (Precaution--See Section 8.) Discard the tissue, into a container of water. DO NOT allow acid to drip into the circulating-bath water. 10.13 Remove the completed titration beaker from the cooling bath. 10.14 Lower the electrodes and pipet into a beaker of clean H2S04 for soaking. Make sure the acid is not contam inated with FeS04. (It may bleed from the dispenser tip giving a reddish tint to the acid) Replace with clean H2S04 if this occurs. No t e--It is important to soak the electrodes in between each analysis and while the tiitrators are not in use. Cleanliness of equipment is of the utmost importance in this method of analysts. 10.15 Calculate the nitrogen equivalence factor F for the standard KN03 as. follows: F -- (A x I3.855)/5 where: A = weight of KN03, g, 13.855 = nitrogen equivalence of nitrogen in KN03 or in the standard material used, and B = amount of FeS04 used to titrate KN03, mL. 11. Specimen Preparation 11.1 Cutting: 11.1.1 Use a sample size of approximately 2 heaping tablespoons of wet nitrocellulose. 11.1.2 For high viscosity types, place the sample into a small (8-oz) plastic blender jar. Fill to the fill line with tap water, and screw on the cap with a 4-blade cutter unit inside. 11.1.3 Place on the blender base and blend for 7 min at high speed. . 11.1.4 For lt % nitrogen and low viscosity types, grind in a tissue disintegrator using a 16-oz glass jar about 3/t full of tap water. 11.1.5 Grind each sample at high speed for their respec tive times as follows: Hercules Designation Time, min SS, all RS `A RS `A RS Vfe A.S, all 5 4 4' 3 3 11.2 At the completion of cutting, remove the .sample container and draw off the excess water from the nitrocellu lose by filtering on a Buchner funnel through a circular filter paper. 11.3 Dry the material in accordance with the paragraph on small quantities in the Procedure section for Drying Samples of Methods D 301. 11.4 After drying, weigh 3 replicate specimens of 0.4500 0.0075 g each into a weighing can or bottle. 507 DUP050297027 D 4795 TABLE 1 Suggested Settings for Fisher Titralyzer II EP-1 Select EP-1 Setting, mV Proposed Minimum Band* Delivery* Standardizations with -mV EP-1 350 80 100 KN03 Analysis of nitro- -mV EP-1 200 80 100 celluiose * These are approximations only. Settings can vary between instruments. 11.5 It is desirable to analyze the specimens as soon as they are taken out of the oven. Allow time for cooling in a desiccator before weighing. If specimens are out of the oven for more than 2 h, redry for V2 h at 100C. 12. Procedure 12.1 Prepare specimens in accordance with Section 11. 12.2 Repeat 10.1 through 10.15, using the settings for the specimen given in Table 1. 12.3 Dispose of any excess H2S04 standard down the sink and rinse with large quantities of water. 13. Calculation 13.1 Calculate the percent of nitrogen N as follows: y = (CX F)/D where: C = FeS04 to titrate specimen, mL, F = equivalence factor from 10.15, and D = weight of specimen, g. 14. Precision and Bias6 . -14.1 Tests by two laboratories on two samples gave results equivalent to the nitrometer in precision and bias. No more extensive interlaboratory testing has been undertaken as yet. 6Supporting data available from ASTM Headquarters. Request RR: D01-1056. The American Society for Testing and Materials takes noposition 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 oi 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 live 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 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. 508 DUP050297028 Designation: D 4827 - 88 Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography*1 This standard is issued under the fixed designation D 4827; 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 reapprovaJ. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. Scope ,1 This test method is for the determination of the -eacted monomer content of acrylic latexes. Monomers at have been successfully determined by this procedure -lude w-butyl methacrylate, n-butyl acrylate, styrene, and ethyl methacrylate. The determination of other monomers not been evaluated, but this test method is believed to be jjjplicable. The established working range ofthis test method from 100 to 1000 pg/g, but there is no reason to believe it i not work outside ofthis range, provided that appropriate flutions and adjustments in specimen size are made. ,i 1.2 The unreacted monomer in acrylic latexes is expected o change with time and environmental factors. This time itependence of the determination may be seen as an artifi cially large deviation of results, making the test method Inostly applicable for in-house quality control, where sam pling and analysis conditions can be better controlled. ' 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 7. 2. Referenced Documents 2.1 ASTM Standard: D1193 Specification for Reagent Water2 3. Summary of Test Method 3.1 A suitable aliquot of the latex is internally standard ized with isobutyl acrylate, diluted with water, and then injected onto a capillary gas chromatographic column con taining a stationary phase that separates the internal standard and monomers in question from each other and from other volatile compounds. 4. Significance and Use 4.1 Excessive amounts of unreacted monomer may cause concerns relating to toxicity and odor. This test method is designed to measure the unreacted monomer content of latexes. The results may be used to monitor the extent of polymerization during manufacture, as well as to establish maximum unreacted monomer content for regulatory pur poses. 5. Apparatus 5.1 Gas Chromatograph--Any gas-liquid chromato graphic instrument having a flame ionization detector and linear temperature programming and a capillary column inlet capable of split operation. The split liner should be constructed of glass and be replaced or cleaned as needed. On-column injection into a wide bore capillary column was not evaluated but is expected to also be satisfactory for this procedure. 5.2 Column--30-m by 0.25-mm inside diameter fused silica coated with a 1 pm thick film of a phenyl methyl silicone polymer. A bonded phase is preferred. Other col umns having equivalent or superior performance may also be used. 5.3 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 level of 0.03 % of full scale. 5.4 Liquid Charging Devices--A microsyringe, 1.0-pL capacity, or an automatic liquid sampling device using a suitable syringe and appropriate change in split ratio. 5.5 Dropper Pipettes, glass, disposable. 5.6 Vials, approximately 7 mL capacity, with caps. Open top screw-cap vials fitted with PTFE/silicone septa are preferred. 5.7 Autosampler Vials, 2 mL capacity (optional). 5.8 Analytical Balance, accurate to 0.1 mg......... 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 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 II of Specification D 1193. 6.3 Carrier Gas--Helium of 99.995 % or higher purity. High purity nitrogen may also be used. 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 27, 19S8. Published November 1988. 1 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 "Reagent Chemicals, American Chemical Society Specifications" by Am. Chem. Soc,, Washington, DC. For suggestions on the testing of reagents not listed by the Am. Chem. Soc., see "Reagent Chemicals and Standards" by Joseph Rosen, D. Van Nostrand Co., Inc., New York, NY, and and the "United States Pharmacopeia." 509 DUP050297029 4827 6.4 Acetone, 6.5 Isobutyl Acrylate (internal standard), 99+ % pure. No t e 1--Isobutyl acrylate was found to be a suitable internal standard, but any other monomer not found in the sample may be substituted. The internal standard chosen should yield a clear chromato- graphic separation, and should be free of interferences. 6.6 Monomers ofInterest, 99+ % pure. 7. Hazards 7.1 Acrylic and methacrylic monomers are considered hazardous. All sample preparations should be done in a well ventilated area, such as a fume hood. 8. Preparation of Apparatus 8.1 Column Conditioning--Attach one end of the column to the inlet side of the instrument leaving the exit end of the column disconnected. This prevents the contamination of the detector due to column bleed. Set the helium flow rate at 0.5 ml ./min (approximately equivalent to a linear velocity of 20 cm/s) and purge the column at 220C for 1 h. 8.2 After conditioning, connect the exit end of the column to the detector and establish the operating condi tions required to give the desired separation (see Table 1). Allow sufficient time for the instrument to reach equilibrium as indicated by a stable baseline. 8.3 Control the detector temperature so that it is constant to within 1C without thermostat cycling whicli causes an uneven baseline. Adjust the carrier gas flow rate to a constant value. 9. Calibration 9.1 Determine the retention time of each component expected to be present by injecting small amounts either separately or in known mixtures. Retention times should be determined each day that the test method is used. 9.2 Standardization--Determine iri duplicate the relative response of the monomers of interest to the isobutyl acrylate internal standard as follows: 9.2.1 Weigh to within 0.1 mg about 0.05 g of isobutyl acrylate and each monomer of interest into a vial (see 5.6). Weigh approximately 5 g of acetone into the vial and niix well. 9.2.2 Weigh approximately 0.05 g of the solution pre pared in 9.2.1 into another vial, add approximately 5 g of acetone, and mix well. 9.2.3 Inject a 0.5-pL aliquot of the solution from 9.2.2 onto the column and record the chromatogram. The elution order for acetone and each of the monomers using the conditions given in Table 1 is shown in Fig. 1. 9.2.4 Measure the peak areas of the individual compo nents and calculate the relative response factor, RF, for the monomers of interest as follows: RF~(Wy xAJKfT'XAO where: RF = relative response factor for each monomer, Ay = peak area produced by the monomer, As => peak area produced by the internal standard, Wy = weight of monomer used for calibration (see 9.2.1), g, and Ws = weight of internal standard (see -9:2.1), g. 10. Procedure 10.1 If the composition of the latex is not known or if the approximate level of monomers in the latex is not known, a preliminary analysis must be performed by diluting approx imately 0.5 g of latex with approximately 5 g of water and injecting a 0.5 pL aliquot into the chromatographic column. Using the Same conditions as for standardization, record the peaks ofall components at attentuation settings (hat provide maximum peak heights. Use the relative retention times to identify the monomers present If the specimen has a component eluting at the same retention time as isobutyl acrylate, choose a different internal standard (see Note 1). 10.2 Prepare a dilute solution of the internal standard by weighing to 0.1 mg about 0.05 g of isobutyl acrylate and 5 g of acetone into a septum vial. Take care to minimize losses due to evaporation. Prepare this Solution fresh each day that the test method is used. TABLE 1 Instrument Conditions Detector Airflow, mL/min Hydrogen flow, mL/min Column:* Length, m Inside diameter, mm Him thickness, pm Carrier gas Flow rate Temperatures: Injection port, C Detector block, C Column: Initial, C Hold time, min Program rate, C/min Final, C . Final hold, min Injection volume, pL Split ratio ______ flame ionization ' 240 30 30 0.25 1 helium 0.5. mL/min 220 250 60 4 8 200 (or higher as needed) 10 (or longer) 0.5 20:1 * Cross-linked 50 % phenyl 50 a methyl silicone. A column ot equivalent or better performance may also be used. 510 DUP050297030 # D 4827 10.3 Weigh to within 0.1 mg an appropriate amount of sample into a septum vial using Table 2 as a guide to `specimen size. Also weigh to within 0.1 mg 50 mg of the dilute solution prepared in 10.2 into the vial. Add about 3 to 5 g of water or acetone. Shake the vials, on a; wrist action, shaker or other suitable device for 15 min. No t e 2--The viscosity of a number of latexes increases upon the ' addition of an organic solvent. If acetone (or another organic solvent) is found to be compatible with the specimen, it should be used as the I diluent instead of water. It should be kept in mind that some organic (solvents may interfere with the chromatographic separation. 10.4 Inject 0.5 pL of the solution prepared in 10.3 and record the chromatogram using the conditions given in 10.1. ? Measure the peak areas (Note 3) ofthe internal standard and relevant monomers, multiplying each-area by the appro priate attenuation factor to express the peak areas on a common basis. No t e 3--Peak areas may be determined by any method that meets the precision requirements given in Section 12. Electronit integration is recommended for best results. 10.5 Repeat 10.3 and 10.4 and calculate the mean values. 11. Calculations 11.1 Calculate the weight of the internal standard present in the diluted specimen (see 10.3) as follows: W4 =.{WjWbWi where: W4 = weight of internal standard in diluted specimen pre pared in 10.3, g, Ws = weight ofinternal standard used to prepare solution in 10.2, g, Wb = weight of acetone plus weight of internal standard used to prepare solution in 10.2, g, and W1 = weight of the dilute internal standard solution in 10.2 added to the. specimen in 10.3, g. 11.2 Calculate the concentration of each monomer present in the latex specimen from the results obtained in 10.5 as follows: C = HA3 xw4x RF)/(Ws x a 4)} x 10s where: A3 -- peak area produced by the monomer, A4 = peak area produced by the internal standard, C = concentration of unreacted monomer, g/g, RF = relative response factor for each monomer calculated in 9.2.4, W4 = weight of internal standard calculated in 11.1, g, and W3 =*= weight of specimen prepared in 10.3, g. 12. Precision and Bias4 12.1 In an interlaboratory study of this test method by five laboratories using four specimens, each containing variable concentrations of four different monomers, the following duplicates, repeatability, and reproducibility coef ficients of variation were obtained for each monomen Monomer Precision, % Duplicates Repeata bility (Single Labora tory) Reproduc ibility (Between Labora- tory) Methyl methacrylate 11.7 34.3 86.2 (MMA) rt-Bmyl acrylate (BA) 13.3 21.7 49.2 Butyl methacrylate (BMA) 14.5 33.5 96.5 Styrene (STY) 11.3 30.5 71.5 No t e 4--Variation in results may be due to the changing composi tion ofthe specimens used for the study. This precision statement should only be used as a guide since it oiily represents the fnagnitude of variation that is posable, which will vary with time'tiepending on the latex and the particular monomers being determined. 12.2 Bias cannot be determined for this test method. TABLE 2 Suggested Dilutions No t e--This tablets to be used only as a guide. If the monomer concentrations are outside the range given, appropriate adjustments must be made in terms of specimen size, dilution, and amount of internal-standard added. ______ Level of Unreacted Monomer Expected', g/g . Specimen Size, g .. piluent, g 250 2 3 500 1 4 750 0.7 4.3 1000 0.5 4.5 13. Index Terms 13.1 This test method is indexed under the following terms: chromatography--gas; chromatography--gas (pap illary column); .Jatex paints; latex vehicles; monomer (unreacted); unreacted monomer content. 4 Supporting data is available from ASTM Headquarters. Request RR: D01-1059. 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 ifnot revised, either reepproved or withdrawn. Your comments are Invited either forrevision ofthis,standard or for additionalstandards and should be addressed to ASTM Headquarters. Your commenfs 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. 511 DUP050297031 Designation: D 5097 - 90 Standard Test Method for Filter-Retained Solids Content of Polymer Latexes1 This standard is issued uijder the fixed designation D 5097; 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 the determination of the filter-retained solids (grit) content of polymeric latex vehi cles, that is, material present in a latex specimen that is retained on a 200-mesh screen. ' 1.2 The values stated in SI units are to be regarded as standard. 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 Standard: E 11 Specification for Wire-Cloth Sieves for Testing Purposes12 E 145 Specification for Gravity-Convection and Forced- Convection Ovens2 3. Summary of Test Method 3.1 A specified weight of a polymer latex, first filtered through a 20-mesh screen to.remove skins and large agglom erates, is water-washed through a preweighed 200-mesh stainless screen. The dried residue on the screen, defined as the filter-retained solids, is expressed as parts per million (ppm) of the polymer latex. No t e 5-- Other screens or sample sizes, or both, may be used upon agreement,of producer and user. Precision may vary with differing mesh size and sample weight. 4. Significance and Use 4.1 The amount of excessive oversized particulate matter present in polymer latexes can detract from the appearance properties of applied formulated coatings and may reduce filtration rates or clog filters in processing or application processes. 4.2 This test method may be useful as a quality control test for latex manufacture and for product characterization. 5. Apparatus 5.1 Analytical Balance, capable of weighing to 0.1 mg. 5.2 Balance, capacity of 500 g, capable of weighing to 0.1 g. 5.3 Dessicator. 1 This test method is under the jurisdiction of ASTM Committee D-I on Paint and Reiated Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.33 on Polymers and Resins. Current edition approved July 27, 1990. Published September 1990. 2 Annual Book ofASTM Standards, Vol 14.02. 5.4 Forced-Ventilation Oven, Type II B conforming to Specification E= 145. 5.5 Forceps. 5.6 Spectra Mesh Filtration Unit,3 (90-mm size). 5.7 Graduated Cyclinder, 500-mL. 5.8 Polyethylene Water Wash Bottle, 500-mL. 5.9 Two Beakers, 800-mL. 5.10 Screen,. stainless steel, 90-mm diameter, 200-mesh (as defined in Specification E 11). 5.11 Screen, cloth or stainless steel, 20-mesh (as defined in Specification E 11). 7. Procedure 7.1 Weigh the clean, dry, 200-mesh screen to the nearest 0.1 mg. Record the weight, A. 7.2 Place the screen into the filtration apparatus. No t e 2--The screen should be held firmly in place while screwing down the filter chamber to ensure that the screen seats smoothly on the plastic ring. 7.3 Weigh 500 g of water into the 800-riiL beaker and set aside. 7.4 Hand-stir the polymer latex sample for about 15 s using a wide blade spatula to ensure adequate mixing, taking care not to beat in air. Filter about 150 g of the latex sample through a standard 20-mesh cloth or stainless-steel sigve to remove skins or large pieces of coagulum. 7.5 Stir the filtered sample gently with the spatula. Imme diately weigh out by difference about 50 weighed to 0.1 g, of the latex into an 800-mL beaker. Record the latex specimen weight, B. ~ 7.6 Transfer the 500 g of water from 7.3 to the beaker with the specimen and stir the mixture with the spatula. No t e 3--If the latex coagulates on water dilution,.the test is not applicable. 7.7 Slowly pour the mixture onto the 200-mesh screen, water-washing the sample from the beaker onto the screen with the polyethylene wash bottle. 7.8 Wash the residue on the screen with 1000 g of water, using the wash bottle to wash down the sides of the filtration apparatus and to move the solid toward the screen center. 7.9 Specimen Drying: 7.9.1 Carefully remove the screen from the apparatus using forceps, place the screen in the oven and dry for 1 h at i io rc. 7.9.2 Remove the screen from the oven using the forceps and allow the screen to cool for 10 min in a dessicator. 3 Available from Fisher Scientific, catalog number 08-670-173. 512 DUP050297032 7.9.3 Weigh the screen plus dried solids to the nearest 0.1 Record the weight, C. '7.10 Repeat 7.1 to 7.9.3 using a duplicate sample of the :ex. Calculation 8.1 Calculate the parts per million of filter retained solid ontent, S, in the analysis samples as follows: S = -(C-AB) 106 'ere: = mass of screen and solid residue, g, -- mass ofscreen, g, and = mass of latex sample, g. , 8.2 Calculate the average filter-retained solids content From the duplicate analysis. 9. Report 9.1 Report the following information: 9.1.1 The filter-retained solids content to the nearest 10 ppm as the average of the two determinations and 9.1.2 The mesh size and sample weight used, if other than 200 mesh and 50 g. 10. Precision and Bias 10.1 The precision of this test method will be determined. 10.2 Since there is no accepted reference material for determining the bias of the procedure for measuring filterretained solids no statement on bias is being made. 11. Keywords 11.1 filter-retained solids; grit; polymer latexes 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.sublect to revision at any time tty tha responsible technical committee and must be reviewed every five years end Ifnot revised, eitherreapproved or withdrawn. Yourcomments are Invited either for revision ofthis standard orfor addi'tional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ol 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. 513 DUP050297033 Designation: D 5166 - 91 Standard Practice for Laboratory Preparation of dialled Vehicle Samples Using a Microwave Oven1 This standard is issued under the fixed designation D 5166; 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 ofjast reapproval. A superscript epsilon (s) indicates an editorial change since the last revision or reapptoval. 1. Scope 1.1 This practice outlines a procedure for preparing gelled vehicle samples using a microwave oven. 1.2 The test samples can be used for characterizing the gelability or reactivity of resins, gelling agents, and vehicles used in the manufacture of oil based printing inks, or both. 1.3 Evaluation of the gelled vehicles may, depending upon preference, be either visual or instrumental. ... . ' * 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 of this standard to establish'appro priate safety and health practices anddetermine the. applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D154 Guide for Testing Varnishes12 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method3 D1725 Test Method for Viscosity of Resin Solutions4 D4040 Test Method for Viscosity of Printing Inks and Vehicles by Falling Rod Viscometer5 E 1 Specification for ASTM Thermometers6 3. Terminology 3.1 Description of Terms Specific to This Standard: 3.1.1 gel--Any resin solution, or more complex blend of resins and alkyds that has been cooked or reacted with a gelling or cross-linking agent to build molecular weight and that exhibits a pseudoplastic rheology. (Also called "gelled vehicle.") 3.1.2 gelling agent--in the context of ink resins and vehicles, gelling agents or gellants are typically organoaluminum compounds that react with carboxylic add and hydroxyl groups present on the backbone of resins and alkyds to form cross-linked networks. (Also called "gellant".) 3.1.3 gel length--References to long, medium, and short gel length refer to the length of a string of gelled vehicle observed when pulling apart a small sample of vehicle with a spatula (that is, a long gel is very fluid and forms a "long" 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 1.37 on Ink Vehicles. Current edition approved Sept. 15, 1991. Published November 1991. 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 06.02. 5 Annual Bock ofASTM Standards, Vols 06.01 and 06.02. 6 Annual Book ofASTM Standards, Vol 14.03. filament; a short gel has little flow and forms a "short" filament). - ;',T - * * ' > 3.1.4 pregel--The resin solution or. vehicle components comprising the vehicle prior to the addition of gelling agent andviscosity adjusting solvent. (Also called?"pfegel vehicle".i 4. Summary of Practice 4.1 Prepare a pregel resin solution pt Vehicle. 4.2 Separate the pregel veliicle into five or more aliquots to which various levels of gellant are added. Alternately, various gellants can be added at a given concentration to compare th&r effectiveness;''; y 4.3 Place the test ^amples on a tumtable in the microwave < oven and heat the samples at full power until the desired test temperature is attained. 4.4 After the prescribed waiting period, test and rate samples for gelability. *' f | ?! ! 5. Significance and Use 5.1 This practice provides a means of preparing a number ' S of gel vehicle samples with minimum use of materials and time. It provides a means of quickly 'characterizing and ! comparing the gelability or reactivity of resins, vehicles, and gelling agents. 6. Apparatus 6.1 Mercury Thermometer, capable of reading from 0 to 250C and conforming to Specification E 1-. 6.2 Jars, (40 mm in diameter by mm in height), 70 cm3 with nonmetallic screw-on lids. 6.3 Microwave Oven, common 750-watt.7 6.4 Microwave Oven Carousel, if not contained in the microwave oven. 6.5 Glass Dish, 15.2 cm in diameter. 6.6 Balance or Scale, capable of weighing to 0.1 g accuracy. 6.7 Ink Knife or Rigid Spatula. 6.8 Rheology Testing Apparatus, at the discretion of the user. 7. Reagents and Materials 7.1 Nonvolatile materials including resins, alkyds, gellants, etc consistent with those used in the manufacture of lithographic ink vehicles, for example, aromatic hydrocarbon resins, modified rosin ester resins, long oil linseed isophthalic 7 Microwave oven, such as the Amana Radarrange Model RR-9TA, Amana Refrigeration, Inc., is available from most appliance stores, and has been found suitable for this purpose. 514 DUP050297034  alkyds, and aluminum compounds. * 7.2 Solvents typically used in the manufacture of litho- graphic ink vehicles, for example, hydrocarbon petroleum distillate with carbon numbers in the range of Cl 2 to Cl6 and initial boiling point above 150C. TABLE 1 Microwave Gelability Test, Weights and Concentrations for 50-g Samples Gellant Solution, % Actual Gellant Concentration, % Weight Gellant Solution, gA (at 33.3% Gellant in Ink Oil) Weigh! Ink Oil, gA [ 8. Procedure | 8.1 Plhce 45 g (or the calculated; weight) of previously j prepared; pregel vehicle-into each of five or more 30-cm3 bottles. ; ' No t e i--Any vehicle, even a very Complex formulation, without the gellant added may be used as the pregel vehicle portion for the microwave oven gelability process. ' 8.1.1 In the absence of a vehicle formula agreed upon between iuser and seller, the following test vehicle formula is? * 0 1 2 3 ... .4 ' S 6 '7 8 .9 to 0.00 0.33 0.67 1.00 1.33 1.67 2.00 2.33 2.67 ... 3.00 3.33 A Weight added to 45-g pregel sample. 0.0 0.5 1.0 1.5 2.0 25 35 35 4.0 4.5 . 5.0 5.0 45 4;o 3.5 3.0 25 2.0 15 1.0 0.5 0.0 suggested:8,9 i Pregel Vehicle Resm Alkaline refined Unseed oil (ARLO) C12.C16 hydrocarbon petroleum distillate CeUant/Solvent Addition 33.3t% oxyaluminum octoate/66.7 % C12-CI6 hydrocarbon petroleum distillate " Parts 35 30 25 90 10 too No t e 2--If more than one serof samples is to be run, allow the microwave oven to cool between runs. Heat is retained in the oven and ifa second set ofsamples is run immediately it will be subjected to more heat than the first set 9. Evaluation 9.1 Samples should be tested immediately after prepara tion and after 24 h to determine .the effects of post gelation, if 8.2 Estimate the amount of gellant required to make an any. acceptable gel vehicle. Add gellant solution (betweeif 30 and .; 9.2 Guide D 154 outlines many methods applicable to the 50 % gellant in major vehicle solvent recommended) in 1 % testing of varnishes. It is an excellent guide for those looking increments plus additional solvent to ddjuSf'the1 vehicle to' aE : ifomspecififeareas of evaluation. 100 % formula. If the amount ofgellant required can not be 9.3 Lightly gelled resin solutions and vehicles can be estimated, use a larger range of gellant concentration;.^ tested for changes in viscosity by using either Test Method 8.2.1 Ifusing thcipregel fortnulaasjustrecommended.ithe D 1545 or D 1725. These test methods both.use Gardner required amount of gellant can be estimated from Table 1, bubble tubes to determine the viscosity of liquids. > 8.2.2 A sample containing no (6 %)>geliaint solution^.is 9.4 Another test method for testing gelled ink vehicles is always prepared as the standard for each resin. Test Method D4040. This method utilizes a falling-rod 8.3 Mix the added.liquids, into the pregel very well using viscometer and. can be used to determine the non-Newtonian an ink knife or rigid spatula. - ^ * nature of yefiicies. Other viscometers used for determining 8.4 Place the five sample bottles, without tops, into the '-.-the'rheology .of gelled vehicles include;-.variable shear rate 15.2-cm glass dish and place on the carousel in the micro- viscometers, and cone and plate viscometers. wave oven. 's.; / ; % -'*''Z'..''*-. ' ''i- 8.5 Turn on the carousel and. ensure that %it is .turning' 9:5 For thb trained analyst-the occurrence of gelation is eyideiit aha gels. can be rqted: visually (for example, long, before starting the heating cycle: Turn on the--light in the . medium,, medium, short, short gel body). oven to observe the process. 8.6 Set the timer on the oven for "5.00" min and start the cooking cycle. 8.7 Upon completion of the cooking cycle, check the temperature of the samples to determine whether a temper ature of 105 to 110C was obtained. If not, continue the heating cycle in I-min intervals until the samples have reached this temperature. 8.8 Remove the samples from the microwave oven, and allow to cool. 8.9 Seal cooled samples with jar lids.8 9 10. Report 10.1 Report the following information: 10.1.1 Sample identification, 10.1.2 Test run, 10.1.3 Brief summary of procedure, 10.1.4 Conditions oftest procedure, and 10.1.5 Results of the analyses made. In the case of falling rod viscometer determinations, the following data could be obtained using Test Method D 4040 (see also the Apparatus Section of this test method): 10.1.5.1 Apparent viscosity at 2500 at 25C, s, 8 This formula works best with higher molecular weight ink resins (for example, phenolic modified rosin esters). It is suggested that the resin solids be increased for low molecular weight resins (for example, simple rosin estets, modified hydrocar bons, etc). 9 When a resin is insoluble, reformulate replacing 5 parts of C12-CI6 hydrocarbon petroleum distillate with TX1B (2,2,4-trimethyl-1,3-pentanediol, diisobutyrate) or TDA (tridecyl alcohol). Caution: TDA may hinder the reactivity of the resin system tested. 10.1.5.2 Pseudo-Bingham Yield value at 254C, 10.1.5.3 Shortness ratio (yield value/viscosity), and 10.1.5.4 Slope (non-Newtonian parameter). No t e 3--For a measurement of relative resin, vehicle, or geilant reactivity, lots of rheology versus gellant concentration (see Fig. i) provide an excellent comparison. 515 DUP050297035 # D 5166 FIG. 1' Determination of-Lithographic ink Resin Gelability No t e 4--Falling rod viscosity slope (non-Newtonian parameter), shortness ratio, and visual degree of shortness? if used properly, are all suitable measures of rheology. 11. Keywords ... 11.1 gel; gelability; gelled varnish; gelled vehicle; micro wave oven; ndn-NeWtonian fluid; pregel; pregel varnish; pregel vehicle; shortness ratio; slope, yield value 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 ofthe 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 ifnot revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additionat$tandards 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 die ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 516 DUP050297036 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. DUP050297037 List by Subjects 1992 ANNUAL BOOK OF ASTM. STANDARDS, VOLUME 06.01 0 5 7 --Tes t s f o r Fo r mu 7 Pr o d u c t s 7 Ap p l ie d C 7 n g 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 Volume 06.02 and 06.03, see pp, xxSv and 527 A complete Subject Index begins on p. 561 Specifications for D 5098-90 D4302 - 90 D 5067 - 90e! Test Methodsfor: D 969 -85 (1989)1 D 4399 -90 D 1210 -79(1988)61 D 1316 -87 D 2243 90 D 2337 84 D 3793 -89 D 2574 -86 D 185 -84(1989)fl D 5062 -90l D 869 - 85 (1989)6' D 1309 -88 D4144 82 (1987) D1849 -80(1987)C1 D4948 -89 Practicefor: 0 3925 - 91 Test Methodsfor: D 4958-91 D 2353-83 D2801 -69(1981)fl D 4062 - 88 D 4400 - 89a 0 2376 - 84(1989) D 4707 - 87 Practicefor: 04941-89 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 Conduct!vityof Electrocoat Baths, Measuring Fineness of Dispersion of Pigment-Vehicle Systems Fineness of Grind of Printing 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, Mutability 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 How 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, ifindicated on the standard, replaces corresponding Federal or Military document. Consult the DoD Index ofSpecifications 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 information only. 519 DUP050297038 i Test Methodsfor: tl D 1209 - 84 (1988)ei D 1544 -80 (1989)1 D 4838 - 88 D 2090 -88 Test Methodfor: D 1475-90 Test Methodsfor: D 562-81 (1990)ei D 4359-90 D2196-86 (1991)1 D 4212 -88 D 4287-88 D 1200-88 D4040-91 D 1545 - 89 Test Methodsfor: D 2697-86 D 5145-90 D 5095 - 90 D4713-8761 D 1644 - 88 Guidefor: D 2832-83 (1991)el Test Methodsfor: D4451 -85 (1991)el D2371 -85 (1990)el D 2698 -90 D3723-84<1990)) Test Methodsfor: D 2369-90 D 5200-91 D 5087-91 Practicefor: D 3960 - 91 Test Methodsfor: D 3792-91 D4017-90 D 4942 -89 Test Methods for: 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 | 1 I | j 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 520 DUP050297039 West Methods for: I'D 4370- 84(1990)1 D 2348 - 91 fD3133- 72(1989)l i D3718- 85a 1 D4457- 85 (1991)1 | D2621- 87 D 3335 - 85a {! 99 l)ei ; D3618- 8Sa(1991)1 D 4834 - 88 D 3624 - 85a(l99l)el D 4584 - 86 (I991)l !D 1542 - 60 (1988)1 i D 2349 - 90 i D 4764 ' 88 I D 4563 86 (1991)I ! D 2921 - 88 2)3432- 89 |Practicesfor: D 3271-87 D 3168-85 (1990)1 D2372-85 (1990)1 D 2743-68 (1987) D3272 - 76(1988)C1 1 Guidefor: D 1978 - 91 Test Methodsfor: D 215-91 Specification for: D 358-83(1988) Test Methodsfor: D 4940-89 D 1734 -- 63 (1980)61 04262-83(1988) D2201-65(1987)l 04417-84 D 609 -90 02200-91 Practices for: D1730-67(1984)I D1731 -67(1984)1 D 5107-90 D 4259 - 88 D 4260 - 88 D4258 - 83 (1988) D4261 - 83 (1988) 0 3891-90 D 1732 - 67(1984) 02092-86 Guidefor: 0 4610 - 86 Test Methods for: 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 Dichlorometbane 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 Prepalymers and Coating Solutions by Gas Chromatography (see Vol 06.02) 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 Solidsfey Spectroscopy and Gas Chromatography Vacuum Distillation of Solvents &om Solvent-Reducible Pints for Analysis 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 i 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 Films of Uniform Thickness of Paint,-Varnish, and Related Products on Test Panels, Producing Thickness, Wet Film, Measurement, ofOrganic Coatings 521 DUP050297040 Practices for: D 4147-82 (1987) D4414 - 84 (1990)" D 4708 -91 Test Methods,for: D 1640-83(1989)" D 1643-60 (1988) D 3793-89 D 711-89 D 4752-87 Practices for: D 3732-82 (1989)" D3259-84(1990)" 1 D 2454 - 91 Test Methodsfor: D4138-88 D 1186-87 D 1400 - 87 D 1005 - 84 (1990)" D 2691-88 G 12-83(1988) Test Methodsfor: D 2065-91 D 3258 - 80(1987)" D 1653 - 91a E 96 - 90. Practicefor: D 5162-91 Test Methods for: E 97-82(1987) D 3928-89 D 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 Curing fl Drying Times of OrganicCoatings at Room Temperature Gas Checking and Draft Resistance of Varnish Films . Low-Temperature Coalescence ofLatex 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 . Infrared 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 Ttiickness of Protective Coating Systems Measurement of Dry Film Thickness on Ferrous Base; . . Measurement of Dry Film Thickness on Nonferrous 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, Reflectqnce, and Hiding Power. 45-deg 0-deg, Directional Reflectance Factor of OpaquoSpecimens by Broad-Band Filter Reflectometry Gloss or Sheen Uniformity, Evaluation of . j. , .. Gloss Differences Between Surfaces of Similar Appearance, Visual Evaluation of Gloss of High-Gloss Surfaces Using Abridged Goniophotometry Gloss, Specular . . Hiding Power of Architectural Paints Applied by Roller '! Hiding Power of Paints by Reflecfometry Hiding Power, Relative, of Paints by the Visual Evaluation.of Brusbouts Print Resistance of Architectural Paints Reflection Haze of High-Gloss Surfaces. > Wet-to-Dry Hiding Change Absolute Calibration ofReflectance Standards (see Vo! 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 from Instrumentally Measured Color Coordinates Color Permanence of White Architectural Enamels (Discontinued 1992f) 522 DUP050297041 LIST BY SUBJECTS, VOLUME 06.01 -91 `968 -81 (1991)" |4060 -90 15181 -91 p4213 -87 3359 90 gl97 -86 (1991)el Bl79 -91 H541 - 85 (1989)l l 10 -83(1988) >2793 -69(1987) J34946 -89" 4796 -88 >3170 -87(1991)" H642 70(1987) 522 88" >5178 -91 BJ4145 - 83 ID 3281 -84(1989) .>4146 -83(1989)" 3363 -74(1989)" p 1474 -85(1991)" |Ij y -91 m 14 -88 i!? -89 - 88 D 3003 -71(1987) D 2091 -88 1 D 2794 -90 I'D 4518 -91 !D 2370 - 82(1987)" I'D 913 -88 test Methodsfor: D3260 -82(1991) D4938 -89 D3623 -78a (1987) G 8 -90 G 42 -90 D1540 -82(1987)" D 1308 -87 G 20 -- 88 D2933 -74(1986)" D 1654 -79a (1984)" D4256 -89 D3719 -87 G 19 D2803 -82(1987) D 1360 -90a D 3806 -90a D 2485 -91 D 3459 -87 D 2246 -87 G 18 -88 D4303 -91 D 3424 - 75 D2620 -87 D4939 -89 Color 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 the 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 Coatings Block 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 (Falling Weight Test) . Impact Resistance^ 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 oitOrganic Coatings to the Effects of Static Friction of Coating Surfaces,' Measuring Tensile Properties of Organic Coatings Wear Resistance of Traffic.Pai-pt, 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 Disbonding of Pipeline Coatings;- Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures Chemical Agents, Effect on Organic Finishes Used in the Transportation Industry Chemicals, Household, Effect of, on Clear and Pigmented Organic Finishes Chemical Resistance of Pipeline Coatings - Corrosion Resistance, Dynamically Testing Coated Steel Specimens (Discontinued 1992t) 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 Coatingsby Direct Soil Burial Filiform Corrosion Resistance of Organic Coatings on Metal Fire Retardancy of Faints (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 Fluid Shear Forces in Natural Seawater 523 DUP050297042 Test Methods for: D 3274-82 (1988)*' D 3273 -86(1991)" D 5108-90 D 4828-91 D 4082 -89 B 117-90 D2486 - 89 02134-66(1980)*' D2792 - 69(1987) D2198-84(1989)*` D1211 -87 D 3450 - 90 D 1647-89 G 9-87 E 84-90 E 162-90 Practicesfor: 02248-89 0 3456 - 86 < 199 l)el 03023-88 D 4585 - 87*' D 870-87 D 2247 - 87 D 1735 - 87 Test Methodsfor: D 868-85(1989)*' D 714-87 D 659-86*1 D 660-87 D 661 -86i 0 662 - 86*' D 772 - 86** D 2200 - 85 (1989) D 610-85(1989)*' Practice for: D412I - 82 (1987) Test Methodsfor: D 2830-91 D 1641-59 (1987) 0 1014 - 83(1988)*' 01150-55(1987)*' G 11-88 D 1848-88 Practices for: D 4141-82 (1987)*' D 4587-91 D 1006-73 (1986)*' G 23-90 D 822 - 89 G 53 - 88 D 3361-87 0 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 of Interior Coatings in an Environmental Chamber, Resistance to Organotin Release Rates of Antifouliug Coating Systems in Sea Water Practical Washability of Organic Coatings Radiation, Effect on Coatings Used in Light-Water Nuclear Power Plants Salt Spray (Fog) Testing Scrub Resistance of Interior Latex Flat Wall Paints Softening of Organic Coatings by Plastic Compositions (Discontinued 1990f) 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 Films 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 Paint 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 r Pictorial Surface Preparation Standards for Painting Steel Surfaces j Rusting on Painted Steel Surfaces, Evaluating' Degree of i I i$ :jt 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, Effects of 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 r Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetallic Materials, Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Caibon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Products Using the Dew Cycle, Operating Light- and Water-Exposure, Using Enclosed Carbon-Arc Apparatus, Conducting Tests on Paints and Related Coatings and Materials 524 DUP050297043 LIST BY SUBJECTS, VOLUME 06.01 yesfor: 26-90 if. 113-90 Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Nonmetaliic Materials, Operating Road Service Tests on Traffic Marking Materials, Conducting Miscellaneous Properties Methods for: 1736 - 89 2338 - 84 (1989)*' 199-82(1987) 14797-88 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 m Methodsfor: *11546-62(1987) 333-87 466 - 42(1989) >2066-91 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 idices for: >3794-79" >3002-81 (1987) >3925-81(1985)" >3451 -76(1987)" (3322 - 82(1991) |b 2336-87(1991)" Coil Coatings, Testing Evaluation of Coatings for Plastics 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 guidesfor: D 2833 89 D 3630 89 >3129- 91 D 2932 - 80(1988)" D3730- 78(1988)" D4712- 87a (1991) D 4540 91 > 3323 - 80(1988)" D2931 - 84(1989)" D 5010 91 D5I46- 91 D 3425 - 80(1988)" D 3383 - 79a(1988)" D 2205 - 85(1990)" D 154- 85(1989)" 03358- 88 D2571 - 88 Architectural Paints and Coatings, Index of Methods for Testing Constituents Classified as Hazardous Contained in Protective Coatings Exterior Latex House Paints, Testing Exterior Solvent-Reducible 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 f Printing Inks and Related Materials, Testing j Solvent-Borne Architectural Coatings Solvent-Reducible Interior Semigloss Wall and Trim Enamels, Testing Solvent-Reducible Floor Paints, Testing N Traffic Paints, Testing Varnishes, Testing Water-Borne Floor Paints, Testing Wood Furniture Lacquers, Testing Purchasing and Application of Paint and Related'Coatings ' --- ' if 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 It Specificationsfor: D 4618-87 D 5139 -90 Flue Gas Desulfurization System Components for Protective Lining Application Sample Preparation for Qualification Testing of Coatings to be Used in Nuclear Power Plants Test Methodsfor: 0 3912 - 80(1989) D3911-89 D 4256-89 D4138-88 D 4263-83 (1988)" D4285-83(1988) D 4262 -83 (1988) D 4082-89 Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants Coatings Used in Light-Water Nuclear Power Plants, Evaluating Decontaminability 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 or Etched Concrete Surfaces Radiation on Coatings Used in Light-Water Nuclear Power Plants, Effects of 525 DUP050297044 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) Guidesfor: D5161-91 D 3842-86 (1991) D4537-91 D 5163-91 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 1990f) Surface Cleaning Concrete for Coating Surface Cleaning Concrete Unit Masonry for Coating 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 Specifications for: D 3924-80 (1991){1 E 171-87 Test Methodsfor: D 5043 -90 D 5009-89 D 5066-91 D 95 - 83 (1990) E 306-71(1976)ej E 337 - 84(1990) Practices for: 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 Standard Environment for Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials Standard Atmospheresfor Conditioning and Testing Materials (see Vol 15:09) 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) __ 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 of Objects and Materials (see Vol 14.02) Natural Light Exposure Tests (Sunlight and Daylight), Conducting Under Glass (see Vols 07.01 and 14.02) Definitions of Terms 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 Practicefor: E 380-91 Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Material section) DUP050297045 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.03 P --F7 7 Oil s 7 Ac id s , N77 St o r e s , So l v e n t s , Mis c e l 7u s ; A( !7"#c H9$%&'7%)o n s jpl . ; Since the standards in this book are arranged in alphanumerical sequence, no page numbers are given in this list. I 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. 519 and xxiv A complete Subject Index begins on p. 561 'Specificationsfor: D1539 60(1988) P 961- 86 D 960- 79(1988) D1841 63 (1988)" D1842- 63(1988) D1843 - 63 (1988)l D 1538 - 60(1988)" D 260- 86(1990) D 234- 82 (1991)" D 601- 87 (1991)" D1392 - 87 D1537 - 60(1988)" D 124- 88 D 1462- 87 D3169- 89 D1984 - 69(1988) D 12- 88 Test Methodsfor: D 1950-86 D1980 - 87(1991) D 1951-86 D 1952-86 D 2090-88 D 1967 - 86 D 1981-86(1990) D 1544 - 80 (1989)" D 1358 - 86 D1983-90 D 3457-87 (1991)" D 2800 - 87 D 3725 - 78(1988)" D 93- 90 D 3278 - 89 D 1966- 69(1991)" D 1954- 86 01955- 85(1989)" D 1957 - 86 D 2245 - 90 D 1959- 85(1989)" D1541 - 86 FATTY OILS AND ACIDS, DRYING AND NONDRYING Castor Adds, Dehydrated Castor Oil, Dehydrated Castor Oil, Raw Coconut Fatty Adds, Distilled Com Fatty Acids, Distilled - .. Cottonseed Fatty Adds, Fractionated and Distilled ' Linseed Fatty Acids, Distilled ' ' Linseed Oil, Boiled Linseed Oil, Raw ' Oiticica Oil (Permanently Liquid) Safflower Oil - Soybean Fatty Adds, Distilled Soybean Oil, Degumrned Soybean Oil, Refined Sunflower Oil t- Tall Oil Fatty Acids Tung Oil, Raw .' Acetone Tolerance of Heat-Bodied Drying Oils Acid Value of Fatty Adds Ash in Drying Oils and Fatty Adds 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 Adds, 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 Adds for Determination of Fatty Add Composition by Gas-Liquid Chromatography, Preparation of Methyl Esters from Oils for Determination of Fish Oil in Drying Oils and Drying Oil Fatty Adds 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 Adds Iodine Value, Total, of Drying Oils and Their Derivatives Approved for use by agencies ofthe 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. 527 f DUP050297046 Test Methodsfor; 0 1960 - 86(1990) D 1958-86(1990) D 2575-70 (1987) D 1240 - 82 D 1466 -86 D1962-85(1989)fl D 1963 - 85 (1989)" D 803-82(1987) D 1585-82 D 1982-85 (1989)" D 1964-85 (1989)" 0 1965 - 87 (1991)" 0 1545 - 89 Guidesfor: D 555-84(1988)" D 1467 - 89 D4I40-82(1991)" Test Methodsfor: D2076-64(1987)" D 2074-66 (1987)" D 2073 - 66 (1987)" D 2077 -64 (1987) 0 2071-87(1991) 0 2075 - 89 0 2078 - 86(1990) D 2080-64 (1987) D 2082 -82 (1987) D 2079-82 (1987) D2081 -64 (1987) D 2083-66 (1987) D 2072-66 (1987)" D 235-87" D 3735-87 D 13 - 82 (1987) D 836-84 D 835 - 85 D 2359 -85a 0 3055 - 86 D 3734 - 91 D 4077 - 81 (1986)" D 2827-88" D 362-84 D 841-85 D 4076 - 86 D 843-80(1985)" D 846-84 D 319-90 D 330-89 D 304 - 90 D1007 - 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 Oitidca Oil, Chloroform Insoluble Matter in Polymerized Fatty Acids Rosin Acids in Fatty Adds Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Related Materials Saponification Value ofDrying Oils and Fatty Adds Sperific Gravity of Drying Oils, Varnishes, Resins, and Related Materials Tall Oil Tall Oil Rosin, Fatty Adds Content of Titer of Fatty Adds Tung Oil Quality Unsapdriifiable Matter in Drying Oils and Fatty Acids Viscosity of Transparent Liquids by Bubble Time Method Drying Oils, Testing Fatty Acids 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 o-Xylene 950 Xylene, Nitration Grade Xylene, Ten-Degree (Discontinued 1991) Alcohols and Ether Alcohols Amyl Alcohol (Synthetic) 2-Butoxyethanol -Butyl Alcohol (1-Butanol) sec-Butyl Alcohol (2-Butanol) Diethylene Glycol Dipropylene Glycol (Discontinued 1992f--Replaced by Specification D 5164) Dipropylene Glycol Monomethyl Ether 2-Ethoxyethanol DUP050297047 D 2693 -87 D 2636 - 91 01719-90 D 770-90 D3160-9I D 3128-89 D 1152-89 D 2635 - 91 D 3622 - 90 D 2695-87 D4837-89 D 329-90 D 2627 -91 D2916-88 D 4360-90 D 740-89 D 3729-84 02917-91 D1153-90 D 3540-86 D4615-86et D 3728-88 04614-86 D 5137-90 D 1718-86 D3131 -88 D 2634-86 03130-86 D 4835-89 | Test Methodsfor: D 801-57(1987) D 233-65 (1981)el D 268-90 i Test Methodsfor: D1612-90 D 1613-91 D 847- 87 01614- 91 01492- 87 D 2324 - 81 (1989)61 D 848- 81 (1989)1 D 849- 88 D 130- 88 D 1617 - 90 D 853- 82 (1987)el 0 1363- 88 D3961- 89 D1685 - 86 D 890- 58 (1987) 01364- 90 E 203- 75 (1986)tl Test Methodsfor: D 3545 - 90 LIST BY SUBJECTS, VOLUME 06.03 Ethylene Glycol Hexylene Glycol Isobutyl Alcohol (Isobutanol) Isopropyl Alcohol (Isopropanol) Isopropylbenzene (Cumene), Phenol Content 2-Methoxyethanol Methanol (Methyl Alcohol) Methyl Isobutyl Carbinol n-Propyl Alcohol (1-Propanol) Propylene Glycol (Discontinued 1992|--Replaced by Specification D 5164) Propylene Glycol Monomethyl Ether Ketones Acetone Diacetone Alcohol Isophorone Methyl n-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) -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 w-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 Alcohbl) Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, taequer, 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 Vol 15.05) Physical Tests Acetate Esters, Alcohol Content and Purity by Gas Chromatography t Although this standard has been officially withdrawn from Society approval, a brief descriptioin is included for information only. 529 r DUP050297048 LIST BY SUBJECTS, VOLUME 06.03 Test Methods for: D 3257-88 D2935-81 (1985) D 4367 - 89 D 1209 -- 84 (1988)ei 0 3054-81 (1985) D 850-86 D 86-90 D 1078-86 D 5008-89 D 3539-87 D 3934 -90 0 1310 - 86(1990)" D 93-90 D 56-87 D 3941-90 D 3278 - 82" D 3893 - 90 D 2804 - 88 D 3329-89 D 2360-82 (1987)" D 1353 - 90 D 1296-84 (1988)" 0 4773 - 89 D 852 - 87 D 1493 - 84 (1988) D 4206 - 89 D4207 - 91 D3962 - 80(1989)l D3009-72(1981)l D 1555 - 83 D 95 - 83 (1990) D 2306 - 81 (1985) D 3797-88 D 3798-89 D1217-86 D 1015 -84 01016-84 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) 11 Cyclohexane, Purity and Benzene Content by Gas Chromatography Instillation of Aromatic Hydrocarbons ^ Distillation of Petroleum Products t Distillation Range of Volatile Organic Liquids i '* 2-Ethylhexonal, Ethyl Methyl Pentanol Content' ahd Purity Value by Gas Chromatography Evaporation Rates of Volatile Liquids (See Vot 06.01) Flash/No-Flash--Equilibrium Method by-a Closed-Cup Apparatus Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus Flash Point by Pensky-Martens Closed Tester Flash Point by Tag Closed Tester `. Flash Point of Liquids by Equilibrium Method With Closed-Cup ApparatasT Hash Point of Liquids by Setaflash Closed-Cup Apparatus ' Methyl Amyl Ketone and Methyl Isoamyl 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 ahd Diluents . .. Purity of Propylene Glycol Monomethyl Ether, Dipropylehe Glycol Monomethyl Ether, and Ptbpyjene Glycol Monomethyl Ether Acetate '' ' 1,: Solidification Point of Benzene ^ Solidification Point of Industrial Organic Chemicals ' SustainedBumingofLiquidMixturesby Setaflash Apparatus (Open Cup) ' ' Sustained Burning of Low-Viscosity Liquid Mixtures by Wick Test Styrene Analysis by Gas Chromatography v" 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 o-Xylene 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) , o >' . Solubility and Miscibility Tests! Test Methods for: D 611-82(1987)" D 1720-88 D 1476 - 88 0'll 33-90 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 Splvejitsr. i . __' Kauri-Butanol Value of Hydrocarbon Solvents Water Miscibility of WaterrSoluble Solvents- ----- . , Liquid Naval Stores i t Test Methodsfor: D 801 -57 (1987) D 86 - 822 D 56-87 D 802-82 (1987) D 856 - 49(1987) D 1131 -53(1981)" D 803-82 (1987) D 233 -- 65 (1981)ei D3009-72(1981)l D 890-58(1987) Dipentene, Sampling and Testing r . f. Distillation of Petroleum Products ' ' Flash Point by Tag Closed Tester Pine Oil, Sampling and Testing' Piffc Tars and Pine-Tar Oils ' ' J Rosin Oils Tall 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 ir 530 \ \ DUP050297049 LIST BY SUBJECTS, VOLUME 06.03 pj Specificationsfor: I D 4710-87 i D 3620-90 I D 4416-89 II D 3547-91 ji! D 608-90 I D 3548-86 | D 3193 -91 f D3541 - 91 | D 1969-91 1 D2378-84(1987) ! D1257 -90 f D 3504-91 f D 3845-89 | D 4709-87 I D 600 - 90 02403-68(1982)" D 363-90 02190 - 89 I Test Methodsfor: D 3362-84 (1987) D4415-91 D 2192-89 D2119-87 D 2613-85 (1990)" D 3970-80 (1990)" D 2373-85 (1990)" D 2379 - 84 (1987) D 2194-89 i D 2087-89 D 2380 -84(1987) 0 3546 - 90 ! 0 1258 - 90 0 1728 - 83 D 3804-86 (1991)" D 2374-85(1990)" D 2375 - 85 (1990)" D 3125-83 (1987) D 2999-85 D 564-87(1991)" D 2195-84 D 3989-81a (1990)" D 3962-80 (1984)" D 2119-87 D 2120-87 D 2340 - 82 (1987)6! 02121-84 D 1721-84(1988)" 0 1399 - 90 0 1468 - 84(1988)" D 1638 - 74" D 3988 -85 (1990)" D2191-84 D 2086-84 D 2193 -84 0 1631-850 3969 - 85(1990)" Terminology Relating to: I D 16-91 j Test Methodsfor: f 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 Add, 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 s < Formaldehyde Solutions, Concentration of Formaldehyde Solutions, Iron in , >> Formaldehyde Solutions, Methane! Content of Formic Acid in Glacial Acetic Acid Glycerin, High-Gravity, Testing '> Glycerin, Phthalate Ester Color of High Gravity (Discontinued 1991f) Iron in Paint Driers by EDTA Method Lead iri Pdint Driers by EDTA K&thod' 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 1989f- Replaced by Test Method D 2195) Paint Driers, Liquid-'. ' 5' : Pentaerythritol - 1 '' Rare Earth Metals, Total, in Paint Driers by EDTA-Method Styrene Analysis by Gas Chromatography ' - ! Styrene Monomer, Aldehydes in' Styrene Monomer, p-rert-Butylcatechol Inhibitor in Serene Monomer, Peroxides in '' Styrene Monomer, Polymer Content of Tricresyl Phosphate, Permanganate Time of Tricresyl Phosphate, Unsaponifiable Content of Tricresyl Phosphate, Volatile Matter in 1 Urethane Foam Isocyanate Raw Materials (Discontinued 199If) 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 531 DU P0502 97050 Test Methodsfor: D1063-51 (1987) D 1585-82 0 1064 - 58(1981) D 3008 -90 D 1240 - 82 D 509-70(1987) D 464-91 E 28 -- 67 (1982)61 D 269 - 52(1987)" D 1065 - 82 D 889-58(1987) Specifications for: D 3264 - 86 D 836-84 D 835-90 D 2359-90 D 4734 - 90 0 3055 - 90 D4C77- 91 D 3504-87 D 2439-91 D 2403 - 91 D2323-84(1989)I D2827 - 88" D 362-84 D 841-90 D 5211 -91 D 843-90 D 846-84 0 4076 - 86(1990) D5136-90 Test Methodsfor: D 847 - 91 D 848-81 (1989)" D 2119-87 D 2935-91 D 4492-85 (1989)" D 4534-89 D 1492-91 D 2324 - 81 (1989)" 0 5194 - 91 0 3627 - 82(1987)" 04789-88 D 3366-90 D 1686-81 (1990) D 4590-86 D 849-88 D 3439-89 D 3505-84" D 850-91 0 2232-81 (1986)61 D 1015-89 D 2870-86 D 853-91 D 5060-90 D 4961 -89 0 2120 - 87 D 3760-79 (1984) D2930-80(1989)" D 2360 - 82 (1987)" 0 4589 - 91 D 2340-82 (1987)" D2121-90 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 Roan Softening Point by Ring-and-Ball Apparatus Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark) Unsaponifiable Matter 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 199 It) Benzene-485, Refined (Nitration Grade) Benzene-535, Refined Benzene-545, Refined Cyclohexane 995 Isopropylbenzene (Cumene) .. Maleic Anhydride Phenol, Refined Pbthalic Anhydride-1308, Refined Pyridine, Refined Styrene Monomer 996 ,. Toluene, Industrial Grade (Discontinued 199 It) Toluene, Nitration Grade Xylene, Feedstock for p-Xylene Xylene, Nitration Grade Xylene, Ten-Degree (Discontinued 199It), o-Xylene 950 p-Xylene, High Purity Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons Add 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 , Qirbon Disulfide in Benzene Chloride, Trace, in Liquid Aromatic Hydrocarbons ... Color of CresyEc 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-tert-Butylcatechol 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 Adds 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-rert-Butylcatechol, in Styrene Monomer Isopropylbenzene (Cumene) by Gas Chromatography , Maleic Add 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 532 DUP050297051 ^ I cut mc(r((/Wi) ji/f. ' D3054-81 (1985) ? D1016-89 r D 4471 -85(1989)" * D 2031-84(1989)" D 852-87(199!) D1493 - 90 D 4493-89 D 5135-90 D 3962 -80 (1989)" D 3799-89 D 3961 -89 D 3626-85 (1990)" D1685-86 (1990) D4735-87 (1991)" D 1555-91 D 1631 -85 (1989)" D2030-84(1989)" D2306- 81 (1985) D 3797-88 D 3798 - 89 D1217-86 D1218-87 Practices for: D 3436 -91 D 4297 - 89 D 3437-89 D 3438 - 89 D 3852 - 90 Guide for: D 4588-87 Terminology of: D 4790-89a LIST BY SUBJECTS, VOLUME 06.03 Purity and Benzene Content of Cyclohexane by Gas Chromatography Purity of Hydrocarbons from Freezing Points Pyridine Bases in Cresylic Acid by Direct Titration Reducing Substances in Refined Pyridine Solidification Point of Benzene Solidification Point of Industrial Organic Chemicals Solidification Point of 4,4'-Isopropylidenediphenol (Bisphenol A) Styrene, Analysis of, by Capillary Gas Chromatography Styrene, Analysis of, by Gas Chromatography 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, Using Isatin 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 o-Xylene by Gas Chromatography p-Xyiene by Gas Chromatography Density and Relative Density (Specific Gravity) ofLiquids by Bingham Pycnometer (see Vol 05.01) Refractive Index and Refractive Dispersion ofHydrocarbon Liquids (see Vol 05.01) Aniline, Sampling and Handling 4,4'-Isopropylidenediphenol (Bisphenol A), Sampling and Handling Liquid Cyclic Products, Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride, Sampling and Handling Phenol and Cresylic Acid, Sampling and Handling p-Xylene, Analysis of (Discontinued 1992f--Replaced by Specification D 5136) Aromatic Hydrocarbons and Related Chemicals Specifications for: D 1193-91 E 100 - 81(1986) E 1-90 E 133-86 Reagent Water ASTM Hydrometers (see Vol 14.03) ASTM Thermometers (see Vol 14.03) Distillation Equipment (see Vol 14.02) Test Methodsfor: 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 Interlaboratory Study to Determine the Precision of a Test Method, Conducting Definitions of Terms Relating to: E 12 - 70 (1986) Density and Specific Gravity ofSolids, Liquids, and Gases (see Vols 04.02 and 15.05) METRIC PRACTICE Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related' Material section) 533 DUP050297052 Excerpts from Standard Practice for Use of the International System of Units (SI) (the Modernized Metric System)1 Following are excerptsfrom Standard Practicefor Use ofthe International System ofUnits (SI) the ModernizedMetric System E 380, which is available as a separate publication and which appears in its entirety in Volume 14.02. Deleted areAppendixesXI, X2, X3. and X4. Added is a table ofselected conversion factors from Appendix X3. CONTENTS ' . Section Scope................................................................................................................................. .................................. 1 SI Units and Symbols.................................................... ................... . ...................... ............:............. 2 Classes of Units............................. ............................... ......... .......... ,............... ,...................................... . 2.1 Base Units............................................................................................ ................. ................ .................... . 2.2 Supplementary Units ................................................... ........................ --............................... 2.3 Derived Units ..................................................................................................................... ............................... . 2.4 SI Prefixes............................................................................................ ^......... f..................'................................. 2.5 Application of the Metric System....................................... ;....................................................................................... 3 General..................................... ............................. ........................................................................................... 3.1 Application of SI Prefixes......................................................................................................................................... 3.2 Other Units.......................................................................................................................................................... . 3.3 Other Recommendations Concerning Units ........................................ ........................ ............. ..;......................... 3.4 Style and Usage...........................:.................................................. ......... ;............. ...................................... . 3.5 Rules for Conversion and Rounding............................. --' ............. ................ v.................... ........................... 4 General .................................... :................................................. ,.................................................................... . 4.1 Accuracy and Rounding..............................................................:........ ............................... ............................. . 4.2 Significant Digits..................................................................................................................................................... ,4.3 Rounding Values.......................... .................. .................................................. ............................................... 4.4 Conversion of Linear Dimensions of Interchangeable Parts............................. ............ ............................................ 4.5 Other Units............................................................................................................................................................ 4.6 Terminology ................................................................................................................................ ............................ 5 Appendixes Development of the International System of Units............... .................................................................................... XI Organs of the Metre Convention: BIPM, CIPM, CGPM............................................................................................. X2 Conversion Factors............................................................................................................................................... X3 Supplementary Metric Practice Guides......................................................................... X4 Bibliography Index - r f 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 Mesures). The name International System of Units and ihe international abbreviation SI2 were adopted by the 11th CGPM in 1960. 1.2 Information is included on 1, 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 general guidance on proper style and usage. 1.3 It is hoped that an understanding ofthe 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.JO 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, Le 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- 534 DUP0502970S3 E 380 TABLE 1 Base SI Units i Quantity3 Unit gength fjnass ftime iielectric current ^thermodynamic temperature'1' ^amount of substance ;iumlnous intensity metre kilogram second ampere kelvin mole candela * For a discussion of Celsius temperature see 3.4.2. Symbol m kg $ 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 j 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~`), and that for angular velocity, is the radian per second (rad/s or rad; s-1). 2.4.2 Those derived SI units which have special names and symbols approved by the CGPM 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 Om 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 dr 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 meads 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 Inductance Celsius temperature luminous flux illuminance activity (of a radionuclide) absorbed dose3 dose equivalent Unit hertz newton pascal joule watt coulomb volt farad ohm siemens weber tesla henry degree Celsius31 lumen lux becquerel gray sievert Symbol Hz N Pa J w c V Formula 1/s kg* m/s2 N/m2 N-m J/s A*s W/A F C/V Q V/A s AN Wb Vs T Wb/m2 H Wb/A C K(see 3.4.2] Im cd-sr lx lm/m2 Bq 1/s Gy J/kg Sv J/kg * Inclusion in the table of derived SI units with special names approved by the CIPM in 1976. 0 Related quantities using the same unit are: specific energy imparted, Kerma, and absorbed dose Index. stood and properly applied. Obsolete metric units and practices are widespread, particularly in those countries that long ago adopted the metric system, and much usage is improper. This section gives guidance concerning the limited number of cases in which units outside SI are appropriately used, and makes recommendations concerning usage and style. 3.2 Application ofSI Prefixes: 3.2.1 General--la general the SI prefixes (2.5) should be used to indicate orders of magnitude, thus eliminating^ nonsignificant digits and leading zeros in decimal fractions, and providing a convenient alternative to the powers-of-ten notation preferred in computation. For example:. 12 300 mm becomes 12.3 m 12.3 x 10? m becomes 12.3 km 0.00123 jxA becomes 1.23 nA 3.2.2 Selection--When expressing a quantity by a numer ical value and a unit, a prefix should preferably be chosen so that the numerical value lies between 0.1 and 1000. To minimize variety, it is recommended that prefixes repre senting 1000 raised to an integral power be used. However, three factors may justify deviation from the above: 3.2.2.1 In expressing area and volume,ithe prefixes hecto-, deka-, deci-, and centi- may be required, for example, square 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 millimetre is used for linear dimensions in mechanical engineering drawings even when the values lie far outside the range 0.1 to 1000 mm; the centimetre is often used for body 535 DUP050297054 E 380 TABLE 4 Quantity3 absorbed dose rate acceleration angular acceleration angular velocity area concentration (of amount of substance) current density density, mass electric charge density electric held strength electric flux density energy density entropy exposure (X and gamma rays) heat capacity Some Common Derived Units of SI Unit 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 par cubic metre volt per metre coulomb per square metre joule per cubic metre joule per kelvin coulomb per kilogram joule per kelvin heat flux density irradlance watt per square metre luminance magnetic field strength molar energy molar entropy molar heat capacity moment of force-4 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 mote kelvin newton metre henry per metre farad per metre watt per square metre watt per square metre stenadlan 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 4 See 3.4.4. Symbol Gy/s m/se rad/s2 rad/s m2 mol/ms A/m2 kg/m3 C/m3 V/m C/m2 J/m3 J/K C/kg J/K W/m2 cd/m2 A/m J/md J/(mol-K) J/(md-K) I'hm H/m F/m W/m2 W/(m2-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 t/m 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: V/m, not mV/mm, and MJ/kg, not kJ/g 3.2.4 Compomd Prefixes--Compound prefixes, formed by the juxtaposition of two or more SI prefixes are not to be used. For example, use 1 nm, riot 1 mum 1 pF, not 1 u j iF If values are required outside the range covered by the prefixes, they should be expressed by using powers of ten applied to the base unit. 3.2.5 Powers ofUnits--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. 1 cm3 =(10-2m)3 1 ns-1 = (10~9 s)-' 1 mm2/s = (I0~3 m)2/s =10_6m3 ?= IO9 s_l = tO-6 m2/s 3.2.6 Calculations--Errors in calculations pan be mini mized if thebase and the coherent derived"SI units are used and the resulting numerical values are expressed in powers- of-ten notation instead of using prefixes.. 3.3 Other 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 SJ (see Tabled): 3.3.2.1 Time--The SI unit oftime is the second. This unit is preferred and should be used ifpractical, 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 536 DUP050297055 TABLE 5 SI Prefixes Multiplication Factor Prefix 1 000 000 000 000 000 000 = 10' 1 000 000 000 000 000 = 10' 1 000 000 000 000 =10' 1 000 000 000 - 10 1 000 000 = 10 1 000 = 10 too = 10 10 = 10' 0.1 = 10-' 0.01 = 10" 0.001 = 10- 0.000 001 =10" 6.000 000 001 = 10- 0.000 000 000 oof = 10-' 0.000 000 000 000 001 = 10-' 0.000 000 000 000 000 001 = 10-' exa peta tera giga mega kilo hactc4 daka* deci'* centi'* milli micro nano pico femto atto * To be avoided where practical, except as noted in 3.2.2. Symbol E P T G M k h da d c m F n p f a K the minute and second is discouraged except for special fields Itsuch as cartography. K 3.3.2.3 Area--The SI unit of area is the square metre jjl(m2). The hectare (ha) is a special name for square hectometre (hm2). Large land or water areas are generally 1 expressed in hectares or in square kilometres (km2). It 3.3.2.4 Volume--The SI unit of volume is the cubic B- metre. This unit, or one of the regularly formed multiples M such as the cubic centimetre, is preferred. The special name fi litre1 (L)6 has been approved for the cubic decimetre, but use of this unit is restricted to volumetric capacity, dry measure, Xand measure of fluids (both gases and liquids). No prefix It other than milli* or micro- should be used with litre. 3.3.2.5 Mass--The SI unit of mass is the kilogram. This unit, or one of the multiples formed by attaching an SI prefix to gram (g), is preferred for all applications. The megagram jp (Mg) is the appropriate unit for measuring large masses such Iff as have been expressed in tons. However, the name ton has H been given to several large mass units that are widely used in H commerce and technology--the long ton of 2240 lb, the 1| short ton of 2000 lb, and metric ton of 1000 kg (also called m the tonne). None of these terms are SI. The term metric ton H. should be restricted to commercial usage, and no prefixes B| should be used with it. Use of the term tome is deprecated. | 5See Appendix XI.11.1. 1 4 The OGPM in October 1979 approved L and 1 as alternative symbols for litre. f. 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 Unit Symbol Definition time minute min 1 min a 60s hour h 1 h ae 60 min = 3600 s day d 1 d = 24 h = 86 400 s week, month, etc. plane angle degree O 1 - (*/180) rad minute'' ' 1' (1/60) second** (x/10 800) rad u 1" -- (1/60)' = (vr/648 000) rad volume mass litre metric ton L 1 L OB 1 dm3 = 10" m t 11 = 10 kg area hectare ha 1 ha 1 hm = 10* m A Use discouraged except for special fields such as cartography. 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 ofSI units) are to be avoided. Various categories of deprecated units are discussed in 3.3.4.1 to 3.3.4.4. 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 TAB(-E 7 Units in Use with SI Temporarily Quantity3 Unit Symbol energy [see 3.3.3.1] cross section pressure [see 3.3.0.2] activity (of a radionuclide) exposure (X and gamma rays) absorbed dose dose equivalent kilowatthour barn bar curie roentgen rad rem kWh b bar Cl R rd rem Definition 1 kWh SB 3.6 MJ 1 b nr 10_ m = 100 fm 1 bar - 10s Pa 1 Ci = 3.7 x 10' Bq 1 R 2.58 x 10-' C/kg 1 rd as 0.01 Gy 1 rem SB 0.01 Sv = 10 mSv DUP050297056 multiples and submultiples of SI units are to be avoided except for the litre (3.3.2.4), metric ton (3.3.2.5), and hectare (3.3.2.3). For example, do not use: fermi...........................1 fermi micron........................ 1 micron millimicron..................1 millimicron are..............................1 are gamma........................ 1 gamma . (magnetic flux density) 7 (mass).................... 1 7 X (volume)....................IX mbo............................ 1 mho candle................. ........ 1 candle candlepower................. I candlepower = 1 fm = 1(TIS m = 1 pm = 10"6 m = 1 nm = 10-9 m = 1 dam2 = 100 m2 -- 1 nT =1 pg = 1 pL =?. 1 mm3 =1 S = 1 cd = l ed 3.3.4.4 Miscellaneous Units--Other non-SI units that are deprecated include the following: calorie grade [1 grade = (t t /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: I 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 is used 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 FIG. 1 Illustration ot Difference Between Mass (Unit = kilogram = kg) and Force (Unit = newton = N) (see 3.4.1) 538 DUP050297057 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 offree 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 ofgravity") 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 ofgravity. 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 ofgravity 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 is 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 (r) is related to thermodynamic tem perature (7) by the equation: t=t -- t q 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 of1968. 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 Outside Diameter, inches (mm) Wall Thickness, inches (mm) Sch Sch Sch 40 80 160 1 1JI5 0.133 0.179 0.250 (33.40) (3.38) (4.55) (6.35) Likewise, a "2 by 4" is that in name only and refers to the approximate dimensions in inches of a rough-sawn piece of green lumber, the finished dimensions of which are consid erably less. A Va-20 UNC screw thread should continue to be identified in this manner. However, the controlling dimen sions of the part, such as the pitch, major, and minor diameters ofa screw thread, should be converted to SI values in accordance with 4.1 and 4.2. 3.4.3.2 Surface texture should be expressed in microm etres. 3.4.4 Quantities and Units used in Rotational Mechanics: 3.4.4.1 Angle, Angular Velocity, andAngularAcceleration. Their SI units are rad, rad/s, and rad/s2 respectively. In accordance with Sec. 2.3, since the radian is here taken to be dimensionless, the units 1, 1/s, and 1/s2 are also used when appropriate. 3.4.4.2 Moment ofForce (Torque or Bending Moment) is force times moment arm (lever arm). Its SI unit is N-m. 3.4.4.3 Moment of Inertia (/) is a property of the mass distribution of a body about an axis (/ = 2mr2). Its SI unit is kg-m2. 3.4.4.4 Angular Momentum (moment of momentum) is 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) times the angular velocity <a (rad/s or 1/s). 3.4.4.5 Rotational Kinetic Energy of a rotating body is equal to Its SI unit is J. 3.4.4.6 Rotational Work is equal to torque (N-m) times angle of rotation (rad). Its SI unit is J. 3.4.4.7 Torsional Stiffness (torsion constant) of a body is applied torque (N-m) divided by angle of twist (rad). ItrSI unit is N-m/rad.. 3.4.4.8 Centripetal Acceleration, v2/r or ofr, where v is the 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. No t e--Centripetal Force, equal to mass times centripetal accelera tion, is, like any force in SI, measured in newtons. 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: 539 DUP050297058 E 380 3.4.7.1 The values of so-called dimensionless quantities, as for example refractive index and relative permeability, are expressed by pure numbers. In these cases the corresponding SI unit is the ratio of the same two SI units and may be expressed by the number I. 3.4.7.2 Terms such as percent, parts per thousand, and parts per million may also be used. 3.4.7.3 In all cases, the meaning must be unequivocal. Expressions like "The mole fraction of C02 in the sample was 1.2 parts per million" or "The mass fraction of C02 in the sample was 1.2 parts per million" are permissible, but would not be permissible if the word "mole" in the first expression or "mass" in the second expression were not present. 3.5 Style and Usage--Care must be taken to use unit symbols properly, and international agreement provides uniform rules. Handling of unit names varies because of language differences, but use of the rules included here will improve communications in the United States. 3.5.1 Rulesfor Writing Unit Symbols: 3.5.1.1 Unit symbols should be printed in upright type regardless of the type style used in the surrounding text 3.5.1.2 Unit symbols are unaltered in the plural. 3.5.1.3 Unit symbols are not followed by a period except when used at the end of a sentence. 3.5.1.4 Letter unit symbols are written in lower-case (for example, cd) unless the unit name has been derived from a proper name, in which case the first letter of the symbol is capitalized (for example, W, Pa). The exception is the symbol for litre, L. Prefix symbols use either lower-case or upper-case letters as shown in 2.5.1. Symbols retain their prescribed form regardless of the surrounding typography. For symbols for use in systems with limited character sets, refer to ANSI X3.50 or ANSI/IEEE 260, as applicable. The symbols in ANSI X3.50 are intended for applications in the 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 this standard. 3.5.1.5 When a quantity is expressed as a numerical value and a unit symbol, a space should be left between them. For example, use 35 mm, not 35 mm, 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 threemetre 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 Rulesfor 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, kilohm, 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. i 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 ot 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 No t h --To avoid ambiguity in complicated expressions, symbols are preferred over words. 3.5.3.2 With unit symbols: Product, use a raised dot: -m for newton metre In the case of W j, 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 fortns: m/s or m'S 1 or-- In no case should more than one solidus be used in the same 540 DUP050297059 Session unless parentheses are inserted to avoid ambi|y. For example, write: J/(mol K) or J mol"' K~1 or (J/mol)/K, . nol J/mol/K 1.5.3.3 Symbols and unit names should not be mixed in same expression. Write: joules per kilogram or J/kg or J-kg~` fnot joules/kilogram nor joules/kg norjoules-kg-1 3.5.4 Numbers: f|3.5,4.1 The recommended decimal marker is a dot on the tie. When writing numbers less than one, a zero should be ritten before the decimal marker. 3.5.4.2 Outside the United States, the comma is often sed as a decimal marker. In some applications, therefore, he common practice .in the United States of using the ffpmma to separate digits into groups of three (as in 23,478) aay cause ambiguity. To avoid this potential source of anfusion, recommended international practice calls for eparating the digits into groups of three, counting from the decimal point toward the left and the right, and using a small pace to separate the groups. In numbers of four digits on father side of the decimal point the space is usually not pnecessary, 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 States but a million million (prefix tera) 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 ofcubic 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, nameplatesf^pf'labels, and in table headings, it is permissible to use the lS symbol followed by a space and the modifier in parentheses. For example: V (ac) and V (dc); 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 ofseven-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 the 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 concerning1 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 nr, 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 8 Recommended Pronunciation Prefix Pronunciation (USA)r* exa............................................................ex'a (a as in about) peta.................... ........... ..........................pet' a (a as in pet. a as in about) tera..........................................................as in terra firma giga........................................ ............. jig' a (/as in jig, a as in about) mega........................................................as In megaphone kilo............................................................kill' oh hecto....................................................... heck'toe deka............................... .......................... deck'a(aaslnabout) dec!......................................................... asincfec/mal cerrti......................................................... as In centipede mtlli...................Xs:.................................. as In military micro............. /...................................... as In microphone nano............. j......................................... nan' oh (an as in ant) pico..........................................................peek' oh femto.......................................................fern' toe (fern as in feminine) atto ..........................................................as in anatomy Selected Units Pronunciation candela. joule ... kilometre pascal. . siemens can dell' a rhyme with tool Still ' oh metre rhyme with rascal same as seamen's A The first syllable of every prefix is accented to assure that the prefix will retain its identity. Therefore, the preferred pronunciation of kilometre places the accent on the first syllable, nor the second. 541 DUP050297060 # E380 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 Vie 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 axe used to guide the determination of the proper number of significant digits in the converted values. Two different approaches to rounding of quantities are here described--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 IVts 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 V2 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) 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: l7/8 in = 47.625 mm exact 47.6 mm normal rounding 47.5 mm (approx) rounded to preferred number 48 mm (approx) rounded to whole number 4.2.2.2 A quantity stated as a limit, such as "not more than" or "maximum," must be handled so that the stated limit is not violated. For example, a specimen "at least 4 in wide" requires a width of at least 101.6 mm, or at least 102 mm. 4.3 Significant Digits: 4.3.1 When converting integral values of units, consider ation must be given to the implied or required precision of the integral value to be converted. For example, the value "4 in" may be intended to represent 4, 4.0, 4.00, 4.000, or 4.0000 in, or even greater accuracy. Obviously, the converted value must be carried to a sufficient number of digits to maintain the accuracy implied or required in the original quantity. 4.3.2 Any digit that is necessary to define the specific value or quantity is said to be significant. When measured to the nearest 1 m, a distance may be recorded as 157 m; this number has three significant digits. If the measurement had been made to the nearest 0.1 m, the distance may have been 157.4 m; this number has four significant digits. 4.3.3 Zeros may be used either to indicate a specific value, like any other digit, or to indicate the order of magnitude of a number. The 1970 United States population figure rounded to thousands was 203 185 000. The six left-hand digits of this number are significant; each measures a Value. The three right-hand digits are zeros which merely indicate the order of magnitude of the number rounded to the nearest thousand. The identification of significant digits is only possible through knowledge of the circumstances. For ex ample, the number 1000 may be rounded from 965, in which case only one zero is significant, or it may be founded from 999.7, in which case all three zeros are significant. 4.3.4 Occasionally data required for an investigatiorTmdst be drawn from a variety of sources where they have been recorded with varying degrees of refinement. Specific rules must be observed when such data, are to be added, sub tracted, multiplied, or divided. 4.3.4.1 The'rule for addition and subtraction is that the answer shall contain no significant digits farther to the right than occurs in the least precise number. Consider the addition of three numbers drawn from three sources, the first of which reported data in millions, the second in thousands, and the third in units: 163 000 000 217 885 000 96 432 768 477 317 768 Thermal indicates a precision that is not valid. The numbers should first be rounded to one significant digit farther to the right than that of the least precise number, and the sum taken as follows: 163 000 000 217 900 000 96 400 000 477 300 000 \ i ? 542 DU P050297061 E380 total is then rounded to 477 000 000 as called for by rule. Note that if the second of the figures to be added 'been 217 985 000, the rounding before addition would produced 218 000 000, in which case the 0 following would have been a significant digit. .3.4.2 The rule for multiplication and division is that the iduct or quotient shall contain no more significant digits are contained in the number with the fewest significant its used in the multiplication or division. The difference en this rule and the rule for addition and subtraction d be noted; the latter rule merely requires rounding of that lie to the right of the last significant digit in the precise number. The following illustration highlights difference: ultipiication: fi3.2 x 1.43 - 161.876, rounded to 162 ^vision: 5113.2 -s- l .43 = 79.16, rounded to 79.2 Mition: 113.2 + 1.43 = 114.63, rounded to 114.6 Subtraction: 113.2 - 1.43 = 111.77, rounded to 111.8 ae above product and quotient are limited to three signifiant 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. FJ 4.3.43 Numbers used in the above illustrations have all [Sjjbeen estimates or measurements. Numbers that are exact counts are treated as though they consist of an infinite plumber of significant digits. More simply stated, when a jjeount is used in computation with a measurement the Ipumber 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 1408. 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 Values'1: 4.4.1 When a figure is to be rounded to fewer digits than the total number available, the procedure should be as follows: 4.4.1.1 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 contaiiiing 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 converted 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 original gage. Method A--The use of this method ensures that even in 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 into 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., - 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 may increase the lower limit a maximum of 10 % ofthe tolerance arid decrease the upper limit a maximum of 10 % of the tolerance. (a) Proceed as in Method A step (a). (b\ Proceed as in Method A step (b). (cjRound each limit toward the interior of the tolerance, that is, tcTthe next lower value for the upper limit and to the next higher value for the lower limit.8 Examples: ' Adapted from ISO R370 (7). 8 If the digits to be rounded are zeros, the retained digits remain unchanged. 543 DUP050297062 E 380 A dimension is expressed in inches as................ 1.950 0.016 The limits are..................................................... 1.934 and 1.966 Conversion of the two limits into millimetres gives............................................................... 49.1236 and 49.9364 Method A--The tolerance equals 0.032 in and 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 for these two 49.13 and 49.93 limits are......................................................... This reduces the tolerance to 0.80 instead of 0.82 mm given by Method A. 4.5.2 Special Methodfor Dimensions with Plus and Minus Deviations--In order to 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 basic size and two deviations. However (except 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 toward 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. 4.5.3 Special Methods for Limitation Imposed by Accu racy ofMeasurements--If the increment of rounding for 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 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. 4.5.4 Positional Tolerance--If the dimensioning consists solely of a positional tolerance around a point defined by a nontoleranced basic dimension, the basic dimension must be converted to the nearest rounded value and the positional variation (radius) separately converted by rounding down 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 basic or gage dimension, such as when dimensioning certain conical surfaces, proceed as follows: (a) Round the converted reference gage arbitrarily, to the nearest convenient value. (b) 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. K (c) Round these limits in conformity with the rules in 4v& 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 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 employ 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 ordegrees 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) I (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 convertedjo 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 2.111TC rounds to 38 3"C. 1000 50F; implied accuracy estimated to be 20F. 537.7777 27.7777"C 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 0.000 04 0.000 4 0.004 0.04 0.4 0.000 4 0.004 0.04 0.4 Fineness of Rounding, mm 0.0001 0.001 0.01 0.1 1 544 DUP050297063 # E 380 spends 5.2 Certain terms used in this standard are defined as its of /Hows: terrain accuracy (as distinguished from precision)--the degree of ii fronj>nformity of a measured or calculated value to some irable cognized standard or specified value. This concept involves certaje systematic error of an operation, which is seldom mater/egligible. I limit approximate value--a value that is nearly but not exactly ally tjorrect or accurate. origfru coherent system of units--a system of units of measurej. ment in which a small number of base units, defined as :s g00dimensionally independent, are used to derive aU other units Ps thjpthe system by rules of multiplication and division with no jxsioj^iuwencal factors other than unity (see Appendix XI.9). md deviation--variation from a specified dimension or design eaci'fequirement, usually defining upper and lower limits (see also tolerance). digit--one of the ten arabic numerals (0 to 9). g to], dimension--a geometric element in a design, such as ilsius 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-pound units--units based upon the yard and the pound commonly used in the United States of America and defined by the National Institute of Standards and Tech nology. Note that units having the same names in other countries may differ in magnitude. nominal value--a value assigned for the purpose of con venient designation; existing in name only. precision (as distinguished from accuracy)--the degree of 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. of' .5 ' ic n! 545 / DUP050297064 # E 380 E 380 SELECTED CONVERSION FACTORS To convert from to atmosphere (760 mm Hg) board foot Btu (International Table) Btu (International Table)/h Btu (International Table)-in./s-ft2-F (fc, thermal con ductivity) calorie (International Table) centipoise centistokes circular mil degree Fahrenheit foot ft2 ft3 ft-lbf ft-lbf/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) lbf/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 metre (m2) degree Celsius metre (m) square metre (m2) cubic metre (m3) joule (J) watt (W) metre per second squared (m/s2) cubic metre (m3) 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 10-1 5.192 204 X 102 4.186 800* 1.000 000* x 10-3 1.000 000* 10~5 5.067 075 X lO"10 fC = (IT -- 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 0Q0* X 10-1 3.785 412 x 10"3 7.460 000* x 10+2 2.540 000* x 10~2 6.451 600* X 10-" 1.638 706 x 10"s 3.376 85 x 103 2.488 4 X 102 9.806 650* x 104 4.448 222 x 103 6.894 757 X 10s 2.957 353 X 10~5 2.780 139 x 10"1 2.834 952 X 10"2 3.051 517 X 10_1 3.390 575 X 10-2 7.489 152 4.731 765 X10-4 4.448 222 4.535 924 x 10~1 6.894. 757 x 103 --2.767 990 X 104 1.601 846 X 10 9.463 529 x 10~4 9.071 847 X 10z 1.333 22 X 102 3.600 000* x I03 9.144 000* x 10"1 8.361 274 x lO-1 7.645 549 X 10"1 546 r DUP050297065 Condensed Index of Committee D-l Standards--19921 This index references all standards under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, plus several others of auxiliary usefulness. It attempts to include what is relevant and exclude what is incidental to the concept of each standard. Being designed for Committee D-l usage it omits much of the detailed information provided in the regular more comprehensive index, the latter being intended for users with a broader range of product concern. It's structure employs cross-indexing from specific to general and vice-versa, with the objective of avoiding redundancy while guiding the user with dispatch to the desired and related material. The criterion for the selection of index terms is whether they might reasonably occur to an index user familiar with the technology of organic coatings. Index users encountering errors or other deficiencies should report them promptly by writing to ASTM Subcommittee DO 1.18 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 1 This index was developed by ASTM Committee D-l 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 lest, D96801) . Taber Abraser teat, D4060< I) wear resistance, of traffic paint, D913(I) wet abrasion/scrubbing, D2486,4213(1) Accelerated exposure tests See Exposure - accelerated Acetaldehyde acetaldehyde, spec., D47W(3) acidity, test, 02086(3) Acetate ester solvents purity, alcohol content. D3S45(2> Sa Amyl acetate n-Butyi acetate Ethyl acetate Hexyl acetate Isobutyl acetate Isopropyl acetate Methyl amyl acetate n-Propyl acetate Sa Glycol ether acetates Acetic add (glacial) formic acid in gl'aciai acetic acid, D3546{3) specification, D3620(3) Acetone acetone tolerance, of bodied oils, D19$0(3) alkalinity, test, 131614(3) permanganate time, test, D1363(3) specification, D329(3) Acetylene black, See Carbon black Acidity/alkalinity, (pH) acetaldehyde, spec., 04710(3) acetone, test, 01613,1614(3) chemically cleaned/etched, concrete, 04262(1) electrocoat baths, 04584(1) fatty quaternary ammon. chlorides, D208K3) formaldehyde solutions, test, D2379(3) hydroxypropyl methylcellulose, 02363(2) miliiequivalence, electrocoat baths, 04370(1) phenol-formaldehyde, 04613(3) pigments, D1203(2) volatile solvents, 01613(3) Acid number (value) fatty acids, 01980(3) lac resins, test, 029(2) organic coating materials, 01639(1) pine tars and pine tar oils, test, 0856(3) rosin oil, test, 01131(3) rosin test, 0465(3) tall oil, test, 0803(3) turpentine and pinene, test, 0233(3) Sa Saponifies dotvnumber Acid resistance (of patfhts/related coatings) clear coatings on aluminum, test, 03260(1) Acrylate esters, purity, D3362C3) Acrylic acid dimer content, 04415(3) specification, 04416(3) Acrylic emulsion paints, See Artists' Paints Adhesion/Cohesion by cut tape test, 03359(1) EHllon dynometer test, 04796(1) HIPAC coatings, 03730(1) portable tester, pull-off strength, 04541(1) prepainted fabricated metal, 04145(1) scrape test on smooth surfaces, 02197(1) traffic marking paints, materials,.04796(1) zinc-rich primer on steel D4146(1) Air blast abrasion tester, 0658(1) Alcohol resistance,'furniture lacquer, D2571(l) Alcohol solvents See Amyl alcohol 0319(3) n-Butyl alcohol (1-Butanol), 0304(3) sec-Butyl alcohol (2-Butanol), 01007(3) 2-Ethylhexanol, D50Q8(3) isobutyl alcohol (isobutanol), 01719(3) Isopropyl alcohol (isopropanol), 0770(3) Methyl isobutyl carbino!, 02635(3) Methanol (Methyl alcohol), D1152(3) n-Propyl alcohol (n-propanol), 03622(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, 01647(1) Alkyds/alkyd resins carboxylic acids content, 02455(2) fatty acids content 01398(2) isophthalic add content, 02690(2) phthalic anhydride content, 0563, 01306(2) pplyhydric alcohol, 01615,2456, 2998(2) Alkyds/alkyd resins (cont'd) rosin add content, 01469(2) silicon content 03733(2) test methods, selection of, 02689(2) unsaponifiable matter content, D1397(2) Sa Paints,solvent-reducible Aluminum (metal surfaces) add/mortar resistance^ coatings,D3260(l) preparation for painting, D1730, 01731(1) Aluminum powder and paste sampling/testing, 0480(2) . , specification, D962{2), Aluminum silicate (anhydrous) _ analysis, 0718(2) specification, 03619(2) Sa Pigments,general properties Aluminum silicate (hydrous) analysis, 0718(2) .specification, 0603(2) Sa Pigments, genera! properties Amidoamines, See Fatty amines Amino resins free formaldehyde content, D1979(3) test procedures, practice, D4277(2) nitrogen content, 01013(2) solvent tolerance test, 01198(2) Amines/amine values See Fatty amines Fatty quaternary/amine chlorides Amyl acetate, synthetic primary, D3540(3) Amyl alcohol (synthetic), spec., D319C3) Analysis See Chemical analysis Aniline sampling and handling, practice, 03436 (3) specification, 03264(3) 547 DUP050297066 Condensed index of Committee D-1 Standards Aniline point dipentene, related terpene solvents, D801(3) petroleum hydrocarbon solvents,D611(3) Anticorrosion 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(1) erosion test, high velocity water, D4938{1) erosion test, rotating drum, D4939(l) organotin release rate, D5108O) Anti-fungal pigments See Calcium borosilicate Zinc Oxide Antimony oxide analysis, D2350(2) analysis by spectrophotometry, 03717(1) Sa Figments,general properties Anti-sag meter, multinotch blade, D4400(l) Applicators, film See: Film application/applicators Architectural paints and coatings block resistance, D4946(l) color permanence, white enamels, D1543(l) brushability (brush drag), D4958(l) efflorescence of wall paints, D1736(l) film failures, exterior latex paint,' D1848(l) film porosity, 03238(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-borne, D3323(-l) water-borne, D3129(l) flat paints, solvent-borne, 03323(1) water-borne, D243K1) floor paints, solvent-borne, 03383(1) water-borne,03358(1) gloss and S/G, solvent-borne, 03425(1) water-borne, D4540(l) high performance (HIPAO, D3730(1) solvent-borne (general), 05146(1) water-borne (general), ih prep, guide for purchasing: . state and institutional, D3927(l) hiding power: brush application, visual, 0344(1) drawdown, reflectometric, D2805(l) roller application, visual, in prep, wet-to-dry hiding change, 05007(1) leveling, D4062(l) minimum film formation temp., D2345(l) package stability, D1849(l) porosity of films, 03258(1) print resistance, D4207(l) roller spatter, resistance to, D4707(l) sag resistance, D4400(l) washability: soilant, mechanical test, D3450(l) practical multi-stain test, D4828(l) wet abrasion (scrub) resistance: scrub-to-failure test, D2486(l) weight-loss test, 04213(1) Aromatic hydrocarbon solvents See High-flash aromatic naphtha Toluene Xylene Arsenic content in paint, 02348(1) Artists' paints drawdowns, preparation of, D4941(l) labeling for health hazards, D4236(l) lightfastness of pigments, D4303O) specifications acrylic emulsion, D5098(l) oil, acrylic, alkyd, resin-oil, 04302(1) water colors, D5067(l) tinting strength, D4838(l) Asbestine See Magnesium silicate Atlas Weatherometer, D5031(l) Automotive painting spray transfer efficiency, D5066(l) Bacterial resistance See Biodeterioration Baking, effect of overbaking, D2454(l) Ball drop method, for viscosity ,01343(2) Barium sulfate (barite, barytes) analysis, 0715(2) specification, 0602(2) Sa Pigments,general properties Basic carbonate white lead analysis, 01301(2) specification, 081(2) S a Pigments; general properties Basic lead silicochromate analysis, D1844(2) specification, D1648(2) S a Figments, general properties Basic sulfate white lead analysis, D1301(2) S a Pigments, general properties Bend testing mandrel bend test, 0522(1) Berlin white See Basic carbonate white lead Biocidal pigments See Ante-fouling pigments Anti-fungal pigments Biodeterioration (microbiological attack), emulsion paints in container, D2574(l) paint films: discoloration - exterior exposure, D3456(l) mold - environmental chamber, D3273(l) removal of fungal/algal growth, D4610 (1) soil/dirt/fungal accumulation,03274(1) Sa Anti-fouling paints Bituminous materials' water content, by distillation, D95(l) Black box exposure test accelerated outdoor exposure, D414K1) 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 See 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, D45S5(1) water fog test D1735(l) Blocking (block resistance) of architectural coatings, D4946<1) lacquers on metal substrates 03003(1) on wood substrates D2793(l) / Blue pigments, mixture, analysis of, 01135(2) Sa Iron blue Phthalocyanine blue Ultramarine blue Boiled oils (drying) See Linseed oil Bonding strength. See Adhesion/cohesion Bone black solvent extractable matter, D305(2) spec., D210(2) Sa Pigments, general properties Break test. See Fatty oils Bronze powders. See Gold bronze powder Brookfield viscometer, See Viscometers Brown pigments See Iron oxide Sienna, raw and burnt Umber, rawand burnt S 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(l) Brushes, paint See Paint brushes Bubble time method See Viscometers Burning Characteristics of liquid ingredients Equilibrium method, closed cup flash/no flash, D3934(3) flash point, D3941(3) Pensky-Martens (closed cup), D93(l,3) Seta flash tester (closed cup), D3278(3) Seta flaah tester (open cup) 04206(3) Sustained burning tes t, 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, D3806(l) Burnt sienna/umber - See Sienna, burnt and raw Umber, burnt and raw 1- Butanol Sec n-Butyl alcohol 2- Butanol See sec-Methyl ethyl alcohol _ 2-Butanone See Methyl ethyl ketone 2-Butoxy ethanol, spec., 0330(3) Butyl acetate alcohol content/purity, D35450) specification, D4615(3L- i ,_ Butyl acrylate purity test, D33620) specification, 03547(3) Butyl acrylatefmethacrylate monomer content of latexes, 04747(2) n-Butyl alcohol, specification, 0304(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, D3335(l) Calcium borosilicate analysis, D4487(2) specification, 04288(2) S a Pigments, general properties Calcium carbonate specification, D1I99(2) Sa Pigments,general properties Calcium content cellulose pulp (from wood/cotton), 04085(2) paint driers, by EDTA method; 02613(3) Calcium paint driers See Driers 548 DUP050297067 Condensed Index of Committee D-1 Standards Carbon-arc lamps See Exposure, accelerated Carbon blade pigment for paint, spec., D561(2) solvent extractable material, D305{2) Sa Pigments, general properties Carboxyl content, of cellulose, D1926(2) Carboxymethyl cellulose, sodium, DH439(2) Carboxylic acids, identification in alkyd resins, D2455(2) Castor oil, dehydrated spedficadon, D961(3) diene value, 01358(3) Sa Fatty oils Castor oil, raw specification, D96C(3) hydroxyl content, D19570) Sa Fatty oils Caulking/glazing compoundsand sealants viscosity, falling-rod-viscometer, 04040(1) Cellulose and cellulose derivatives acetate, butyrate and proprionate, P817(2) alcohol-benzene-soluble content, D1729(2) ashing, test methods, D3516(2) carboxyl content, test, D1926(2) cellulose acetate, test, D871(2), D365(2) cellulose nitrate. See Nitrocellulose chain length uniformity, D1716(2) chlorine content, test D264H2) chromatographic analysis, D1915(2) cold check resistance, lacquers, D121M1) definition of terms, D1695(2) dichloromethane-solubie matter, D397K2) ethoxyl substitution in cellulose, 194794(2) ethyl cellulose (EC) plastics, D914(2) ethyl cellulose pulp, metals content, 1)4085(2) hydroxyethyl cellulose, D2364(2) hydroxypropyl methylcellulose, D 2363(2) hydroxypropyl substitution, D3876(2) methoxy substitution, D3876(2) methylcellulose, test methods, D1347(2) moisture content, test, D1348(2) nitrocellulose. See Nitrocellulose silica content, test D2438(2) sodium carboxymethylcellulose, D1439{2) solubility in sodium hydroxide, D1696(2) sulfur content, D2929(2) viscosity, bail-drop method, D1343(2) viscosity, intrinsic, D1795(2) volatile/non-volatile of solutions, D4209(2) Centrifuge, See Vehicle separation Cerium paint driers. See Driers Certification ofconformance, form, D5063(l) Chalk, See Calcium carbonate Chalking exterior paints, D659, D4214(l) Channel black See Carbon black Char index See Burning characteristics Checking (check resistance) exterior paints, test D660(l) S a Cold checking Chemical Analysis See Pigments; analysis White pigments, analysis Chemical resistance, to: acid & mortar, of coated aluminum, D3260(l) alkali, of varnish films, D1647(l) alcohol, of wood furniture lacquers, D2571(l) household chemicals, of coatings, D1308(l) China day See Aluminum silicate (hydrous) Chinese blue See Iron blue China red See Chrome orange Chinese white See Zinc oxide Chip (chipping) resistance of coatings, D3170(l) of traffic paint, D913(l) Chlorinated phenol preservative content in wood products, D2921(l) Chlorine content cellulose, test, D2641(2) epoxy resins/compounds, test, D4301(2) hydrolyzable,of liquid epoxy resins, D1726(2) polyvinyl chloride. Dll56(2) toluene diisocyanate, D1638(3) total, of liquid epoxy resins, D1847(2) Chromaticity, See Color Chromatography See individual analysis references Chrome green analysis, D126(2) specification, D212(2) Sa Pigments (general properties) Chrome yellow and orange : analysis, D126(2) specification, D211(2) Sa Pigments, general properties Chromium content-lowconcentrations in air particulate filter samples, D4358{2) in paint, D3718(l) Chromium oxide green analysis, D126(2) specification, D263(2) Sa Pigments (general properties) Chromium pigments See Chrome green Chrome yellow and orange Chromium oxide green. Lead silicochrornate, Strontium chromate Zinc chromate CIE color system See Color-opaque materials Citron yellow See Strontium Chromate Clarity/cleanliness of paint and ink liquids, D2090 (3) Clay, See Aluminum silicate Cloud point aromatic hydrocarbon solvents, D4790(3) Coalescence latex paint films, low temperature, D3793C1) Coarse particle analysis See Dispersion (of pigments) Particle size (analysis/distribution)- Cobalt content paint driers, by EDTA method, D2373(3) paint, in low concentrations, D3335(l) liquid drier, analysis, D564(3) Coconut oil, See Fatty acids, tests, specs. Coefficient of friction See Slip resistance Coefficient of retroreflection See Retrore/lection/retroreflectors Coffee stains, resistance to of furniture lacquer, D2571C1) Cohesion, See Adhesion/Cohesion Coil coatings wire-wound bar application, D4717<1) guide for testing D3794<1) 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 materials CIE color system, E308(14.02) color difference,mstrumental, D2244C1) Colour Index, artist pigments, D4302C1) defining and evaluating tolerances, D3134C1) evaluating color change,gray scale, D2616(l) metamerism, visual evaluation, D4086(l) Munsell system, D1535(l) tristimulus values, D2244(l) visual evaluation of differences, D1729(l) Color retention discoloration: microbiological discoloration, D 3456(1) clear coatings in sunlight, D2620(l) household Chemicals, effect of, D1308(l) white architectural enamels, D1543(l) light fastness (fading): pigments in artists paints, D4303C1) printed matter, D3424(l) Color- transparent liquids and solids Gardner color scale, D1544 (1, 2,3) standard solutions for color tests: caramel/platinum-cobalt, D365(2) platinum-cobalt scale D1209(l,3) Compatability, coatings. Patch test, D5064(l) Concrete and masonry test panels, Dl743(l> pH, chemically cleaned/etched, D4262(l> surface cleaning (for coating), D4261,4258(1) Conditioningenvironment for !estingD3924(l) Conductance and conductivity of electrocoat baths, D4399(l) Cone-and-plate viscometers See Viscometers, 1CI Conformanceicerlification of, D5063(l) Conjugated oils See Dehydrated castor oil Oiticica oil Tung oil Sa Fatty oils, conjugated diene value Consistency, by Stormer viscometer, D562(l) Contrast ratio hiding power by reflectomehry, D2805(l) Copal content, of lac resins See Shellac - copal resin content Copper content cellulose pulp (from wood/cotton), D408512). copper pigments, test, D283(2) pine tars and pine tar oils, D856(3) Copper corrosion in aromatic solvents, D849(3)............. in dipentene & related tgfpenes, D8Ctl<3) - in petroleum products, D130(3) S a Exposure tests Copper phthaiocyanine blue and green See Phthaiocyanine blue Phthaiocyanine green Copper powder analysis, D283(2) specification, D964(2) 5s Pigments, general properties Com oil. See Fatty acids - tests, specifications Corrosion resistance See Exposure' Cotton seed oil See Fatty acids - tests, specifications Covers, paint roller See Faint rollers; covers Cracking (crack resistance) exterior paints, evaluating, D661(l) mandrel bend test, D522(l) Cross-cut, cross-hatch tape test adhesion of paint, test, 03359(1) Cuprous oxide analysis, D283(2) specification, D912(2) See Figments, general properties 549 DU P0502 97068 Condensed index of Committee D-1 Standards Cure time, thermosetting resins, D4640(2) Sa Drying/curing Curtain coating, water reducible, D4712(l) Dark chrome yellow See Chrome yellow and orange Definitions of terms related to paint, varnish, etc., D16(l,2,3) Dehydrated castor oil See Castor oil, dehydrated Fatty acids - tests, specifications Density--apparent (bulk) hydroxyethelcellulose, 02364(2) hydroxypropyl tnethylcellulose, D2363(2) methylceliulose, D1347(2) sodium carboxymethylcellulose, D1439(2) Density-true dipentene/terpene solvents, D80K3) " industrial aromatics, D2935(3) paints and related coatings, D1475(l) paint liquids, D1963(3) pigments, tests, Dl53(2) pine oil, 0802(3} pine tars and oils, D8S6(3) turpentine arid pinene, D233(3) Deposition efficiency of powder coatings, D3451(1) Detergent resistance, D22480) Dew cycle. See Exposure tests - accelerated Diacetone alcohol, spec., D2627(3) Diamines, See Fatty diamines Diatomaceous silica. See Silica Dibutyl phthalate, spec, D608(3) Dichlormethonc, determination of by gas chromatography, D4457(l) Diethlene glycol, spec. D2694(3) Pillon Dynamometer, See Adhesion/cohesion Dilution ratio/Dilutability cellulose nitrate solutions,D1720(3) cellulose nitrate, with toluene, D30K2) resin solutions, D5062(3) Dimethyl ketone. See Acetone Dip application water reducible coatings, D4717(l) Dipentene (and related terpene solvents) sampling and testing, D8Q1(3) Dipropylene glycol specification, D2696<3) Dipropylene giycoi monomethyl ether (DPGME) specification. D4836(3) purity, D4773(3) - Dip-type viscosity cups, See Viscometers Directional reflectance See Reflectance and reflectivity Dirt/Soil resistance exterior white coatings, D3719C1) practical washability, D4828(l) 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(l), (2) dispersion stability, phthaio blue, D963(2) in pigment-vehide systems, Dl210(l) in printing inks, NFIR1 grindometer, D1316(l) in titanium dioxide slurries, D3926(2) Distillation dipentene, terpene solvents, D80H3) distillation range, D1078(3) ethyl acetate, spec.,D4614(3) in vacuum, solvent-type paints, D3272(l) petroleum products, D86(3) pine oil, D802(3) pine tars and tar oils, 0856(3) turpentine and pinene, D233(3) Dolomite, See Calcium carbonate Draft test, varnish films, D1643(l) Drawdown bars and rods See Film application/applicators Draw-down tests, multi-notch applicators leveling characteristics of paints, D4062(l) leveling of paints, D2801 (discontinued) sag resistance of paints, D440O(1) Driers calcium/zinc content, EDTA, 02613(3) cerium content test D3970(3) darity/cleanness, visual, D2190(l,3) cobalt content EDTA method, D2373(3) iron content, EDTA method, D2374(3) manganese content EDTA method, D2375(3) ; rate earths content, EDTA method, 03989(3) selection of test methods, D564(3) specification, D600(3) vanadium content EDTA method,D3988(3) volatile/nonvolatile content, D4140(3) zirconium content EDTA method, D39690)' Drop black, See Bone black Dry film thickness^ee Film thickness, dry film Drying oils. See Fatty oils Drying /curing cellulose nitrate, 0301(2) MEK resistance, zinc-rich primers) D4752(l) room temperature, film formulation, D1640(l) shellac varnish, D1650(2) temperature during curing by I.R., 03259(1) thermosetting resins/cure time, D4640(2) ultra-violet cured coatings, D3732(l) Durability, See Exposure tests Dutch white. See 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 EDTAmethod, paint driers caidum content, D2613(3) cobalt content, D2373(3) iron content, D3804(3) lead content, D2374(3) manganese content, D2375(3) rare earths content, D3989(3) vanadium content, D3988(3) zinc content, D2613(3) zirconium content, D3969(3) Efficiency , See Deposition efficiency (powder coatings) Transfer efficiency-spray application Efflorescence exterior latex paints, D1848(l) interior wall paints ,D1736(1) Elasticity, of varnishes, test, D 1642(1) Electrical insulating solids shellac specifications, D784(2) shellac, test methods, D411(2) Electrocoat baths Add/base milliequivalency, D4370(l) Guide for testing, D1978(l) pH measurement, D4584(l) Electrostatic deposition See Powder Coatings Electrostatic spray water-redudble coatings, D4712(l) Elongation mandrel bend test, D522(l) tensile strength/stiffness,free films, D2370(l) Emulsion vehicles (for paints/related coatings) freeze-thaw resistance, D2243(l) minimum film formation temp., D2354(2) Sa Latex vehicles Environment, standard conditioning for testing coatings, D39240) thermosetting (molding) compounds,01013(2) Erosion resistance of exterior paints, D662(l) 5 a 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, D1652(2) epoxy content, D1652(2) guide for testing, D4142(2) hydrolyzable chlorine content, D1726(2) Ester Value of solvents and thiiihers, 01617(3) Ether-alcohols See Glycol ethers 2-Ethoxy ethanol, specification, D331(3) 2-Ethoxyethyl acetate alcohol content/piirity, D3545(3) specification, D3728(3) Ethyl acetate alcohol content/purity,'D3545(3). specification, D4614(3) Ethyl acrylate ethyl acrylate, spec., D3548(3) purity, D3362(3) Ethylene giycoi -* ." specification, D2693(3) Ethyleneglycol monobutyi ether See 2-Butoxyethanol -- Ethylene glycol monoeihyl ether . Sec 2-Ethoxy ethanoh * Ethylene glycol monomethyl ether See 2-Metboxy ethanol 2-Ethylhexanol, analysis, D5008(3) 2-EthylhexyI acrylate, spec., D3541(3) Ethyl silicate, zinc-rich primer - MEK resistance, D4752(l) Evaporation rate, volatile liquids, D3539(l) Exposure - accelerated-corrosive environment cyclic salt spray/humidity/cold D2933(l) filiform corrosion on steel, 02803(1) method for evaluating corrosion, D1654(l) Exposure - accelerated -water/humidityrtight black box/Fresnel reflector rack, D4141(l) carbon arc lamp - dew cycle, 03361(1) carbon arc lamp/unfiltered, D822(l) carbon arc lamp, enclosed. Atlas, D503K1) controlled condensation, D4585(l) fluorescent UV/condensation, D4S87(1) 100% humidity chamber, D2247 (1) wood panel substrates, D3S8 (06. xenon arc/water spray, G26(l) 550 - DUP050297069 Condensed Index of Committee D-1 Standards Exposure testing* exterior Fatty ails (drying oils) Fischer reagent method (for water content) house paints on new wood, D1O06(1) absorption (by pigments), 0281,1483(2) See Karl Fischer reagent method paints on steel surfaces, D1014,5065(1) acetone tolerance (heat-bodied oils), D195O0) Fish oil in drying oils and fatty acids, 037250) quantifying dirt collection, D3719<1) ash content, 01951(3) Sa Fatty oils recording results on standard forms, 01150(1) break test, 01952(3) Flake brass See Gold bronze powder wood panel substrates, D358(l) darity/cleanliness, visual, 02090(1 3) color after heating, test, D19670) Flaked powders See Aluminum powder and paste Extender pigments conjugated diene value, D13580) Flake white See Basic carbonate white lead See Aluminum silicate (clay) content, of solvent paints, 022450) Flaking (flake resistance) Barium Sulfate (barytes) definition of terms, 0555(3) exterior paints 0722(1) Calcium carbonate (whiting) film formation rates, drying, D1640(l) Flammability/fire retardancy Magnesium silicate (talc) Gardner color scale, 01544(1,2,3) See Burning characteristics Mica Pumice gel time, test, D19550) iodine value, test, D19590) Flash point--liquids See Burning characteristics Silica, diatomaceous loss on heating, D196O0) Flat paints, interior Exterior paints and coatings sampling, D14660) solvent-home, test guide, D3323 See Architectural paints and coatings. saponification value, D19620) water-borne, test guide, D2931 Exposure testing selecting test procedures, guide, D414O0) specific gravity at 25/25"C, test, D19630) Flexibility impact resistance, 02794(1) Fatty oils (drying oils) - (cont'd) mandrel bendtest, 0522(1) testing methods, D5550) on prepainted metal sheets,D4145(l) Factory applied finishes S ee Industrial finishes, water-borne unsaponifiable matter content, D19650) Flocculation - of pigments, test for, D963(2) unsaturation, Rosenmund-Kuhnhenn, D15410) Floor paints/coatings Wood finishes unsaturation, Wijs method, D19590) clear floor sealers, 01546(1) See Color retention Sa Castor oil, raw solvent-borne, test guide, 03383(1) Falling-rod viscometer See Viscometers Castor oil, dehydrated water-borne, test guide, 03358(1) Falling sand method. See Abrasion resistance Fish'oil ' Flow and flow rate Fatty adds--general Linseed oil See Rheological properties definition of terms, D14670) Oiticica oil Foots, in raw linsded oil sampling, D1466(3) Safflower oil gravimetric method, 01966(3) testing methods, D2575(3) Soybean oil volumetric method, D19540) Fatty acids--specifications Sunflower oil Ford cup. Sec Viscometers coconut oil, t>1841(3) Tall oil Formability com oil, D18420) Tung oil Impact-Wedge bend test, 03281(1) cottonseed oil, Dl843(3) Fatty quaternary ammonium chlorides zinc-rich primer on steel, D4146(l) dehydrated castor oil, 01539(3) add value, tests, D2076(3) Formaldehyde linseed oil, D1538(3) . amine value, test, D2O7B0) ' acidity test, D23790) soybean oil, D1537(3) ash content, test, D2077C3) in amino resins, D19790) tall oil, 01984(3) iodine value, D2078(3) iron content, test, 02087(3) Fatty acids--tests nonvolatile matter, D2O790) methanol content, test, 02380(3) acid value, 01980(3) molecular weight, D2O8O0) specification, 02378(3) ash content, D195K3) pH, test, D2O810) Forms clarity/cleanness, D2090(l, water content, D2O720) certification of conformance, 05063(1) color after heating, 01981(3) recording exposure test results, 01150(1) fish oil content, D3725(3) Ferric oxide/Ferrite See Iron oxide pigments Fouling _ Gardner color scale, D1544C1,2,3) Ferrous iron in iron oxides, 03872(2) See Anti-fouling paints hydroxyl content, D1957(3) Field identification/anaiysis Free films (organic coatings) iodine value, D19590) of structural coatings, D5043(1) preparation, tensile properties, 02370(1) rosin add content, D11240(3) Filiform corrosion resistance , preparation of, D4708(l) saponification value, 01962(3) of organic coatings, 02803(1) ' Freeze - thaw resistance -- solidification point, D19820) S a Exposure tests-accelerated-corrosive multicolored lacquers, 02337(1) specific gravity, test, D19630) Film application/applicators water-borne paints, 02243(1) titer test, 01982(3) artists' paste paints, practice, 04941(1) French blue See Iron blue unsaponifiable matter, 01965(3) blade applicators, D823(l) French chalk See Magnesium silicate Fatty acids content producing uniform films, D823(l) French ocher See Ocher alkyd resins, D1398(2) t. methyl esters, D1983,3457(3) wire-wound (Meier) rods, 04147(1) Film formation, emulsion vehicles Fresnel reflector rack exposure accelerated outdoor metal exposure D414K1) solvent paints, D2245(3) minimum temperature (MFFT), 023540) Friction, static coefficient. See Slip resistance tall oil rosin, test, D1585(3) Film porosity. See Porosity Fuel oil t solvent resistance tall oil test, D803(3) Film thickness gages of traffic paints, D2792(l) Fatty amines, amidomines, diamines dry films Fungicidal (fungistatic) pigments amine content, D2083(3) by indsion cut, Tooke gage, 04138(1) See Anti-fungal pigments amine values, D2073,2074(3) on non-ferrous metals (eddy), 01400(1) Fungus resistance/fungirides iodine value, Wijs, D2075(3) on steel, magnetic gage, D1186 See Biodeterioration isocyanates test, 01638(3) using micrometers, 01005(1) Furnace black. See Carbon black non-amine content, D2082C3) wet films test methods, amidomines, 02071(3) eccentric wheel, 01212(1) water content, 020720) Interchemical and Pfiutd gages, 01212(1) notched gages, 04414(1) Galvanized surfaces Fatty nitrogen compounds Films, organic coatings. See Free films See Steel panels/pipe/tube/sheet identification in solvent paints, 02245(3) Fineness of grind (dispersion) Gardner-Coleman method non-amine content, D2O820) See Oispersion oil absorption of pigments, D14830) test methods, D2071(3) Fire retordancy/flammability Gardner color scale water content, test,02072(3) See Burning characteristics transparent liquids, test, 01544(1,2,3) 551 DUP0502 97070 Condensed Index of Committee D-1 Standards Cardncr-Holdt viscometer tubes Halo-silane coated glass plates See Viscometers for preparation of free films, D4708(l) Gas checking, draft test, varnish films, D1643(l) Halphen-Hicks test Gasoline resistance, of traffic paints, D2792{1) rosin content of varnishes, D1542(l,2) Gel time Handling material See Materials handling drying oils, test, D1955(3) Hardness testing, of organic films tar adds, test D2870(3) Glass panels Knoop indentation tester, KHN, D1474(D Koenig pendulum test, D4366(l) surface prep for testing coatings, D389H1) pencil test, D3363(l) Class beads (in traffic paint) Persoz pendulum test, D4366(1) analysis for D4797(l) Pfund indentation tester, PHN, D1474(l) sieve analysis, D1214(2) Sward rocker test, D2134(l) test for roundness of, D1155(2) Hazards, fire and health Gloss (specular) and Sheen . change, washability of coadngs, D4823(l) handling analine, 03436(3) handling cresyiic acid, phenol, D3852(3) effect of household chemicals, D1308C2) handling naphthalene, D343S(3) gloss differences, visual evaluation, D4449(l) in protective coatings, D3630(l) haze of high gloss finishes, D4039(l) labeling art materials, D4236(l) high gloss, goniophotometer, test, E430O) Haze See Gloss measurement of gloss and sheen, D523(l) Heat resistance of organic coatings tolerances, conformance evaluation, D3134(l) on steel, D2485 (1) uniformity of brushouts, test, 03928(1) effect of overbaking, D2454(l) Gloss paints Heatset-type printing inks See Architectural paints non-volatile content, D4713(l) Glycerin--high gravity Hegman scale sampling/testing, D1258(3) fineness of dispersion, pigments, D 1210(1) spedfication, D1257(3) Hematite See Iron oxide red . Glycidal ethers n-Heptane chlorine content in epoxy resins, D4301(2) flash/fire point of liquids, test, 01310(3) Glycols Heptane miscibility See Miscibiity See Diethylene glycol, D2694(3) Hexanes commercial, specification, D1836(3) Dipropylene giycol, 1)2696(3) Hexyl acetate, spec., D51370,). Ethylene glycoi, D2693(3) Hexylene glycoi, specification, DZ636(3) Hexylene glycoi, D2636(3) Hiding power (of paints/coatings) Propylene glycol, D2695(3) brushouts, visual, relative, D344(l) Glycol ethers drawdowns, reflectometry, D2805(l) See Dipropylene glycol monomethyi ether roller application, pracfical, visual. In Prep, Ethylene glycoi butyl ether wet-to-dry change, visual, P5007(l) , Ethylene glycol ethyl ether High-flash aromatic naphthas, D37340) Propylene glycol monomethyl ether High performance (HIPAC) coatings, D3730(l) Glycol ether acetates High-purity (reagent) water, spec., D1193(3) See Ethylene glycol ethyl ether acetate High shear (IQ) viscosity, D4287(l) , Propylene glycoi methyl ether acetate Sa Brushability Gold bronze powder Horizontal pull test, static friction, D4518(l) analysis, D283(2) Household chemicals, specification, D267{2) resistance to, of organic coatings, D1308(l) S a Pigments, general properties House Paints See Architectural paints Green pigments , Humidity resistance , of coatings See Chrome green humid-dry cycling, on wood, D345911) Chromium oxide green humidity, on steel, D2247(l) Phthalocyanine green humidity-thermal cycle on steel, D2246(l)__ Grind, of pigment, dispersions S a Water resistance See Dispersion/fineness of grind Hunter, visual gloss differences, D4449(l) Grindometer, NP1RI Hydrocarbon solvents See Printing inks See Aliphatic hydrocarbon, solvents Dispersion/fineness of grind Aromatic hydrocarbon solvents Guide for Solvents, general test procedures assessing aged coatings on steel, D5065(l) Hydroquinone content in vinyl acetate, D2193(3) painting inspectors, metal substrates,D3276(l) Hydroxyethylcellulose, testing, D2364(2) Guides for testing (selection of methods) Hydroxyl content See Architectural paints and coatings cellulose acetate, D871(2) Coil coatings cellulose acetate, butyrate, D817(l) Electrocoat baths fatty oils and acids, D1957(3) Epoxy resins Hydroxypropyl methylcellulose, D2363(2) Industrial finishes Hydroxypropyl substitution Lacquers in cellulose ether products, D3876(2) Latex vehicles Powder coatings IC1 cone/plate viscometer, D4287(l) Solvents Sa Brushability Impact resistance, flexibility test, D2794(l) Gum rosin Imprinting See Print resistance See Rosin Inclined plane test, static friction, D451S(1) Halogenated solvents Indentation hardness See Hardness Testing analysis for, in paint, D4457(l) Index of refraction See Refractive index Indexes, specialized, of standards and tests Architectural coatings, D2833(l) Sa Guides for testing Indian red See Iron oxide red Industrial finishes water-borne, lest guide, D1712(l) Inert pigments See Extender pigments Infrared pyrometry (thermometers) for wood coatings, cure cycle, D3259(l) 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, D154K3) fatty amines, Wijs test, D2075(3) fatty quaternary ammon. chlorides, D2078(3) lac resins, test, D29(2) Wijs test, D1959(3) Iron blue analysis, D1135(2) spedfication, D261(2) Iron oxide black natural/synthetic-analysis, D3872(2) synthetic., spec., D769(2) See Pigments, general properties Iron oxide brown (natural) analysis, D50(2) specification, D3722(2) S a Pigments, general properties Iron oxide brown (synthetic) analysis, D3872(2) specification, D3724(2) Sa Pigments, general properties Iron oxide red (natural) analysis, D50(2) spedfication, D3722(2) Sa Pigments, general properties Iron oxide red (synthetic) analysis, D50(2) ----- specification, D3721(2) S a Pigments, general properties Iron oxide yellow analysis, D50(2) " specification, D76S(2) - ,' S a Pigments, general properties Iron paint driers See Driers Iron Oxides, ferrous iron content, D3872(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, D163813) isocyanate groups in urethanes, D2572(2) Isophorone, specification, D2916(3) Isophthalic acid content alkyd and polyester resins, test, D2690X2) Isopropanol See Isopropyl acetate Isopropyl alcohol alcohol content/purity, D3545(3) Isopropyl acetate (99% grade), spec., D3131(3) Isopropyl alcohol, specification, D770(3) Kaolinite, Kaolin See Aluminum silicate Karl Fischer reagent, water content, D4017(l) Kauri-butanol value, D1133(3) 552 DUP050297071 Condensed Index of Committee 0-1 Standards methyl n-amyl ketone, spec., D436O0) purity, test, D2192(3) Ketone solvents See Acetone, D329(3) Diacetone alcohol, D2627(3) Isophorane, D261913) Methyl amyl ketone, D4360(3) Methyl ethyl ketone, D740(3) Methyl isoamyl ketone, D2917(3) Methyl isobutyl ketone, D1153{3) Knife test, for paint adhesion, 03359(1) Knoop hardness tester, D147411) Koenig pendulum test, hardness, D4366(1) Sa Hardness testing Labeling art materials for health hazards, 04236(1) Lacquer cellulose nitrate content, D3133(l) definition of, D16(l,2,3) ester value, of lacquer solvents, D1617(3) freeze/thaw test, multicolored, D23370) guide for testing, D333(l) imprint resistance (of dried films), D2091(l) particle size analysis(multicolored),P233B(l) plasticizer migration, vinyl fabrics, D2199(1) selection of test methods, D333(l) stain removal (multicolored lacquer) D2198(l) temperature-change resistance, test, D1211(l) testing wood furniture lacquers, D2571(l) viscosity by dip type viscosity cups, D4212(l) viscosity by Ford viscosity cup, D1200(l) Lac resins See Shellac Lampblack solvent extractable matter, test, 0305(2) specification., 0209(2) Lampblack content, test, D305(2) Lapis lazuli See Ultramarine blue latex paints -- See Architectural paints Latex vehicles filter-retained solids content, D5097(2) guides to test procedures, 04143(2) nonvolatile content, 04758(2) unreacted monomer content, 04827,4747(2) 5 a Emulsion vehicles Lead chromate pigments See Chrome yeltowand orange Chrome green Molybdate orange Lead content, analysis air particulate filter samples, D4358(2) basic lead silico-chromate, D1844(2) leaded zinc oxide, test, 03280(2) paint driers, D2374, 564(3) red lead pigments, test, 049(2) traffic marking material/ D4797(l) white linseed oil paints, D215(l) yellow, orange, and green pigments, 0126(2) Lead pigments See White lead Lead chromate pigments Basic lead silicochromate Red lead Leaded zinc oxide Lead silicochromate See Basic lead silicochromate Lead molybdate See Molybdate orange Lead oxide See Red lead Leaded zinc oxide, analysis, D3230(2) Leafing properties aluminum powders/pastes, D4B0(2) Leveling (ropiness) of paints, test, 04062(1) Lleberman-Storch test rosin content of varnishes, 01542(1,2) Lightfastness of printed matter, D3424(l) of pigments used in Artists' Faints, 04303(1) S a Artists' paints Color retention Limonite See Ocher Linseed oil boiled, specification. D260(3) raw, specification, D23413) Sa Fatty oils Foots in raw linseed oil Oil absorbtion (ofpigments) Fatty acids - tests, specifications Liquids, darity/cleanliness, visual, D2090C1, 3) color, by Gardner scale, 01544 (1,2,3) density and specific gravity, D3505(3) liquid/solid state, characterization, D4359(l) S a Burning characteristics Magnesium silicate analysis, D717<2) specification, 0605(2) Sc Pigments, general properties Maleic anhydride color, by platinum cobalt scale, 03366(3) maleic arid content, 02930(3) sampling and handling; practice, D343SO) specification, D3504(3) Mandrel bend test flexibility of organic coatings, D522(l) Manganese content of drier, D564, 2375(2) of cellulose pulp, 04085(2) Mar resistance under development by D0123 Marine coatings See Antifouling paints Masonry exposure test panels, prep., D1734(l) Masonry treatments See Water repellents MEHQ content See Methyl ether of hydroquinone Meier rods See Film applicators MEK resistance of ethyl silicate-zinc rich primer, 04752(1) Menhaden fish oil See Fatly oils Mercuric oxide analysis, 0284(2) specification, D911(2) Mercury content in mercuric oxide, D284(2) in paint (low concentrations), D3264(l) Metal powder pigments See Aluminum powder and paste Copper powder Gold bronzepowder Zinc dust Metal substrates,coatings on accelerated outdoor exposure, D4141CU adhesion, by cut/tape test, D3359(l) blistering-evaluation of, 0714(1) coil coatings, D3794(l) flexibility/adhesion-deformed, D4145(l) mandrel bend test, D522(l) primers, testing practices, 03322(1) Metamerism, visual evaluation, D4086(l) Methacryiic acid (glacial 98.5%) specification, D3845(3) Methanol (methyl alcohol) acetone content of, D1612 (3) content, in formaldehyde solutions, 02380(3) permanganate time, test, D1363(3) specification, 01152(3) Methoxyl content hydroxypropyl methylcellulose, 02363(2) methylcellulose, 01347(2) Methoxyl/hydroxypropyl substitution by Zeisel-gas chromatography, D387612) Methyl acrylate, specification, D4709(3) Methyl alcohol. See Methanol Methyl amyl acetate, D2635(3) Methyl amyl alcohol See Methyl isobutyl carbinol Methyl amyl ketone purity, by gas chromatography, D3893(3) Methyl butyl ketone purity, by gas chromatography, D3893(3) Methylcellulose See Cellulose and cellulose derivatives Methytcyclohexone purity from freezing point, test, D1016(3) Methyl esters, fatty arid composition, D1983(3) preparation from fatty acids,, 03457(3) preparation from oils, D2800(3) Methyl ether of hydroquinone (MEHQ) content of monmomeric acrylate esters, D3125(3) Methyl ethyl ketone 99.5% grade, spec., D3729(3) purity, by gas chromatography, D2S04C3) spec., 0740(3) Methyl isoamyl ketone purity, by chromatography, D3893(3) spec., 02635(3) Methyl isobutyl carbinol, spec., D2635(3) Methyl isobutyl ketone analysis by gas chromatography, 03329(3) spec., D1153(3) Methyl methacrylate unreacted monomer in latexes, 04827,4747(2) Methyl n-amyl ketone 98% grade, spec., 04360(3) Methylo! group content in phenolic resins, test, 04706(2) Metric practice--SI Units, excerpts, E3800,2,3) MFFT See Film formation, emulsion vehicles Mica pigment analysis, D716(2) ., spec., 0607(2) Microbiological attack See Biodeterioration Microcoulomelry See Coulometiy Micro-organism resistance See Biodeterioralion Migration of plasticiser from vinyl fabrics to lacquers, test, D2199C1) Milliequivalency, acid/base Bee Electrocoat baths MUori 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 sandmill method color and strength of pigments, 03022(2) Minimum film formation temperature (MFFT) See Him formation, emulsion vehicles Miscibility lacquer solvents, with heptane, D1476(3) water soluble solvents, with water, D1722(3) Mixed aniline point dipentene/terpene solvents, test, 0801(3) 553 DUP0502 97072 Condensed Index of Committee D-1 Standards Modulus of elasticity, 2370(1) Moisture content blue pigments, D1135(2) capillary moisture in concrete, 04263(1) cellulose acetate, test, D871 (2) cellulose, test, D1348C2) ethylcelluiose, test, D914(2) hygroscopic moisture in pigments, 0280(2) hydroxyethylcellulose, test, D2364(2) hydroxypropyl methylcellulose, D2363(2) Karl Kscher method, D4017O) lac resins, test, D29(2) liquid naval stores, D890(3) methylcellulose, test, 01347(2) pine oil, D890(3) pine tars and pine tar oils, test, D856{3) sodium carboxymethylcellulose, D1439(2) tall od, test, D803(3) Moisture vapor permeability See Permeability Mold resistance See Biodetefioratibn Molybdate orange analysis, D126(2) spedflcation, D2218(2) S a Pigments, general properties Molybdenum content molybdate orange, D126,2218(2) Mortar resistance of dear coatings on aluminum, D3260(l) Mottling failure, exterior latex paints, D1848(l) Mud-cracking failure, exterior latex paints, D18480) Muller device color/tinring strength of pigments, D387(2) Multinotch applicator tests sag resistance of paints, D4400(l) leveling of paints, 04062(1) Multi-panel forms for recording results, D1150(l) Munsell color system specifying color by, D1535(l) Nacreous pigments, no standard Naphtha and naphtha derivatives high-flash aromatic naphthas, 03734(3) VM&P naphtha, D3735(3) Sa Hydrocarbon solvents National Printing Ink Research Institute NPIRI, See Printing Inks Naval stores def. of terms, 0804(3) volatile/nonvolatile content, D4140(3) water content, D890(3) S a Terpene solvents Newtonian liquids See Viscometers (viscosity) Nitrocellulose base solutions, test methods, 0365(2) content in alkyd lacquers, D3133(l) dilution ratio for solutions, D1720(3) testing, D301(2) Nitrogen content cellulose nitrate, test D301(2) nitrogen-containing plastics, D1013(2) resins and plastics(total), test, 01013(2) Nonleafing aluminum pigment See Aluminum powder and paste Nonvolatile/volatile content aluminum powders/pastes, 0480(2) coatings, by volume, D2697(l) driers/naval stores, 04140(3) emulsions, resin solutions, 04209(2) guide to test methods, 02832(1) latices, test, D475B(2) pigment dispersions, D4139(2) printing inks/resin solutions, test, D4713(l) resin solutions, test, 01289(2) shellac varnish, test, D1650(2) silane/siloxane masonry treatments, D5095(1) titanium dioxide slurries, D3926(2) varnishes, test, D1644(l) volatile solvents, test, 01353(3) Notched gages Him thickness measurement, 04414(1) Notched film applicators See Multinotch applicator tests NPIRI See Printing inks Ocher analysis, D50(2) spedflcation, D65(2) Odor test volatile solvents and diluents, 01296(3) Oil absorption (of pigments) Gardner-Coleman method, D1483(2) Spatula rub-out test, D28H2) Oil content artists' paints, spec., 04302(1) solvent-borne paints, D2245(3) Oil resistance electrical insulating varnish, D115(l) wood furniture lacquers, 02571(1) Sa Fuel oil resistance Oils See Fatty oils (Drying oils) Mineral oil Pine oil Rosin oils Oiticica oil chloroform-insolubles, D1958(3) gel rime, 01955(3) specification, D60H3) Orange pigments See Molybdate orange Chrome yellow and orange Organotin release rate of anti-fouling paints, D5103(l) Overbaking (of paints/related coatings) effects of overbaking, D2454(l) Oxirane epoxy content of epoxy plastics, 01652(2) Package stability coatings for ultraviolet curing, D4144(l) emulsion paints, biodegradation, D2574(l) freeze-thaw resistance, D2243(l) sampling liquid paints, D3925(l) settling of traffic paint, D869(l) solvent and water-bome paints, 01849(1) Paint brushes preparation for evaluation, 05068(1) Paint inspection See Inspection of paint application work Paint thinners Set' Thinners Paint rollers, covers preparation for evaluation, 05069(1) Panel forms (single/multi), D1150(l) Panel preparation for tests See Steel panels Para (paranitraniline) red analysis, 0970(2) spedflcation, 0475(2) S a Pigments, general properties Paris red See Red lead Paris white See Calcium carbonate Paris yellow See Chrome yellow and orange Particle size (analysis/distribution) coarse particle content, 0185(1,2) pigments, reporting characteristics, D1366(2) polymeric powder properties, D3451(l) white extender pigments, D3360(2) Pastes in oil (ofpigments) See Pigment dispersions Patch test, coating compatability, D5064(l) Pavement marking paint See Traffic paint Peariescent pigments See Nacreous pigments Peen plating See Coatings--mechanically deposited Pencil test, film hardness, 03363(1) Pendulum test hardness of coatings, D4366(l) Penetration--paint films See Porosity Pensky-Martens closed, flash point, D93 (1,3) Pentaerythfltol/peittaerythritoi content methods for testing, D2195(3) monopentaerythritol content, D2999(3) of alkyd resins, D1615(2) Permanganate time acetone and methanol, test, 01363(3) tricresyl phosphate, test, D1721(3) Permeability, to moisture vapor, of organic films, 01653(1) Peroxide content of styrene monomer, test, D234CK3) Persian gulf oxide See Iron oxide red Pfirsoz pendulum test See Hardness Perspiration resistance of HIPAC coatings, D3730(l) Petroleum spirits See Mineral spirits Ffund gage See Film thickness measurement Pfund indentation hardness See Hardness pH See Acidity/Alkalin ity Phenol, in phenolic resins, 01312(2) __ Phenolic resins (Phenol formaldehyde) apparent pH, D4613(3) free phenols content, Di312(2) methylol group determination, 04706(2) stroke cure time, 04640(2) ... ' volatile content, 04639(2) Phthalic anhydride color in molten state, D3366(3) content in alkyd resins, D563,1306(2) sampling and handling, D3438(3) spedflcation, D2403(3) Phthatocyanine (phthalo) blue analysis, D1135, D3256(2) spedflcation, 0963(2) 5 a Pigments, general properties Phthalocyanine (phthalo) green chemical analysis, D3256(2) specification, D3021(2) S a Pigments, general properties Pictorial stds, steel surfaces, 02200(1) Pigment content/paints and dispersions paint/traffic marking material, 04451(1) pigment pastes in oil, test, 01208(2) solvent paints, D2371, 2698(1) titanium dioxide slurries, D3926(2> water-based paints, D3723(l) Pigments--analysis and specifications see individual pigment names 5s Pigments-coior categories White pigments, chemical analysis 554 DU P050297073 Condensed Index of Committee D-1 Standards `[Figments--color categories ` See Black pigments i Blue pigments I-. Brown pigments Glass beads Green pigments Inert pigments (Extenders) Metal powder pigments Nacreous pigments Orange pigments ' Red pigments White hiding pigments Yellow pigments I "Pigments--composition categories See Earth pigments Iron oxide pigments Lead chromate pigments Chromium pigments .* Pigments--function categories : See Anti-corrosion pigments Anti-fouling pigments 1 Anti-fungal pigments Colorant pigments j Extender pigments (inerts) " White hiding pigments Pigments--general properties fj bleeding characteristics, D279(2) composition acidity/alkalinity, 01208(2) > ignition loss 01208(2) moisture content, 0280,01208(2) volatile content; 04139(2) s. water soluble salts content, D2448(2) lightfastness in artist paints, 04303(1) oil absorption Gardner-Coleman method, 01483(2) Spatula, rub-up test, D281(2) particle size characteristics, reporting of, D1366(2) j course particle content, 0185(2) fineness of dispersion paint, D1210(l) fineness of grind, printing ink, D1316(l) particle size distribution, D3360(2) specific gravity, D153(2) tinting strength and color colored pigments -- with mechanical muUer,D387(2) with miniature sand mill, 03022(2) white pigments-- visual method, 0332(2) instrumental method, D2745{2) Pigments--in paints and dispersions See Dispersion/fineness of grind Lightfastness Pigment content Slurries White pigments/rhemical analysis Pine oil moisture content, D89CK3) sampling/testing, D802(3) Pine tar/pine tar oils sampling and testing, D856(3) Pinholing film failures of exterior latex paints, 01848(1) Plasticizer migration ' vinyl fabrics to lacquers, D2199(l) j Plastics coatings for plastic substrates, D3002(l) epoxy content, D1652(2) Platinum-cobalt solutions, color scale See Color Polyester resins See alkyds Polyhexafluoropylene (FEP) substrate for preparation of free films, 04708(1) 1 Polyhydric alcohols content See Alkyds Polymeric powders/powder coatings test procedures, practices, 03451(1) Polymerization cellulose nitrate, test, 01716(2) dipentene/terpene solvents, test, D233(3) unreacted monomer of latexes, D4747(2) Polymerization inhibitors butylcatechol in styTene, D2120(3) Polymerization time electrical insulating shellac, D411(2) Polymers silicons^ilicon content, 03733(2) solubility range, test, D3132(2) Polyurethanes See Urethanes Polyvinyl butyral resins See Resins--polyvinyl butyral Polyvinyl chloride (PVC) chlorine content, test, D1156(2) residual vinyl chloride, D368CK2) test procedures, guide; D4368(2) Porosity, of paint films, 03258(1) Potash blue See Iron blue Powder coatings See Polymeric powders/powder coatings Practices See individual standard practices 5 u Guides for testing Precisian See Statistical methods Primers ethyl silicate - zinc rich MEK resistance, cure test, 04752(1) formahility on steel, D4146(l) test guide, on pre-formed metal, 03322(1) Primrose chrome/yetlow See Chrome yellow and orange Print resistance of lacquers, D209K1) of architectural coatings, in preparation Printed matter evaluating lightfastness, 03424(1) Printing inks and vehicles apparent tack, inkometer test, 04361(1) fineness of grind, NIP1RI method, D1316(l) Ughtfastness, printed matter, D342401) nonvolatile content, D4713(l) tinting strength, in prep, viscosity, by falling-rod, D4040O) water pick-up, D4942(l) S a Resins, Resin solutions 1- Propanol See n-Propyl alcohol 2- Propanone See Acetone Propionyl content cellulose acetate propionates, D817(2) Propyl acetate, normal alcohol content/purity, D3545(3) 90-92% grade, spec., D3130(3> n-Propyl alcohol, spec., D3622(3) Propylene glycol monomethyl ether PGME, purity, D4773(3) spec., 4837(3) Propylene glycol monomethyl ether acetate PGME acetate, purity, D4773(3) spec, 04835(3) Propylene glycol, spec., D2695(3) Prussian blue See Iron blue Pull-off strength (bond strength) See Adhesion/Cohesion Pull test, static friction, 04318(1) Pumice/pumice stonefpumacite specification, D867(2) Purchasing, state/institutional, D3927(l) Rare earths content -wwJ! paint driers, by EDTA method, 03989(3) Raw oils (drying oils) See Fatty oils Raw sienna/umber See Sienna, burnt and raw Umber, burnt and raw Reagent water microelectronic processing, spec., 01193(3) reagent water, spec., D1193(3) Red copper oxide (77402) See Cuprous oxide Red iron oxide See Iron oxide red Red lead analysis, D49(2) specification, 083(2) Sa Figments, general properties Red oxide of mercury See Mercuric oxide Red pigments See Iron oxide red (synthetic/natural) Para (paranitraniline) red Red lead Toluidine red Venetian red Reflectance and reflectivity gray scale, evaluating color change, D2616(l) hiding power by reflectometry, 02805(1) instrumental color difference, D2244(l) Munsell color system, D1535(l) of opaque specimens, E97(l) preparation of reflectance standards, E259(l) specific luminance, traffic coatings, 04061(1) Reflective markers in traffic paint See Glass beads Refractive index dipentene/terpenes, 0801(3) pine oil (natural/synthetic), D802(3) turpentine and pinene, test, D233C3) Repellents, See Water repellents Reporting paint film failures ^ of exterior latex paints, D1848(l) Reproducibility and Repeatability See Statistical methods Resin solutions, general properties clarity/cleanness, 02090(1,3) cloud point, 05062(3) ___ dilutability (solvent tolerance), .05062(3) Gardner color scale, 01544(1,2,3) nonvolatile, ink vehicles, D4713(l) nonvolatile matter content, test, 01259(2) std. color solutions, 0365(2), D1209(l,3) unsaponifiable matter, D1397(2) viscosity, test, D1725(2) Resins,general properties softening, ring and ball, E28(3) solubility/range, test, 03132(2) volatile/nonvolatile, D4209(2) volatile resin adds, 03008(3) water content, Karl Fischer, test, D40X7(1) Resins, various types See Aikyd resins Amino resins Epoxy resins Phenolic resins Rosin Shellac (lac) Urethanes Vinyl resins 555 DUP050297074 m Condensed Index of Committee D-1 Standards Resistance properties/resistance to See Abrasion resistance Acid resistance Alcohol resistance Alkali resistance Bleeding Biodeterioration Blistering Blocking Checking Chemical resistance Chip (chipping) resistance Coffee stains Corrosion resistance Cracking (crack resistance) Detergent resistance Discoloration Erosion resistance Exposure (weathering) Flaking' Fuel oil/resistance Fungus resistance Gas checking Gasoline resistance ' Heat resistance Household chemicals Humidity resistance Impact resistance Light resistance Mar resistance Microbiological attack Microorganisms Mold resistance Mortar resistance Oil resistance Overbaking Perspiration resistance Print resistance Sag/sagging resistance Salt spray resistance Scratch See Mar resistance Scrub resistance Slip resistance Soil/dirt resistance Solvent resistance Spattering (spatter resistance) Stain resistance Water resistance Wear resistance Wet abrasion (scrub) resistance Retroreflection (horizontal coatings) traffic paints, specific luminance, D4061(l) Rheological properties/non-Newtonian coatings Brookfield viscometer, D2196(l) ICI core/plate viscometer, D4287(l) S a Viscometers (viscosity) Ring-and-ball apparatus softening point, of resins, E28<3) Road service testing See Traffic paint Rocker hardness test (Sward) See Hardness Roller application, of paint hiding power,practical, D5150(l) spatter resistance, D4707(l) Rollers, paint See Paint rollers^ covers Ropiness (of paints). See Leveling Rosenmund-Kuhnhenn method iodine value of drying oils, D15410) Rosin add number, D46S(3) ash, burning residue iron content, D1(IM(3) sampling and grading, D509(3) saponification number, D464(3) tall oil rosin-fatty adds, D1585(3) unsaponifiable matter, D1Q65(3) toluene insolubles, D2693(3) volatile oil conte,n, D889(3) volatile resin adds content, D300S(3) Rosin add content coating vehicles, D7469(2) fatty adds, test, D1240(3) rosin oil, test, D1131(3) tall oil, test, D803O) lac resins, test, D29(2) Lieberman-Storch test, D1542(I,2) Rosin esters rosin adds contend D1469(2) Rosin oils, testing of, D1131(3) Rouge See Iron oxide red Rub-out test (pigments) , See Oil absorption (pigments) Rusting-degree-photographic standards on painted steeLsurfaces, D610(l) Safflower oil spedfication, D1392{3) Sa Fatty oils Sag resistance test Using a multinotch applicator, D4400(l) Salt spray (fog) resistance with acetic acid, B287, 117(1) Sampling liquid paints & pigmented coatings, D3925(l) Sand abrasion test falling sand method), D968(l) Sandstone, architectural preparatory surface deaning, D5107(l) Saponification number/value drying oils, fatty adds, D1962(3) lac resins, test, D29(2) rosin, test, D464(3) tall oil, test, D803(3) 5 a Unsaponifiable matter content Saybolt viscometer See Viscosity Scaling See Flaking Scattering coefficient _____ absolute values (hiding power), D2805(l) white pigments, relative values, D2745(2) Scratch resistance See Mar resistance Scrub (wet abrasion) resistance See Wet abrasion (scrub) resistance Sealants See Caulking/glazing compounds Sealers (floor) See Floor paints/coatings Semi-gloss paints See Architectural paints Seridte See Mica Setaflash tester See Burning Characteristics Settling traffic paint, accelerated, D1309 traffic paint, in containers, D869(l) Set-to-touch-time See Drying properties Sheen See Gloss and Sheen Sheet metal (with organic coating) flexibility/adhesion of the coating, D4145(l) mandrel bend test, 0522(1) Shellac (lac resin) bleached shellac spec., D207(2) copal resin content, D29(2) for electrical insulation, D411, 784(2) orange shellac and other lacs, spec., D237(2) sampling and testing, D29(2) shellac varnishes sampling and testing, D16S0(2) spedfication, D360(2) volatile/non-volatile content, D4209{2) SI units (International System of Units) metric practice, excerpts, E380,(l,2,3) Sienna (burnt and raw) analysis, D50(2) specification, D765(2) Sa Figments, general properties Sieve analysis glass spheres, used in traffic paint, D1214(2) pigments, practice for reporting, D1366(2) pigments and dispersions, (D185(2) Silanes, siloxanes See Water repellents Silica, diatomaceous analysis, D719(2) spedfication, D604(2) Silicate pigments See Aluminum silicate Caldum borosilicate Calcium silicate Magnesium silicate , . Silicone-coated paper preparation of free films, D4708(l) Silicone polymers silicon content by spectrophotometry, D3733 Skinning See Stability--package Slip resistance, static friction test D2518(l) Slurries titanium dioxide conten~D3926(2) Soapstone See Magnesium silicate Softening point organic coatings, test, D21340) -- resins, ring and ball apparatus, E28(3) Soil accumulation, on paint films degree of surface disfigurement, D3274(l) Soil/dirt resistance (removal)' ' practical washability,~D4828(l) . -- Solid/Liquid state, characterization, D4359(l) Solids content See Nonyolatile/volatile content Solubility tests cellulose in sodium hydroxide, D1696(2) cellulose nitrate, D301(2) solubility range (resins/polymers), D3132(2) Solvents See Solvents-chemical types Solvent resistance Solvents, test procedures, general Solvents-chemical types See Acetate ester solvents Alcohol solvents . Aliphatic hydrocarbon solvents' Aromatic hydrocarbon solvents Ester solvents Glycols Glycol ether acetates Glycol ethers (ether-alcohols) Halogenaied solvents Hydrocarbon solvents Ketone solvents Terpene solvents 556 DU P050297075 Condensed Index of Committee D-1 Standards . Solvent resistance Steel surfaces, unpainted Texture alcohol, cm furniture lacquer, 02571(1) pictorial standards of condition, D2200(l) gloss differences of similar surfaces, 04449(1) gasoline/fuel oil, on traffic paint, 02792(1) profile of abrasive - cleaned steel, D44170) Thermalvoltaic infrared thermometers MEK, of ethyl silicate primer D4752{1) - test panels, preparation of, D609(l) See Infra-red pyrometry So'lvents-iest procedures, general Steel surfaces, painted Thermistor infrared radiation `*'"TM'"deters analysis, cluomotography, 03271(1) See Exposure, accelerated See Infra-red pyrometr clarity/cleanness, D290(1, 3) Exposure^ exterior Thermosetting resins evaporation rate, D3S39 Stiffness of free 0ms, D237Q(1) stroke cure dine of phenolics, D4640(2) halogenated, in paints, analysis, D4457(l) Stormer viscosity (consistency) Thickness--paints/related coatings hydrocarbon solvents of paint, D562(l) producing uniform films, D823(l) acidity, test, D1613(3) of pine -ars and pine tar oils, 0856(3) 5a Film thickness measurement aniline point, 0611(3) Strip (copper tarnish) test Thinners See Mineral spirits. Turpentine, benzene content, 04367(3) copper corrosion in petroleum products, D130(3)| VM &P Naphtha Kauri-butanol test, 01133(3) Stroke cure time S a Solvents odor (characteristic/residual), 01296(3) thermosetting phenolic resins, D4640{2) Thixotropy sampling/test procedures, D268(3) Strontium chromate, analysis, D1845(2) rotational (Brookfield) viscometer, D2196(l) water content, by Fischer reagent, Dl365(3) S a Pigments, general properties Sa Viscometers identification in paint, 02349(1) Structural coatings Tinting strength lacquer solvents,heptane miscibility, Dl476(3)j field identification/analysis, 05043(1) chromatic paints, 04838(1) water miscibility, D1722(3) Sulfide content printing inks, in prep, Solvent tolerance See Resin solutions white pigment, bom paint, D235H2) white pigments, instrumental, 02745(2) Sulfur content white pigments, visual, D332(2) Soybean oil cellulose materials, D2929(2) colored pigments, D387,3022(2) degummed, specification, 0124(3) white pigment, from paint, D2352(2) Sa Pigments, general properties refined, specification, 01462(3) Sunflower oil Titanium dioxide So Fatty oils specification, D3169(3) Sa Fatty oils analysis of and for Fatty acid tests, specifications Surface analysis anatase/rutile ratio, D3720(2) Spattering (spatter resistance) adhesion, tests, D454K1) atomic absorption spectroscopy, D 4563(1) roller application test, D4707C1) gloss differences, visual evaluation, D4449(l) by X-ray spectroscopy, 0 4764(1) Spatula rub-out test gloss goniephototneter, E430(l) chemical analysis, D1394(2) See Oil absorption, pigments profile, blast cleaned steel, D4417(l) in traffic marking paint, D4797(l) Specific gravity static friction, D4518(l) slurry-solids content, D3926(2) of pigments, D153(2) Surface preparation^--for painting specification, 0476(2) Specific luminance, horizontal coating abrading of concrete, D4259(l) tinting strength, instrumental, 02745(2) traffic stripe paint, 04061(1) acid etching of concrete, D4260(l) dnting strength, visual, D332(2) Specific permeability aluminum (hot-dip), D1731(l) Sa Pigments, general properties See Moisture vapor permeability aluminum/aiuminum-alloy surfaces, D1730(l) Titer Spectroscopic analysis architectural sandstone, D5107(l) fatty adds, test, t>1982(3) acrylic polymer in emulsion paint, 03168(1) concrete/masonry panels, D1734(l) Toluene antimony content flow cone), D3717(l) galvanized steel, non-passivated, D220K1) industrial grade, spec. 0362(3) cellulose nitrate in alkyd lacquers, D3133(l) glass panels, D389H1) toluene insolubles in rosin, D269(3) chromium content (low cone), D3718(l) magnesium alloys, D1732C1) volume and weight calcuiatiSns, D15555(3) diene value, dehydrated castor oil, D13S8(3) steel test panels, D609(l) Toluidine red identifying separated vehicle solids, D2621(l)| Sustained burning test analysis, D970(2) iron content (of rosin), 01064(3) Seta-flash tester (open cup), D4206(3) specification, D656(2) lead/cadmium/cobalt, D3335(l) Wick test, D4207(3) Tooke gage. See Film thickness, dry films _ lead/chromium in pigment dust, 04358(2) Sward rocker See Hardness testing lead content in paint, 04834(1) mercury contentflow concentration), D3624C1) Traffic paint metal content of cellulose pulp, 04085(2) Taber abraser test. See Abrasion resistance adulteration of vehide solids,'D2743(l) sulfur content of cellulosics, D2929(2) Tack, ofprinting inks, Inkometer, D436K1) bleeding, over tar and' asphalt, D969(l) titanium dioxide in paint, 04563,4764(1) Tag cup See Burning Characteristics bleeding, photographic standards 0868(1) traffic paint vehicle adulteration, D27430) Talc See Magnesium silicate conducting road sendee tests, D7130) Specular gloss See Gloss and Sheen Tall oil, test methods for, 0803 degree of chipping, D913C1) Spoilage See Biodeterioration Sa Fatty oils degree of settling, 0869(1) Package stability Tall oil rosin glass spheres, roundness, 01155(2) Spray application Fatty acids--tests, specifications glass spheres, sieve analysis, D1214(2) See Transferefficiency Tall oil rosin fuel oil/solvent resistance, D2792(l) Spreading rate fatty adds content, D1585(3) gasoline resistance, D2792(l) hiding power of paints, D344, 2805(1) volatile resin acids content, D3008(3) no-pick-up (drying) time,D711(l) Stability--package See Package stability pigment content, by ashing, D445K1) Stain resistance practices for testing, D2205(l) coffee stains, D 2571(1) Tar See Pine tar/pine-tar oils retroreflectance/specific luminance, D406K1) of factory applied wood finishes,.D3023(l) Temperature tests settling during storage, D1309(l) of multicolor lacquers, 02198(1) freeze-thaw resistance, D2243(l) wear life/resistance, D913.(l) of organic finishes, 01308(1) low-temperature coalescence, D3793CU Transfer effidency-spray application . -- of transportation industry finishes, D1540CU minimum film formation temp. D2345(2) under laboratory conditions, D5009(l) of wood furniture lacquer, D2571(l) Tensile properties, of free films, D2370(l) under production conditions, D5066(1) 5a Washability, Porosity Terpene solvents Tribasic lead phosphosilicate Static friction tests (slip resistance) See Dipentene, Pine Oil, Turpentine analysis, 02742(2) inclined plane/horizontal pull, D4518(l) Terra alba See Calcium sulfate spedfication D2744(2) Statistical methods Terra de sienna See Sieruia (burnt and raw) Tributyltin See Organotin release rate for interlaboratory testing, E691(3), D3980(l) Test results See Forms for recording Trichloroethane determination Steel blue pigment See Iron blue Testing, interlaboratory practice, D3980(l) by gas chromatography, D4457(l) 557 DUP050297076 Condensed Index of Committee D-1 Standards Tricresylphosphate permanganate time, 01721(3 specification, D363(3) unsaponifiable matter content, 01399(3) volatile matter content, D1468(3> Tristimulus values See Color - opaque materials Tung Oil gel time, test, D1955(3) quality determination, D1964(3) raw, specification, D12(3) Tunnel methoditwo foot tunnel) fire retardancy of paints, 03806(1) Turkey red See Iron oxide red Turkish umber See Umber (burnt and raw) Turpentine pinene composition, 03009(3) sampling and testing, D233(3) specification,.013(3) Two-foot tunnel method fire retardancy of paints, D3806(l) Ultramarine blue analysis, D1135(2) specification, D262(2) Ultraviolet-cured coatings cure time, reporting of, D3732(l) package stability, 04144(1) Ultraviolet exposure, D4587(l) Umber (burnt and raw) analysis, 050(2) specification, D763(2) Units, SI, metric, E380OA3) Unsaturation (in drying oils and derivatives) Rosenmund-Kuhnhenn method, D1541(3) Wijs method, D1959(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, 02572(2) isocyanate raw materials, D1638<3) methyl ethyl ketone in, spec., D3729(3) UV See Ultraviolet-cured coatings Ultraviolet exposure Vanadium content paint driers, EDTA method, D3988(3) Varnishes abrasion resistance:. air blast, D658(l) falling sand method, D968(l) acid value, test, D1639(l) acrylic acid, spec, 04416(3) bleached lac varnish, testing, D1650(2) clarity/cleanness, visual, D2090(l,3) def. of terms, 016(1,2,3) density, test, D1475(l) discoloration (light stability), 02620(1) household chemicals, effect, D13Q8(1) elasticity or toughness, D1642(l) elongation/tensile strength, 02370(1) exterior durability, test, 01641(1) drying at rpom temperature, D1640(l) flash point, test, 03278(3) Gardner color scale, D1544(l, 2,3) gas checking and draft test, D1643(l) humidity resistance, D2247(l) indentation hardness, test, D1474(1) moisture vapor permeability, 01653(1) nonvolatile matter content, D1644(l) preparation of free films, D4708(l) preparing glass panels for testing, D389K1) Varnishes (continued) preparing steel panels for testing, D609(l) rosin adds content, D1469(2) rosin content, Ueberman-Storch, D1542(l,2) rosin content, Halphen-Hicks, D1S42(1, 2) scrape adhesion test, D2197(l) selection of test procedures, D154(l) shellac varnish, testing, D1650(2) specific gravity at 25/25C, 01963(3) test environments, D3924(l) viscosity, dip-type viscosity cups, 04212(1) viscosity. Ford cup, D1200(l) volatile/nonvolatile content, 04209(2) water and alkali resistance, D1647(l) water immersion test, D670(l) weathering tests on wood, D358(l) wet film thickness, D1212,4414(1) Vehicles, solvent type, pigmented . centrifuge for pigment content, D2371,2698(1) centrifuge for vehide separation, D2372(l) non-volatile content, printing inks, D4713 solids identification, infra-red, 02621(2) Venetian red, analysis, D50(2) S a Pigments, general properties Vinyl acetate acetaldehyde content, D2191(3) acidity, test, 02066(3) hydroquinone content, D2193(3) spedfication, D2190(3) Vinyl chloride monomer (residual) content in polyvinyl chloride resins Vinyl resins polyvinyl butyral, D1396{2) polyvinyl chloride, D4368(2) Viscometers (viscosity) ball drop method, cellulose, Dl343(2) Brookfield (rotational), 02196(1) bubble time, clear liquids, 01545(1,2,3) dip type viscosity cups, 04212(1) falling rod (printing inks/vehicles), D4040(l) Ford cups (paints/varnishes), 01200(1) Gardner-Holdt, D803(3) ICI cone/plate (high sheaf), D4287(l) ISO flow cups, D51250) Saybolt, 0856(3) ', Stormer (Krebs tmits), D856(3) Weissenberg, rheogoniometer, D3451(l) Zahn cups (coil coatings), D3794(l) VM & P Naphtha specification, 03735(3) VOC (Volatile organic compounds) paints and related coatings, D3960(l) automotive coatings, abatement, D5087C1) Volatile liquids rate of evaporation, D35390) Sa Solvents Volatile matter content See Nonvoiatile/volatile content Volatile organic compounds (VOC), D396(HI) Wick test (low viscosity mixtures), D4207(3) Washability, of architectural paints soilant - mechanical'washing, D3450(l) 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 Water content--paints/related materials by gas chromatography, D3792(l) by iodine reagent method, D1631(3) crude cresylic add, D3439(3) fatty nitrogen compounds, D2072(3) in compressed air, 04285(1) Karl Fischer reagent method, D4017(l) liquid naval stores, D890(3) petroleum products, by distillation, D95(l, 3) pigments, and pigment pastes, D1208(2) solvents, by Fischer reagent method, D1364(3) terpene solvents, D 890 Water fog test, organic coatings, D1735(l) Water immersion test paints on steel, D870(l) Water miscibility See Miscibility Water pickup test See Printing Inks Water-reducible coatings industrial type, testing guide, D4712(l) Water repellents for wood, evaluation of, D--(1) in prep, masonry treatments,silane,non vol,D5095(l) qualitative test for in wood, D2921(l) Water resistance of coatings boiling water, of furniture lacquer, D2571(l) controlled condensation, D4585(l) of varnishes, D1647(l) water-fog test, D1735(l) water immersion test, D870(l) Sa Humidity resistance Water-soluble matter, content dry pigments, D1208, 2448(2) lac resins, D29(2) pigments (lead chromate type), D126(2) salt content, blue pigments, D113S(2) salt content of pigments, D2448(2) Water spotting,exterior latex paints,D1848(l) Water vapor permeability, D16S3(1) Wear resistance (Wear life) of traffic paint, D9i3(l) 5 a Abrasion resistance Weathering See Exposure Weatherometer, See Exposure-accelerated Weissenberg rheogoniometer test viscosity of powder coatirigs, D3451(l) Wet abrasion (scrubrfesistance " scrub-to-failure method, 1)2486(1) weight loss method, D4213(l) Wet film thicknesii gages See Film thickness gages, wet film Wet ground muscovite mica See Mica Wet-to-dry hiding change of paints, D5009(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 558 DUP050297077 Condensed index of Committee D-1 Standards t, White pigments, analysis extracted from paint antimony oxide content, D2350 combined sulfur, D2351, D2352(02) general, DM5 (01) practices and methods, list, D34(02) So White hiding pigments Extender pigments White zinc See Zinc oxide Whiting See Calcium carbonate Wick test See Burning Characteristics Wijs procedure--iodine value drying oils and derivatives, D1959(3) fatty amines/diamines, test, 02075(3) Wire-wound drawdown bar (Meier rod) coating application method, 04147(1) Wolfe-potentiometric method fatty acids in tall oil rosin, 01585(3) Wood chlorinated phenol in, test for, 02921(1) exposure tests on wood, D100(l) panels for weathering tests, 0358(1) water repellents for, under devel. by 00142 water repellents in, test for, D2921(l) Wood finishes blocking test, D2793(l) dry film thickness, D269M1) exposure tests, practices, D1006(l) factory applied: liquid/fresh film, properties, D2336(l) factory primed, durability tests, 02830(1) humid-dry cycling, D34590) preservative, chlorinated phenol, D2921(l) temperature of coating cure cycle, D3259(l) weathering tests, panels for, D356(l) S a Factory applied finishes Wood rosin. See Rosin Wood sash glazing compounds See Caulking/glazingfsealant compounds Wood turpentine. Sec Turpentine Xenon lamps exposure, nonmetallic materials, G26(l) lightfastness of pigments, D43030) Xylene ten-degree, spec.,D846(3) Yellow ocher See Ocher Yellow pigments See Basic lead silicochromate Chrome yellow Iron oxide yellow Ocher Strontium chromate Zinc chromate Zinc driers See Driers Zinc dust pigment analysis, D521(2) specification, D520(2) Zinc hydroxy phosphite analysis, D4450(2) specification, D4462(2> Zinc oxide analysis, D3280(2) specification, D79(2) Sa Pigments,general properties Zinc-rich primer. See Primers Zinc sulfide analysis, D3280(2) specification, D477(2) Sa Pigments,general properties Zinc white See Zinc oxide Zinc yellow See Zinc chromate Zirconium drier. See Driers Zahn viscometers See Viscometers Zeisel technique, chromatography, ethoxyl substitution, D4794(2) methoxy] hydroxypropyl sub.,, D3876(2) Zinc chromate analysis, D444(2) specification, D478(2) Sa Pigments, general properties Zinc-coated (galvanized) surfaces preparation for painting, D2092(l) Zinc content driers, EDTA method, D2613(3) white linseed oil paints, D2150) white zinc pigments, D3280<2) zinc dust pigment, D521(2) zinc hydroxy phosphite, D445012) 559 DU P050297078 ANNUAL BOOK o f ASTM STANDARDS Index Section 6 PAINTS, RELATED COATINGS, AND AROMATICS This index covers the standards, and related material appearing in Volumes 06.01,06.02, and 06.03. The boldface references are to the I ASTM designations; the standards appear in each volume in alphanumeric order. Proposed methods and specifications carry the index ; reference, "(Proposed)"; they appear, as does other ancillary material, in the Related Material (gray-edged) section in the back of the book. 1 A triangle (A) preceding the ASTM designation denotes that Adjunct Material for the standard is published separately; the Adjunct No. is : given in the standard. A Combined Index, covering the standards appearing in all volumes ofthe 1992 Annual Book ofASTM Standards, is I issued as Volume 00.01. I Alphabetization in the index is letter-for-letter, with no consideration to punctuation or word division. Initial prepositions of (indented) | subentries are ignored for alphabetization. f In the preparation of indexes, every attempt has been made to index standards on three levels: (1) by main subject, using general and l specific search terms; (2) by test methods or other significant sections of ASTM standards; and (3) by cross-references to locate main subject j! entry terms. {See also references are abbreviated as Sa and appear under main entry terms.) Specification F451, for Acrylic Bone Cements jl (Volume 13.01), illustrates ASTM's method of indexing. Ij INDEX TERMS FOR MAIN SUBJECT I ENTRY Adhesives--surgical implant materials acrylic bone cements (for internal orthopedic prostheses), self-curing, spec., F 451 Orthopaedic medical devices--bone acrylic bone cements (for internal orthopedic prostheses), I self-curing, spec., F 451 INDEX TERMS FOR TESTS Compressive strength acrylic bone cements, test, F 451 Doughing time acrylic bone cements, test, F 451 CROSS-REFERENCES Bone--cement See Adhesives--surgical implant materials Fixation materials Sa Orthopaedic medical devices (headings) 561 DUP050297079 Index of ASTM Standards, Sectioh 6 A Ablative antifouling paint systems See Antifouling coating system Abrading abrading concrete, practice, D 4259 (06.01) Abrasion resistance abrasion resistance of organic coatings, by falling abrasive, test, D968 (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-faiiure 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) Abrasives/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/ 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, by direct aspiration atomic absorption spectroscopy, test, D 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/vamishes/lacquers/related products, using filtered open flame 'carbon-arc light/water exposure apparatus, practice, D 822 (06.01) coatings (applied 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, D1654 (06.01) nonvolatile content of latexes, test, D 4758 (06.02) wet abrasion resistance of interior paints to scrubbing, 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 coatings cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (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) 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., D 358 (06.01) Acetaldehyde (AA) Sa Aldehydes acetaldehyde content of vinyl acetate, test, D 2191 (06D3) acetaldehyde, spec., D 4710 (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 acid (glacial) formic acid in glacial acetic acid, test, D 3546 (06.03) glacial (99.8 %) acetic acid (for use in paint/vamish/ lacquer/related products), spec., D 3620 (06.03) Acetone acetone in methanol (methyl alcohol), test, D1612 (06.03) acetone, spec., D 329 (06.03) acetone tolerance of heat-bodied drying oils, test, D1950 (06.03) alkalinity in acetone, test, D1614 (06.03) apparent pH of water insoluble phenol-formaldehyde resin, test, D4613 (06.02) permanganate time of acetone/methanol, test, D1363 (06D3) Acetophenone analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06X13) Acetyl content acetone in methanol (methyl alcohol), test, D1612 (06.03) apparent acetyl content of cellulose acetate proprionate/ butyrate, test, A D 817 (06.02) combined acetyl/acetic acid content of cellulose acetate, test, D871 (06.02) Acetylene black See Carbon black {headings) Acid content acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) Acid-insoluble extenders acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Acidity, alkalinity, pH--paints/related coatings/materials acetaldehyde, spec., D 4710 (06.03) acid/amine value of fatty quaternary ammonium chlorides, test, D 2081 (06.03) acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test,-D 4370 (06.01) acidity in vinyl acetate and acetaldehyde, test, D 2086 (06.03) acidity in voiatile solvents/chemical intermediates (used in paint/vamish/lacquer/nelated products), test, D1613 (06.03) acidity of benzene/toluene/xylenes/solvent riaphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03)-alkalinity in acetone, test, D 1614 (06.03) apparent pH of electrocoat baths, test, D 4584 (06.01) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) cellulose acetate propionates/butyrate, test, A D81T(06.02) cellulose acetate, test, D 871 (06.02) ethylcellulose, test, D 914 (06.02) formaldehyde solutions, test, D 2379 (06.03). hydrogen sulfide/sulfur dioxide (qualitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methyl acrylate, spec., D 4709 (06.03) methylcellulose, test, D1347 (06.02) moisture content of pigments, D1208 (06.02) pH of chemically cleaned/etched concrete surfaces, D 4262 (06.01) Acidity, alkalinity, pH--plastics cellulose acetate propionates/butyrate, test, A D 817 (06.02) - - Acid number Sa Saponification number/value rosin oil, test, D1131 (06.03) rosin, test, D 465 (06.03) sampling and testing pine tars/pine-tar oils, method, D 856 (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 562 DUP050297080 Index of ASTM Standards, Section 6 Alkyds/alkyd resins |cid resistance | acid/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) dd-soluble extenders " acid-soluble extenders in (iron/copper pbthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) idd value acid/amine value of fatty quaternary ammonium chlorides, test, D 2076 (06.03) acid value of organic coating materials, test, D1639 (06.01) fatty acids and polymerized fatty adds, test, D1980 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet r lac/bleached lac), test, D 29 (06.02) lad wash color aromatic hydrocarbons/related chemicals, terminology, 04790(061)3) ylate esters purity, by gas chromatography, test, D 3362 (06.03) Acrylic acid acrylic add dimer in acrylic acid/unsaturated organic adds, test, D 4415 (06.03) glacial acrylic add (99.0 % grade), spec., D 4416 (06.03) fjAcrylic latex paints Sa Latex paints artists' acrylic emulsion paints, spec., D 5098 (06.01) artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) preparing drawdowns of artists' paste paints, practice, D4941 (06.01) water content of water-redudble paints, by direct injection into gas chromatograph, test, D3792 (06.01) j: Acrylic polymer content qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D3168 (06.01) I Active oxygen content--organic solvents trace peroxides (2:5-80 ppm), using spectrophotometer, test, 209(06.03) Adhesion--paints/related coatings/materials 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) clear/pigmented organic coatings, test, D1308 (06.01) evaluation of painted/coated spedmens subjected to corrosive environments, method, D1654 (06.01) mar resistance of organic coatings, using balanced beam scrape adhesion and mar test, D 5178 (06.01) organic coatings on prepainted deformed metallic sheets, test, D 4145 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) by scrape test, D 2197 (06.01) zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) Adhesive bonding bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Adhesives amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) commercial hexanes, spec., D 1836 (06.03) Adhesives--structural trace peroxides (>5-80 ppm), using spectrophotometer, test, E 299 (06.03) Adulteration See Purity African ocher See Ocher Aged coatings assessing the condition of aged coatings on steel surfaces, guide, D5065 (06.01) Aggregate impact resistance of pipeline coatings, by limestone drop test, G 13 (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), D 4285 (06.01) Air-cooled xenon-arc lamp 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 of latexes, test, D 4758 (06.02) Airless spray application Sa Spray--Applied coatings testing industrial water-reducible coatings, guide, D 4712 (06.01) 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-solnble content alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) Alcohol content alcohol content/purity of acetate esters, by gas chromatography, test, D3545 (06.03) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) Alcohol resistance wood furniture lacquers, test, D 2571 (06.01) Alcohols (C4-C13) plasticizer grade, chemical/physical analysis (selection/use oftest procedures), E 852 (06.03) Aldehydes peroxides in styrene monomer, test, D 2119 (06.03) purity of aldehydes and ketones, test, D 2192 (06.03) Algae presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) Aliphatic hydrocarbons See Hydrocarbons--aliphatic Alkaline cresyiate solutions cresylic acid contest (of alkaline cresyiate solutions), chemical analysis, D 3439 (06.03) Alkaline earth carbonates acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Alkalinity alkalinity in acetone, test, D1614 (06.03) Alkali resistance clear/pigmented organic coatings, test, D1308 (06.01) dried varnish films, test, D1647 (06.01) Alkyds/alkyd resins alkyd resins, selection of test methods, practice, D 2689 (06.02) artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) fatty arid content, test, D1398 (06.02) glycerol/ethylene giycof/pentaerythritol in alkyd resins, test, D1615 (06.02) identification of carboxylic acids in alkyd resins D 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) 563 DU P050297081 Index of ASTM Standards, Section 6 Ash content--paints/related coatings/materials shallow submergence test, D 3623 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) /Antifouling paint pigments--copper powder chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) copper powder (for antifouting paints), spec., D 964 (06.02) Antifouling paint pigments--cuprous oxide chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) cuprous oxide (for antifouling paints), spec., D 912 (06.02) Antifouling paint pigments--mercuric oxide analysis, D 284 (06.02) mercuric oxide for use in antifouling paints, spec., D 911 (06.02) Antimony content antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) Antimony 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) Anti-sag meter sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) Apparent acetyl content apparent acetyl content of cellulose acetate proprionate/ butyrate, test, A D 817 (06.02) Apparent tack apparent tack of printing inks/vehicles, by inkometer, test, D4361 (06.01) Appearance of materials bleeding characteristics, of dry pigments, test, D 279 (06.02) Mistering (of paints/related coatings), A D 714 (06.01) chalking (of white/lightly tinted exterior paint films), practice, AD 4214 (06.01) checking (of exterior paints), test, A D 660 (06.01) darity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test; D 2090 (06.02, 06.03) dear/pigmented organic coatings, test, D 1308 (06.01) cracking (of exterior paints), test, A D 661 (06.01) degree of rusting on painted steel surfaces, method, AD 610 (06.01) erosion (of exterior paints), A D 662 (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 reflectometry, test, A D 2805 (06.01) hiding power -relative dry hiding power (of paints/related 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, D4941 (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, D 4712 (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/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Aqueous coatings sag resistance of paints, using a multinotch applicator, test, D 4400(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 oftesting 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 washability 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, D5007 (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, D5107 (06.01) Aromatic hydrocarbons See Hydrocarbons (headings) Aromatic potentiometer titrator acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) Aromatics content aromatics (ethylbenzene and eight-carbon (Cj/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 Orpiment content Artists' paints artists' acrylic emulsion paints, spec., D 5098 (06.01) artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) artists' watercolor 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, D 4303 (06J)l) 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 acid/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 acids, test, D1951 (06.03) 565 DUP050297082 Index of ASTM Standards, Section 6 Ash content--paints/related coatings/materials ethylcellulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (qualitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) methylcellulose, test, D1347 (06.02) moisture content of pigments, D 1208 (06.02) rosin, after burning and ignition, test, D1063 (06.03) sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) sampling/testing lac resins (orange shellac/button Iac/garnet lac/bleached lac), test, E> 29 (06.02) tall oil, methods of testing, D 803 (06.03) Atmospheres--conditioning/testing standard environments for conditioning/testing paint/ vamish/lacquer/related materials, spec., D3924 (06:01) Atmospheric analysis design/fabrication of flue gas desulfurization system components (for protective lining applicatipn), spec., D 4618 (06.01) inspection of linings in operating flue gas desulfurization , systems, practice, D 4619 (06.01) Atomic absorption See Spectrophotometry--atomic absorption Atomic absorption spectrophotometry r See Spectrophotometry--atomic absorption Atomic absorption spectroscopy See Spectroscopy--atomic absorption. Automatic spray producing films of uniform thickness-of paint/varnish/related products on test panels, test, D 823 (06.01) Automotive coatings/paints 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) gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) transfer efficiency under production conditions.for spray application of automotive paints, by weight basis, practice, D 5066 (06.01) viscosity of paints/related materials, by ISO flow cups, test,. D 5125 (06.03) B Bac-dray bleached lac See Bleached lac , Backfill impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G 17 (06.01) Bacteria/bacterial control . resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (0'6.01) Bacteria/bacterial control--paints/related coatings/materials resistance of emulsipn 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, D 3273 (06.01) Baked coatings nonvolatile content of latexes, test, D 4758 (06.02) Baker-Philippoff equation intrinsic viscosity of cellulose acetate, using modified Baker-Philippoff equation, test, D 871 (06.02) Baking (paints/related 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 viscosity of cellulose derivatives, by ball-drop method, teat D1343 (06.02) Bar codes abrasion resistance of printed matter, by the ga-cat conij sive abrasion test, D 5181 (06.01) Barite See Barium sulfate pigments Barium sulfat? acid-soluble extenders in (irdn/copper phthaiocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Barium sulfate content barium sulfate content in barium sulfate pigment, test, D 715 (06.02) Barium sulfate pigments Sa Pigments (general properties) barium sulfate pigment, analysis, test, D715 (06.02) barium sulfate pigments, spec., D 602 (06.02) Barriers comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Bartlet white lead.. See Basic sulfate white ,lead Barytes barium sulfate pigments, spec., D 602 (06.82) Base content acid/base milliequivalent content of(anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) Basic carbonate white lead basic carbonate white lead pigment, spec., D 81 (06.02) white lead- chemical analysis, test, D1301 (06.02) Basic lead silicochrorhate basic lead silicochromate pigment, spec., D1648 (06.02) chromium trioxide content of basic lead silicor.chromate pigment, test, D1844 (06.02) Basic sulfate white lead white lead- chemical analysis, test, D1301 f06.02) BeUstein analysis . field identification of coatings; test,.D 5043 (06.01) Bend testing--coatings effects of outdoor weathering on pipeline coatings, test, G11 (06.01) mandrel bend test of attached organic coatings; test, , D 522 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) *53$ acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847(06.03) acid wash color, test, B 848 (06.03) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) , carbon disulfide content of aromatic hydrocarbons, using spectrophotometry, test, D 2324 (06.03) chemical analysis ofbenzene, by gas chromatography, test, D 4492 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) cyclic hydrocarbon products, by gas chromatography, test, D4534 (06.03) distillation, test, D 850 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, D 3054 (06.03) 566 DUP050297083 Index of ASTM Standards, Section 6 Broad-band filter reflectometry purity of hydrocarbons from freezing points, test, D1016 (06.03) refined benzene-485 (nitration grade), spec., D 835 (06.03) refined benzene-535, spec., D 2359 (06.03) refined benzene-545, spec., D 4734 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) solidification point, test, D 852 (06X3) thiophene content of benzene, by spectrophotometry, test, D1685 (06X3) thiophene content of refined benzene, by gas chromatography (with flame photometric detection), test, D 4735 (06X3) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D 2360 (06X3) I volume/weight of industrial aromatic hydrocarbon's, method, t D1555 (06.03) Berlin white See Basic carbonate white lead Biocidal pigments See Antifouling paint pigments (headings) Biodeterioration See Deterioration Biological data analysis subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Bisphenol A sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) Bituminous materials (general) penetration resistance of pipeline coatings, by blunt rod test, G17 (06X1) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) water in petroleum products/bituminous materials, by distillation, test, D 95 (06X1, 06X3) Black box exposure test accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06X1) Black iron oxide See Iron oxide black $ Black pigments See Bone black pigment Sa Carbon black pigment Lampblack pigment Blade applicator producing films of uniform thickness of paint/varnish/related products on test panels, test, D 823 (06.01) Blanc fixe See Pigments (headings) Blast-cleaned steel profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) Blast cleaning standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) Bleached lac dry, regular and refined, spec., D 207 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) Bleeding bleeding characteristics, of dry pigments, test, D 279 (06.02) evaluating degree of bleeding of traffic/pavement marking paint, test, A D 868 (06X1) laboratory evaluation of degree of bleeding of traffic/pavement marking paint, test, D 969 (06X1) 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 D 714 (06X1) testing water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06X1) Blocking blocking resistance of trade sales paints, test, D 4946 (06X1) organic coatings on wood substrates, test, D 2793 (06.01) pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06X1) Blotching reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06X1) Blue-light reflectance See Reflectance and reflectivily (headings) Blue pigments Sa Iron blue/Phthalocyanine blue Ultramarine blue chemical analysis of (iron/copper phthaloc.yanine/ultramarine) blue pigments, test, D1135 (06X2) Blunt rod test penetration resistance of pipeline coatings, by blunt rod test, G 17 (06X1) Boiled oils (drying) See Oils (headings) Boiling point industrial aromatic hydrocarbons, test, D 850 (06X3) Boiling water resistance wood furniture lacquers, test, D 2571 (06X1) Bonding comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06.01) Bond strength bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D4796 (06X1) Bone black bone black pigment, spec., D 210 (06X2) solvent extractable material in black pigments, test, D 305 (06X2) Bone-dry bleached lac See Bleached lac--dry ". Book covers ----abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Boron trioxide (B?03) calcium borosilicate, test, D 4487 (06X2) Brabeuder moisture tester moisture content of (iron/copper phthalocyanine/ultramarine) blue pigments, by Brabender test, D1135 (06X2) Break drying oils, test, D1952 (06X3) Breaks cathodic disbonding of pipeline coatings, accelerated procedure,-. test, G 8 (06X1) 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 reflectometiy, test, E 97 (06X1) 567 s1 DUP050297084 Index of ASTM Standards, Section 6 Bromide content Bromide content titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D4764 (06.01) Bromine index aromatic hydrocarbons, by coulometric titration, test, D1492 (06.03) Bronze blue See - Iron bine 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 (06.02) synthetic brown iron oxide pigment, spec., D3724 (06.02) Brunswick blue See Iron blue Brunswick green See Chrome green Brush-application behavior testing industrial water-reducible coatings, guide, D 4712 (06.01) Brush drag comparison of the brush drag oflatex 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) Bulk density See Density--apparent (bulk) Burning characteristics--paints/related coatings/materials fire retardancy of paints, by cabinet method, test, AD 1360 (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 (oflow viscosity liquid mixtures), by Wick test 0 4207(06.03) Burnt sienna Sa Figments (headings) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) raw/bumt 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, D1016 (06.03) 1- Butanol See n-Butyl alcohol 2- Butanol See sec-Butyl alcohol 2-Butanone See Methyl ethyl ketone (MEK) Butoxyethanol 2-butoxyethanoI, spec., D 330 (06.03) Button lac orange shellac and (button lac/gamet lac), spec., D 237 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) n-Butyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) n-butyl acetate (all grades), spec., D 4615 (06.03) n-Butyl acrylate n-butyl acrylate, spec., D3547 (06.03) purity, by gas chromatography, test, D 3362 (06.03) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) n-Butyl acrylate/methacrylate unreacted monomer content oflatexes, by gas-liquid chromatography, test, D 4747 (06.02) n-Butyl alcohol n-butyl alcohol (butanol), spec., D 304 (06.03) .scc-Butyl alcohol sec-butyl alcohol, spec., D1007 (06.03) Butylated melamine-formaldehyde resins See Resins Butylcatechol inhibitor content p-teri-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) Butyl glycol See Butoxyethanol n-Butyl methacrylate unreacted monomer content oflatexes using capillary column gas chromatography, test, D 4827 (06.02) Butyraldebyde Sa Resins (headings) poly(vinyl butyral)- chemical analysis, test, D1396 (06.02) Butyryl content cellulose acetate propionates, test, A D 817 (06.02) c C4-C,3 alcohols chemical/physical analysis, selection/use of test procedures, E 852 (06.03) Cabinet method fire retardancy of paints, by cabinet method, test, A D 1360 (06.01) Cadmium content lead/cadmium/cobalt content (Low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) Cblcium borosilicate analysis,- B-4487 (06.02) `--- .- calcium borosilicate pigments, spec., D 4288 (06.02) Calcium carbonate calcium carbonate pigment, spec., D1199 (06.02) Calcium content calcium/zinc content, by EDTA method, test, D 2613 (06.03) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) zinc dust (metallic zinc powder), test, D 521 (06.02) Calcium oxide (CaO) content calcium borosilicate, test, D 4487 (06.02) calcium oxide in magnesium silicate pigment, test, D 717 (06.02) Calcium paint driers See Driers Calculating test results calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Calibration conductivity cell for conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) 568 DUP050297085 Index of ASTM Standards, Section 6 Chain length uniformity jration--paints/related coatings instrumentation pipment/standards for measuring purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) eacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) osity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) itance Imparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) r gas chromatography ilysis of styrene by capillary gas chromatography, test, 05135(06.03) eacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) fillary-moisture relations apillary moisture in concrete, by plastic sheet method, test, D 4263 (06.01) on-orc lamps derated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) inducting tests on paint/varnish/lacquer/related products, using enclosed carbon-are 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) operating unfiltered apparatus (for testing paints/related coatings), using the Dew cycle, practice, D 3361 (06.01) Inmate content dd-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) ion black carbon black pigment for paint, spec., D 561 (06.02) I solvent extractable material in black pigments, test, D 305 (06.02) bon black content solvent extractable material in black pigments, test, 0 305(06.02) bon disulfide content carbon disulfide content of aromatic hydrocarbons, using spectrophotometry, test, D 2324 (06.03) boxyl content carboxyl content of cellulose, test, D 1926 (06.02) 'bffixylic add identification of carboxylic acids in alkyd resins D 2455 (06.02) boxylie adds content resins, test, D 2455 (06.02) tor oil dehydrated castor oil, spec., D 961 (06.03) hydroxyl value of fatty oils/acids, test, D1957 (06.03) raw castor oil, spec., D 960 (06.03) spectrophotometric diene value of dehydrated castor oil/derivatives, test, D1358 (06.03) fellular plastics See Urethanes (headings) Cellulose 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, D 1926 (06.02) cellulose/cellulose derivatives, terminology, D1695 (06.02) cellulose (chemically refined), composition by chromatographic analysis, method, D1915 (06.02) chain length uniformity, by fractional precipitation of cellulose nitrate, test, D1716 (06.02) chlorine content, test, D 2641 (06.02) dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) dichloromethane-soluble matter content of cellulose, test, D3971 (06.02) ethoxyl substitution in cellulose ether products, by gas chromatography, test, D 4794 (06.02) hydrogen sulfide/sulfhr dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) in cellulose ether products methoxy] and hydroxypropyl substitution, by Zeisel-gas chromatographic technique, test, D3876 (06.02) intrinsic viscosity of cellulose, test, D1795 (06.02) methylcellulose, testing, D1347 (06.02) moisture in cellulose, test, D1348 (06.02) nitrogen content of soluble nitrocellulose, by ferrous sulfate procedure, test, D4795 (06.02) pentosans content of cellulose, test, D1787 (06.02) silica content, test, D 2438 (06.02) sodium glycolate content of sodium carboxymethylceMose, test, D1439 (06.02) solubility in sodium hydroxide, test, D1696 (06.02) soluble nitrocellulose-base solutions, methods oftesting, D 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/emulsions/rtsin solutions/shellac/varnishes), selecting test procedures, practice, D4209 (06.02) Cellulose and cellulose derivatives--cellulose acetate (CA) cellulose acetate, methods of testing, D 871 (06.02) Cellulose and cellulose derivatives--cellulose nitrate (nitrocel lulose) cellulose nitrate in alkyd lacquers, quantitative determination by infrared spectrophotometry, test, D 3133 (06.01) dilution ratio for solutions, test, D1720 (06.03) soluble cellulose nitrate, testing, methods, D 301 06.02) Cellulose and cellulose derivatives--ethylcellulose (EC) ethylcellulose, methods of testing, D 914 (06.02) Cellulose and cellulose derivatives--pulp metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, 0 4085(06.02) Cellulosic plastics--cellulose acetate butyrate (CAB) cellulose acetate propionate/butyrate, methods of testing, AD 817 (06.02) Cement ...... 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, D 4619 (06.01) Centrifuge (high-speed for vehicle separation) See Vehicle separation--solvent-type paints Ceramic whitewares directional reflectance factor (45-deg (Meg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Cerinm content cerium content (of paint driers), by EDTA method, test, D 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) 569 DUP050297086 Index of ASTM Standards, Section 6 Chalk Chalk See Calcium carbonate Chalking white/lightly tinted exterior paint films, practice, A 0 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 D1360 (06.01) Checking exterior paints, test, A O 660 (06.01) Chemical analysis--paints/related coatings/materials ,3calcium borosilicate, test, D 4487 (06.02) Q-C alcohols, chemical/physical analysis (selection/use of test procedures), E 852 (06.03) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) ethyl methyl pentanol content/purity 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, D 4450 (06.02) Chemical-resistant linings inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) Chemical-resistant materials/products dear/pigmented oiganic coatings, test, D1308 (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 (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) clear/pigmented organic coatings, test, 01308 (06.01) dipropylene glycol monomethyl ether, spec., D 4836 (06.03) propylene glycol monomethyl ether acetate, spec., D4835 (06.03) propylene glycol monomethyl ether, spec., 0 4837 (06.03) China day See Aluminum silicate (hydrous) Chinese blue See 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 O 913 (06.01) Chloride content--paints/related coatings/materials ethylcellulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, 0 2363 (06.02) methylcellulose, test, D1347 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, D 1439 (06.02) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) Chlorinated hydrocarbons dichloromethane/l,l,I-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) Chlorinated phenol preservative content wood products, qualitative test for, D 2921 (06.01) Chlorine content cellulose, test, D 2641 (06.02) epoxy resins/compounds, test, D 4301 (06.02) hydrolyzable chlorine content of liquid epoxy resins, test, D1726 (06.02) total chlorine content of liquid epoxy resins, test, D1847 (06.02) Chloroform-insolnhles content chloroform insoluble matter in oiticia oil, test, D1958 (06.03) Chromate coatings formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) Chromaticity See Color (headings) Chromatic pigments zinc yellow (zinc chromate) pigments, spec., D 478 (063)2) Chromatography--gas (detergents) methoxyl/hydroxypropyl substitution (of cellulose ether products), by Zeisel technique, test, 0 3876 (06.02) Chromatography--gas (paints/related coatings) identification of oils and oil acids in solvent-reducible paints, test 0 2245 (06.03) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) Chromatography--gas (paints/related coatings/materials) acrylate esters, purity, test, 0 3362 (06.03) alcohol content/purity of acetate esters, by gas chromatography, test, 03545 (06.03) analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 0 4961 (06.03) analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06.03) analysis of purities/impurities of styrene, test,' B 3962 (06.03) analysis of p-xylene, method, B 3798 (06.03) analysis of styrene by capillary gas chromatography, test, 0 5135(06.03) aromatics (ethylbenzene and eight-carbon (C8/heavier) in mineral spirits, test, 0 3257 (06.03) benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, 0 4534 (06.03) chemical analysis of benzene, by gas chromatography, test, 0 4492(06.03) '_ dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) ethoxyl substitution in cellulose ether products, by gas chromatography, test, 0 4794 (06.02) ethyl methyl pentanol content/purity value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.03) fatty acid composition, by gas-liquid chromatography of methyl esters, test, 01983 (063)3) identification of carboxylic acids in alkyd resins B 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) impurities in high-purity ethylbenzene, by gas chromatography, test, 0 5060 (06.03) monopentaerythritol in commercial pentaerythritol, test, 0 2195(06.03) phenol content (of tar acid mixtures), by gas liquid chromatog raphy, test, D 3626 (06.03) pinene composition (ofwood/gum/sullate turpentine), test, D 3009 (06.03) purity analysis of isopropylbenzene (cumene), test, 0 3760 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, 0 3054 (06.03) 570 BIB* DUP050297087 Index of ASTM Standards, Section 6 Coatings ity of methyl (amyl ketone/isoamyl ketone), test, D 3893 (06.03) fey of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) dty of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) rity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) tialitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) adual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) fjjvent composition analysis (of solvent-type paints), direct-injection technique, practice, D 3271 (06.01) biophene content of refined benzene, with flame photometric detection, test, D 4735 (06.03) Jjtal non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, test, D 2360 (06.03) fiuiiformity (of traffic paint vehicle solids), practice, *' D 2743 (06.01) [reacted monomer content of latexes, test, D4747 (06.02) reacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) unreacted toluene diisocyanate content of urethane prepoly mers/coatings, test, D 3432 (06.02) /volatile resin acids in toll oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) piwater content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) f xylene isomer analysis, by gas chromatography, test, D 2306 (06,03) [xylene, purity of ortfto-xylene, test, D3797 (06.03) omatography--gas (solvents) | benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) solvent composition analysis (of solvent-type paints), direct-injection technique, practice, D 3271 (06.01) .Chromatography--paper cellulose (chemically refined), composition by chromatographic analysis, method, D1915 (06.02) rome 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) irome yellow and orange chrome yellow/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 yellow) 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, D 126 (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 system 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, D 2090 (06.02,06.03) Classification field identification of coatings, test, D 5043 (06.01) Clay (aluminum silicate) See Aluminum silicate pigments ' Cleaning practical washabiiity 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, D185 (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 of coating-films to metallic substrates, by tape test, D3359 (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 (6.01) accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) 571 DUP050297088 Coatings Index of ASTM Standards, Section 6 assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) certification of coating conformance form, D5063 (06.01) chromium content (low concentrations) in solids ofliquid 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/1,1,1-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) dry film thickness, by microscopical measurement, D 2691 (06.01) dry film thickness of protective coating systems, by destructive means, test, D4138 (06.01) evaluating degree of settling (pigment suspension/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) evaluation of (dear/pigmented) coatings for rigid/semirigid plastics substrates, practice, D3002 (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, D 1210 (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) photographic documentation of coatings/lining defects/failures, D4121 (06.01) porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) producing films of uniform thickness of paint/vamish/rdated products on test panels, test, D 823 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) purity of methyl isobutyl ketone, by gas chromatography, test, D3911 (06.01) sag resistance of paints, using a multinotch applicator, test, D4400 (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, D 5146 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) volume nonvolatile matter in dear/pigmented coatings, test, D 2697 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Coatings--chromate formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) relative tinting strength of chromatic 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, D 3794 (06.01) f Coatings--enamel amount ofliquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test 04948(06.01) 'J| conducting tests on paint/varnish/lacquer/related products, & ^aSusing endosed carbon-arc light/water exposure apparatrci-"} practice, D5031 (06.01) ^Jg gloss of high-gloss metallic/nonmetallic surfaces, by goniodintf^^ }%imetry, method, E 430 (06.01) t UJ Coatings--epoxy subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D4939 (06.01) Coatings--organic See Organic coatings Coatings--ultraviolet-cured cure time, practice, D 3732 (06.01) estimating package stability of coatings for ultraviolet curine .., test, D 4144 (06.01) !e Coatings monitoring program establishing;procedures to monitor performance of safety related^ coatings in operating nuclear power plant, guide, D 5163 (06.01) * Coating thickness disbonding characteristics of pipeline coatings, by direct soil buriali'test, G19 (06.01) .' dry film thickness of protective coating systems, by destructive mearif test, D4138 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Cobalt conteijff lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by; atomic absorption spectroscopy, test; |) 3335 (06.01) paint driers, by EDTA method, test, D 2373 (06.03) SH 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,.D4518 (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, cement bricks/steel cubes, test, D4796 (06.01) Coil coatings application using a wire-wound drawdown bar, practice, D 4147 (06.01) coil coatings, testing, practice, D 3794 (06.01) Cold-check resistance temperature-change (high-low) resistance of clear nitrocelluli lacquer films applied to wood, test, D1211 (06.01) Cold resistance temperature-change (high-low) resistance ofclear nitrocelluli lacquer films applied to wood, test, D1211 (06.01) Colloidal black See Carbon black (headings) Cologne yellow See Chrome yellow Color cellulose acetate propionates/butyrate, test, A D 817 (06.02) 572 DUP050297089 Index of ASTM Standards, Section 6 Conformance discoloration boatings, by sunlight-through-glass test, D 2620 (06.01) 'pigmented organic coatings, test, D1308 (06.01) . s of paints/related coatings (by microbiological attack), Practice for determining by exterior exposure tests, >3456(06.01) in flight exposure imping carbon-arc light-exposure apparatus with and without pyater for exposure of nonmetaliic materials, practice, 23 (06.01) astness of pigments (in artists' paints), test, D4303 (06.01) 1 matter, D 3424 (06.01) srganic/inorganic chemicals ,,dehyde, spec., D 4710 (06.03) plose acetate propionates/butyrate, test, A D 817 (06.02) or of cresylic acids ("C" series standards), test, D 3627 (06.03) r adds (after heating), test, D1981 (06.03) leic/phthalic anhydride (in molten state/after heating), by platinum-cobalt scale, test, D 3366 (06.03) thyl acrylate, spec., D 4709 (06.03) pling and testing dipentene, method, D 801 (06.03) -paints/related coatings/materials ainum silicate (hydrous/anhydrous) pigment, analysis, test, 0718(06.02) r sts' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) nzene/toluene/xylenes/refined solvent naphthas/similar industrial aromatic hydrocarbons, test, D848 (064)3) eflulose acetate, test, D 871 (06.02) larity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) "ear liquids, by platinum-cobalt scale, test, D1209 (06.01, 06.03) "olor differences from instrumentally measured color differences of opaque materials, test, D 2244 (06.01) /Colored pigments (dry/pastes in oil), with a mechanical mulier, test, D 387 (06.02) /color of transparent liquids by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) color pigments, by miniature sandmill method, test, AD3022 (06.02) .drying oils (after heating), test, D1967 (06.03) evaluation of color for thermoplastic traffic marking materials, test, D 4960 (06.01) ' magnesium silicate pigment, analysis, test, D 717 (06.02) , preparation of standard color solutions (caramel/platinumcobalt), for color test on soluble nitrocellulose-base solutions, D 365 (06.02) quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) reflection haze (of high gloss surfaces), test, D 4039 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) 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/garnet lac/bleached lac), test, D 29 (06.02) 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, D4712 (06.01) Colorfastness lightfastness of printed matter, D 3424 (06.01) Colorimeter relative tinting strength ofprinting ink dispersions, test, D 2066 (06.01) Color index artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) 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 moisture stress, test, D 2065 (06.01) Composition analysis--paints/related coatings/materials chemical analysis of yellow/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/abrastve 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, D4260 (06.01) capillary moisture, by plastic sheet method, test, D4263 (06.01) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) making and preparing concrete/masonry 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, D4258 (06.01) surface cleaning concrete unit masonry (for coating), practice, D4261 (06,04) -- ' Condensation water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) Conditioning standard environments for conditioning/testing paint/ vamish/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 4389 (06.01) Conductivity bridge/cell electrical conductivity of electrocoat baths, test, D 4399 (06.01) Cone-and-plate viscometers Set Viscometers {headings) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D4287 (06JB1) Conformance certification of coating conformance form, D 5063 (06.01) 573 DUP050297090 Index of ASTM Standards, Section 6 (Conical mandrel apparatus Conical mandrel apparatus mandrel bend test of attached organic coatings, test, 0522 (06.01) Conjugated diene spectrophotometric diene value of dehydrated castor oil/derivatives, test, D1358 (06.03) Conjugated oils See Oils (headings) Consequence of coatings failure specifying inspection requirements for coating/lining work on metal substrates, guide, 0 5161 (06.01) Consistency consistency of paints, using Stormer viscometer, test, 0 562(06.01) Containers--aerosol volatile organic compounds (VOC) of solvent reducible paints in aerosol cans, test, 0 5200 (06.01) Containers--fiberboard . abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 0 5181 (06.01) Containers--tank cars/wagons sampling and handling aniline, practice, 0 3436 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, 0 3437 (06.03) sampling procedures--for paints/pigmented coatings, practice, D 3925 (06.01) sampling/unloading procedures--for cresylic acid/phenol, practice, 0 3852 (06.03) sampling/unloading procedures--for naphthalene/maleic anhydride/phthalic anhydride, practice, 0 3438 (06.03) Contamination--nuclear use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, 0 5144 (06.01) Contamination--paints/coatings applications chemical resistance of pipeline coatings, test, G 20 (06.01) conductimetric analysis of water-soluble ionic contamination of . blasting abrasives, test, 0 4940 (06.01) decontaminability of coatings used in light-water nuclear power plants, test, D 4256 (06.01) Continuity verification continuity verification of liquid/sheet linings applied to concrete substrates, practice, 0 4787 (06.01) Contractors coating contractor qualification (for nuclear-powered generation facilities), practice, 0 4286 (06.01) Contrast ratio hiding power of paints, by reflectometry, test, A O 2805 (06.01) Copal content sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) Copper--corrosion copper corrosion of industrial aromatic hydrocarbons, test, 0 849(06.03) detection of copper corrosion from petroleum products, by copper strip tarnish test, A 0130 (06.03) sampling and testing dipentene, method, 0 801 (06.03) Copper content chemical analysis of cuprous oxide/copper pigments, test, 0 283(06.02) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, 0 4085 (06.02) sampling and testing pine tars/pine-tar oils, method, 0856(06.03) Copper phthalocyanlne blue Sa Phthalocyanlne blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, 01135 (06.02) Copper phthalocyanlne green ., See Phthalocyanlne green 7 Copper powder chemical analysis of cuprous axide/copper pigments, test, D 283 (06.02) copper powder (for antifouling paints), spec., 0 964 (06.02) Copper strip test detection of copper corrosion from petroleum products, by copper strip tarnish test, A 0130 (06.03) Copy materials/products--lithographic water pickup of lithographic printing inks/vehicles in. a laboratory mixer, test, 0 4942 (064)1) Corn oil com oil, spec., 01842 (06.03) Corrosion--atmospheric testing ;\ evaluation of painted/coated specimens subjected to corrosive' environments, method, 01654 (06.01) ; Corrosion--eiectrodeposited coatings cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Corrosion--paints/related coatings/materials copper corrosion of industrial aromatic hydrocarbons, test, 0849(06.03) detection of copper corrosion from petroleum products, by copper strip tarnish test; A 0130 (06.03) evaluation of painted/coated specimens subjected to corrosive environments, method, 01654 (06.01) filiform corrosion resistance, test, 0 2803 (06.01) sampling and testing dipentene, method, 0 801 (06.03) water resistance of coatings, using controlled condensation, practice, 0 4585 (06.01) Corrosion--pipeline coatings cathodic disbonding of pipeline coatings, accelerated procedure;! test, G 8 (06.01) comparative corrosion preventive characteristics of materials used forjomts/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Corrosion--pitting/crevice salt spray (fog) testing, method, B117 (06.01) Corrosivity detection of copper corrosion from petroleum products, by copper strip tarnish test, A 0130 (06.03) Corrugated fiberboard boxes abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 0 5181 (06.01) Cotton metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, if. test, 04085(06.02) Cottonseed oil Sa Fatty acids--specifications cottonseed oil, spec., D1843 (06.03) * Coulometric titration aromatic hydrocarbons, for bromine content, test, D1492 (06.03) Coulometry sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, 03961 (06.03) Coulometry--microcoulometry sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, 0 3961 (06.03) Couplings comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06.01) 574 DUP050297091 Index of ASTM Standards, Section 6 Degradation--paints/related coatings/materials jty verification of liquid/sheet linings applied to concrete J>strates, practice, D 4787 (06.01) jerformance of composite wood products under surfactant .ccelerated moisture stress, test, D 2065 (06.01) of outdoor weathering on pipeline coatings, test, ll&ll (06.01) Vpar paints, evaluating, test, A D 661 (06.01) garel bend test of attached organic coatings, test, jgte 522 (06.01) Jgpc bendability of pipeline coatings, test, G10 (06.01) reidi tger content, by iodine reagent method, test, 01631 (06.03) Bile add Mphenol, sampling and handling, practice, D 3852 (06.03) jiff of cresylic acids ("C" series standards), test, Ip) 3627 (06.03)' Sylic acid content (of alkaline cresylate solutions), chemical M dialysis, D 3439 (06.03) lyridine base content in cresylic acid, by direct titration, test, f.'D4471 (06.03) gSoss-eut tape test .fadhcsion of coating films to metallic substrates, by tape test, D 3359 (06.01) i^-hatch tape test {lesion of coating films to metallic substrates, by tape test, 0 3359(06.01) index idex of ASTM methods equivalent/related to methods in Federal Standard 141 ("Paint, Varnish, Lacquer, and Related Materials; Methods for Sampling and Testing"),s;: (Related Material) (06.01,06.02, 06.03) ide far adds See Tar adds--crude/refined 'Stallization solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, 0 4493(06.03) specimen testing [adhesion of coating films to metallic substrates, by tape test, 0 3359(06.01) iene (isopropylbenzene) See Isopropylbenzene (cumene) ene process jfanalysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 0 4961 (06.03) iu s oxide chemical analysis of cuprous oxide/copper pigments, test, 0 283 (06.02) cuprous oxide (for antifouling paints), spec., O 912 (06.02) Bring characteristics MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, 0 4752 (06.01) Curing of organic coatings See Orying or curing Curing time stroke cure time of thermosetting phenol-formaldehyde resins, test, 0 4640 (06.02) Current 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) Curtain coat testing industrial water-reducible coatings, guide, 0 4712 (06.01) Cut 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, 0 2935(06.03) benzene content of cyclic 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, O 3437 (06.03) trace (total) chloride (organic/inoiganic) in liquid aromatic hydrocarbons, test, 0 5194 (06.03) volume/weight of industrial aromatic hydrocarbons, method, 01555 (06.03) Cyclohexane 995 cyclohexane 995, spec., 0 3055 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, 03054 (06.03) Cylindrical mandrel apparatus mandrel bend test ofattached organic coatings, test, 0522(06.01) D Damping hardness test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, 0 4366 (06.01) Dark chrome yellow See Chrome yellow and orange Oata analysis--recording/reporting results recording results on singie-/multi-panel forms, method, AD 1150 (06.01) Daylight Sa Reflectance and reflectivity (headings) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (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 (06i01) Defects--coatings .... ... photographic documentation of coatings/lining 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. ofterms, D 804 (06.03) protective coating/lining work for power generation facilities, terminology, D 4538 (06.01) Deformation--paints/related coatings/materials flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) fonnability/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, G17 (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, D 4141 (06.01) 575 DUP050297092 Index of ASTM Standards, Section 6 Driers (ability value in solution dilutability, test, D 5062 (06.03) tion ratio/value ellulose nitrate solutions, for active solvents, hydrocarbon diluents, and cellulose nitrates, test, D 1720 (06.03) luble cellulose nitrate, testing, methods, D 301 (06.02) er erylic aeid dimer in acrylic acid/unsaturated organic acids, test, D 4415 (06.03) ethyl-benzyl alcohol alysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) imethyl ketone See Acetone ip application testing industrial water-reducible coatings, guide, D 4712 (06.01) `p coater - producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) ipentene (and related terpene solvents) sampling and testing dipentene, method, D 801 (06.03) ipropylene glycol ' dipropylene glycol, spec., D 2696 (06.03) propylene glycol/dipropylene glycol, spec., D 5164 (06.03) ipropylene glycol monomethyl ether (DPM) dipropylene glycol monomethyl ether, spec., D 4836 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Dip-type viscosity test viscosity (of paints/vamishes/iacquers/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 atomic absorption spectroscopy, test, D 4834 (06.01) Directionality gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) Directionality of surface gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) Directional reflectance See Reflectance and reflectivity (headings) Dirt accumulation Sa Soil accumulation quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) Dirt resistance See Resistance--soil Disbonding disbonding characteristics of pipeline coatings, by direct soil burial, test, G 19 (06.01) specific bendability of pipeline coatings, test, G10 (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 to 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, D 185 (06.01, 06.02) copper phthalocyanine blue pigment, spec., D 963 (06.02) fineness of grind of printing inks, by NPIRJ grindometer, 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 cresylic 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 (06.03) 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 (06.01) Distillation--petroleum products distillation of petroleum products, method, D 86 (06.03) water in petroleum products/bituminous materials, by distiliation, test, D 95 (06.01,06.03) Distilled fatty adds See Fatty acids--specifications Distilled water acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D847 (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 coil coatings, application using a wire-wound drawdown bar, practice, D 4147 (06.01) leveling characteristics of architectural paints/coatings (aqueous/nonaqueous), in white/light 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, D4400(06.01) Driers ealdum/zinc content, by EDTA method, test, D 2613 (06.03) cerium content, by EDTA method, test, D 3970 (06.03) clarity/cleanness of (nonpigmented) 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.,' D 600 (06.03) manganese content, by EDTA method, test, D 2375 (06.03) rare earths content, by EDTA method, test, D 3989 (06.03) 577 DUP050297093 Index of ASTM Standards, Section 6 Driers vanadium content, by EDTA method, test, D3988 (06.03) y%iitynnnvolatile 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, G 13 (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, 0 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, D 1650 (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, D 3259 (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, D4I41 (06.01) comparison of the brush drag of latex paints, test, D 4958 (06.01) exterior durability (of varnishes), test, D 1641 (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/steel cubes, test, D4796 (06.01) E Earth pigments See Ochre Sa Sienna (burnt and raw) Umber (burnt and raw) Ease of brushing comparison of the brush drag of latex paints, test, D4958 (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, D 2613 (06.03) cobalt content in paint driers, test, I) 2373 (06.03) iron content in paint driers, test, D 3804 (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 driers), test, D 3989 (06.03) vanadium content in paint driers, test, D 3988 (06.03) zinc content in paint driers, test, D 2613 (06.03) zirconium content in paint driers, test, D 3969 (06.03) Efflorescence interior coatings (of water-base paints), test, D 1736 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Efflux cups viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) Elasticity elasticity/toughness of varnishes, test, D1642 (06.01) Electrical insulating solids orange shellac/other indian lacs for electrical insulation, spec., D 784 (06.02) shellac (dry/powdered) used for electrical insulation, selecting test methods, D 411 (06.02) Electrical measurements--coating applications cathodic disbonding of pipeline coatings, accelerated procedure, test, G8 (06.01) 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, G 19 (06.01) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) effects of outdoor weathering on pipetine coatings, test, G 11 (06.01) impact resistance of pipeline coatings, by falling weight test, G14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G 13 (06,01) water penetration into pipeline coatings, test, G 9.(06.01) Electrical stress cathodic disbonding of pipeline coatings, accelerated procedure, test, G8 (06.01) Electrochemical measurements nitrobenzene in aniline, test, D 4589 (06.03) Electrocoat baths acid/base milliequivalent content of'(anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) analysis of electrocoat bath samples, guide, D 1978 ,(06.01) apparent pH of electrocoat baths, test, D 4584 (06.01) electrical conductivity of electrocoat baths, test, D 4399 (06.01) nonvolatile andT>igment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) Electrostatic spray evaluating and comparing transfer conditions-laboratory conditions, test, D 5009 (06.01) Electrostatic spray application testing industrial water-reducible coatings, guide, D4712 (06.01) Elongation mandrel bend test of attached organic coatings, test D 522 (06.01) Elongation--attached organic coatings elongation/tensile strength/stiffness, test, D 2370 (06.01) . Emergent stem temperature corrections distillation of industrial aromatic hydrocarbons, test, 0 850(06.03) Emulsion vehicles (for paints/related coatings) blocking resistance of trade sales paints, test, D 4946 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) minimum film formation temperature (MFFT) of emulsion vehicles, test, D 2354 (06.02) 578 DUP050297094 Index of ASTM Standards, Section 6 Exposure tests--carbon-arc apparatus gi-; Itesting industrial water-reducible coatings, guide, D 4712 (06.01) fvoJatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (06.02) lame] coatings See Coatings--enamel bgiish china clay See Aluminum silicate poxide equivalent weight (EEW) epoxy content of epoxy resins, test, D1652 (06.02) ipoxy content epoxy resins, selecting test procedures, practice, D 4142 (06.02) Ethylbenzene aromatics (ethylbenzene and eight-carbon (C8/heavier) content in mineral spirits, by gas chromatography, test, D 3257 (06.03) ethylbenzene, spec., D 3193 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, 0 5060 (06.03) purity of hydrocarbons from freezing points, test, 01016(06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) |poxy (EP) plastics--coatings ' subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) poxy resins selecting test procedures, practice, D4142 (06.02) uilibrium method flash point of liquids, test, D 3941 (06.03) 'osion erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) exterior paints, method for evaluating, A D 662 (06.01) practical washability of organic coatings, test, D 4828 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) ter content alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) | Esters tf-butyl acetate (alt grades), spec., D 4615 (06.03) ester value of solvents and thinners^ test, D1617 (06.03) ethyi acetate (all grades), spec., D4614 (06.03) hexyl acetate, spec., D 5137 (06.03) hydroxyl content of pyridine-soluble esters, by spectrophoto metry, test, A D 817 (06.02) isobutyl acetate (95 % grade), spec., D1718 (06.03) H-propyl acetate (96 % grade), spec., D 3130 (06.03) phthalic anhydride content- in presence of dibasic acids, by gravimetric test, D1306 (06.02) primary (synthetic) amyl acetate (98 % grade), spec., D 3540 (06.03) Ester value ester value of solvents and thinners, test, D1617 (06.03) Etching acid etching concrete, practice, D 4260 (06.01) Etherification sodium glycolate content of sodium carboxymethyicellulose, test, D 1439 (06.02) Ethoxy ethanol 2-ethoxyethanol, spec., D 331 (06.03) Ethoxyethyl acetate 2-ethoxyethyI acetate (99 % grade), spec., 03728 (06.03) alcohol contem/purity of acetate esters, by gas chromatography, test, D354S (06.03) Ethoxy! 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, 03545 (06.03) ethyl acetate (all grades), spec., D 4614 (06.03) Ethyl acrylate ethyl acrylate (98.5 % grade), spec., D 3548 (06.03) purity, by gas chromatography, test, D 3362 (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, D1615 (06.02) Ethylene glycol monobutyl ether See Butoxyethanol Ethylene glycol monoethyl ether See Ethoxy ethanol Ethylene glycol monomethyl ether See lyiethoxy ethanol 2-Ethylhexanol 2-ethylhexanoi (synthetic), spec., D1969 (06.03) ethyl methyl pentanol content/purity value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.03) 2-Ethylhexyl acrylate 2-ethylhexyl acrylate, spec., D3541 (06.03) Ethyl iodide ethoxyl substitution in cellulose ether products, by gas chromatography, test, 0 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) primer Sa Primer MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Evaporation--rate/time volatile liquids with low viscosity, test, D 3539 (06.01) Exempted solvents - Sa Solvents ^headings) dichlororiiethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D4457 (06.01) 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 (06.0.1) 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, D 4585 (06.01) Exposure tests--carbon-arc apparatus accelerated testing of paints/varnishes/Iacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) carbon-arc light- and water-exposure apparatus, unfiltered, by Dew cycle, practice for operating, D 3361 (06.01) 579 DUP0502 97095 Index of ASTM Standards, Section 6 Exposure tests--carbon-arc apparatus 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 water for exposure of nonmetaliic 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 of coatings (applied to metal substrates), practice, D 4141 (06.01) conducting exterior exposure tests of (exterior) paints on steel, test, D1014 (06.01) conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D1006 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) quantifying dirt collection on coated exterior panels, test, D3719 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) Exposure tests--fluorescent-UV apparatus exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetaliic materials, practice, G 53 (06.01) Exposure tests--light 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/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) lightfastness of pigments (in artists' paints), test, D4303 (06.01) lightfastness of printed matter, D 3424 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetaliic materials, practice, G 26 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetaliic 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, D 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, D1654 (06.01) recording results on single- and multi-panel forms, standard, A D 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 humiditythermal 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, D 1735 (06.01) water resistance of coatings on steel, using water immersion, practice, D 870 (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, D 3732 (06.01) ij* estimating package stability of coatings for ultraviolet curine test, D 4144 (06.01) s` Exposure tests--water erosion testing of antifouling paints, using high velocity water test, D 4938 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Exposure tests--xenon-arc apparatus operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetaliic materials, practice, G 26 (06.01) Extender pigments Sa Aluminum silicate/Barium suIfate/Calcium carbonate/Calcium sulfate Magnesium silicate Pigments (general properties) Silica (diatomaceous) particle size distribution, by hydrometer of common white extender pigments, test, D 3360 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Exterior durability See Durability Exterior paints/coatings conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D1006 (06.01) degree of checking, evaluation, test, A D 660 (06.01) degree of cracking, evaluation, test, A D 661 (06.01) degree of erosion, evaluation, A D 662 (06.01) degree of flaking, evaluation, A D 772 (06.01) house and trim coatings, solvent-based, practices for selecting/using test procedures, practice, D 2932 (06.01) latex house paints, selecting/using test procedures, practice, D 3129 (06.01) quantifying dirt collection on coated exterior panels, test, 03719(06.01) reporting paint film failures characteristic ofexterior latex paints, classification, D1848 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) Extraction methods unsaponifiable matter content of rosin, testi-D 1065 (06.03) Extractives content dichloromethane-soluble matter content of cellulose, test, D 3971 (06.02) ii ^ Fabrication design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) Face glazing and bedding compounds;--metal sash slump of face glazing/bedding compounds on metal sash, test, D 2376 (06.01) Factory-applied organic coatings See Organic coatings Failure end point photographic documentation of coatings/linings defects and failures, D4121 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) reporting paiiit film failures characteristic of exterior latex paints, classification, D1848 (06.01) 580 DUP050297096 Index of ASTM Standards, Section 6 Fiber-optic light ' rod viscometer sity of printing inks/vehicles, by falling-rod viscometer, test, 0 4040(06.01) , sand abrasion test non resistance of organic coatings, by falling abrasive, test, D 968 (06.01) ; stones ' act resistance of pipeline coatings, by limestone drop test, G13 (06.01) g weight test -pact resistance of pipeline coatings, by falling weight test, r* G14 (06.01) -at ' g industrial water-reducible coatings, guide, D 4712 (06.01) -acids--general ' add composition, by gas-liquid chromatography of methyl esters, test, D1983 (06.03) tty adds used in protective coatings--terminology and selecting test methods, guide, D 1467 (06.03) entification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) Reparation of methyl esters from fatty adds, for fatty acid it composition analysis, test, D 3457 (06.03) npling liquid oils/fatty acids (commonly used in paints/ f varnishes/related materials), test, D1466 (06.03) / adds--specifications " eonut oil, spec., D 1841 (06.03) rn oil, spec., D1842 (06.03) bttonseed oil, spec., D1843 (06.03) hydrated castor oil, spec., D1539 (06.03) -seed oil, spec., D1538 (06.03) oybean oil, spec., D1537 (06.03) loil, spec., D1984 (06.03) / acids--tests dd value of fatty adds/polymerized fatty acids, test, D1980 (06.03) sh content, test, D1951 (06.03) jiarity/cleanness of (nonpigmented) paint and ink liquids, by s 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, D 1544 (06.01, 06.02, 06.03) fatty acids used in protective coatings--terminology and ; selecting test methods, guide, D1467 (06.03) fish oil content, by gasrliquid chromatography, test, D 3725 (06.03) hydroxyl value of fatty oils/acids, test, D 1957 (06.03) ipdine value, test, D1959 (06.03) polymerized fatty acids, selecting test methods, D 2575 (06.03) 1 rosin acid content, test, D 1240 (06.03) saponification value of drying oils/fatty acids/polymerized fatty adds, test, D1962 (06.03) . solidification (titer) point of fatty adds, test, D1982 (06.03) . specific gravity at 2S/25C, test, D1963 (06.03) unsaponifiable matter in drying oils/fatty adds/polymerized fatty acids, test, D 1965 (06.03) atty acids content , alkyd resins and alkyd resin solutions, test, D1398 (06.02) fatty add composition, by gas-liquid chromatography of methyl esters, test, D 1983 (06.03) ; oleic acid content of tall oil rosin, test, D 1585 (06.03) preparation of methyl esters from fatty acids, for fatty add composition analysis, test, D 3457 (06.03) / tall oil, methods of testing, D803 (06.03) -atty 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/diammes, by referee potentiometric 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 fatty amines/nonamines, test, D 2082 (06.03) percent of amines (primary/secondary/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/tertiary amine values of fatty amines, by alternative indicator method, test, D 2074 (06.03) water content, test, D 2072 (06.03) Fatty diamines fatty 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/nonamines, test, D 2082 (06.03) total/primary/secondap'/tertiary amine values of fatty amines/amidoamines/diamines, by referee potentiometric method, test, D 2073 (06.03) water content, test, D 2072 (06.03) Fatty matter content sampling/testing flaked aluminum powders/pastes, methods, D480 (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, D 2079 (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 ("Paint, Varnish, 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 methyiol 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 581 DUP050297097 Fibrous magnesium silicate Index of ASTM Standards, Section 6 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 UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) Aim hardness (of factory-applied organic coatings on metal substrates), by pencil test, D 3363 (06.01) mandrel bend test of attached organic coatings, test, 0 522(06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (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 coatings (applied to nonferrous metal base), nondestructive measurement, test, D1400 (06.01) dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01); 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, D 4938 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G 12 (06.01) nonmagnetic coatings (paint/varnish/lacquer), applied to a ferrous base, D1186 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) subjecting marine antifoulijig 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, D1640 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) Film--wet film thickness wet film thickness of organic coatings, D1212 (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, D1366 (06.02) Fineness of grind (dispersion) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) printing inks, by NPIRI method, test, D1316 (06.01) Finger-rub test field identification of coatings, test, D 5043 (06.01) Finite closed-cup flash point methods See Flash point (headings) Fire retardancy See Fire testing--fire/flame retardancy Fire testing--paints/related coatings/materials fire retardancy of paints, by cabinet method, lest, A D1360 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (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) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) Fire testing--petroleum products flash/fire point ofliquids, by Tag open-cup apparatus, test, D1310 (06.03) First aid handling/sampling phenol and cresylic acid, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) Fischer reagent method (for water content). See Karl Fischer reagent method Fish oil content fish oil content of drying oils and their fatty acids, by gas-liquid chromatography, test, D 3725 (06.03) Fittings comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) < Five-degree xylene/5 xylol See Xylene (five-degree) Fixed alignment adhesion tester pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) -- Flake brass See Copper powder/Gold bronze powder Flaked powders sampling/testing flaked aluminum powders/pastes, methods, - D 480 (06JB3) ~ Flake white See Basic carbonate white lead Flaking exterior paints, A D 772 (06.01) Flame cleaning standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) 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) Flammability--paints/related coatings/materials fire retardancy of paints, by cabinet method, test, A D 1360 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (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) 582 DU P050297098 Index of ASTM Standards, Section 6 Fungal influence--paints/reialed coatings/materials ained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06,03) ability--petroleum products h/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Kb/no flash method compliance by liquids of closed-cup flash point specifications, ft D 3934 (06.03) psh point--liquids liquilibrium method, test, D 3941 (06.03) Iflash/fire point of liquids, by Tag open-cup apparatus, test, I D1310 (06.03) Kash/no flash equilibrium method, D 3934 (06.03) -flash point by Tag closed tester, test, D 56 (06.03) flash point (of fud'oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) flash point of liquids, by Setaflash closed-cup apparatus, test, D 3278 (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) tall oil, methods Of testing, D 803 (06.03) t interior latex paint See Latex paints lexibility 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) oor paints/coatings clear floor sealers, performance tests, D1546 (06.01) solvent-thinned paints, practice for selection and use of test procedures, D 3383 (06.01) water-thinned floor paints, selection and use of test procedures, practice, D 3358 (06.01) {Flow and flow rate--paints/related coatings/materials high shear viscosity (of paints/vamishes/related products), by 1CI cone/plate viscometer, test, D 4287 (06.01) shellac (dry/powdered) used for electrical insulation, selecting test methods, D 411 (06.02) testing industrial water-reducible coatings, guide, D 4712 (06.01) viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) Flowcoat testing industrial water-reducible coatings, guide, D 4712 (06.01) Flow cup viscosity of paints/related materials, bv ISO flow cups, test, D 5125 (06.03) 'v viscosity of paints/vamishes/lacquers, by Ford viscosity cup, test, D 1200 (06.01) Flue gas desulfurization system design/fabrication (for protective lining application), spec., D 4618 (06.01) Fluorescent UV-condensation apparatus exposure of paints/related coatings to fluorescent UVcondensation 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) Foil film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Foots foots in raw linseed oil, by gravimetric method, test, D1966 (06.03) foots in raw linseed oil, by volumetric method, test, Di954 (06.03) Ford cup viscosity of paints/vamishes/lacquers, by Ford viscosity cup, test, D1200 (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) Formabiiity 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 of formaldehyde solutions, test, D 2194 (06.03) formaldehyde- 50 % grade (unhibited) and 37 % grade (ihhibited/uohibited), spec., D 2378 (06.03) free formaldehyde content of amino resins, test, D1979 (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 adds See Fatty adds--specifications Free formaldehyde See Formaldehyde Free monomers unreacted monomer content oflatexes, by gas-iiquid 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, D 3432 (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 (06.0i) Freezing point freezing points of high-purity hydrocarbons, test, D1015 (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, D 4141 (06.01) Friction/frictional 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, AD 3274 (06.01) 583 DUP050297099 Index of ASTM Standards, Section 6 Heating tests--paints/related coatings/matemls n pigments Sa Chrome green/Chromium oxide green Phthalocyanine green How/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) d (pigments) See Fineness of grind (dispersion) ilter-retained solids content of polymer latexes, test, D 5097 (06.02) t content t content of mica pigment, test, D 716 (06.02) and dolomite/limestone/oyster shell f See Calcium carbonate ties for testing paints/related coatings/materials likyd resins, practice, D 2689 (06.02) latino resins, selecting test procedures, practice, D 4277 (06.02) analysis of electrocoat bath samples, guide, D1978 (06.01) architectural paints/coatings (solvent-/water-thinned), " D 2833 (06.01) chemical analysis of white pigments, selection of test methods, guide, D34 (06.02) clear/pigmented lacquers, D 333 (06.01) (coil coatings, testing, practice, D 3794 (06.01) J ^drying oils, selecting test methods, guide, D 555 (06w3) 5 epoxy resins, selecting test procedures, practice, D 402 (06.02) I evaluation of (clear/pigmented) coatings for rigid/sgnairigid plastic substrates, practice, D 3002 (06,01) 11 k ' exterior latex house paints, practice, D 3129 (06.0f}' exterior solvent-based house/trim coatings, practice^ D 2932 (06.01) fatty adds used in protective coatings--terminology and selecting test methods, guide, D1467 (06.03)' - fatty nitrogen products, D 2071 (06.03) <,*,!<, ^ i; . floor paints (solvent-thinned), practice, O 3383 (06.01)' floor paints (water-thinned), practice, D 3358 (06,01) Interior flat wall paints (latex), practice, D 2931 (06.01) interior flat wall paints (solvent-thinned), practice, D 3323 (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, D 4143 (06.02) nonvolatile matter content (of paint/raw paint materials), practice, D 2832 (06.01) polymeric powders/powder coatings, practice, D 3451 (06.01) polymerized fatty acids, selecting test methods, D 2575 (06.03) poiy(vinyl chloride) resins, guide, D 4368 (06.02) printing inks/ink fUms/related materials, selecting test methods, guide, D 5010 (06.01) i sampling/testing volatile solvents/chemical intermediates (for paints/lacquer/vamish/related material), selecting test methods, D 268 (06.03) testing industrial water-reducible coatings, guide, D 4712 (06.01) testing primers/primer surfacers over preformed metal, selection/use of procedures, practice, D 3322 (06.01) traffic paints, practice, D 2205 (06.01) traffic paint, uniformity of vehicle solids, by speetroscopy/gas chromatography, practice, D 2743 (06.01) varnish, D 154 (06.01) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (06.02) volatile/nonvolatile content (of driers/diying 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* paitits (Oil/resin-oil/alkyd), spec., 04302 (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/Halphen-Hicks tests, D1542 (06.01, 06.02) Handling materials See Material handling Hardness (indentation) indentation hardness of organic coatings, by Rnoop and Pfund methods, test, D1474 (06.01) Hardness tests--organic coatings film hardness, by pencil test, D 3363 (06.01) hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D 4366 (06.01) indentation hardness of organic coatings, by Rnoop and Pfund methods, test, D1474 (06.01) Hazardous constituents analytical procedures for determining hazardous constituents in protective coatings, selecting test methods, guide, D3630 (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 acid and phenol, practice, D 3852 (06.03) handling naphthalene, maleic/phthalic anhydride, practice, D 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 diphenoi (bisphenol-A), practice, D 4297 (06.03) Haze ...... . Sa Gloss ._ cellulose acetate propionates/butyrate, test, A D817 (06.02) cellulose acetate, test, D 871 (06.02) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metry, method, E 430 (06.01) reflection haze (of high gloss surfaces), test, D 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, D 4141 (06.01) Heating tests--paints/related coatings/materials cellulose acetate propionates/butyrate, test, A D817 (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, D 850 (06.03) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) loss on heating of drying oils, test, D 1960 (06.03) 585 DUP05029710O Index of ASTM Standards, Section 6 Heating tests- -paints/related coatings/materials stroke cure time of thermosetting phenol-formaldehyde resins, test, D4640 (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, 0 4207(06.03) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) water resistance of coatings, using controlled condensation, practice, D458S (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, D1210 (06.01) Hematite See Iron oxide red n-Heptane flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) heptane miscibility of lacquer solvents, test, D 1476 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06.03) Heptane miscibility Sa Miscibility heptane miscibility of lacquer solvents, test, D 1476 (06.03) Herring content fish oii content (ofdrying oils and their fatty acids), by gas-liquid chromatography, test, D 3725 (06.03) n-Hexane purity of hydrocarbons from freezing points, test, D1016 (06.03) Hexanes commercial hexanes, spec., D 1836 (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 ofthe brush drag of latex paints, test, D 4958 (06.01) hiding power of paints, by reflectometry, test, A D 2805 (06.01) relative dry hiding power, D 344 (06.01) 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, D4958 (06.01) High-speed centrifugal vehicle separations See 'Vehicle separation High velocity water erosion testing of antifouling paints, using high velocity water" test, D 4938 (06.01) High voltage continuity testing continuity verification of liquid/sheet linings applied to concre substrates, practice, D 4787 (06.01) High voltage spark testing discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Holiday detection cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) ' continuity verification of liquid/sheet linings applied to concrete J substrates, practice, D 4787 (06.01) > disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) impact resistance of pipeline coatings, by limestone drop test, G 13 (06.01) Horizontal pull test static friction of coating surfaces, test, D 4518 (06.01) Humidity humid-dry cycling for coatings on wood/wood products, method, D 3459 (06.01) humidity-thermal cycle cracking, testing finishes on steel surfaces, D 2246 (06.01) Humidity--relative testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) Hunter appearance gloss'diflsrences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) Hydrated iron oxide ochre pigment, spec., D 85 (06.02) - Hydrocarbon content---nonaromatic 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) Hydrocarbons acidity in volatile solvents/chemical intejmediates (used in . paint/vamish/lacquer/related products), test, D 1613 (06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, D 4534 (06.03) .. dichloromethane/l,l,l-trichioroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) high-flash aromatic naphthas, spec., D 3734 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) VM & P naphthas, spec., D 3735 (06.03) Hydrocarbons--aromatic aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) bromine content, by coulmetric titration, test, D1492 (06.03) color (of solid aromatic hydrocarbons/related materials in molten state), by platinum-cobalt scale, test, D 1686 (06.03) solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) 586 DUP050297101 Index of ASTM Standards, Section 6 Industrial aromatic hydrocarbons (jion-aroinatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed fcienes, by gas chromatography, test, D 2360 (06.03) jfltotal) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) irbons--high-purity aercial density (of pure liquid chemicals), test, >3505(06.03) j points of high-purity hydrocarbons, test, D1015 (06.03) iy of hydrocarbons from freezing points, test, If 1016 (06.03) Scation point of industrial organic chemicals, test, 11493 (06.03) rbons--industrial aromatic Mty of benzene/toluene/xylenes/solvent naphthas/similar gf industrial aromatic hydrocarbons, test, D 847 (06.03) jwash color, test, D 848 (06.03) ent density of industrial aromatic hydrocarbons, test, p-D 2935 (06.03) iimercial density (of pure liquid chemicals), test, I D 3505 (06.03) hper corrosion of industrial aromatic hydrocarbons, test, D 849 (06.03) illation, test, D850 (06.03) idrogen sulfide and sulfur dioxide content (qualitative), test, Jjs D 853 (06.03) Edification point of industrial organic chemicals, test, I D1493 (06.03) [fur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, D 3961 (06.03) piume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) ifpcarbons--light Blume/weight of industrial aromatic hydrocarbons, method, D 1555 (06.03) rodynamic stress fibjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) progen sulfide content Industrial aromatic hydrocarbons, test, D 853 (06.03) filrolyzable chlorine content jiydrolyzable chlorine content of liquid epoxy resins, test, ft, D 1726(061)2) ijjlroquinone content aiydroquinone in vinyl acetate, test, D 2193 (06.03) jproxyacetone content pialysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06.03) proxyethylcelluiose jhydroxyethylcellulose, test, D 2364 (06.02) |droxyI (hydroxide ion) content iJhydroxyl 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) f hydroxyl value of fatty oils/acids, test, D1957 (06.03) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) 3ydroxypropoxyi content hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) Hydroxypropyl methylcellulose 1 hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) ydroxypropyt substitution f methoxyl/hydroxypropyl substitution in cellulose ether products, by Zeisel-gas chromatography, test, D3876 (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, D1631 (06.03) 1 ICI cone/plate viscometer high shear viscosity (of paints/vamishes/related products),-by ICI cone/piate viscometer, test, D4287 (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/coupiings/fittings/patches in pipeline coatings, test, G18 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Impact testing--pipeline coatings effects of outdoor weathering on pipeline coatings, test, GII (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 organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06,03) analysis ofp-xyleae, by gas chromatography, method,' D3798(06.03) - chemical analysis of benzene, by gas chromatography' test, D4492 (06.03)~ impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) pyridine base content in cresylic acid, by direct titration, test, D4471 (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 1 Ocher Indian red See Iron oxide red Industrial aromatic hydrocarbons See Hydrocarbons--industrial aromatic 587 DUP050297102 Index of ASTM Standards, Section 6 Industrial grade benzene/toluene/xylene Industrial grade benzene/toluene/xylene See Benzene/Toluene/Xylene (headings) Industrial materials/applications--chemicals Sa Chemicals solidification point of industrial organic chemicals, test, D1493 (06.03) Industrial materials/applications--paints/related coatings testing industrial water-reducible coatings, guide, D 4712 (06.01) viscosity of paints/related materials, by ISO' flow cups, test, 05125(06.03) Inert pigments See Extender pigments Infrared (IR) analysis qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) Infrared (IR) analysis--paints/related coatings/materials 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) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) Infrared pyrometer temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D3259 (06.01) Infrared spectrophotometry See Spectrophotometry--infrared Infusorial earth See Silica--diatomaceous Inhibitor zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Inhibitor content p-rert-butylcatechol (TBC) in styrene monomer, test, D 2120 (06.03) residual p-tof-butylcatechol (TBC) in styrene monomer, by addition of NaOH, test, D 4590 (06.03) Ink apparent tack of printing inks/vehicles, by inkometer, test, D4361 (06.01) clarity/cieanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) lightfastness of printed matter, D 3424 (06.01) nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, D 4942 (06.01) Inkometer. method apparent tack of printing inks/vehicles, by inkometer, test, D4361 (06.01) Inorganic colored pigments chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) Inorganic linings inspection of linings in operating flue gas desulfurization systems, practice, D4619 (06.01) Insoluble matter content lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) Inspection--coating applications design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, D 4537 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) painting inspectors (metal substrates), guide, D3276 (06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) Inspection personnel establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, D 4537 (06.01) Instrumental measurement--color/light See Light--exposure Instrumental measurement--paints/related coatings/materials accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) cathodic disbonding of pipeline coatings, accelerated procedure test, G 8 (06.01) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) evaluation of color for thermoplastic traffic marking materials, test, D 4960 (6.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) testing industrial water-reducible coatings, guide, D 4712 (06.01) Insulating coating systems cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Interchemical wet film gage ^ wet film thickness of organic coatings, D1212 (06.01) Interior mold environments See Resistance--bacteria Interior paints/coatings efflorescence (of interior wall paints), test, D1736 (06.01) interior latex semigloss/gloss paints, selecting test methods, guide, D 4540 (06.01) latex flat wall paint, practice for selection and use of test procedures, D 2931 (06.01) - ' practical washability of organic coatings, test, D 4828 (06.01) scrub-to-failure of interior latex flat wall paints, test, D 2486 (06.01) solvent-thinned flat wall paint, practice for selection and uSe of test procedures, D 3323 (06.01) solvent-thinned wall/trim semigloss enamels, practice for selection and use of test procedures, D 3425 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Interlaboratory testing * conducting interlaboratory study to determine precision of test method, practice, E 691 (06.03) paints/related coatings, practice, D 3980 (06.01) Internal indicator method acid number of rosin, test, D 465 (06.03) saponification number of rosin, test, D 464 (06.03) >; Internal voids continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) \ J588 DUP050297103 Index of ASTM Standards, Section 6 Isopropylbenzene (cumene) ic viscosity Sa Viscosity (headings) 'nsic viscosity of cellulose acetate, using modified Baker-PhilippofF equation, test, D 871 (06.02) Sting viscosity number of cellulose acetate propionate/ butyrate, test, A D 817 (06.02) e-pyridine-sulfur dioxide reagent ter in liquid naval stores, test, D 890 (06.03) , reagent method : content, in phenol and related materials, test, D1631 (06.03) value "d/amine value of fatty quaternary ammonium chlorides, test, D 2078 (06.03) r amines, amidoamines, and diamines, Wijs procedure, test, D 2075(06.03) pling and testing shellac varnish, D1650 (06.02) apling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) e value--drying oils and their derivatives codified Rosenmund-Kuhnhenn method, test, D 1541 (06.03) Jijs method, test, D 1959 (06.03) c contamination |i See Contamination (headings) /burnt sienna pigments, spec., D 765 (06.02) 1 blue emical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) hemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) i blue pigment* spec., D 261 (06.02) content--paint driers rmaidehyde, test, D 2087 (06.03) ' drogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) |pn in liquid iron paint driers, by EDTA method, test, D 3804 (06.03) i oxide black (natural)- chemical analysis, test, D 3872 (06.02) fhetals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) ethylcellulose, test, D1347 (06.02) osin, test, D1064 (06.03) i oxide black lack synthetic iron oxide pigment, spec., D 769 (06.02) ,.fon oxide black (natural)- chemical analysis, test, D 3872 (06.02) ^ oxide brown (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) i oxide brown (synthetic) /iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) jsynthetic brown iron oxide pigment, spec., D 3724 (06.02) n oxide content ^calcium borosilicate,.test, D 4487 (06.02) 'on oxide red (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) on oxide red (synthetic) analysis, D 50 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) on oxide yellow analysis, D 50 (06.02) yellow iron oxide (hydrated), spec., D 768 (06,02) on 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) Isadn thiophene content of benzene, by spectrophotometry, test, D 1685 (06.03) Isobutanol See Isobutyi alcohol Isobutene (isobutylene) purity of hydrocarbons from freezing points, test, D1016 (06.03) Isobutyi acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) isobutyi acetate (95 % grade), spec., D1718 (06.03) Isobutyi alcohol isobutyi alcohol, spec., D 1719 (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, 0 5125(06.03) Isocyanates isocyanate group- content of urethane materials/prepolymers, test, D 2572 (06.02) ISO (International Standards Organization) index of standards by ISO/TC 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/polycstcr resins, test, D 2690 (06.02) Isoprene purity of hydrocarbons from freezing points, test, D1016 (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, D 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) isopropvtbenzene (cumene), test, D3160 (06.03) purity analysis of isopropylbenzene (cumene), by gas chromatography, test, D 3760 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) 589 DUP050297104 Index of ASTM Standards, Section 6 4,4* Isopropylidene diplienol 4,4* Isopropylidene diphenol sampKng/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) solidification point, test, D 4493 (06.03) solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) Ivory black See Bone black J Jaune de zinc See Zinc yellow Joints comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06.01) Jones redactor 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, D 4017 (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, 0 4790(06,03) MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D4752 (06.01) methyl ethyl ketone, spec., D 740 (06.03) methyl isoamyl ketone, spec., D 2917 (06.03) methyl isobutyl ketone, spec., D11S3 (06.03) methyl n-amyl ketone (98 % grade), spec., D 4360 (06.03) purity of aldehydes and ketones, test, D 2192 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D3893 (06.03) purity of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, D3329 (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 tape test, D 3359 (06.01) Knoop hardness indentation hardness of organic coatings, by Knoop and Pfund methods, test, D 1474 (06.01) Konig pendulum test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D 4366 (06.01) Krems white See Basic carbonate white lead Kubelka-Munlt equation relative tinting strength of printing ink dispersions, test, D 2066 (06.01) L Labeling abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) drt materials for chronic health hazards, practice, D 4236 (06.01) Laboratory evaluating and comparing transfer conditions-iaboratory conditions, test, D 5009 (06.01) profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) Laboratory mixer water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, D 4942 (06.01) LAC orange shellac and (button lac/gamet lac), spec., D 237 (06.02) Lacquer abrasion resistance, by air blast abrasion test, A D 658 (06.01) abrasion resistance of organic coatings, by falling abrasive, test D 968 (06.01) acidity in volatile solvents/chemical intermediates (used in paint/vamish/Iacquer/related products), test, D1613 (06.03) adhesion (to smooth surfaces), by scrape adhesion test, D 2197 (06.01) amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) cellulose nitrate in alkyd lacquers, quantitative determination byj^ infrared spectrophotometry, test, D 3133 (06-01) clarity/cleanness of (nonpigmented) paint and ink liquids, by, At visual examination, test, D 2090 (06.02,. 06.03) t, . clear and pigmented, selection of test methods, P 333 (06.01) ` clear/pigmented organic coatings, test, D1308 (06.01) conducting tests on paint/vamish/Iacquer/related products, using enclosed carbon-arc light/water exposure apparatus;t, * practice, D 5031 (06.01) discoloration (light stability), test, D 2620 (06.01) dry film thickness of nonconductiye coatings (applied to ,, nonferrous metal hase), nondestructive measurement, tesfc^M? D1400 (06.01) dry film thickness (of nonmagnetic organic coalings applied ferrous base), D1186 (06.01) dry-film thickness of organic coatings, using micrometers, test D1005 (06.01) effects of overbaking on organic coatings, practice, D 2454 (06.01) elongation/tensile strength/stiffness, test, D 2370 (06.01) . t ester value of solvents and thinners, test, D1617 (06.03) i field identification of coatings, test, D 5043 (06-01) film formation rates in drying or curing process, at room temperature, test, D1640 (06.01) flash pointofliquids, by Setaflash closed-cup apparatuS. Wst* D3278 (06.03) freeze-thaw stability of multicolor lacquers, test, D 2337 (G6.01)[f glacial acrylic acid (99.0 % grade), spec., D 4416 (06.03) heptane miscibility of lacquer solvents, test, D1476 (06.03) imprint resistance, of dried films, test, D 2091 (06.01) * indentation hardness of organic coatings, by Knoop and Pfiux1J1 methods, test, D 1474 (06.01) methyl n-amyl ketone (98 % grade), spec., D 4360 (06.03) moisture vapor transmission of organic coating films, test, D 1653 (06.01) paint/vamish/Iacquer/related products, terminology, D16 (06.01, 06.02, 06.03) a paint/vamish/Iacquer/related products, test, A D 1475 (06.0l)jJ particle size analysis (of multicolored/nitrocellulose-base lacquer), test, A D 2338 (06.01) plasticizer migration from vinyl fabrics to lacquers, method, D 2199 (06.01) , tii preparation of free films of organic coatings, practice, D 4708 (06.01) preparing glass panels for testing, D 3891 (06.01) resistance to failure (on steel surfaces), by water immersion D 870 (06.01) 590 DUP050297105 Index of ASTM Standards, Section 6 Lead chromate stain removal (of multicolored lacquer on primed steel panels), test, D2198 (06.01) standard environments for conditioning/testing paint/ varnish/lacquer/related materials, spec., D3924 (06.01) temperature-change (high-low) resistance of dear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) viscosity of paints/vamishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) viscosity (of paints/vamishes/lacquers/related 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, D 4414 (06.01) wood furniture lacquers, test, D 2571 (06.01) ac resins See Resins--lac iampblack lampblack pigment, spec., D 209 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) Lampblack content solvent extractable material in black pigments, test, 0 305(06.02) Lapis lazuli See Ultramarine blue atex paints antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, 03717(06.01) artists' acrylic emulsion paints, spec., D 5098 (06.01) blocking resistance of trade sales paints, test, D 4946 (06.01) chromium content (low concentrations) in solids of liquid 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 brush 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 0-deg) of opaque specimens, by broad-band, filter reflectometry, test, E 97 (06.01) drying/curing/film formation (at room temperature), test, D1640 (06.01) efflorescence (of interior wail paints), test, D 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, D 1210 (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 D 2805 (06.01) hiding power (relative dry), visual evaluation of brushouts, test, D 344 (06.01) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D 4287 (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) leveling, by draw-down method, test, D 4062 (06.01) low temperature coalescence, test, D 3793 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D 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, D 4707 (06.01) paint/vamish/lacquer/related products, test, A D1475 (06.01) preparing drawdowns of artists' paste paints, practice, D4941 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) sag resistance, using multinotch applicator, test, D4400 (06.01) sampling liquid paints/related pigmented coatings, practice, D 3925 (06.01) scrub-to-failure of interior latex flat wall paints, test, D 2486 (06.01) specular gloss of nonmetaQic 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 (VOC) of paints/related coatings, selecting test procedures, practice, D 3960 (06.01) volume nonvolatile matter in clear/pigmented 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, D 4017 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (Q6.01) water-thinned 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, D 4213 (06.01) ._ wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) 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/ieaching 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) 591 DUP050297106 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) 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, D 3618 (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) lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (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, D 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, D 126 (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, D 49 (06.02) Lead salt infrared radiation thermometers 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/chromium 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, 0 480(06.03) Leveling characteristics architectural paints/coatings (aqueous/nonaqueous), in white/light tints, by draw-down method, test, 0 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, D822 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) cure time of ultraviolet-cured coatings, practice, D 3732 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D4587 (06.01) lightfastness of pigments (in artists' paints), test, D 4303 (06.01) lightfastness of printed matter, D 3424 (06.01) operating carbon-arc light-exposure apparatus with and without water for exposure of nonmetallic materials, practice, G 23 (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) Light--lightfastness lightfastness 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 evaluation, 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 2620 (06.01) Lightening power See Tinting strength Ligbtfastness 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 location^ in coating/lining industry, practice, A D 4257. (06.Q!) 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/lining 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, D1483 (06.02) absorption (by pigments), spatula rub-out test, D 281 (06.02) boiled linseed oil, spec., D 260 (06.03) linseed oil, spec., D1538 (06.03) raw, foots, by gravimetric method, test, D1966 (06.03) 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) 592 DUP050297107 Index of ASTM Standards, Section 6 Marine (shipboard) coatings alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) ({Liquid chemicals | See Chemicals Liquid coating properties testing solvent-borne architectural (interior/exterior) coatings, J guide, D S146 (06.01) Liquid cyclic products sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) liquid driers See Driers Liquid epoxy resins Sa Resins--repoxy epoxy content of epoxy resins, test, D1652 (06.02) Liquids 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) claxity/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, D1544 (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/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) liquid/solid status (of viscous materials), test, D 4359 (06.01) oiticia oil (permanently liquid), spec.,D 601 (06.03) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D4206 (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, test, D1545 (06.01,06.02, 06.03) Lithium methoxide identification of carboxylic acids in alkyd resins D 2455 (06.02) Loading tests pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) Loading tests--metals/alloys salt spray (fog) testing, method, B117 (06.01) Loss of adhesion See Adhesion--loss of adhesion Loss 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 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 coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D3624 (06.01) Low hiding strontium chromate See Strontium chromate Low temperature bake coatings nonvolatile content of latexes, test, D 4758 (06.02) Low voltajge wet sponge test discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Luminous reflectance See Reflectance and reflectivity (headings) M Magazine covers abrasion resistance ofprinted matter, by the ga-cat comprehen sive abrasion test, D5181 (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 phthalocyanine/ ultramarine) blue pigments, test, D1135 (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 silicate 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, D5163 (06.01) Maleic acid content . maleic acid content of maleic anhydride, by potentiometric titration, test, D 2930 (06.03) Maleic anhydride color in molten state/afier heating, by platinum cobalt scale (includes phthalic 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, D 564 (06.03) raw/burnt sienna pigments, spec., D 765 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) Manganese content metals (iron/copper/manganese/calcium) content ofcellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D4085 (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, D5066 (06.01) Marine (shipboard) coatings See Antifouling paint pigments (headings) 593 DUP050297108 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, D4261 (06.01) Masonry water repellents nonvolatile content in silanes/siloxanes/silane-siloxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) Material handling impact resistance of pipeline coatings, by falling weight test, G14 (06.01) naphthalene, maleic/phthalic anhydride, practice, D 3438 (06.03) phenol and cresylic add, practice, D 3852 (06.03) sampling and handling aniline, practice, D3436 (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 oitida oil, test, D1958 (06.03) Mechanical damage specific bendability of pipeline coatings, test, G10 (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 Mercaptans 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., D 911(06.02) Mercury content dry mercuric oxide pigment, test, D 284 (06.02) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D 3624 (06.01) Mesityl oxide analysis of major organic impurities in phenol 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 metallic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) Metal powder pigments See Aluminum powder and pastc/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 substrates, by tape test, D3359 (06.01) coil coatings, testing, practice, D3794 (06.01) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metry, method, E430 (06.01) mandrel bend test of attached organic coatings, test, 0 522(06.01) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) painted surfaces- evaluating degree of blistering, A D 714 (06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) testing primers/primer surfacers over preformed metal, selection/use of procedures, practice, D 3322 (06.01) Metaxylene See meta-Xylene Methacrylic acid (glacial) glacial (98.5 %) methacrylic acid (for use in paint/varnish/ lacquer/related products), spec., D 3845 (06.03) Methanol (methyl alcohol) Sa Chemicals/Petroleum and petroleum products (headings) acetone in methanol (methyl alcohol), test, D1612 (06.03) methanol content of formaldehyde solutions, test, D 2380 (06.03) methanol (methyl alcohol), spec., D1152 (06.03) permanganate time of acetone/methanol, test, D1363 (06.03) solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) Methoxy ethanol 2-methoxyethariol, spec., D 3128 (06.03) Methoxyl content hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D 1347 (06.02) Methoxyl/hydroxypropyl substitution cellulose ether products, by Zeisel-gas chromatography, test, 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 carbinol Methyl amyl ketone (MAK) methyl n-amyl ketone (98 % grade), spec., D 4360 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) Methylbenzofuran analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) Methyl butyl ketone purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) Methylcellulose See Cellulose and cellulose derivatives Methylcyclohexane purity of hydrocarbons from freezing points, test, D 1016 (06.03) Methylene chloride dichloromethane/l.l.l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D4457 (06.01) DUP050297109 Index of ASTM Standards, Section 6 rs Moisture content--paints/related coatings/materials fatty acid composition, by gas-liquid chromatography of methyl esters, test, D 1983 (06.03) preparation from oils, for fatty acid composition determination by gas-liquid chromatography, D 2800 (06.03) preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) Methyl ether of hydroquinone (MEHQ) content methyl- ether of hydroquinone (MEHQ) content of colorless monomeric acrylate esters, test, D 3125 (06.03) 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) purity of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) Methyl isoamy) ketone (MIAK) methyl isoamyl ketone, spec., D 2917 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) Methyl isobutyl carbinol methyl isobutyl carbinol, spec., D 2635 (06.03) Methyl isobutyl ketone (MIBK) methyl isobutyl ketone, spec., D1153 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) Methyl methacrylate 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) Methylol group content methylol group determination (qualitative) in phenolic resins, test, D4706 (06.02) Methylstyrene analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (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, D 716 (06.02) wet ground mica pigments, spec., D 607 (06.02) Microbiological attack--paints/related coalings discoloration susceptibility (in exterior exposure tests), practice, D 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, D 3273 (06.01) Microbiological examination presence of and removing microbial (fungal/algal) growth on paint/relaled coatings, guide, D 4610 (06.01) Microcoulometry See Coulometry--microcoulometry Microelectronic device processing--water reagent water, spec., D 1193 (06.03) Micrometer disbonding characteristics of pipeline coatings, by direct soil burial, test, G 19 (06.01) dry-film thickness of organic coatings, using micrometers, test, D 1005 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Microscopic examination--paints/related coatings dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) reporting particle size characteristics of pigments, practice, D1366 (063)2) Microwave procedures laboratory preparation ofgelled vehicles, using microwave oven, practice, D 5166 (06.02) Migration plasticizer migration from vinyl fabrics to lacquers, method, D 2199 (06.01) Milliequivalency acid/base miliiequivalent content of(anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D4370 (06.01) Milori blue See Iron blue Minerals field identification of coatings, test, D 5043 (06.01) Mineral spirits aromatics (ethylbenzene and eight-carbon (Cs/heavier) content in mineral spirits, by gas chromatography, test, D3257 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) porosity of paint films (to indicate coating penetration), test, D3258 (06.01) Miniature sandmill 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, D 1722 (06.03) Mixed aniline point sampling and testing dipentene, method, D801 (06.03) Mixed xylene See Xylene (mixed) MMFT See Film Model 'C' wet film thickness gage wet film thickness of organic coatings, D1212 (06JD1) . 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 2065 (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, D 871 (06.02) ethylcellulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (06.02) methylcellulose, test, D1347 (06.02) moisture content of (iron/copper phthalocyanine/ultramarine) blue pigments, by Brabender test, D1135 (06.02) moisture in cellulose, test, D1348 (06.02) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) pine tars and pine tar oils, test, D 856 (06.03) sampling and testing dipentene, method, D 801 (06.03) 595 DUP050297110 Index of ASTM Standards, Section 6 Moisture content--paints/related coatings/materials sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, D1439 (06.02) tall oil, methods of testing, D 803 (06.03) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) water in liquid naval stores, test, D 890 (06.03) Moisture degradation conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) Moisture passage water penetration into pipeline coatings, test, G 9 (06.01) Moisture vapor permeability moisture vapor transmission of organic coating films, test, D1653 (06.01) Molar substitution (MS) hydroxyethylcellulose, test, ID 2364 (06.02) Molecular weight--average acid/amine value of fatty quaternary ammonium chlorides, test, D 2080 (06.03) Molybdate pigment molybdate orange pigments, spec., D 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Molybdenum content molybdate orange pigments, spec., D 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Monocyclic aromatic hydrocarbons See Hydrocarbons (headings) Monocyclic terpene hydrocarbons See Dipenteue (and related terpene solvents) (headings) Monomeric acrylate esters (colorless) methyl ether of hydroquinone (MEHQ) content of colorless monomeric acrylate esters, test, D3125 (06.03) Monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D4747 (06.02) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) Monomer (unreacted) 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/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) Mottling pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Mud-cracking reporting paint film failures characteristic of exterior latex paints, classification, D1848 (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, D 4797 (06.01) Muller device color/tinting strength (of dry colored pigments/pastes in oil), test, D 387 (06.02) Multinotch applicator sag resistance of paints, using a multinotch applicator, test, D4400 (06.01) wet film thickness of organic coatings, by notched gages, practice, D4414 (06.01) Multipanel forms recording results on smgle-/multi-panel forms, method, A D1150 (06.01) N Naphtha and naphtha derivatives acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color of industrial aromatic hydrocarbons, test, D 848 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) evaporation residue determination, test, D 2232 (06.03) high-flash aromatic naphthas, spec., D3734 (06.03) sampling and handling aniline, practice, D 3438 (06.03) VM & P naphthas, spec., D 3735 (06.03) water content, by iodine reagent method, test, D1631 (06.03) Natural drying oils See Oils--drying Natural iron oxide pigments See Iron oxide black Natural pigments iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) pure para red toner pigment, spec., D 475 (06.02) pure toluidine red toner, spec., D 656 (06.02) Natural pine oil See Oils--pine (natural/synthetic) Natural yellow oxide See Ocher Naval stores ^ naval stores/related products, def. of terms, D 804 (06.03) volatile/nonvolatile content (ofdriers/drying oils/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) water in liquid naval stores, test, D 890 (06.03) Negative BeUstein field identification of coatings, test, D5043 (06.01) Neutral salt spray test See Salt spray (fog) testing ., Newtonian liquids viscosity ofpaints/vamishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) Nitration grade/pure benzene/benzol See Benzene Nitration grade/pure toluene/toluoi See Toluene Nitration grade xylene See Xylene (nitration grade) Nitrobenzene nitrobenzene in aniline, test, D 4589 (06.03) Nitrocellulose See Cellulose and cellulose derivatives (headings) Nitrogen-containing plastics nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) Nitrogen content nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) soluble cellulose nitrate, testing, methods, D 301 (06.02) 596 DUP050297111 Index of ASTM Standards, Section 6 Nuclear reactor vessels- coatings applications soluble nitrocellulose, by ferrous sulfate procedure, test, D 4795 (06.02) Nitrogen imparities pyridine base content in cresylic acid, by direct titration, test, 04471 (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, D4492 (06.03) Nonconductive coatings dry film thickness of nonconductive coatings (applied to nonferrous metal base), nondestructive measurement, test, D1400 (06.01) Nonconductive linings continuity verification of liquid/sheet linings applied to concrete substrates, practice, D4787 (06.01) Nonconductive protective coatings discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Nonconjligated oils--iodine valne See Iodine value Noncontact thermometer temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D3259 (06.01) Nondestructive evaluation (NDE) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Nondestructive evaluation (NDE)--x-ray diffraction See X-ray diffraction Nonheat-reactive resins See Besins (headings) Non-human control--algae See Algae Nonleafing aluminum pigment See Aluminum powder and paste 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/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniopbotometry, 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) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of uonmetallic materials, practice, G 26 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetallic materials, practice, G S3 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G 17 (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) 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/resin soiutions/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 silanes/siloxanes/silane-siloxane blends used in masonry water-repellent treatments, test, D5095 (06.01) nonvolatile content of latexes, test, D 4758 (06.02) nonvolatile content of resin solutions (in volatile organic solvents), test, D1259 (06.02) printing inks/resin solutions/vehieles, test, D 4713 (06.01) sampling and testing shellac varnish, D1650 (06.02) sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) varnishes, test, D1644 (06.01) 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 (06.01) volatile solvents, test, D1353 (06.03) volume nonvolatile matter in clear/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 coatings, by notched gages, practice, D4414 (06.01) NPIR1 method fineness of grind of printing inks, by NP1RI method, test, D1316 (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, D 4121 (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) 597 DUP050297112 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 flue gas desulfurization system components (for protective lining application), spec., D4618 (96.01) design/use of safety alert system for hazardous work locations in coating/lining industry, practice, A D4257 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) effects of radiation on coatings (for light-water nuclear power plants), test, D4082 (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, D4619'(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, D 4262 (06.01) photographic documentation of coatings/lining defects and failures, D 4121 (06.01) purity of methyl isobutyl ketone, by gas chromatography, test, D 3911(06.01) quality assurance, practice, D 3843 (06.01) sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D5139 (06.01) selecting test methods, guide for, D 3842 (06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) surface cleaning concrete (for coating), practice, D 4258 (06.01) surface cleaning concrete unit, masdnry (for coating), practice, D 4261 (06.01) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (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, D4227 (06.01) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D4228 (06.01) Ocher chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) ochre pigment, spec., D 85 (06.02) tt-Octane purity of hydrocarbons from freezing points, test, D 1016 (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, D1296 (06.03) Oil absorption calcium borosilicate, test, D4487 (06.02) pigments, by Gardner-Coleman method, test, D 1483 (06.02) pigments, by spatula rub-out test, D 281 (06.02) Oil adds identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) Oil-base paints See Solvent-reducible paints/coatings Oil content artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) oil/water presence in compressed air (used for coating application/air blast cieaning/abrasive blast cleaning), 0 4285(06.01) Oil resistance wood furniture lacquers, test, D 2571 (06.01) Oils Sa Hydraulic fluids coconut oil, spec., D 1841 (06.03) com oil, spec., D1842 (06.03) cottonseed oil, spec., D1843 (06.03) fish oil content (of drying oils and their fatty acids), gas-/liquid chromatography/test, D3725 (06.03) identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) rosin oils, testing, D 1131 (06.03) safflower oil, spec., D 1392 (06.03) sunflower oil (once-refined, technical grade), spec., D 3169 (06.03) water in liquid naval stores, test, D 890 (06;03) Oils--castor dehydrated castor oil, spec., D 961 (06.03) hydroxyl value of fatty oils/acids, test, D1957 (06.03) raw castor oil, spec., D 960 (06.03) spectrophotometric diene value of dehydrated castor oil/derivatiyes, test, D 1358 (06.03) Oils--drying acetone tolerance of heat-bodied drying oils, test, D1950 (06.03) ash content, test, D1951 (06,03) boiled linseed oil, spec., D 260 (06.03) break, test, D 1952 (06.03) color after heating, test, D1967 (06.03) color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) degummed soybean oil, spec., D124 (06.03) dehydrated castor oil, spec., D961 (06.03) drying oils, selecting test methods, guide, D 555 (06.03) film formation rates in drying or curing process, at room temperature, test, D 1640 (06.01) fish oil content; by gas-liquid chromatography, test, 0 3725(06.03) foots, by gravimetric method, test, D1966 (06.03) foots, by volumetric method, test, D1954 (06.03) gel time, test, D. 1955 (06.03) iodine value, test, D1959 (06.03) loss on heating of drying oils, test, D i960 (06.03) methyl esters, preparation for fatty acid composition analysis gas-liquid chromatography, D 2800 (06.03) oiticia oil (permanently liquid), spec., D 601 (06.03) raw castor oil, spec., D 960 (06.03) raw linseed oil, spec., D 234 (06.03) raw tung oil, spec., D12 (06.03) refined soybean oil, spec., D 1462 (06.03) safflower oil, spec., D1392 (06.03) sampling liquid oils/fatty acids (commonly used in paints/ vamishes/related materials), test, D1466 (06.03) saponification value of drying oils/fatty acids/polymerized fatty. acids, test, D 1962 (06.03) specific gravity at 25/25C, test, D 1963 (06.03) unsaponifiable matter in drying oils/fatty acids/polymerized fatty acids, test, D 1965 (06.03) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D4140 (06.03)' Oils--fatty clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) 598 DUP050297113 Index of ASTM Standards, Section 6 Organic linings Oils--fuel flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (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 drycleaning solvent, spec., D 235 (06.03) Oils--oiticica chloroform insoluble matter in oiticia oil, test, D1958 (06.03) gel time, test, D1955 (06.03) oiticia oil (permanently liquid), spec., D 601 (06.03) Oils--pine (natural/synthetic) sampling and testing pine oil, method, D 802 (06.03) sampling/testing pine tars/pine-tar oils, test, D 856 (06.03) water in liquid naval stores, test, D 890 (06.03) Oils--soybean degummed soybean oil, spec., D124 (06.03) refined soybean oil, spec., D 1462 (06.03) Oils--tell distilled fatty acids, spec., D 1984 (06.03) tall oil, methods of testing, D 803 (06.03) Oils--tall oil rosin oleic acid content of tall oil rosin, test, D1585 (06.03) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.031) Oils--tung gel time, test, D1955 (06.03) quality determination, test, D1964 (06.03) raw castor oil, spec., D12 (06.03) Oily matter content sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) Oleic acid content oleic acid content of tall oil rosin, test, D 1585 (06.03) Once-refined sunflower oil (technical-grade) sunflower oil (once-refined, technical grade), spec., D 3169 (06.03) Opacity hiding power of architectural paints applied by roller, test, .. D5I50(06.0I) Opacity/opaque materials directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) Open-cup dash point methods See Flash point (headings) Optical materials/properties/tests Sa Clarity/cleanness//Gloss/Haze Hiding power/Luminance/Metamerism Reflectance and reflectivity Refractive index/Tinting strength printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) Orange pigments chrome yeliow/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, D 126 (06.02) .Orange shellac See Shellac Organic coatings abrasion resistance, by Taber abraser, test, D 4060 (06.01) add value of organic coating materials, test, D1639 (06.01) adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) adhesion, to smooth panel surfaces, by scrape test, D 2197 (06.01) clear/pigmented organic coatings, test, D1308 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) detergent resistance, practice, D 2248 (06.01) dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) effect of staining agents, for products 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, <i 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 drying or curing process, test, D 1640 (06.01) film hardness, by pencil test, D 3363 (06.01) flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic 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 Konig/Persoz pendulum hardness tests, D 4366 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) moisture vapor transmission of organic coating films, test, D1653 (06.01) practical washability of organic coatings, test, D 4828 (06.01) preparation of free films of organic coatings, practice, D4708 (06.01) producing films of uniform thickness of paint/vamish/related 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 cracking, method, D 2246 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) water immersion test, D 870 (06.01) wet film thickness of organic coatings, D1212 (06.01) wet film thickness of organic coatings, by notched gages, practice, D 4414 (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, D 4619 (06.01) 599 DUP050297114 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/related 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 (GF-AAS), test, D 5108 (06.01) Orpiment content sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) Orthoxylene See ortho-Xylene Outdoor weathering See Weathering--outdoor Ovens nonvolatile content of printing inks/resin solutions/vehicles, test, D4713 (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, D 1652 (06.02) Oxygen (active) content See Active oxygen content Oxygen degradation conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) P Package stability estimating package stability of coatings for ultraviolet curing, test, 04144(06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) package stability of solvent-reducible/water-reducible paint, test, D 1849 (06.01) resistance of emulsion paints (in containers) to attack by microorganisms, test, D 2574 (06.01) sampling liquid paints/related pigmented coatings, practice, D 3925 (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/painits Paint--chromatic See Chromate coatings Paint--curing See Curing characteristics Paint--general acidity in volatile solvents/chemical intermediates (used in paint/vamish/lacquer/related products), test, D1613 (06.03) clear/pigmented organic coatings, test, D 1308 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) 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, D 1005 (064)1) erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) evaluating degree of settling (pigment suspension/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) field identification of coatings, test, D 5043 (06.01) 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) flash point by Tag closed tester, test, D 56 (06.03) index of ASTM methods equivalent/related 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 of standards by ISO/TC 35 on Paint and Varnishes, (Related Material) (06.01, 06.02,06.03) paint/vamish/lacquer/related products, terminology, D16 (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., D3924 (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-base pigment content, by low temperature ashing! test, D 3723 (06.01) testing industrial water-reducible coatings, guide, D4712 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) Paint--inspectors Sa Qualifications painting inspectors (metai substrates), guide, D 3276 (06.01) Paint--latex See Latex paints Paint--primer See Primer Paint--selection/use of test procedures See Guides for testing paints/related coatings/materials Paint--solvent-reducible See Solvent-reducible paints/coatings Paint--thinners ester value of solvents and thinners, test, D1617 (06.03) evaporation rate, test, D 3539 (06.01) nature of thinners in solvent-reducible paints, qualitative determination, method, D 2349 (06.01) Paint brashes preparation of paint brushes for evaluation, practice, D 5068 (06.01) 600 DUP050297115 Index of ASTM Standards, Section 6. Petroleum/petroleum products Paint roller preparation of paint roller covers for evaluation, D 5069 (06.01) 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 (064)1) Pale gold bronze See Gold bronze powder Panel evaluation evaluation of painted/coated specimens subjected to corrosive environments, method, D 1654 (06.01) mandrel bend test of attached organic coatings, test, 0522(06.01) Panel forms recording results on single-/multi-panel forms, method, A D1150 (06.01) Panels wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Paper and paperboard directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (064)1) lightfastness of printed matter, D 3424 (06.01) Para (paranitramline) red Sa Pigments (general properties) pure para red toner pigment, spec., D 475 (06.02) Para red pigment para red/toluidine 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 233(8 (06.01) polymeric powder properties, by multiple sieve method, practice, D 3451 (06.01) reporting partide 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/pastes/paints, test, D 185 (06.01,064)2) Pastes in oil (of pigments) See Pigment dispersions (paint)--white pigment analysis Patches comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Patch test conducting a patch test to assess coating compatibility, practice, D 5064 (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, D 4366 (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, D93 (06.03) Pentaerythritol glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D1615 (06.02) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D2195 (06.03) Pentane purity of hydrocarbons from freezing points, test, D1016 (06.03) Pentosans content pentosans content of cellulose, test, D 1787 (06.02) Percent dilatability resin solution dilutability, test, D 5062 (06.03) Percent epoxide epoxy content of epoxy resins, test, D1652 (064)2) Performance--coatings clear floor sealers, D 1546 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D5163 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Performance--nuclear materials/applications 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 ofacetone/methanol, test, D1363 (06.03) tricresyl phosphate, test, D1721 (06.03) Permeability--films moisture vapor transmission of organic coating films, test, D1653 (06.01) Permeability absorption reporting particle size characteristics of pigments, practice, D1366 (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 (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, D 4366 (06.01) Petroleum--mineral spirits See Mineral spirits Petroleum/petroleum products cresylic acid content (of alkaline cresylate solutions), chemical analysis, D3439 (06.03) 601 DUP050297116 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, D 1474 (06.01) w Pfund wet film thickness gage wet film thickness of organic coatings, D1212 (06.01) pH Sa Addity, alkalinity, pH (headings) apparent pH of electrocoat baths, test, D45S4 (06.01) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (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, D4961 (06.03) and cresylic add, sampling and handling, practice, D 3852 (06.03) apparent free phenols, in synthetic phenolic resins/solutions (used in paints/related coatings), test, D1312 (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, D3160 (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/reiated coatings), test, D1312 (06.02) apparent pH of water insoluble phenol-formaldehyde resin, test, 0 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 add content zinc hydroxy phosphite, test, D 4450 (06.02) Photographic processing photographic documentation of coatings/lining defects and failures, D4121 (06.01) Photographic standards for surface preparation standard pictorial surface preparation standards for 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, E 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 (0603) Phthalic 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 (06103) Phthalic anhydride--refined refined phthalic anhydride-1308, spec., D 2403 (06.03) Phthalic anhydride content alkyd resins/resin solutions in absence of dibasic acids ti D 563 (06.02) ^ alkyl resms/resin solutions containing dibasic acids bv gravimetric test, D1306 (06.02) 'y Phthalocyanine blue chemical analysis of phthalocyanine blue/green Diems.,,. . D 3256 (06.02) 8 nts' te, Phthalocyanine green chemical analysis of phthalocyanine blue/green Diemm,,. . D 3256 (06.02) togments, test, Phthalocyanine (phthalo) blue chemical analysis of (iron/copper phthalocyanine/ultramar;..^ blue pigments, test, D H35 (064)2) anne> copper phthalocyanine blue pigment, spec., D 963 (06.02) Phthalocyanine (phthalo) green phthalocyanine green pigment, spec., D 3021 (06.02) Physical constants calculating formulation physical constants of paims/coatinTM practice, D 5201 (06.01) ^ Physical strength/resistance (nonchemical) printing inks/ink films/reiated materials, selecting test rnwhsa. 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 (064)2) 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 ashing, test, D 4451 (06.01) pigment content of solvent-reducible paints, test, D 2371 (06.01) solvent-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 pigments (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 pngments/pastes/paints, test, D185 (06.01, 06.02) evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (064)1) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) ' fineness ofgrind, printing ink, test,-D 1316 (06.01) infrared identification of vehicle solids from solvent-reducible: paints, by infrared spectroscopy, test, D 2621 (064)1) 602 r r V W Pig r rPig 1 rPig \ V rKg a Pig 1 Pig I V Pig 1 v Pig 1 c rr Pig % Pig Pig 1 Pi: Pit Pit Pig c Pig t \ Pig c DUP050297117 Index of ASTM Standards, Section 6 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 (06.02) white linseed oil paints- chemical analysis, selecting test methods, practice, D 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 4358 (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 602 (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., D 81 (06.02) white lead- chemical analysis, test, D1301 (06.02) Pigments--basic lead silicochromate basic lead silicochromate pigment, spec., D1648 (06.02) chromium trioxide content of basic lead silico-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--bene black bone black pigment, spec., D 210 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) Pigments---calcium borosilicate analysis, D 4487 (06.02) calcium borosilicate pigments, spec., D 4288 (06.02) Pigments--calcium carbonate calcium carbonate pigment, spec., D 1199 (06.02) Pigments--carbon black carbon black pigment for paint, spec., D 561 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) Pigments--chrome green chrome green pigment, spec., D 212 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Pigments--chrome yellow and orange chrome yellow/orange pigment, spec., D 211 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Pigments--chromium oxide green chrome oxide green pigment, spec., D 263 (06.02) yellow/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 (for antifouling paints), spec., D 964 (06.02) Pigments--cuprous oxide chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) cuprous oxide (for antifouling paints), spec., D 912 (06.02) Pigments--ferrous ochre pigment, spec., D 85 (06.02) Pigments--gold bronze powder chemical analysis of cuprous oxide/copper pigments, lest, D 283 (06.02) gold bronze powder, spec., D 267 (06.02) Pigments--iron blue chemical analysis of (iron/copper phthalocyanine/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, D 3872 (06.02) Pigments--iron oxide black (synthetic) black synthetic iron 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., D 3722 (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, O 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 of white/yellow thermoplastic . traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) Pigments--leaded zinc oxide analysis of white zinc pigments, test, D 3280 (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., D 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Pigments--ocher , lV analysis, D 50 (06.02) ` ochre pigment, spec., D 85 (06.02) . .. Pigments--para red para red/toluidine red pigments, testing, D 970 (06.02) pure para red toner pigment,spec., D 475 (06.02) . Pigments--phthalocyanine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) 603 DUP050297118 Index of ASTM Standards, Section 6 pigments--phthalocyanine blue copper phthalocyanine blue pigment, spec., D 963 (06.02) Pigments--phthalocyanine green chemical analysis of phthalocyanine blue/green pigments, test, D3256 (06.02) phthalocyanine green pigment, spec., D 3021 (06.02) Pigments--pumice pumice pigment, spec., D 867 (06.02) Pigments--red lead lead peroxide/true red 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/burnt sienna pigments, spec., D 76S (06.02) Pigments--silica diatomaceous silica pigment, analysis, test, D 719 (062)2) Pigments--silica, diatomaceous diatomaceous silica pigment, spec., D 604 (06.02) Pigments--strontium chromate chemical analysis of strontium chromate pigment, test, D 1845 (06.02) strontium chromate pigment, spec., D1649 (06.02) Pigments--titanium dioxide chemical/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, D 3720 (06.02) titanium dioxide content of pigments (recovered from whoie paint), by atomic absorption spectroscopy, test, D 4563 (06.01) titanium dioxide pigments, spec., D476 (06.02) white titanium pigments, chemical analysis, test, D1394 (06.02) Pigments--toluidine red para red/toluidine red pigments, testing, D 970 (06.02) pure toluidine red toner, spec., D 656 (06.02) Pigments--ultramarine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) ultramarine blue pigment, spec., D 262 (06.02) Pigments--umber, burnt and raw analysis, D 50 (06.02) raw/burnt umber pigments, spec., D 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, D 3280 (06.02) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (062)2) chemical analysis of white pigments, selection of test methods, guide, D 34 (06.02) particle size distribution, by hydrometer of common white extender pigments, test, D 3360 (06.02) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, D 3720 (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) sulfide in white pigment separated from solvent-reducible paints, test, D 2351 (06.02) sulfur dioxide in white pigment separated from solventreducible paints, test, D 2352 (06.02) white lead- chemical analysis, test, D1301 (062)2) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) white titanium pigments, chemical analysis, test, D 1394 (06.02) zinc oxide pigments, spec., D 79 (06.02) Pigments--zinc chromate analysis, D 444 (06.02) zinc yellow (zinc chromate) pigments, spec., D 478 (062)2) Pigments--zinc dust analysis, D521 (06.02) zinc dust pigment, spec., D 520 (06.02) Pigments--zinc hydroxy phosphite analysis, D 4450 (06.02) zinc hydroxy phosphite pigment, spec., D4462 (06.02) Figments--zinc oxide analysis of white zinc pigments, test, D 3280 (06.02) zinc oxide pigments, spec., D 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/resin-oil/alkydj, spec., D 4302 (06.01) bleeding characteristics, of dry pigments, test, D 279 (062)2) chemical analysis of yellow/orange/red/brown pigments containing.iron/maganese, test, D 50 (06.02) coarse particles in pigments/pastes/paints, test, D185 (06.01,06.02) common properties of pigments, test, D1208 (06.02) evaluation of (clear/pigmented) coatings for rigid/semirigid plastic substrates, practice, D 3002 (06.01) field identification of coatings, test, D 5043 (06.01) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (06.02) lightfastness of pigments (in artists' paints), test, D 4303 (06.01) ofi absorption, by Gardner-Coleman method, test, D1483 (06.02) oil absorption, by spatula rub-out, test, D 281 (06.02) particle size- fineness of grind- printing inks, test, D1316 (062)1) relative tinting strength of chromatic paints, test, D 4838 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) repotting particle size characteristics of pigments, practice, D1366 (06.02) specific gravity, test, D 153 (06.02) tinting strength/color of colored pigments, by mechanical muller, test, D387 (06.02) tinting strength/color of colored pigments, by miniature sandmill, test, A D 3022 (06.02) volatile/nonvolatile content (of pigments), selecting test procedures, guide, D 4139 (06.02) water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (062)1) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Pigments (general properties)--dispersions Sa Pigment dispersion (paint) evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 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 of common white extender pigments, test, D 3360 (06.02) Pinene sampling and testing turpentine, method, D 233 (062)3) Pinene--alpha and beta wood, gum, and sulfate turpentine, by gas chromatography, test, D 3009 (06.03) Pine tars/pine tar oils sampling and testing pine oil, method, D 802 (06.03) 604 DUP050297119 Index of ASTM Standards, Section 6 Polyurethane raw materials sampling and testing pine tars/pine-tar oils, method, D 856 (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 (06.0!) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Pipeline coatings cathodic disbonding of pipeline coatings, accelerated procedure, 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/patches in pipeline coatings, test, G18 (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) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G 12 (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, G 10 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Plasticizer grade alcohol C4-C13 alcohol, chemical/physical analysis (selection/use of test procedures), E 852 (06.03) Plasticizers plasticizer migration from vinyl fabrics to lacquers, method, D2199 (06.01) Plastics (general) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E97 (06.01) evaluation of (clear/pigmented) coatings for rigid/semirigid plastic substrates, practice, D 3002 (06.01) methyiol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) operating light-/water-exposure apparatus (fluorescent-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 ofthermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) evaluation of color 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, D 1209 (06.01, 06.03) color of maleic/phthalic 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, D4789 (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, D 4948 (06.01) Polycyclic hydrocarbons See Hydrocarbons {headings) Polyester resins . identification'of carboxylic acids in alkyd resins D 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) isophthalic add content of alkyd/polyester resins, test, D 2690 (06.02) Polyhexafluoropylene (FEP) substrate preparation of ftee films of organic coatings, practice, D4708 (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, D 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, D3451 (06.01) Polymerization. cellulose nitrate, test, D1716 (06.02) sampling and testing turpentine, method, D 233 (06.03) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) Polymerization inhibitors p-tert-butylcatechol (TBC) in styrene monomer, test, 02120(06.03) Polymerized fatty adds See Fatty adds--tests Polymer latexes Sa Latex paints filter-retained solids content of polymer latexes, test, D 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 of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) silicone polymers- silicon content, by atomic absorption spectrophotometry, test, D3733 (06.02) solubility range, test, D 3132 (06.02) Polyol acetates identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) Polyurethane raw materials See Urethanes--polyurethane raw materials (headings) 605 DUP050297120 / Index of ASTM Standards, Section 6 PolyOinyl acetate) coating systems Poly(vinyl acetate) coating systems water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) Poly(vinyl butyrai) resins Sa Resins (headings) poiy(vinyl butyrai)- chemical analysis, test, D1396 (06.02) Poly(vinyl chlorideXPVQ plastics--resins ooly(vinyl chloride) resins, selecting test procedures, guide, D 4368 (06.02) residual vinyl chloride monomer content of polyvinyl chloride) resins/compounds/copolymers by solution injection technique, test, D36S0 (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 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Porosity--coating porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) Portable adhesion testers pull-off strength ofcoatings, 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) Fowdered chemicals directional reflectance factor (45-deg O-deg) of opaque specimens, by broad-band filter reflectometry, test, 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, D 4138 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (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) Power law viscosity of printing inks/vehicles, by falling-rod viscometer, 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, 0 4236(06.01) Precision conducting interlaboratory study to determine precision of test method, practice, E691 (06.03) Precision--instrumentation directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E97 (06.01) ............................ -.................. Preformed tape (for traffic marking) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) Pregel vehicle laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) Preparing specimens (for testing) See Specimen preparation (for testing) (headings) Prepolymers isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02) Pressure mottling pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Primary amyl acetate See Amyl acetate Primary hydroxyl content primary hydroxyl content of cellulose acetate, test, D871 (06.02) primary hydroxyl content of cellulose esters, test, A D817 (06.02) Primer formability/adhesion of zinc-rich primer/cbromate complex coatings (on steel), test, D 4146 (06.01) MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) testing primers/primer surfacers over preformed metal, selection/use of procedures, practice, D3322 (06.01) zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Primrose chrome/yellow See Chrome yellow and orange Printed matter abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) method for evaluating lightfastness, D 3424 (06.01) Printing ink resins resin solution dilutability, test, D 5062 (06.03) Printing inks abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) apparent tack of printing inks/vehicles, by inkometer, test, D 4361 (06.01) commercial hexanes, spec., D1836 (06.03) fineness of grind of printing inks, by NPIR1 method, test, D1316 (06.01) nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) relative tinting strength of printing ink dispersions, test, D 2066 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) ` water pickup oflithographic printing inks/vehicles'in a , laboratory mixer, test, D4942 (06.01) Printing substrates printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) Print resistance print resistance of architectural paints, test, D 2064 (06.01) Print resistence of lacquers See Lacquer ,, Procedures establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, D4S37 (064)1) Production method transfer efficiency under production conditions for spray application of automotive paints, by weight basis,,practice, D 5066 (06.01) 2-Propanone See Acetone 606 Pr Pt Pi Pi P P P f I ] 1 DUP050297121 Index of-ASTM Standards, Section 6 Quality assurance ! propionyl content acetyl and propionyl/butyral contents of cellulose mixed esters, test, A D817 (06.02) n-Propyi acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) rt-propyl acetate (96 % grade), spec., D 3130 (06.03) K-Propyl alcohol -propyl alcohol (1-propanol), spec., 03622 (06.03) propylene glycol propylene glycol/dipropylene glycol, spec., D 5164 (06.03) propylene glycol, spec., D 2695 (06.03) propylene glycol monomethyl ether acetate (PMA) propylene glycol monomethyl ether acetate, spec., 04835(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., D 4837 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Protective 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, 0 4538 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D4541 (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) Protective linings design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) Prussian blue See Iron blue Pull testing 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, D4541 (06.01) Pulp solubility in sodium hydroxide, test, 0 1696 (06.02) Pumice/pumice stone/pumacite pumice pigment, spec., 0 867 (06.02) Purity acetaldehyde, spec., 0 4710 (06.03) acrylate esters, by gas chromatography, test, 0 3362 (06.03) alcohol content/purity of acetate esters, by gas chromatography, test, 0 3545 (06.03) analysis of p-xylene, by gas chromatography, method, 0 3798 (06.03) chemical analysis of benzene, by gas chromatography, test, 0 4492(06.03) ethyl methyl pentanol content/purity value of 2-ethylhexanol, by gas chromatography, test, 0 5008 (06.03) methyl acrylate, spec., O 4709 (06.03) ortho-xylene, by gas chromatography, test, 0 3797 (06.03) purity analysis of isopropylbenzene (cumene), by gas chromatography, test, 0 3760 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, 0 3054 (06.03) purity of aldehydes and ketones, test, 0 2192 (06.03) purity of hydrocarbons from freezing points, test, 01016(06.03) . 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 ketone, by gas chromatography, test, 03329(06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, 04773 (06.03) purity of styrene, by freezing point method, test, 03799 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, 0 1439 (06.02) solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, 04493 (06.03) styrene, by gas chromatography, test, 0 3962 (06.03) Pyridine aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) hydroxyl content of cellulose acetate, by spectrophotometry, test, 0 871 (06.02) hydroxyl content of pyridine-soluble cellulose esters, by spectrophotometry, test, A 0 817 (06.02) pyridine base content in cresyiic acid, by direct titration, test, 0 4471 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, 0 3437 (06.03) water content, by iodine reagent method, test, 01631 (06.03) water content of paints/paint materials, by Karl Fischer method, test, 0 4017 (06.01) Pyridine--refined reducing substances in, test, 0 2031 (06.03) refined pyridine (1 degree), spec., 0 2323 (064)3) water solubility, test, 0 2030 (06.03) Pyrolysis field identification of coatings, test, 0 5043 (06.01) Pyrophyllite See Magnesium silicate Q Qualifications--nuclear facilities coating contractors (for nuclear-powered generation facilities), practice, 0 4286 (06411) establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, 0 4537 (06.01) journeyman painters for application ofcoatings to concrete surfaces of safety-related areas in nuclear facilities, practice, 04227(06.01) journeyman painters for application ofcoatings to steel surfaces of safety-related areas in nuclear facilities, practice, 04228(06.01) sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., 0 5139 (06.01) Qualification testing use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, 0 5144 (06.01) Qualitative analysis/measurement white titanium pigments,, chemical analysis, test, O 1394 (06.02) Quality assurance coatings for light-water cooled nuclear power plants, practice, 0 3843(06411) DUP050297122 Index of ASTM Standards, Section 6 Quality assurance 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, D 215 (06.01) Quinoline water content, by iodine reagent method, test, D1631 (06.03) R Radiation exposure accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) effects of radiation on coatings (for light-water nuclear power plants), test, D 4082 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 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, D 3732 (06.01) use of protective coating standards in nudear power plants, selecting ASTM standards, guide, D 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--rate/time Raw oils (drying oils) See Oils (headings) Raw sienna Sa Pigments (headings) chemical analysis of yeUow/orange/red/brown pigments 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 producls, practice, D3023 (06.01) Reagents presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) Reagent water--microelectronic processing microelectronic device processing, spec., D1193 (06.03) Records management single-/multi-panel forms for recording results of exposure tests of paints, A D1150 (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) red/Toluidine red/Venetian red chemical analysis of yellow/orange/red/browh pigments containing iron/maganese, test, D 50 (06.02) lead peroxide/true red lead content of dry red lead pigments, test, D49 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) para red/toluidine red pigments, testing, D 970 (06.02) pure para red toner pigment, spec., D 475 (06.02) pure toluidine red toner, spec., D 656 (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 (0603) Redwood wood used as panels in weathering tests of coatings, spec., D 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 cresylie-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 wbite/lightly tinted exterior paint films), practice, A D 4214 (06.01) gloss differences between surfaces of similar appearance, metliod for visual evaluation, D 4449 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by gomophotometry, method, E 430 (06.01). hiding power of paints, by reflectometry, test, A D 2805 (0601) instrumental color difference, test, D 2244 (06.01) porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) reflection haze (of high gloss surfaces), test, D 4039'(0601) 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 v ii See Haze Reflective markers in traffic paint See Glass spheres (in traffic paint), jI Refractive index gloss differences between surfaces ofsimilar appearance, method for visual evaluation, D 4449 (0601) sampling and testing dipentene, method, D 801 (0603). : sampling and testing pine oil, method, D 802 (0603) sampling and testing turpentine, method, D 233 (0603) Regular bleached lac See Bleached lac--dry ' Relative dry hiding power (at paints/coatings) See Hiding power--paints/coatiiigs * 608 DUP050297123 Index of ASTM Standards, Section 6 Resistance Relative humidity See Humidity--relative Relative tinting strength Sa Tinting strength relative tinting strength of printing ink dispersions, test, D 2066 (06.01) Reporting paint Him 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 white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) Residue--evaporation naphthalene, test, D 2232 (06.03) sampling and testing turpentine, method, D 233 (06.03) Resins alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) amine resins--solvent tolerance, test, D1198 (06.02) amino resins, selecting test procedures, practice, D 4277 (06.02) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 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, 01310(06.03) free formaldehyde content of amino resins, test, D 1979 (06.02) poly(vinyl butyral)- chemical analysis, test, D1396 (06.02) poly(vinyl chloride) resins, selecting test procedures, guide, 04368(06.02) residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) resin solution diiutability, test, D 5062 (06.03) softening point, by ring-and-bai apparatus, test, E 28 (06.03) solubility range, test, D 3132 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (06.02) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) water content of paints/paint materials, by Karl Fischer method, test, D4017 (06.01) Resins--alkyd artists' paints (oil/resm-od/alkyd), spec., D 4302 (06.01) fatty acids content, test, D1398 (06.02) glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D1615 (06.02) identification of carboxylic acids in alkyd resins D 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) phthalic anhydride content (in absence of dibasic acids), test, D 563 (06.02) phthalic anhydride content (in presence ofdibasic acids), by gravimetric test, D1306 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) rosin adds content, test, D1469 (06.02) silicone-modified-silicon content, by atomic absorption spectrophorometry, test, D 3733 (06.02) specific gravity at 25/25'C, test, D1963 (06.03) testing, practices, D 2689 (06.02) unsaponifiable matter content, test, D1397 (06.02) Resins--epoxy bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) epoxy content of epoxy resins, test, D1652 (06.02) epoxy resins, selecting test procedures, practice, D 4142 (06.02) hydrolyzable chlorine content of liquid epoxy resins, test, D1726 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) total chlorine content in epoxy resins/compounds, test, D 4301 (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, D 29 (06J>2) Resins--nitrogen amino resins, selecting test procedures, practice, D 4277 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) Resins--phenolic apparent free phenols, in synthetic phenolic resins/solutions (used in paints/related coatings), lest, D1312 (06.02) apparent pH ofwater 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) Resins--resin solutions laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) Resin solution cloud point resin solution diiutability, test, D 5062 (06.03) Resin solutions color of transparent liquids, by Gardner color scale, test, D1544 (06.01,06.02,06.03) glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D1615 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, D1013 (06.02) nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) nonvolatile content of resin solutions (in volatile organic solvents), test, D1259 (06.02) phthalic anhydride content, in absence of dibasic adds, test, D 563 (06.02) resin solution diiutability, test, D 5062 (06.03) unsaponifiable matter contend test, D1397 (06.02) viscosity, test, D1725 (06.02) Resistance See Resistance--abrasion Sa Resistance--add Resistance-ralcohol 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 609 DUP050297124 Index of ASTM Standards, Section 6 Resistance 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 658 (06.01) practical washability of organic coatings, test, D 4828 (0601) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) Taber abtaser, test, D 4060 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D4213 (06.01) Resistance--acid arid/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, D1647 (06.01) Resistance--bacteria 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, 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, D4585 (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 (HzO) 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, 03912(06.01) Resistance--chipping paints and related coatings, A D 31170 (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--fuel solvent/fuel resistance of traffic paint, test, D 2792 (06.01) Resistance--heat evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) Resistance--imprinting print resistance of architectural paints, test, D 2064 (06.01) print resistance of lacquers, test, D 2091 (06.01) Resistance--mar mar resistance of organic coatings, using balanced beam scrape adhesion and mar test, D 5178 (06.01) Resistance--mortar acid/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) Resistance--oil wood furniture lacquers, test, 1> 2571 (06.01) Resistance--paint spatter paint spatter resistance to roller application, test, D 4707 (06.01) Resistance--penetration porosity ofpaint films (to indicate coating penetration), 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 for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (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) specific bendabiiity of pipeline coatings, test, G10 (06.01) Resistance--pressure mottling pressure mottling/biocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Resistance--reagent factory-applied coatings on wood products, practice, 0 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, 02486(06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Resistance--slip static friction ofcoating surfaces, test, D 4518 (06.01) Resistance--soil practical washability oforganic coatings, test, D 4828 (06.01) Resistance--solvent solvent/fuel resistance of traffic paint, test, D 2792 (06.01) Resistance--stein factory-applied coatings on wood products, practice, D 3023 (06.01) practical washability oforganic coatings, test, D 4828 (0601) Resistance--temperature temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test* D1211 (0601) Resistance--water . coatings using controlled condensation, practice, D 4585 (0601) coatings, using water immersion, practice, D870 (0601) dried varnish films, test, D1647 (06.01) testing water resistance,of ebatings at 100 % relative humidity, practice, D 2247 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735' (0601) ________ __ 610 Re Re Re Re R1 R R B E I DUP050297125 Index of ASTM Standards, Section 6 Sampling--hydrocarbons Resistance--wear See Wear testing (headings) Resistance--wet abrasion practical washability of organic coatings, test, D 4828 (06.01) Retort pine tars See Pine tars (kiln and retort) Retroreflection/retroreflectors sieve analysis of glass spheres (for retroreflective pavements markings/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, AD 3274 (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 D868(06.01) evaluating degree of chipping of traffic paint, method, A 0 913(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 (064)1) Roller coat testing industrial water-reducible coatings, guide, D 4712 (06.01) Rosenmund-Kuhnhenn method iodine value of drying oils and their derivatives, test, 01541(06.03) Rosin acid number, test, D 465 (06.03) ash content, after burning and ignition, test, D1063 (06.03) iron content, test, D1064 (06.03) oleic add 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 (06.03) unsaponifiable matter content, test, D1065 (06.03) volatile oil in rosin, test, D 889 (064)3) volatile resin adds in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) Rosin adds content coating vehicles (rosin esters, varnishes, and alkyd resins), test, D1469 (06.02) fatty acids, test, D1240 (06.03) rosin oils, testing, D1131 (06.03) sampling/testing lac resins (orange sheliac/button lac/gamet lac/bleached lac), test, O 29 (06.02) tali oil, methods of testing, D 803 (06.03) Rosin content qualitative detection of rosin in varnishes, by LiebermanStorch/Halphen-Hicks tests, 01542 (06.01, 06.02) Rosin esters rosin adds content, test, D1469 (06.02) Rotational viscometer rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, 02196 (064)1) Ronge See Iron oxide red Roundness of glass spheres embedded in traffic paint, test for, D1155 (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 (064)2) Rupture/rapture 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 hazardous work locations in coating/lining industry, practice, A D 4257 (064)1) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, 05163(06.01) handling naphthalene, maleic/phthalic anhydride, practice, 03438 (06.03) handling phenol and cresylic acid, practice, D3852 (06.03) handling polymeric powders, practices, D 3451 (06.01) sampling and handling aniline, practice, D 3436 (064)3) sampling/handling liquid cyclic products (at ambient temperature), practice, D3437 (06.03) Safflower oil safflower oil, spec., D1392 (06.03) Sag resistance paints, using a multinotch applicator, test, 04400(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, B117 (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, D 3852 (06.03) naphthalene, maleic anhydride, and phthalic anhydride, practice, 03438(064)3) --......... sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) 611 DUP050297126 Index of ASTM Standards, Section 6 Sampling--hydrocarbons 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 3925 (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/drums), test, D 509 (06.93) sampling liquid oils/fatty acids (commonly used in paints/ vamishes/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/chemical intermediates (for paints/lacquer/vamish/related material), selecting test methods, D 268 (06.03) Sampling--petroleum products purity of hydrocarbons from freezing points, test, D1016 (06.03) Sand abrasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) Sandstone preparatory surface cleaning of architectural sandstone, practice, D5107 (06.01) Saponification number/value Sa Unsaponifiabie matter content apparent acetyl content of cellulose acetate proprionate/ butyrate, test, A D 817 (06.02) rosin, test, D 464 (06.03) sampling and testing shellac varnish, D1650 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet 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, D803 (06.03) Saybolt viscometers See Viscometers--Saybolt Scaling See Flaking Scattering coefficient hiding power of paints, by reflectometfy, test, A D 2805 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) Scrub resistance scrub-to-feilure of interior latex flat wail paints, test, D 2486 (06.01) Sealers (floor) See Floor paints/coatings Secondary butyl acetate (85-88 % grade) See n-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) Seif-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 volatile solvents and diluents, test, D1296 (06.03) Service Level I establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) Service level I and II use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Setaflash testers flash point of liquids, by Setaflash closed-cup apparatus, test, D3278 (06.03) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01,06.03) Settlement evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) traffic paint, in containers, by laboratory simulation, test, D1309 (06.01) Set-to-touch-time See Drying time Shear testing--paints/related coatings/materials consistency of paints, using Stormer viscometer, test, D562(06M) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) viscosity of printing inks/vehicles, by felling-rod viscometer, test, D4040 (06.01) Shear thinning rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Sheen Sa Gloss gloss/sheen uniformity evaluation, test, D3928 (06.01) practical washability of organic coatings, test, D 4828 (06.01) specular gloss of nonmetahic specimens, test, D 523 (06.01) Sheet materials (general) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D4787 (06.01) Sheet metal flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) Shellac sampling and testing shellac varnish, D1650 (06.02) shellac varnishes, spec., D 360 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/sheilac/vamishes), selecting test procedures, practice, D 4209 (06.02) Shellac--electrical insulating orange shellac/other indian lacs for electrical insulation, spec, D 784 (06.02) shellac (dry/powdered) used for electrical insulation, selecting test methods, D 411 (06.02) Shellac--orange orange shellac and (button lac/garnet lac), spec., D 237 (06J)2) sampling and testing shellac varnish, D1650 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet 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) 612 Sh SI Si. Si. Si. SI Si Si Si Si Si Si s S S S S s DUP050297127 Index of ASTM Standards, Section 6 Solid phase materials--paints/related coatings/materials Short-radius bends Slurries specific bendability of pipeline coatings, test, G10 (06.01) conductimetric analysis of water-soluble ionic contamination of SI (International System of Units) blasting abrasives, test, D 4940 (06.01) ted use of international system of units (SI) (modernized metric resistance of steel pipeline coatings to abrasion, by slurry of system), excerpts, coarse abrasive/water, test, G 6 (06.01) (Related Material--all volumes) (06.01, 06.02,06.03) Sienna (burnt and raw) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D3926 (06.02) Smudging abrasion resistance of printed matter, by the ga-cat comprehen raw/burnt sienna pigments, spec., D 765 (06.02) sive abrasion test, D 5181 (06.01) Sieve analysis Soapstone sieve analysis ofglass spheres (for retrorefiective pavements See Magnesium silicate markings/industrial uses), test, D1214 (06.02) Sodium carboxymethylceilulose ,en Sieve analysis--subsieve sodium glycolate content of sodium carboxymethylceilulose, reporting particle size characteristics of pigments, practice, test, D1439 (06.02) D1366 (06.02) Sodium glycolate content .. " Silanes/Siloxane nonvolatile content in silanes/siloxanes/silane-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, D1135 (06.02) sodium glycolate content of sodium carboxymethylceilulose, test, D1439 (06.02) Sodium hydroxide (caustic soda) residual p-tm-butylcatechol (TBC) in styrene monomer, by addition of NaOH, test, D4590 (06.03) solubility in sodium hydroxide, test, D1696 (06.02) cellulose, test, D 2438 (06.02) Sodium sulfite chromium trioxide content of basic lead silico-chromate free formaldehyde content of amino resins, test, D1979 (06.02) pigment, test, 01844 (06.02) Softening point free silica in barium sulfate pigment, test, D 715 (06.02) clear/pigmented organic coatings, test, D1306 (06.01) white titanium pigments, Chemical analysis, test, D1394 (06.02) resins, by ring-and-bail apparatus, test, E 28 (06.03) Silica (diatomaceous) Soi] accumulation diatomaceous silica pigment, spec., D 604 (06.02) paint films, evaluating degree of surface disfigurement, nal Silicon content AD3274 (06.01) silicon polymers and silicon-modified alkyds, by atomic Soil burial test absorption spectrophotometry test, D 3733 (06.02) disbonding characteristics of pipeline coatings, by direct soil Silicon dioxide (SiOj) content burial, test, G19 (06.01) silicon dioxide in magnesium silicate pigment, test, D 717 (06.02) Soil removal properties practical washability of organic coatings, test, D 4828 (06.01) te Silicone-coated paper preparation offree films of organic coatings, practice, 04708(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) 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- isopropyiidenediphenol (Bisphenol A), test, D 4493 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) benzene, test, D 852 (06.03) Simulated accident conditions purity of methyl isobutyl ketone, by gas chromatography, test, D 3911 (06.01) solidification point of industrial organic chemicals, test, D1493 (06.03) solidification (titer) point of fatty acids, test, D1982 (06.03) Single-pane] forms recording results on single-/multi-panel forms, method, & D1150 (06.01) Skinning See Stability--package Skins content ciarity/deanness of (nonpigmeated) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) Solid phase materials--paints/related coatings/materials amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) determining liquid/solid status (of viscous materials), test, D 4359 (06.01) Slag filter-retained solids content of polymer latexes, test, 2) conductimetric analysis of water-soluble ionic contamination, of D 5097 (06.02) blasting abrasives, test, D 4940 (06.01) flash point (of fuel oils/lube oils/suspension of solids/liquids), by Sliding scale calibration graph Pensky-Martens closed tester, test, D 93 (06.03) viscosity of printing inks/vehicies, by falling-rod viscometer,: infrared identification of vehicle solids from solvent-reducible test, D 4040 (06.01) paints, by infrared spectroscopy, test, D 2621 (06.01) Slip resistance toluene-insoluble solid matter (sand/chips/dirt/bark) in rosin, static friction of coating surfaces, test, D4518 (06.01) test, D 269 (06.03) Slope laboratory preparation of gelled vehicles, using microwave oven, volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, 05166(06.02) practice, D 4209 (06.02) Slump slump of face glazing/bedding compounds on metal sash, test, D 2376 (06.01) volatile/nonvolatile content (ofdriers/drying ofls/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) 613 DUP050297128 Index of ASTM Standards, Section 6 Solid phase materials--paints/relaited coatings/materials volatile/nonvolatile content (of pigments), selecting test procedures, guide, D 4139 (06.02) weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) Solubility refined pyridine in water, test, D 2030 (06.03) resin solution dilutability, test, D 5062 (06.03) solubility in sodium hydroxide, test, D1696 (06.02) solubility range (of resins/polymers), test, D 3132 (06.02) soluble cellulose nitrate, testing, methods, D 301 (06.02) Solubility--alkali solubility in sodium hydroxide, test, It 1696 (06.02) Soluble cellulose nitrate nitrocellulose soluble cellulose nitrate, testing, methods, D 301 (06.02) Soluble sulfates content lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) Solution injection technique residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) Solvent analysis (of solvent-type paints) direct injection with a gas chromatograph, practice, D3271 (06.01) Solvent and fuel resistance of traffic paints See Traffic paint Solvent brushing and wiping Sa Steel panels preparation of hot-dipped nonpassivafed galvanized steel panels for testing paint/vamish/lacquer/related products, test, D 2201 (064)1) Solvent-extractable matter pigment content of solvent-reducible paints, test, D 2371 (06.01) Solvent naphtha (refined) See Naphtha and naphtha derivatives Solvent-reducible paints/coatings amount of liquid separated as upper layer from a viscous salution/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, D3717 (06.01) antimony oxide content ofwhite 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/coatings, practice, D 5201 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption, spectroscopy, test, D3718 (06.01) commercial hexanes, spec., D1836 (((6.02) conducting tests on paint/varnish/lacquer/reiated 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) 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, D 5043 (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) hiding power of paints, by reflectometry, test, A D 2805 (06.01) identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D 2621 (06.01) interior flat wall paint, selection/use of test methods, practice, D 3323 (06.01) interior semigloss wall/trim enamels, selection/use of test methods, practice, D 3425 (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 content in paint, by direct aspiration atomic absorption spectroscopy, test, D 4834 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D 3624 (06.01) nature of thinners in solvent-reducible paints, qualitative determination, method, D 2349 (06.01) package stability of solvent-reducible/water-reducible paint, test, D 1849(061)1) paint spatter resistance to roller application, test, D 4707 (06.01) pigment content,'high-speed centrifuging, test, D 2698 (06.01) pigment content of solvent-reducible paints, test, D 2371 (06D1) porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) practical washability of organic coatings, test, D 4828 (06.01) preparing drawdowns of artists' paste paints, practice, D4941 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) solvent analysis, by gas chromatography direct injection method, practice, D 3271 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) sulfide in white pigment separated from solvent-reducible paints, test, D 2351 (06.02) sulfur dioxide in white pigment separated from solventreducible paints, test, D 2352 (06.02) testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D4764 (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) volatile matter content determination, test, D 2369 (06.01) volatile organic compounds (VOQ of solvent reducible paints in aerosol cans, test, D 5200 (06.01) volume nonvolatile matter in clear/pigmented coatings, test, D 2697 (06.01) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Solvent release amount of volatile organic compound (VOC) released from solventbome automotive coatings and available for removal in a VOC control device (abatement), test, D 5087(061)1) Solvent rub method MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Solvents field identification of coatings, test, D 5043 (06.01) hexyl acetate, spec., D 5137 (06.03) 614 So Sc i DUP050297129 Index ofASTM Standards, Section 6 Specimen preparation (for testing)--paints/related coatings mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) trace peroxides (>5-80 ppm), using spectrophotometer, test, E 299 (06.03) Solvents--hydrocarbon aniline point/mixed aniline point of petroleum products/ hydrocarbon solvents, test, D 611 (06.03) benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (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 (VOC) 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 constants of paints/coatings, practice, D 5201 (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) dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) ester value of solvents and thinners, test, D1617 (0603) ethyl acetate (all grades), spec., D 4614 (06.03) heptane miscibility of lacquer solvents, test, D 1476 (06.03) hexyl acetate, spec., D 5137 (06.03) isobutyl acetate (95 % grade), spec., D1718 (06.03) methyl isobutyl ketone, spec., D1153 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) nonvolatile content of resin solutions (in volatile organic solvents), test, D1259 (06.02) nonvolatile matter content, test, D 1353 (06.03) n-propyl acetate (96 % grade), spec., D 3130 (06.03) odor (characteristic/residual), test, D1296 (06.03) primary (synthetic) amyl acetate (98 % grade), spec., D 3540 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) sampling and testing dipentene, method, D 801 (06.03) sampling/testing volatile solvents/chemical intermediates (for paints/lacquer/vamish/related material), selecting test methods, D 268 (06.03) solvent composition analysis (in solvent-type paints), by gas chromatography, test, D 3271 (06.01) solvent extractable materia] in Mack pigments, test, 0 305(06.02) solvent/fuel resistance of traffic paint, test, D 2792 (06.01) solvent tolerance, of amine resins, test, D1198 (06.02) trace peroxides (>5-80 ppm), using spectrophotometer, test, E 299 (06.03) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test 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, 01364 (06.03) water miscibility of water-soluble solvents, test, D 1722 (06.03) Solvent tolerance resin solution dilutability, test, D 5062 (06.03) Southern pine wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Soybean oil degummed soybean oil, spec., D124 (06.03) refined soybean oil, spec., D1462 (06.03) Spark-source mass spectrometry Sa Spectrophotometry (headings) color of cresylic acids ("C" series standards), test, 0 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 (06D1) 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., D 3128 (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 adds, and related materials, at 2S/25C, test, D1963 (06.03) pigments, tests, D153 (06.02) sampling and testing dipentene, method, D 801 (06.03) sampling and testing pine oil, method, D802 (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 films, test, D1653 (06.01) Specific resistance (resistivity) water-soluble salts in pigments, by measuring spedfic resistance of pigment leachate, test, D 2448 (06.02) Specimen preparation (for testing)--palnts/related coatings abrading concrete, practice, D 4259 (06.01) add etching concrete, practice, D 4260 (06.01) magnesium alloys, practice, D1732 (06.01) making and preparing concrete/masonry panels for testing paint finishes, method, D1734 (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, D 2201 (06.01) preparation of methyl esters from fatty adds, for fatty add composition analysis, test, D3457 (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, D4941 (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, D 3964 (06.01) 615 DUP050297130 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, D42S8 (06.01) surface cleaning concrete unit masonry (for coating), practice, D4261 <06-01) zinc-coated (galvanized) steel, practice, D 2092 (06.01) Specimen preparation (general)--paints/irelated coatings sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Spectral data conducting tests on paint/varnisb/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (063)1) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- raetry, method, E 430 (063)1) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (063)1) 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), D1064 (06.03) spectrophotometric diene value of dehydrated castor oil/derivatives, test, D1358 (06.03) thiophene content of benzene, by spectrophotometry, test, D1685 (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 metallic/nonmetallic surfaces, by goniophoto- raetry, method, E430 (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 of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) uniformity (oftraffic paint vehicle solids), practice, D 2743 (06.01) Spectroscopy--absorption (of paint) lead/chromium content (in air particulate filter samples of lead 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, D 4563 (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 ofliquid 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, D3335 (06311) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, 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 Sa 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, D 5066 (06.01) Spray method testing industrial water-reducible coatings, guide, D 4712 (06311) Spreading rate hiding power of paints, by reflectometry, test, A D 2805 (06311) Stability--paints/related coatings/materials accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) conducting tests on paint/varaish/iacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06311) 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 of cellulose acetate, test, D 871 (06.02) heat stability of cellulose ester, test, A D 817 (06.02) light stability of clear coatings, by sunlight-through-glass method, test, D 2620 (06.01) package stability of solvent-reducible/water-reducible paint, test, D1849 (06311) Staining effect of staining agents (on organic finishes in the automobile industry), practice, D1540 (06.01) practical washability of organic coatings, test, D 4828 (06.01) stain removal (from multicolor lacquers on primed steel panels), test, D 2198 (06.01) stain resistance of factory-applied coatings on wood products, practice, D3023 (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 (06313) Steam-distilled wood turpentine See Turpentine Steel bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D4796 (06311) Steel--panels paint and related coatings exposure tests, methods for preparation, D609 (06.01) 616 Sri St. S S S $ DUP050297131 Index of ASTM Standards. Section 6 Sulfate content--paints/related coatings 1 preparation of hot-dipped nonpassivated galvanized steel panels | for testing paint/vamish/lacquer/related products, test, ' D 2201 (06.01) 1 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 of rusting on painted steel surfaces, method, A D 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 steel surfaces, in laboratory/ field/fabricating shop, test, D4417 (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, D2201 (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, D4414 (06.01) Sticking blocking resistance of trade sales paints, test, D 4946 (06.01) Stiffness free films of paints and related coatings, test, O 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, test, AD 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, D332 (06.02) Stress pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06311) 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) Strontium chromate pigment Sa Pigments (general properties) chemical analysis of strontium chromate pigment, test, D 1845 (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, D 5135 (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, D 3505 (06.03) peroxides in styrene monomer, test, D 2119 (06.03) peroxides in styrene monomer, test, D 2119 (06.03) polymer content of styrene monomer, test, D 2121 (063)3) p-tert-butylcatechol (TBC) in styrene monomer, test, D 2120 (06.03) purities/impurities, 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 (063)3) residual p-rert-butylcatechol (TBC) in styrene monomer, by addition of NaOH, test, D 4590 (063)3) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) styrene monomer 996, spec., D 2827 (063)3) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (063)2) unreacted monomer content of latexes using capillary column gas chromatography, test, D4827 (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 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) Subsieve analysis See Sieve analysis--subsieve (headings) Substrates--coating applications accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (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, D 5162 (063)1) mandrel bend test of attached organic coatings, test, D 522 (06.01) painting inspectors (metal substrates), guide, D 3276 (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 add-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) cellulose acetate propionates/butyrate, test, A D 817 (063)2) cellulose acetate, test, D 871 (06.02) 617 DUP050297132 Index of ASTM Standards, Section 6 Sulfate content--paints/related coatings lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) yeliow/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, D 2351 (06.02) Sulfur content cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, D 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, D 3961 (06.03) zinc dust (metallic zinc powder), test, D521 (06.02) Sulfur content--petroleum products mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenoi-A), practice, D4297 (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, D 2352 (06.02) Sunflower oil sunflower oil (once-refined, technical grade), spec., D 3169 (06.03) Sunlight/monochromatic light exposure lightfastness of pigments (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, D 4449 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metiy, method, E 430 (06.01) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) static friction of coating surfaces, test, D 4518 (06.01) subjecting marine antifouting coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 03259(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, D 2201 (064)1) preparatory surface cleaning of architectural sandstone, practice, D 5107 (06.01) standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) Surfacers See Primer , Surfaces (of nuclear facilities) coating contractor qualification (for nuclear-powered generation facilities), practice, D 4286 (06.01) qualification ofjourneyman painters for application of coatings to concrete surfaces of safety-related areas in nuclear facilities, practice, D 4227 (06.01) qualification of journeyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 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, D 5163 (06.01) T Suspension fluids flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Tt Sustained burning test sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (064)1,06.03) sustained burning (oflow viscosity liquid mixtures), by Wick test, D4207 (06.03) Swelling clear/pigmented organic coatings, test, D1308 (064)1) Ter c Swelling and cracking edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) Ten: e\ Synthetic amyl alcohol amyl alcohol (synthetic), spec., D 319 (06.03) ex Synthetic black iron oxide (magnetite) See Iron oxide black fre Synthetic drying oils See Oils--drying low Synthetic ethylhexanol See 2-Ethylhexano) mir Synthetic hematite (red) See Iron oxide red Synthetic phenolic resins non 1 opei See Resins--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 ] P'grc , solid! temp ) i temp c I Tack apparent tack of printing inks/vehicles, by inkometer, test, D4361 (06.01) Tag closed-cup tester flash point by Tag closed tester, test, D 56 (064)3) Tag open-cup tester flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Talc (pigment) See Magnesium silicate Tall oil/tall oil rosin tall oil, methods of testing, D 803 (064)3) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) Tank cars/wagons/bther shipping containers See Containers--tank cars/wagons Tanks - cresylic acid and phenol, practice, D3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Tempera operat w. LTen-degpirt * L ** Tension (t I adhesio ten paints/ri ` Preparat ` D4 aromatic i D41 cellulose/ freeze-tha D22 Paint/varr 16 , ferpene aico sampling s 618 DUP050297133 Index of ASTM Standards, Section 6 Thickness--paints/related coatings/materials Tar acids color of cresylic acids ("C" series standards), test, D 3627 (06.03) gel time, test, D 2870 (06.03) phenol content (of tar acid mixtures), by gas liquid chromatog raphy, test, D 3626 (06.03) TBC inhibitor p-tert-butyicatechol (TBC) in styrene monomer, test, D 2120 (06.03) residual p-fert-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 (06.01) chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D4797 (06.01) Temperature service applications--high conducting tests on paint/varnish/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 UVcondensation iight-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) low-temperature coalescence (of latex 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-are 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 (Bisphenoi A), test, D 4493 (06.03) temperature-change (high-low) resistance ofclear 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) paists/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/materials aromatic hydrocarbons/related chemicals, terminology, D4790 (06.03) cellulose/cellulose derivatives, terminology, D1695 (06.02) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) paint/varnish/lacquer/related products, terminology, D16 (063)1,06.02,06.03) 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 and raw) Testing methods recording results on singie-/multi-panel forms, method, A D 1150 (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., D5139 (06.01) Test specimens See Specimen preparation (for testing) (headings) Tetraethyiammonium 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 (063)1) Thermistor-type infrared radiation thermometers temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (063)1) Thermometers thermometer specifications for flash point (of fuel oiis/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D93 (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 (063)1) 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, D4640 (06.02) Thermosetting phenol-formaldehyde See Phenolic resins Thickness--paints/related coatings/materials dry film thickness, of nonmagnetic coatings (paints/ varnish/lacquer) applied to a ferrous base, D1186 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) erosion testing of antifouiing paints, using high velocity water, test, D 4938 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) subjecting marine antifouiing coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) 619 DUP050297134 Index of ASTM Standards, Section 6 Thickness--paints/related coatings/materials wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Thinners (paint) See Paint--thinners Thiophene content refined benzene, by gas chromatography (with flame photometric detection), test, D 4735 (06.03) thiophene content of benzene, by spectrophotometry, test, D1685 (064)3) Thiosulfate method chromium content of strontium chromate pigment, by thiosulfate method, test, D 1845 (06.02) Thixotropy rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Three-degree xylol (3* xylol) See Xylene (nitration grade) Time tests amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) Tinting strength colored pigments (dry/pastes in oil), with a mechanical muller, test, D 387 (064)2) relative tinting strength of chromatic paints, test, D 4838 (06.01) relative tinting strength of printing ink dispersions, test, D 2066 (06.01) 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) Titanium content white titanium pigments, chemical analysis, test, D1394 (06.02) Titanium dioxide slurries weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) Titanium dioxide (Ti02) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, D 3720 (06.02) relative tinting strength of white pigments, by reflectance measurements, test, D 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, D 4563 (06.01) titanium dioxide pigments, spec., D 476 (06.02) weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) white titanium pigments, chemical analysis, test, D1394 (06.02) Titer solidification (titer) point of fatty acids, test, D1982 (06.03) Titrimetric method resin solution dilutability, test, D 5062 (06.03) Toluene acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color, test, D 848 (064)3) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (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) distillation, test, D 850 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (064)3) nitration grade toluene, spec., D 841 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) soluble cellulose nitrate, testing, methods, D 301 (06.02) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gp chromatography, test, D 2360 (064)3) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (064)3) volume/weight of industrial aromatic hydrocarbons, method, D1555 (064)3) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) Toluene insolubles content toluene-insoluble solid matter (sand/chips/dirt/bark) in rosin, test, D 269 (064)3) Tolnidine red pure toluidine red toner, spec., D 656 (06.02) Tolnidine red pigment para red/toluidine red pigments, testing, D 970 (06.02) Toner (para/toliiidine red) para red/toluidine red pigments, testing, D 970 (06.02) Top liquid layers amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) Total chloride content See Chloride content (headings) Total nitrogen oxides content See Nitrogen oxides Total sulfur content See Sulfate content (headings) Total titanium total titanium in white titanium pigments, by Jones reductor/aluminum reduction method, test, D1394 (064)2) Toxicity/toxicology unreacted monomer content of latexes, by gas-liquid chromatography, test, D4747 (06.02) Trace elements contents sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, D 3961 (06.03) Trace elements contents--chloride Sa Chloride content (headings) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) Trace impurities content See Impurities content Sa Purity Trace lead/cadmium/cobalt paint lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (064)1) Trace monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D4747 (064)2) Trade sales paint blocking resistance of trade sales paints, test, D 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 D 868 (06.01) evaluating degree of chipping, A D 913 (06.01) glass spheres in, test for roundness, D 1155 (06.02) laboratory evaluation of degree of bleeding of trafiic/pavement marking paint, test, D 969 (064)1) 620 JL DUP050297135 Index of ASTM Standards, Section 6 Urethanes 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 retroreflective pavements markings/industrial uses), test, D1214 (06.02) solvent and fuel resistance, test, D 2792 (06.01) uniformity of vehicle solids (by spectroscopy/gas chromatog raphy), selection and use of test procedures, practice, D2743 (06.01) Transesterification identification of carboxylic acids in alkyd resins D 2455 (06.02) Transfer efficiency (TE) evaluating and comparing transfer conditions-Iaboratory conditions, test, D5009 (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, 05108 (06.01) TricUorotriiluoroethane-extractable matter permanganate time of acetone/methanol, test, D1721 (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) Tristimulus value Sa Color (headings) calculation of color differences from instrumentally measured color coordinates, test, D 2244 (06.01) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometiy, test, E 97 (06.01) True red lead lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) Tung oil See Oils--tung Tunnel method small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, D 3806 (06.01) Turbidlmetric 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., D13 (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 acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) apparent pH of electrocoat baths, test, D 4584 (06.01) electrical conductivity of electrocoat baths, test, D4399 (06.01) nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) Ultramarine blue pigment chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) ultramarine blue pigment, spec., D 262 (06.02) Ultraviolet-cured coatings cure time, practice for reporting, D 3732 (06.01) estimating package stability of coatings for ultraviolet curing, test, D 4144 (06.01) Ultraviolet (UV) light/radiation accelerated testing of paints/varnishes/lacquers/related products, using-filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-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, D 50 (06.02) raw/burnt umber pigments, spec., D 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/materials Unloading tank cars/wagons/other shipping containers cresylic acid and phenol, practice, D 3852 (06.03) naphthalene, maleic/phthaiic anhydride, practice, D 3438 (06.03) sampling and handling aniline, practice, D 3436 (06.03) Unreacted monomer content unreacted monomer content of latexes, by gas-liquid chromatography, test, D4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D4827 (06.02) Unsaponifiable matter content alkyd resins and resin solutions, test, D1397 (06.02) rosin, test, D1065 (06.03) tall oil, methods of testing, D 803 (06.03) tricresyl phosphate, test, D1399 (06.03) unsaponifiable matter in drying oils/fatty adds/polymerized fatty adds, test, D1965 (06.03) Unsaturation drying oils/derivatives total, by modified RosenmundKuhnhenn method, test, D1541 (06.03) drying oils/derivatives Wijs method, test, D1959 (06.03) Up and down method impact resistance of pipeline coatings, by falling weight test, G14 (06.01) Upper liquid layer amount of liquid 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) 621 DUP050297136 Index of ASTM Standards, Section 6 Urethanes unreacted toluene diisocyanates in urethane prepolymers/ coating solutions, by gas chromatography, test, D3432 (06.02) Urethanes--coatings 2-ethoxyethyl acetate (99 % grade), spec., D 3728 (06.03) isocyanate group content of urethane raaterials/prepoiymers, test, D 2572 (06.02) unreacted toluene diisocyanates in urethane prepolymers/ coating solutions, by gas chromatography, test, D 3432 (06.02) V Vanadium content paint driers, by EDTA method, test, D 3988 (06.03) Vapors chemical resistance of pipeline coatings, test, G 20 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) Variances in manufacturing process sampling industrial chemicals, annex, practice, E 300 (06.03) Varnish acidity in volatile solvents/chemical intermediates (used in paint/vamish/lacquer/related products), test, D1613 (06.03) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) Varnishes abrasion resistance, by air blast abrasion test, A D 658 (06.01) abrasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) acid value of organic coating materials, test, D1639 (06.01) adhesion (to smooth panel surfaces), by scrape adhesion test, D 2197 (06.01) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) dear/pigmented organic coatings, test, D1308 (06.01) color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) discoloration (light stability), test, D 2620 (06.01) dried varnish films, test, D 1647 (06.01) dry film thickness of nonconductive coatings (applied to nonferrous metal base), nondestructive measurement, test, D1400 (06.01) dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01) elastidty/toughness of varnishes, test, D1642 (06.01) elongation/tensile strength/stiffness, test, D 2370 (06.01) exterior durability, test, D1641 (06.01) film formation rates in drying or curing process, at room temperature, test, D1640 (06.01) flash point of liquids, by Setaflash closed-cup apparatus, test, D3278 (06.03) gas checking and draft test, D1643 (06.01) gladal acrylic add (99.0 % grade), spec., D 4416 (06.03) high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) indentation hardness of organic coatings, by Knoop and Pfund methods, test, D1474 (06.01) liquid paint driers, selection of test methods, D 564 (06.03) methyl n-amyl ketone (98 % grade), spec., D 4360 (06.03) moisture vapor transmission of organic coating films, test, D1653 (06.01) nonvolatile matter content, test, D1644 (06.01) paint and related coatings exposure tests, methods for preparation, 0609 (06.01) paint/vamisb/laoquer/related products, terminology, D16 (06.01,06.02, 06.03) paint/varnish/lacquer/related products, test, A D1475 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) preparing glass panels for testing, D3891 (06.01) qualitative detection of rosin in varnishes, by Lieberman- Storch/Halphen-Hicks tests, D1542 (06.01,063)2) rosin acids content, test, D1469 (06.02) sampling and testing shellac varnish, D1650 (06.02) selection and use of test procedures, D154 (06.01) spedfic gravity at 25/25C, test, D1963 (06.03) standard environments for conditioning/testing paint/ varnish/lacquer/related materials, spec., D 3924 (06.01) steel surfaces, resistance to failure, by water immersion test, D 870 (06.01) testing water resistance ofcoatings at 100 % relative humidity, practice, D 2247 (06.01) viscosity of paints/varnishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) viscosity (of paints/vamishes/lacquers/related materials), by dip-type viscosity cups, test, D4212 (06.01) volatile content in phenolic resins, test, 04639 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (06.02) wet film thickness of organic coatings, D1212 (06.01) wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Vegetable origin artists' punts (oil/resin-oil/alkyd), spec., D 4302 (063)1) Vehicles nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) Vehlde separation--solvent-type paints amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) high-speed centrifuge, for pigment content, test, D 2698 (06.01) infrared identification of vehicle solids from solvent-redudble paints, by infrared spectroscopy, test, D2621 (06.01) pigment content of solvent-redudble paints, test, D 2371 (06.01) vacuum distillation (for vehicle separation in solvent-type paints), practice, D 3272 (06.01) vehicle separation from solvent-redudble paints, by centrifuge, practice, D 2372 (06.01) Vehicle solids content See Solids content Venetian red chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) Vinyl acetate acetaldehyde content of vinyl acetate, test, D 2191 (06.03) addity in vinyl acetate and acetaldehyde, test, D 2086 (063)3) hydroquinone in vinyl acetate, test, D 2193 (06.03) vinyl acetate, spec., D 2190 (06.03) Vinyl antifouling coatings See Antifouling coating system Vinyl chloride monomer (residual) content residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D3680 (06.02) Viscometers--Brookfield rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Viscometers--falling rod viscosity of printing inks/vehicles, by falling-rod viscometer, test, D4040 (06.01) 622 DUP050297137 Index of ASTM Standards, Section 6 Volatile matter content Viscometers--Ford viscosity of paints/varnishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) Viscometers--Gardner-Holdt tall oil, methods of testing, D 803 (06.03) Viscometers--ICl cone/plate high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Viscometers--Saybolt viscosity of pine tars/pine-tar oils, by Stonner/Saybolt Furol viscometers, test, D 8S6 (06.03) Viscometers--Stormer viscosity of pine tars/pine-tar oils, by Stormer/Saybolt Furol viscometers, test, D856 (06.03) Viscometers--Weissenberg Rheogoniometer viscosity of polymeric powders/powder coatings, test, D34S1 (06.01) Viscometers--Zahn coil coatings, testing, practice, B 3794 (06.01) Viscosity--paints/related coatings/materials cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, D 871 (06.02) coil coatings, testing, practice, D 3794 (06.01) comparison of the brush drag of latex paints, test, D 4958 (06.01) consistency of paints, using Stormer viscometer, test, D 562 (06.01) dip-type viscosity cup, test, D 4212 (06.01) ethylcellulose, test, D 914 (06.02) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) intrinsic viscosity of cellulose, test, D1795 (06.02) methylcellulose, test, D1347 (06.02) paints/vamishes/lacquers, by Ford viscosity cup, test, D 1200 (06.01) polymeric powders/powder coatings, by Weissenberg rheogoniometer, test, D 3451 (06.01) resin solutions, test, D1725 (06.02) rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (064)1) rosin oil, test, D1131 (06.03) sodium glycolate content of sodium carboxymethyicellulose, test, D1439 (06.02) soluble cellulose nitrate, 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-tiome method, test, D1545 (06.01, 064)2,06.03) viscosity of cellulose derivatives, by ball-drop method, test, D1343 (064)2) viscosity of paints/related materials, by ISO flow cups, test, D 5125 (064)3) viscosity of pine tars/pine-tar oils, by Stormer/Saybolt Furol viscometers, test, D 856 (06.03) viscosity of printing inks/vehicles, by falling-rod viscometer, 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 of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) liquid/solid status (of viscous materials), test, D 4359 (06.01) Visual examination--paints/related coatings/materials clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) color of cresylic acids ("C" series standards), test, D 3627 (06.03) color (of maleic anhydride/phthalic anhydride--in molten state and after heating), by platinum-cobalt scale, test, D 3366 (06.03) color (of solid aromatic hydrocarbons/related materials--in molten state), by platinum-cobalt scale, test, D 1686 (06.03) evaluating degree of bleeding of traffic/pavement marking paint, test, AD868 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (064)1) 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, D 3928 (06.01) laboratory evaluation of degree of bleeding of traffic/pavement marking paint, test, D969 (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, D 4939 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) Visual examination--pipeline coatings cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) effects of outdoor weathering on pipeline coatings, test, G 11 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) VM & P naphthas VM & P naphthas, spec., D 3735 (06.03) VOC abatement 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) VOC calculation volatile organic content (VOC) of paints/related coatings, selecting test procedures, practice, D 3960 (06.01) Volatile acids content sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) Volatile liquids low viscosity, rate of evaporation, test, D3539 (06.01) Volatile matter content calcium borosilicate, test, D 4487 (064)2) cellulosics/emulsions/resin solutions/sheilac/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 of drying oils, test, D I960 (06.03) moisture content ofpigments, D 1208 (06.02) paint/raw paint material, practice, D 2832 (064)1) paints (solvent-reducible), test, D 2369 (06.01) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (064)2) 623 DUP050297138 Index of ASTM Standards, Section 6 Volatile matter content 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/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) Volatile organic compounds (VOC)--paints/related coatings dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) distillation range (between 30 and 350"C) of volatile organic liquids, test, D1078 (06.03) nonvolatile content in silanes/siloxanes/silane-siloxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) nonvolatile content of resin solutions (in volatile organic solvents), test, D 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/related coatings, selecting test procedures, practice, D 3960 (06.01) Volatile organic compounds (VOC)--paints/related materials calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Volatile resin acids content See Resins (headings) Volatile solvents (in paints/coatings) See Solvents--paints/related coatings/materials Volatility distillation range (between 30 and 350"C) of volatile organic liquids, test, D1078 (06.03) Volume--petroleum products volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Volume--volume change wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D4213 (06.01) Volume nonvolatile content volume nonvolatile matter in clear/pigmented coatings, test, D 2697 (06.01) Volume solids calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Volumetric measurement water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, D4942 (06.01) w Washability interior architectural coatings, test, D 3450 (06.01) practical washability of organic coatings, test; D4828 (06.01) Water water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, D 4942 (06.01) Water--high-purity/reagent-grade reagent water, spec., D 1193 (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 antifouling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, D 5108 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in 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, G 18 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Water-base paints See Latex paints Water channel method erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) Watercolor paint Sa Artists' paints artists' watercolor paints, spec., D 5067 (06.01) Water content--paints/related coatings/materials cresylic acid content (of alkaline cresylate solutions), chemical analysis, D 3439 (06.03) fatty nitrogen compounds, test, D 2072 (06.03) Karl Fischer reagent method, test, D4017 (06.01) moisture content of pigments, D1208 (06.02) oil/water presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), D4285 (06.01) phenol/related materials, by iodine reagent method, test, D1631 (06.03) water content ofwater-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) water in liquid naval stores, test, D 890 (06.03) water in volatile solvents, by Fischer reagent titration method, test, D1364 (06.03) Water content--petroleum products water in petroleum products/bituminous materials, by distillation, test, D 95 (06.01,06.03) Water fog test testing water resistance of coatings, using water fog apparatus, practice, D 1735 (06.01) Water immersion resistance to failure of paints and related coatings, on steel surfaces, D 870 (06.01) Water-insoluble impurities content See Impurities (headings) Water-insoluble matter content apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D1347 (06.02) Water miscibility Sa Miscibility water miscibility of water-soluble solvents, test, D1722 (06D3) Water of hydration calcium borosilicate, test, D4487 (06.02) Water penetration water penetration into pipeline coatings, test, G 9 (06101) Water pickup water pickup of lithographic printing inks/vehicles in a laboratory muter, test, D 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-soluble-matter content conductimetric analysis ofwater-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) moisture content of pigments, D1208 (06.02) painting inspectors (metal substrates), guide, D 3276 (06.01) 624 sal' sar wa wa yel Wate VVatc ret Watt mt Watt m< Wax ale Wea re Wea co ev Wea ac cc D te Wet cc o t t c w We ii P ti v We v We P We e DUP050297139 Index of ASTM Standards, Section 6 Wijs procedure--iodine value salt content of blue pigments, test, D 1135 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (06.02) water miscibility of water-soluble solvents, test, D1722 (06.03) water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Water-soluble solvents See Solvents (headings) Water spotting reporting paint film failures characteristic ofexterior latex paints, classification, D1848 (06.01) Water vapor permeance moisture vapor transmission of organic coating films, test, D1653 (06.01) Water vapor transmission moisture vapor transmission of organic coating films, test, D1653 (06.01) Waxes alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) Wear testing resistance to wear of traffic paint, method, A D 913 (06.01) Weathering conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) panel, recording results of exposure tests, single-/multi-panel forms, A D1150 (06.01) Weathering--accelerated and outdoor accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) coatings (applied to metal substrates), practice, D 4141 (06.01) Dew cycle, light-water-exposure apparatus, practice for operating, D 3361 (06.01) testing water resistance ofcoatings, using water fog apparatus, practice, D1735 (06.01) Weathering--outdoor conducting exterior exposure tests of (exterior) paints on steel, test, D1014 (06.01) conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D1006 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Wright impact resistance of pipeline coatings, by falling weight test, 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 aromatic hydrocarbons, method, D1555 (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/lacquer/related products, test, A D1475 (063)1) Weight percent epoxide (WPE) epoxy content of epoxy resins, test, D1652 (06.02) Weight solids calculating formulation physical constants of paints/coatings, practice, D5201 (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 fining application), spec., D4618 (06.01) Western red cedar wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Wet film thickness See Film--wet film thickness Wet film thickness gage wet film thickness of organic coatings, D1212 (06.01) Wet ground muscovite mica See Stone--mica Wet-to-dry hiding change wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) White architectural enamels See Architectural coatings White extender pigments See Extender pigments White hiding pigments See Antimony oxide/Basic carbonate white lead Sa Basic sulfate white lead/Leaded zinc oxide Pigments (general properties)/Titanium 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, D 3280 (06.02) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) basic carbonate white lead pigment, spec., D 81 (06.02) chemical analysis of white pigments, selection of test methods, guide, D 34 (06.02) particle size distribution, by hydrometer of common white extender pigments, test, D3360 (063)2) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, D 3720 (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) sulfide in white pigment separated from solvent-reducible paints, test, D 2351 (06.02) sulfur dioxide in white pigment separated from solventreducible paints, test, D 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, D1394 (06.02) zinc oxide pigments, spec., D 79 (06.02) White pine wood used as panels in weathering tests of coatings, spec., D 358 (06.01) White zinc pigments See Zinc oxide Whiting See Calcium carbonate Wick test sustained burning (oflow viscosity liquid mixtures), by Wick test, D4207 (063)3) Wijs procedure--iodine value drying oils and their derivatives, test, D1959 (06.03) 625 DUP050297140 Index of ASTM Standards, Section 6 Wijs procedure--iodine value fatty amines/diamines, test, D 2075 (06.03) Wire-wound drawdown bar method coil coatings, application using a wire-wound drawdown bar, practice, D 4147 (06.01) Wotfe-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, D 3259 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Wood and wood products--cellulose pulp metals (iron/copper/manganese/calcium) 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, D 2793 (06.01) conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D1006 (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, D3459 (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 (06.01) Wood rosin See Rosin Sa Oils (headings) Wood turpentine See Turpentine X Xenon lamps lightfastness of pigments (in artists' paints), test, D 4303 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials; practice, G 26 (06.01). X-ray diffraction -- ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, D 3720 (06.02) Xylene acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color, test, D 848 (06.03) aromatic hydrocarbons/reiated chemicals, terminology, D 4790 (06.03) distillation, test, D 850 (06.03) flash/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) sampling/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, D 2360 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) xylenes for p-xylene feedstock, spec., D5211 (06.03) meta-Xylene apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) volume/weight of industrial aromatic hydrocarbons, method, 01555(06.03) ortAo-Xylene apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) purity, by gas chromatography, test, D 3797 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) o-xylene 950, spec., D 4076 (06.03) para-Xylene analysis ofp-xylene, by gas chromatography, method, D 3798 (06.03) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) high purity p-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, D1555 (06.03) xylenes for p-xyiene feedstock, spec., D5211 (06.03) Xylene (five-degree) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) Xylene (mixed) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) vohune/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Xylene (nitration grade) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) xylene (nitration grade), spec., D 843 (064)3) Xylene (ten-degree) xylene isomer analysis, by gas chromatography, test, , D 2306 (06.03) Xylenol water content, by iodine reagent method, test, D1631 (06.03) Y Yellow ocher See- Ocher Yellow pigments chrome yellow/orange pigment, spec., D-211 (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) 626 ! | j i I DUP050297141 Index of ASTM Standards, Section 6 ZTO chromate Yield value laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) z Zahn viscometers See Viscometers--Zahn Zeisel technique ethoxyl substitution in cellulose ether products, by gas chromatography, test, D4794 (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 Sa Oils--drying Zinc dust Sa Pigments (general properties) analysis, D521 (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, D4752 (06.01) Zinc sulfide 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, D3969 (06.03) ZTO chromate See Zinc chromate (yellow) 627 DUP050297142 1916 Race Street Philadelphia, PA 19103 Phone: (215) 299-5454 FAX: (2151 977-9679 European Office 27-29 Knowl Piece, Wilbury Way Hitchin, Herts SG4 OSX, England Phone: 0462-437933 FAX:0462-433678 Mmmmmp AmscATim THIS APPLICATION IS FOR SOCIETY MEMBERSHIP ONLY. 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