Document pB7m3vkY5zoprpERddJJBkgQa

N36982 DU PONT DEC 01 199? / HI ANNUAL BOOK* NETWORK la XSTM SMND4RDS B MV Paints, Related Coatings, andAromatics Paint--Fatty Oils and Acids, VOLUME Solvents, Miscellaneous; 06.03 Aromatic Hydrocarbons Includes standards of the following committees: D-1 on Paint and Related Coatings and Materials D-16 on Aromatic Hydrocarbons and Related If Chemicals Publication Code Number (PCN): 01-060392-14 ASTWI 1916 Race Street, Philadelphia, PA 19103-1187 USA (215)299-5400 TWX: 710-670-1037 fl FAX: 215-977-9679 DUP050295640 Director, Editorial Services: Roberta A. Storer Manager, Standards Publications: Joan L. Cornillot 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 0-8031-1709-4 (volume) Copyright 1992 AMERICAN SOCIETY FOR TESTING AND MATERIALS, Philadelphia, PA. Prior editions copyrighted 1991 and earlier, by the American Society for Testing and Materials. All rights reserved. This material may not be reproduced or copied, in whole or in part, in any printed, mechanical, electronic, film, or other distribution and storage media, without the written consent ofthe publisher. Photocopy Rights Authorization to photocopy items for internal or personal use, or the internal or personal use of specific clients, is granted by the AMERICAN SOCIETY FOR TESTING AND MATERIALS for users registered with the Copyright Clearance Center (CCC) Transactional Reporting Service, provided that the base fee of $2.50 per copy, pins $0.50 per page is paid directly to CCC, 27 Congress St., Salem, MA 01970; Tel. (508) 744-3350. 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IV DUP0502 95643 Caveat Statements and Policies in Standards ASTM caveat statements on Safety Hazards and Fire Hazards are required to appear in standards where appropriate. They are located in the scope section of applicable standards. The caveats on General Statement of ASTM Policy and Patents are contained in all standards and located at the end of each standard disclaimer. For more information on the caveats see Section F2 of the Form and Style Manual for ASTM Standards. v DU P050295644 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 RelatedMaterials (I): A 751 to E 354 Volume 03.06 Analytical Chemistry for Metals, Ores, and RelatedMaterials (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 Rock; 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 DUP0502 95645 LISTED BY SECTION AND VOLUME Section 7--Textiles Volume 07.01 Textiles (I): D 76-D 3219 Volume07.02 Textiles (II): D 3333-latest U I Section 8--Plastics Volume 08.01 Plastics (I): C 177-D 1600 Volume 08.02 Plastics (II): D 1601-D 3099 Volume 08.03 Plastics (III): D 3100-latest Volume 08.04 Plastic Pipe and Building Products Section 9--Rubber Volume 09.01 Rubber, Natural and Synthetic--General Test Methods; Carbon Black Volume 09.02 Rubber Products, Industrial--Specifications and Related Test Methods; Gaskets; Tires Section 10--Electrical Insulation and Electronics Volume 10.01 Electrical Insulation (I)--D 69-D 2484 Volume 10.02 Electrical Insulation (II)--D 2518-latest Volume 10.03 Electrical Insulating Liquids and Gases; Electrical Protective Equipment Volume 10.04 Electronics (I) Volume 10.05 Electronics (II) Section 11--Water and Environmental Technology Volume 11.01 Water 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 NonmetalKc Materials Volume 14.03 Temperature Measurement Section 15 General Products, Chemical Specialties, and End Use Products Volume 15.01 Refractories; Carbon and Graphite Products; Activated Carbon Volume 15 02 Glass; Ceramic Whitewares Volume 15 03 Space Simulation; Aerospace and Aircraft; High Modulus Fibers and Composites Volume 15 .04 Soap; Polishes; Leather; Resilient Floor Coverings Volume 15 .05 Engine Coolants; Halogenated Organic Solvents; Industrial Chemicals Volume 15 .06 Adhesives Volume 15 .07 End Use Products Volume 15 .08 Fasteners Volume 15 .09 Paper; Packaging; Flexible Barrier Materials; Business Imaging Products Section 00 Index r Volume 00. 01 Subject Index and Alphanumeric List vu DUP0502 95646 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, Methl.................... 03.02 Aerospace Industry Methods..................................... 15.03 Criteria for the Evaluation of Testing 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............ 11.04 Electrical 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.................... .......................... V.. 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 %............................. 15.08 Cellulose..-..................................... 06.02 Fatigue.,. J.,.................. ...................... . ,.............. ,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 FibeiTCement Products.......... ................................ 04.05 Advanced Ceramics............................................ 15.01 Filtration............ ................ 14.02 Ceramic Whitewares............................................. 15.02 Fire Standards ....-- .................. ....................... 04.07 Ceramics for Electronics ....................................... 10.04 Flexible 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.......................... 04.05Forensic Sciences........................................................ 13.01 Chemicals, Industrial................................................. 15.05 Fracture Testing............ ,................... ........................ 03.01 Chromatography....................................................... 14.01 Gaseous Fuels................ 05.05 Closures........................................... .1.5.09 ..Gaskets........ ....... 09.02 Coal and Coke............................................... 05.05 Geotextiles and Related Products........................... 04.08 Compatibility and Sensitivity of Materials in Oxy Geothermal Resources and Energy........................ 12.02 gen-Enriched Atmospheres.......................... 14.02 Glass.. ........ ...................................................: 15.02 Computerization of Material Property Data........................14.01Graphite Products, Manufactured........................... 15.01 Computerized Systems.............................. 14.01 Graphite Products, Nuclear ..................................... 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 ,f j j ! ij I 1 "| 1 J | 1 j | 1 s i j i vm DUP050295647 LISTED BY SUBJECTS SUBJECT VOLUME SUBJECT VOLUME Index (for all volumes)................................. .......... Industrial Chemicals..................................... .......... Iron Castings................................................. .......... Knock Test Manual ..................................... .......... Laboratory Apparatus.... ........ ...... Leather........................................................... .......... Lime.........;........... ,.. * .............. .......... Magnesium and.Magnesium Alloys ....... ........... 00.01 15.05 01.02 05.04 14.02 15.04 04.01 02.02 Magnetic Properties....................................... Malleable Iron............................................... ........... Masonry Units............................................... ...... Meat and Poultry................................... _____ Medical and Surgical Materials and Devices ...... 03.04 01.02 04.05 15.07 J3.01 Metallic and Inorganic Coatings........ .. <......... 02.05 Metallography ............................ .............. - .......... 03,01. Metal Powders ........................... .................. .......... 02.05 Metals, Chemical Analysis' .;....................... .03.05; 03.06 Metals, Effect of Temperature on Properties 03.01 Metals, Physical' and Mechanical Testing... .......... 03.01 , Metric Practice.................V. -- .......... 14,02 ' Mortars for Unit Masonry ..................... .. ....... 04.05 Naval Stores............................. -- ,.., . 06.03 Nickel and Nickel Alloys ......................................... 02.04 Nondestructive Testing...................... 03.03 Nonferrous Metals, General..................................... 02.04 Nonmetals, General Test Methods........................... 14.02 Nuclear Materials................ .......................... 12.01, 12.02 Occupational Health and Safety .............................. 11.03 Oil Spill Response, Hazardous Substances.......... . 11.04 Ores, Metal Bearing, Sampling and Analysis . 03.05, 03.06 Orthotics, External Prosthetics, and Mobility Aids............................................................... 13.01 Packaging.................................................................... 15.09 Paint and Related Coatings and Materials: Fatty Oils and Acids, Solvents, Miscellaneous... 06.03 'Pigments, Resins, and Polymers........................... 06.02 Tests for Formulated Products and Applied Coat ings.................................................................. 06.01 Paper.......................................................................... 15.09 Pavement Management Technologies...... .............. 04.03 Particle Size Measurement............................................ 14.02 Pesticides.......................... 11.04 Petroleum Products and Lubricants......................... 05.01, 05.02,05.03,05.04 Pldstics............................................... 08.01, 08.02, 08.03 Plastic Pipe and Building Products........................... 08.04 Polishes ...................................................................... 15.04 Porcelain Enamel........................................ 02.05 Pressure Vessel Plate and Forgings........................... 01.04 Products Liability Litigation, Technical Aspects of....................................... 14.02 Protective Clothing................................................... 15.07. Protective Coating and Lining Work for Power Generation Facilities............................. 06.01,12.01 Protective Equipment, Electrical, for Workers........ 10.03 Radioisotopes and Radiation Effects...................... 12.02 Reactive and Refractory Metals............................... 02.04 Refractories...............................................................? 15J}]L; Resilient Floor Coverings....... .......... ...... :............ 15.04 Resinography................................. 14.01 Resource Recovery.................................................... 11.04 Road and Paving Materials.................... 04.03 Robotics...................................................................... 14.01 Roofing, Waterproofing, and Bituminous , Materials .............................................04.04 Rubber ................. .............................................. 09.01,09.02 Security Systems and Equipment.............................. 15.07 Sensory Evaluation of Materials and Products .... 15.07 Shipbuilding................. 01.07 Sintered P/M Structural Parts................. 02.05 Skiing, Snow............. .............................................. 15.07 Soap ............. ..... ...................................... s............ 15.04 Soil and Rock............ ..................,............... 04.08 Solar Energy Conversion.................... 12.02 Space Simulation ..................... ................... 15.03 -Spectroscopy ................................03.06, 14.01 Sports Equipment and Fatalities................. 15.07 Statistical Methods ,. ............... 14.02 Steel: < Bars....................................................................... 01.05 Bearing Steel......................................................... 01.05 Bolting............................................................ 01.01, 15.08 Castings.................................................................. 01.02 Chain ................................................................. , 01.05 Concrete Reinforcing............................................. 01.04 Detention and Correctional Facilities................... 04.07 Fasteners ............................. 15.08 Forgings..................................... 01.04,01.05 Galvanized................. 01.06 , Piping, Tubing, and Fittings .............................. 01.01 Elate* Sheet, and Strip........ .................................. 01.03 Pressure Vessel Plate and Forgings....................... 01.04 Rails, Wheels, and Tires....................................;. 01.04 Springs^........ ..................i.............................. .. 01.05 Stainless' Steel......................................................... 01.01, 01.02,01.03,01.04,01.05 Structural Steel ..................... 01.04 Wire ...:...... ..........,.................................. ... 01.03 Surface Analysis........ ......................................................03.06 Surgical Materials and Devices........................... 13.01 Temperature Measurement.......... 14.03 Textiles ...........................:................................ 07.01, 07.02 Thermal Measurements............................................. 14.02 Thermal Insulation ...................... 04.06 Thermocouples ............ 14.03 Thermostats, Electrical Heating and Resistance, Contacts, and Connectors.................................. 03.04 Tires.......... ................................................................. 09.02 Traveled Surface Characteristics:........... 04.03 Vacuum Cleaners ..;........... 15.07 Vitrified Clay Pipe. `.................. 04.05 Waste Management........... ....... .......... .................. 11.04 Water.......... "... ................... ...................... 11.01, 11.02 Wear and Erosion............ ;...................................... 03.02 Wood.......................................................................... 04.09 * I: H ix l DUP050295648 Contents 19.92 ANNUAL BOOK OF ASTM STANDARDS, Volumes 06.01, 06.02, and 06.03 St a n d ar d s Re l at in g t o Pa in t --Tes t s f o r Fo r mu l at e d Pr o d u c t s a n d Ap p l ie d Co a t in g s ; Pig men t s , Re s in s a n d Po l y mer s ; Ce l l u l o s e ; Fa t t y Oil s a n d Ac id s , Mis c el l an e o u s ; Ar o ma t ic Hy d r o c a r bo n s A complete Subject Index begins on p. 861 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 than one revision during that year, that is 92a indicates the second revision in 1992, 92b the third revision, etc. Standards that have been reapproved without change are indicated by the year of last reapproval in parentheses as part ofthe designation number, for example, (1992). A superscript epsilon indicates an editorial change since the last revision or reapproval--<1 for the first change, <2 for the second change, etc. PAINT AND RELATED COATINGS AND MATERIALS B 117-90 B 287-74(1980)" D 12-88 D 13-82 (1987) D 16-91 D 29-81 (1987)" D 34-91 D 49 - 83 (1990)" D 50 - 90 D 56 - 87 D 79-86 D 81-87 D 83-84(1989) D 85- 87 (1991)" D 86 - 90 D 93 - 90 D ' 95 - 83 (1990) D 124-88 D 126 - 87 (1991)" D 130-88 D 153-84 (1989)" D 154 - 85 (1989)" D 185 - 84 (1989)" D 207 - 55 (1987) D 209-81 (1989) D 210 - 8 la (1991)" D 211 -67 (1989)" D 212-87 D 215-91 D 233 - 65 (1981)" D 234 - 82 (1991)" D 235 - 87" VOLUME Method of Salt Spray (Fog) Testing................................................................................................................... 06.01' Method of Acetic Acid-Salt Spray (Fog) Testing (Discontinued1988f--Replaced by Practice G 85) .. 06.01 Specification for Raw Tung Oil............. 06.03 Specification for Spirits of Turpentine.............................................. 06.03 Terminology Relating to Paint, Varnish, Lacquer, and Related Products .................. .. .06.01,06.02, 06.03 Test Methods for Sampling and Testing Lac Resins............................................................... Practice for Chemical Analysis of White Pigments................................................................................... ..06.02 Test Methods of Chemical Analysis of Red Lead.............................................................................................06.02 Test Methods Of Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and . Manganese......................................................................................................................................................... 06.02 Test Method for Flash Point by Tag Closed Tester............................................... 06,03 Specification for Zinc Oxide Pigments......................................................... 06.02 Specification for Basic Carbonate White Lead Pigment.................................................................................. 06.02 Specification for Red Lead Pigment..................................................................................................................06.02 Specification for Ochre Pigment........................................................................................................................ 06.02 Test Method for Distillation of Petroleum Products ............................ 06.03 Test Methods for Flash Point by Pensky-Martens Closed Tester......................................................... 06.03 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation.............06.01, 06.03 Specification for Degummed Soybean Oil....................................................................................................,.. 06.03 Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green.................................................................................................................................. 06.02 Method for Detection of Copper Corrosion from Petroleum Products by the Copper Strip Tarnish Test.................................... 06.03 Test Methods for Specific Gravity of Pigments...................................................................... 06.02 Guide for Testing Varnishes...:.................................................................................................... 06.01 Test Methods for Coarse Particles in Pigments, Pastes, and Paints............................................................... 06.01,06.02 Specification for Dry Bleached Lac....................................................................... 06.02 Specification for Lampblack Pigment......................................................... 06.02 Specification for Bone Black Pigment................................................................................................................ 06.02 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) ......................06.03 06.0 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 DUP0502 95649 IS P? D 237- 91 . D' 260 86(1990) I*r D .226612- 75(1987)" 81 (1987)" jl D 263 75(1987) D 267 82 (1987)" 268- 90 D 269 (1987)" frv'gD 279 87 (1991)" RDif 5D 228800-81(1987) H- m? j D 281 84(1989) Sy i D 283' 84(1990)" 6* 284- 88 D 301 89 t- 302- 85 AM D 303-85 304-90 305 - 84 (1990)1 319-90 |'D 329.-90, 330 - 89 331-90 332 - 87(1991)" 333 - 87 . i D. 344-89 KW* 0 358 - 83(1988) BWi D 360 - 89 D 362--84 IJk 363--90 D 365-- 84 (1989)" gg m 387--86 D 411--83(1987) ; D 444--88 ; 464--91 D 465--82(1987)" D 475--67(1989) D 476--84(1989) D 477--78 D 478--86(1991)" D 480--88 D 5,09 --70(1987) D 520--84(1989) D 521--90 522--88" 8 523--89 8 555-- 84(1988)" D 561 --82(1989) 8 562--81(1990)" 8 563--88 Si p SD 564--87(1991)" 6.00--90 to. Is is D 601 --87(1991)" D 602--81(1991)" D 603--66(1989) D 604--81(1989) 605--82(1989) 607--82(1987)" S||||||v D 608--90 BaB; D 609--90 yl _ 610-- 85 (1989)" D 611--82(1987)2 ki | I' It If 656--87 D 658--91 8 659--86" 8 660--87 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Specification for Orange Shellac and Other Lacs..........................................................................................06.02 Specification for Boiled Linseed Oil .................................. ............................... ............................... ...... 06.03 Specification for Iron Blue Pigment.......................... ...................................................................................06.02 Specification for Ultramarfme BlueT'fgstgi^,...............................................................................................06.02 Specification for Chrome Oxide Green Pigment ............... .......................................................................... 06.02 Specification for Gold Bronze Powder . ......................................... ....................................................... 06.02 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Materials --........ ............................................ .. -- ................................06.03 Test Method for Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark)........ 06.03 Test Methods for Bleeding of Pigments ........................................................................................................ 06.02 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments.............................................. ..........................................................................................................06.02 Test Method for Oil Adsorption of Pigments by Spatula Rub-Out ................................... ................... 06.02 Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments ....................................06.02 Test Methods for Chemical Analysis of Mercuric Oxide Pigment .................................................. 06.02 Test Methods for Soluble Cellulose Nitrate ..................................................................................................06.02 Specification for Ethyl Acetate (85 to 88 % Grade) (Discontinued 1987f--Replaced by Specification D4614).......................................... ........... .............. .......... .....................................:.................................... 06.03 Specification of n-Butyl Acetate (90 to 92 % Grade) (Discontinued 1987f--Repaced by Specification D4615).......................................................................................... .......................................................06.03 Specification for n-Butyl Alcohol (Butanol)....................... 06.03 Test Method for Solvent-Extractable Material in Black Pigments ............................................... 06.02 Specification for Amyl Alcohol (Synthetic) .................................... 06.03 Specification for Acetone: ........................................................ 06.03 Specification for 2-Butoxyethanol .............. 06.03 Specification for 2-Ethoxyethanol.....................................................................................................................06.03 Test Method for Relative Tinting Strength of White Pigments by Visual Observation............................. 06.02 Test Methods for dear 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...................--.........................:............................................................ 06.02 Specification for Industrial Grade. Toluene (See Section on Aromatic Hydrocarbons)..............................06.03 Specification for Tricresyl Phosphate ............................................... 06.03 Methods of Testing Soluble Nitrocellulose Base Solutions ................................................................... .. 06.02 Test Method for Color and Strength of Color Pigments with a Mechanical Muller ............................... 06.02 Methods of Testing Shellac Used for Electrical Insulation .........................................................................06.02 Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow) ....................... 06.02 Test Methods for Saponification Number of Naval Store Products Including Tall Oil and Other Related Products ...........................................................................................................................................................06.03 Test Methods for Arid Number of Rosin ........... ......................................................................................06.03 Specification for Pure Para Red Toner Pigmeats ....................................................................................... 06.02 Specification for Titanium Dioxide Pigments ............................... ..................................... ..................... 06.02 Specification for Zinc Sulfide Pigmentrs (Discontinued 1988f) ................................................................. 06.02 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 Rosin ..................... . . ..................................................... ............06.03 Specification for Zinc Dust Pigment ...............................................................................................................06.02 Methods for Chemical Analysis of Zinc Dust (metallic Zinc Powder).......................................................06.02 Test Methods for Mandrel Bend Test of Attached Organic Coatings........................................................ 06,01 Test Method for Specular Gloss ........................... ........................... ...........................................................06.01 Guide for Testing Drying Oils ................................................................................ ..................................... 06.03 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 Test Method for Liquid Paint Driers ............................................................................................................ 06.03 Specification for Liquid Paint Driers ........ .................... ............................................................................... 06.03 Specification for Oiticica Oil (Permanently Liquid) ......................................................................................06.03 Specification for Barium Sulfete Pigments.......................................................................................................06.02 Specification for Aluminum Silicate Pigments (Hydrous)........................................................................... 06.02 Specification for Diatomaceous Silica figment ............................................................................................ 06.02 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 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 .................................................................................................... .................................................... 06.03 Specification for Pure Toluidine Red Toner ................................................................................................ 06.02 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive .................................. 06.01 Method of Evaluating Degree of Chalking of Exterior Paints (Discontinued 1990f--Replaced by Test Methods D42I4).................................................................. ....................................................................... 06.01 Test Method for Evaluating Degree of Checking of Exterior Paints........................................................... 06.01 xi DUP0502 95650 D 661 - 86" D 662 -86" D 711-89 D 713-90 D 714-87 D 715 - 86 (1991 f' 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)" 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 (1986) 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)" D 1006-73(1986)" D1007 - 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 1135 - 86 (1991)" D 1150 - 55 (1987)" D 1152 - 89 D 1153 - 90 D 1155 - 89 D 1186 - 87 D 1193-91 D 1198 - 88 D1199 - 86 (1991)" D 1200 - 88 D 1208 - 84 (1989)" D 1209 - 84(1988)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Method for Evaluating Degree of Cracking of Exterior Paints ............................................................. 06.01 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 MarkingMaterials .......................................06.01 Test Method for Evaluating Degree of Blistering of Paints ............................................................................06.01 Test Methods for Analysis of Barium Sulfate Pigment................................................................. ................ 06.02 Test Methods for Evaluating Mica Pigment................. 06.02 Test Methods for Analysis of Magnesium Silicate Pigment.................................. 06.02 Test Methods for Analysis of Aluminum Silicate Pigment ........................................................... 06.02 Test Methods for Analysis of Diatomaceous Silica Pigment ......................................................................... 06.02 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 of Flaking (Scaling) of Exterior Paints................................................. 06.01' Specification for Orange Shellac and Other Indian Lacs for ElectricalInsulation....................................... 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 ....:......................................................................... 06.01 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels ............... ................................................................ ........................................................ .. 06.01 Test Methods for Sampling and Testing Pine Tars and Pine-Tar Oils (Intent to Withdraw)......................06.03 Specification for Pumice Pigment.............................................................................................................. :. 06.02 Test Method for Evaluating Degree of Bleeding of Traffic Paint......... 06.01 Test Method for Evaluating Degree of Settling of Paint.......................................................................... 06.01 Practice for Testing Water Resistance of Coatings Using Water Immersion................................................06.01 Methods of Testing Cellulose Acetate................................................................................................................ 06.02 Test Method for Volatile Oil in Rosin ...................................................................... 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............................................. 06.01 Test Methods for Ethylcellulose................................................................... .............................................06.02 Specification for Raw Castor Oil........................................... 06.03 Specification for Dehydrated Castor Oil.................................................................. 06.03 Specification for Aluminum Powder and Paste Pigments for Paints.................................................... 06.02 Specification for Copper Phthalocyanine Blue Pigment............................... 06.02 Specification for Copper Powder for Usein Antifouling Paints...................................................................... 06.02 Test Methods for Abrasion Resistance of Organic Coatings by FailingAbrasive.......................................... 06.01 Test Method for Laboratory Determination of Degree of Bleeding of Traffic Paint...................................06.01 Test Methods for Para Red and Toluidine Red Pigments .. ............................... 06.02 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers..........06.01 Practice for Conducting Exterior Exposure Tests of Paints on Wood .......................................................... 06.01 Specification for sec-Butyl Alcohol............................................................................................................. 06.03 Test Method for Determining Total Nitrogen in Resins and Plastics .:............................................... 06.02 Test Method for Conducting Exterior Exposure Tests of Paints on Steel ........................................... 06.01 Test Method for Ash in Rosin.............................................................................................................................06.03 Test Method for Iron in Rosin......... ........................................................................................................ 06.03 Test Methods for Unsaponifiable Matter in Rosin ..:..................................................................................... 06.03 Test Method for Distillation Range of Volatile Organic Liquids.......................... 06.03 Methods of Testing Rosin Oils.............................................................................................................................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 Testsof Paints...................................... 06.01 Specification for Methanol (Methyl Alcohol)................................................................................................... 06.03 Specification for Methyl Isobutyl Ketone........... ..............................................................................................06.03 Test Method for Roundness of Glass Spheres..................................................................... 06.02 Test Methods for Nondestructive Measurement of Dry Fjlm Thickness of Nonmagnetic Coatings Applied to a Ferrous Base ........................................................................................................................... 06.01 Specification for Reagent Water ...................................................... 06.03 Test Method for Solvent Tolerance of Amine Resins............................ 06.02 Specification for Calcium Carbonate Pigments............. ........... 06.02 Test Method for Viscosity by Ford Viscosity Cup................... 06.01 Test Methods for Common Properties of Certain Pigments.......................................................................... 06.02 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)................... 06.01,06.03 xii DUP050295651 1210 - 79 (1988)" 1211-87 1212-91 ,1214-89 ,1240 - 82 1257-90 1258-90 1259-85 (1990)" 1296 - 84(1988)" 1301-91 1306-88 1308- 87 1309- 88 1310- 86(1990)" 1312 - 56 (1987)*1 < 1316 - 87 1343- 91 1347 - 72(1989)" D1348 - 89 D 1353 - 90 01358- 86 ,;D 1360 90a D1363 - 88 D 1364 - 90 rD 1366 - 86 (1991)" SO 1392 - 87 |D 1394- 76(1991 )" 01395- 58(1974) D1396 - 73(1987)" "D 1397 - 88 01398- 84 D 1399 90 D1400 - 87 D 1439 83a (1989)" D 1462 -87 D 1466 -86 D1467 - 89 D 1468 -84(1988)" D1469-73 (1988)" D 1474- 85 (1991)" D 1475-90 D 1476 - 88 D1483 - 84 (1989)" 0 1537 - 60 (1988)" 0 1538 - 60(1988)" D1539-60 (1988) D1540 - 82 (1987)" D 1541 -86 D 1542 - 60 (1988)" D1543 - 86 D 1544 - 80 (1989)" D 1545-89 D 1546 - 62 (1987) D1585 - 82 D1612 - 90 D J613-91 D 1614-91 D 1615-60 (1987) 01617-90 D 1638 - 74" D 1639-90 D 1640 - 83(1989)" D 1641 -59 (1987) D 1642-70(1987) CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Method for Fineness of Dispersion of Pigment-Vehicle 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............................. v......................................................... 06.02 Test Method for Rosin Acids in Fatty Acids ............................... .. , -k'.......................................................06.03 Specification for High-Gravity Glycerin ................... ....................... H,..................................................... 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 Resins and Esters Containing Other Dibasic. Acids (Gravimetric)................................................................ 06.02 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes.................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 of Clear Floor Coatings (Discontinued 1989t)............................. 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 Acid Content of Alkyd Resins and Alkyd Resin Solutions....................................06.02 Test Method for Unsaponifiable Content of Tricresyl Phosphate ............................................ 06.03 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive 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 Tricresyl Phosphate.................. 06.03 Test Method for Total Rosin Adds 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 Misdbility of Lacquer Solvents..............................................................................06.03 Test Method for Oil Absorption of Pigments by Gardner-Coleman Method.............................................. 06.02 Spedfication for Distilled Soybean Fatty Adds .............................................................................................. 06.03 Specification for Distilled Linseed Fatty Acids........................... 06.03 Spedfication for Dehydrated Castor Adds..................................................... 06.03 Practice for Effect of Chemical Agents on Organic Finishes Used in the Transportation Industry.........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 (Discontinued 1992f) ................. 06.01 Test Method for Color of Transparent Liquids (Gardner Color Scale)................................06.01, 06.02, 06.03 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 Acidity 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 Pentaferythritol in 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 Acid Value of Organic Coating Materials ....................................................................... 06.01 Test Methods for Drying, Curing or Film Formation of Organic Coatings at Room Temperature .... 06.01 Test Method for Exterior Durability of Varnishes................... .....................................................................06.01 Test Methods for Elastidty or Toughness of Varnishes ......................................................................... .... 06.01 xiu DUP050295652 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)1 D 1650 - 91 D 1652-90 D 1653-91a D 1654-79a (1984)1 D 1695 - 77 (1989)1 D 1696-90 D 1716 - 62(1987) D 1718-86 D 1719-90 D 1720-88 D 1721 - 84 (1988)I D 1722-90 D 1725-62(1989)fl D 1726 - 90 D 1728-83 D 1730 - 67 (1984)l D 1731 - 67 (1984)| D 1732-67(1984) D 1734-63 (1980)ei D 1735 -87 D 1736 - 89 D 1737 - 85 D 1787 - 89 D 1794-89 D1795 - 90 D 1836-91 D'1841 -63(1988)t D 1842 -63 (1988) D 1843-63 (1988)1 D 1844 - 86 (1991)I D 1845- 86 (1991)1 D 1847-87 D 1848-88 D 1849 - 80 (1987)1 D 1915- 63 (1989)I D1926 - 89 D 1950 - 86 D 1951 -86 D 1952 - 86 D 1954 - 86 D 1955 - 85 (1989)t D 1957 - 86 D 1958-86(1990) D 1959 - 85 (1989)I D 1960-86(1990) 0 1962 - 85 (1989)l 01963-.85 (1989)1 0 1964 - 85 (1989)I D 1965 - 87 (1991)l D 1966 - 69 (l-991)l 0 1967 - 86 0 1969 - 91 D 1978 - 91 0^1979-91 D 1980-87 (I991)1 04981 -86(1990) 04982-85 (1989)1 031983 - 90 04984 - 69(1988) O30S4-91 D2065-91 D/2066 - 91 D2071 -87 (199I)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. 3......................... ................................................................................06.03 Test Method for Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions............................. 06.03 Test Method for Permanganate Time bf Tricresyl Phosphate ........................................................ 06.03 Test Method for Water Miscibility of Water-Soluble Solvents ..................................................................... 06.03 Test Method forViscosity 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 of High-Gravity Glycerin (Discontinued 19911). 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 tor Alcohol-Benzene Soluble Matter id Cellulose (Intent to Withdraw!) ............................ 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 Acids........ ......................................................................................06.03 Specification for Fractionated and Distilled Cottonseed Fatty Acids .........................................................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 Reans . -- ................. ........................................ 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 ........................... ...........:........................................... 06B2 Test Method for Acetone Tolerance of Heat-Bodied Drying Oils ........................................................ 06.03 Test Method for Ash in Drying Oils and Fatty Adds ................................................................................... 06.03 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........... ........................................ 06.03 Test Method for Hydroxyl Value of Fatty Oils and Acids ................. 06.03 Test Method for Chloroform Insoluble Matter in Oiticica Oil ............................................. 06.03 Test Method for Iodine Value of Drying Oils and Fatty Adds ................................................ ................ 06.03 Test Method for Loss on Heating of Drying Oils .................................................. 3.............. .................... 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/ 25C .............. 06.03 Test Method for Tung Oil Quality .................................................................................................................06.03 Test Method fdr Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Acids ... 06.03 Test Method for Foots ib Raw Linseed Oil (Gravimetric Method) ...........................................................06.03 Test Method for Measuring Color After Heating of Drying Oils ...............................................................06.03 Spedfication for 2-Ethylhetanol (Synthetic).................................................................................................... 06.03 Guide for Analysis of Electrocoat Bath Samples .......................................................................................... 06.01 Test Method for Free Formaldehyde Content of Amino Resins ................................................................. 06.02 Test Method for Add Value of Fatty Acids and Polymerized Fatty Acids .................................................06.03 Test Method for Measuring Color After Heating of Fatty Acids ................ 06.03 Test Method for Titer of Fatty Adds ....................................................................... 06.03 Test Method for Fatty Add Composition by Gas-Liquid Chromatograph of Methyl Esters ................... 06.03 Specification for Tall Oil Fatty Acids...............................................................................................................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 l f DU P050295653 D 2072 - 66 (1987)" |[ D2073 - 66 (1987)*1 ! D 2074-66 (1987)" b ;D2075 89 ' , D2076 64 (1987)" ' D 2077 64(1987) D2078 86(1990) D 2079 82 (1987) D 2080 64(1987) D2081 64(1987) D2082 82(1987) D 2083 66 (1987) I .D 2086 - 89 D2087--89 D2090--88 D209I --88 |D2092--86 D2I34--66(1980)" D2190--89 D2191--89 D2192--89 D2193--89 D2194--89 1|D2195 --89 |p 2196--86(1991)" D2197 -86(1991)" -mm -84(1989)" D2199 -82(1987) ,02200 -91 J1D2201 -65(1987)" D-2205 -85(1990)" :.D2218 -67(1989)" ,':D2243 -90 'D2244 -89 : 02245 -90 D 2246 -87 02247. -87 D2248 -89 D 2336 -87(1991)" D 2337 -84(1989) D 2338 -84(1989)" D 2348 -91 D 2349 -90 D2350 - 90 02351 -90 : D 2352 - -85(1990)" ' 0 2353 -83 sD 2354 - 91 D2363 - 79(1989)" |!'D 2364 - 89 1*0 2366 - 68(1980)" ;D 2369 -90 0 2370 - 82(1987)" 0 2371 -85(1990)" D 2372-85 (1990)" 0 2373 - 85(1990)" D 2374-85 (1990)" D2375 - 85 (1990)" D 2376-84 (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 Potentiometfic 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 AmmoniumChlorides.... 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 1990t) ...... 06.01 Specification for Vinyl Acetate....................... ....................................................... ....................................... 06.03 Test Method for Acetaldehyde Content of Vinyl Acetate ........................................................................... 06.03 Test Method for Purity of Aldehydes and Ketones...........................: ........................................................06.03 Test Method for Hydroquinone in Vinyl Acetate.......................................................................................... 06.03 Test Method for Concentration of Formaldehyde Solutions............................... ....................................... 06.03 Test Methods for Pentaerythritol.......................................................................................................................06.03 Test Methods for Rheological Properties of Non-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 ofTests for Traffic Paints ................ ......................................................................... 06.01 Specification for Molybdate Orange Pigments............... ........................................................................... 06.02 Test Method for Freeze-Thaw Resistanceof Water-Borne Coatings.............................................................. 06.01 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates.. 06.01 Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints..................................06.03 Test Method for Finishes on Primed Metallic Substrates for Humidity-Thermal 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............................................................................... 06.01 Test Method of Qualitative Determination of Nature of Thinner in Solvent-Reducible Paints.............06.01 Test Method for Antimony Oxide in White Pigment Separated from Solvent-Reducible Paints...........06.02 Test Method for Sulfide in White Pigment Separated from Solvent-Reducible Paints................................06.02 Test Method for Sulfur Dioxide in White Pigment Separated from Solvent-Reducible Paints................. 06.02 Test Method for Flow Ratings of Organic Coatings Using the Shell Flow Comparator (Discontinued 1992t) . :.................................................... ................................................................................................. : 06.01 Test Method for Minimum 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......................................................................... ................. 06.01 Test Method for Tensile Properties of Organic Coatings............................................................................. 06.01 Test Method for Pigment Content of Solvent-Reducible Paints................................................................. 06.01 Practice of Separation of Vehicle from Solvent-Reducible Paints...............................................................06.01 Test Method for Determination of Cobalt in Paint Driers by EDTA Method......... ..............................06.03 Test Method for Lead in Paint Driers by EDTA Method r................................................................ .. 06.03 Test Method for Manganese in Paint Driers by EDTA Method........ .....................................................06.03 Test Method for Slump of Face Glazing and Bedding Compounds on Metal Sash..................................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............................................................... .............................................. 06.02 xv DUP050295654 CONTENTS, VOLUMES 06.01, 06.02; AND 06.03 D 2448 - 85 (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 D2689 - 88 D 2690-89 D 2691 - 88 D 2693 - 87 D 2694 - 87 D 2695 - 87 D 2696 - 87 D2697 - 86 D 2698 - 90 . D 2742 - 79 02743 - 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 0 2805 - 88 D 2830 - 91 *t D 2832-83 (1991)" D 2833 - 89 D 2916 - 88 D 2917 -91 D 2921 - 88 D 2929 - 89 D 2931 - 84(1989)" D 2932-80 (1988)" D 2933 - 74 (1986)" D 2998 - 89 D 2999 - 85 D 3002 - 81 (1987) D 3003 -.71 (1987) D 3008 - 90 D 3009 - 72 (1981)" D 3021 - 82 (1987)" 03022-84(1989)" D 3023 - 88 D 3125 - 83 (1987) D3126-83 Test Method for Water-Soluble Salta 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 of Carboxylic Acids in Alkyd Resins....................................... 06.02 Test Method for Identification of Polyhydric 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 Acids ................ 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-Reducible Paints ........................06.01, Specification for Diacetone Alcohol ................................................................. Specification for Methyl Amyl Acetate (95 % Grade) ....................... 06.03 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 Add in Alkyd and Polyester Resins ....................................... 06.02 Test Methods for Microscopical Measurement of Dry.Film Thickness of Coatings on Wood Products . 06.01 Specification for Ethylene Glycol ............................................... '................................................................. 06,03 Specification for Diethylene Glycol ........................... 06.03 Specification for Propylene Glycol (Discontinued 1992f) ......:.................. 06.03 Specification 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 byHigh-Speed Centrifuging ..................................................................................................................................................06.01 Methods for Chemical Analysis of Tribasic Lead Phosphosilicate (Discontinued 1990t) ................... 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 r.............................................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 Acid Composition . by Gas Chromatography ........ -....... .............................. .................................................. .. 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 .......................... 06.01 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 ............................... :..:.................................... ................................... 06.03 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 Cellulosic Materials by.X-ray Fluorescence ................................ 06.02 Guide for Testing Latex Flat Wall Paints ................. ............. -................ ....................... ,..........06.01 Guide fori Testing Exterior Solvent-Reducible House and Trim Coatings ..:................................................06,01 Test Method for Corrosion Resistance ofCoated Steel Specimens (Cyclic Method) (Discontinued 1992f) .........:.......................... ............................................... .............. ........................................... 06.01 Test Method for Polyhydric Alcohols In Alkyd Resins ...................................... 06.02 Test Method for Monopentaerythritol in Commercial Pentaerythritol (Discontinued1989f--Replaced* by Test MethodD 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 . 06X11 Test Method for Resin Adds 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 Add ............ .............. .......................... ............... .......... ..................... .................. :.................. 06.03 Specification for n-Butyl Acetate (98% Grade) (Discontinued 1987f--Replaced by Specification D4615)...................................................... ...................................... .................................................... 6.03 1 XVI DUP050295655 * CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 83 -89 -91 - 86 " - 88 -84(1990)*' -72 (1989)*' - 83 (1990)*' - 89 -87 (1991)*1 -86(1991)*' -88 -80,(1987)*' - 84(1990)*' -82(1991) -87 -76 (1988)*' -86(1991)*' 24-82(1988)*' 86 8 -- 89 |Q- 85 (1990)*' 1 -84(1989) 2-82 (1991) 383-80(1988)*' 3-89 ^5-85a*' (1991)*' 18-88 59-90 ' jg3fi0 - 80 (1989) / 336 k-87. g i. 62-84(1987) ,3-74(1989)*' 3383 - 79a (1988)*' 414-75 15-80(1988)*' -2-89 W. 450-90 ,1 -76(1987)*' : 56-86(1991)*' $7-87(1991)*' 34)9-87 16-89 "9-87 40-86 "41-91 2-90 46 - 90 "7-91 48-86 )8-85a (1991)*' 19-77(1989) ,20 - 90 21 - 84 i -- 90 , 623-78a (1987) 3624-85a (1991)*' Specification for n-Ethyl Acetate (99% Grade) (Discontinued 1987f--Replaced by Specification D4614) ....................... .................. ......................... ............................ .......... ..............,.................... 06.03 Specification for 2-Methoxyethanol \ ..................... : ................... ............ ......................................06.03 Guide for Testing Exterior Latex House Paints............. .........................................................................06.01 Specification for n-PropyLAcetate (96 % Grade) ............................... .............................................. .. 06.03 Speciflcatiofi'fbr Isopropyl Acetate (99 % Grade)......................................................................................... 06.03 Test Method for the Solubility Range ofResins and Polymers ............... -J.'.............................................. 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 andKJreen Pigments................................. 06.02 Test Method for Aromatics in Mineral Spirits by Gas Chromatography............................. .. 06.03 Test Method for Porosity of Paint Films..................................................j .;.......................................... 06.01 Practice for Infrared Determination of the Temperature of Applied Coatings on Wood Products During 1 ; the Curing Cycle........................................................................................................................................... 06.01 Test Method for Acid and Mortar Resistance ofFactory-Applied Clear Coatings on Extruded Aluminuni Products_____............................................................-............ ................................................v... 06.01 Practice for Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph for Solvent Analysis'....... . . l ................. ....................;.... . ........... i....... ......................... ------ .06.01 Practice for Vacuum Distillation of Solvents from Solvent-Reducible Paints for Analysis----- ........ 06.01 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 and Dirt Accumulation ....................... ..... ....................................... 06101 Guide for Painting Inspectors'(Metal Substrates)............................... .. v.v...................................... 06.01 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus..........................................06.03 Test Methods for Analysis of White Zinc Pigments :......................... .'.......................................... 06.02 Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus...... 06.01 Practice for Testing Primers and Primer Surfaced Over Preformed Metal ................................... 06.01 Guide for Testing Interior Solvent-Reducible. Flat Wall Paints ............................... .. 06.01 Test Method for Purity of Methyl'Isobutyl Ketone by Gas Chromatography .........................................06.03 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy ........................................ ................ .. ----- '................. ........................................................06.01 Guide for Testing Water-Borne Floor Paints ...;...... ............ .........'....!......... .. 1 06.01 Test Methods for Measuring Adhesion by Tape Test........i............... ........ ........................................ 06.01 Test Method for Particle Size Distribution By Hydrometer of the Common White Extender Pig ments v___ ...................... .................... ..........."........ .................... 1 -.;.......................... - 06.02 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Are < Type) for Testihg Paint, Varnish, Lacquer, and Related Products'Using the Dew Cycle.............. 06.01 Test Method for Purity of Acrylate Esters by Gas Chromatography................ ......................................... 06.03 Test Method for Film Hardness by Pencil Test ................... .................... 06.01 Guide.for Testing Solvent-Reducible Floor Paints...................;..;.......................................... 06.01 Method of Evaluating the Lightfastness of Printed Matter---- ........ .......................................................06.01 Guide for Testing Solvent-Reducible Iriterior Semigloss-Wall and Trim Enamels.................................... 06.01 Test Method for Unreacted Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography :,.: ...................................... .:t .a.:........ ....................................06.02 Test Method for Washability Properties bf Interior Architectural Coatings'...... ......................... :v... 06.01 Practices for Testing Polymeric Powders and Powder Coatings...... ........ ......................................... ;-------06.01 Practice for Determining by Exterior Exposure Tests the Susceptibility ofPaint Films to Microbiological ' Attack --------- .............. ................................... ........ ............................ ..........................................:..: 06.01 Test Method for- Preparation of Methyl Esters from Fatty Acids-for Determination of Fatty Acid- -- ) Composition by Gas-Liquid Chromatography .... ...... ......................... .................-........... ..: 06.03 Test Method for Humid-Dry Cycling for Coatings on Wood and Wood Products.......... ........... 06.01 Test Method for Ashing. Cellulose ^............. ...................................................................06.02 Test Methods for Evaporation Rates of Volatile Liquids by Shell Thin-Film Evaporometer................. 06.01 Specification for Primary Amyl Acetate, Synthetic (98 % Grade) ................... .. 06.03 Specification for 2-Ethylhexyl Acrylate .................... ................ .r,;.......... ................ .........'.... 06.03 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography ...........:.... 06.03 Test Method for Formic Acid in Glacial Acetic Acid......... ........ ...................................... i... 06.03 Specification for n-Butyl Acrylate ........... .<........... .................. .................. .............................................06.03 Specification for Ethyl Acrylate.............'....................................................................................................... 06.03 Test Method for Detection of Lead in Paint and Dried Paint Films... . .............................................. .... 06.01 Specification for Aluminum Silicate Pigments (Anhydrous) ................................ ....................................06.02 Specification for Glacial Acetic Add....................................................................................... ^................. 06.03 Practice for Determination of Water in Acetate Esters (Discontinued 1988t--Replaced by Test Method D 1364) ........................................................................................ ............................................................ 06.03 Specification for n-Propyl Alcohol (1-Propanol).......................................... .............................................. 06.03 Method for Testing Antifouling Panels in Shallow Submergence............................................ ............ s 06.01 Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy ........ 06.01 xvii DUP050295656 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 3630 - 89 D 3680 - 89 D 37X7 - 85a (1991)" D 3718 - 85a (1991)" D 3719 - 87 D 3720 - 90 D 3721 - 83 (1991)" D 3722 - 82 (1991)" D 3723 - 84 (1990)" D 3724 - 82 (1987)" D 3725 - 78 (1988)" D 3726 -84 D 3727 - 84 D 3728 - 88 D 3729 - 84 D 3730 - 78 (1988)" D 3732 - 82 (1989)" D 3733-78 (1984)" D 3734 - 91 D 3735 - 87 D 3792-91 D 3793 - 89 D 3794 - 79" D 3804 - 86 (1991)" D 3806-90a D 3842 - 86 (1991) D 3843 - 89 D 3845 - 89 D 3872 - 86 (1991)" D 3876 - 79 (1989)" D 3891 - 90 D 3893 - 90 D 3911 - 89 D 3912 - 80 (1989) D 3924 - 80 (1991)" D 3925 - 91 D3926- 80 (1991)" D 3927 - 87 D 3928 - 89 D 3.934 - 90 D 3941 - 90 D 3960 - 91 D 3964 - 80 (1989) D 3969 - 85 (1990)" P 3970 - 80 (1990)" P 3971 - 89 D 3980 - 88 D3988-85(1990)" D 3989 - 81a (1990)" D 4017 - 90 D 4039 - 87 D 4040 - 91 D 4060 - 90 D 4062 - 88 D 4082 - 89 D 4085 - 81 (1987) D 4121 - 82 (1987) D 4138 - 88 D4139 - 82 (1991)" Guide for Determining Constituents Classified as Hazardous Contained in Protective Coatings............06.01 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 ofAntimony in Paint by Atomic Absorption Spectroscopy------ 06.01 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..................................................... 06.01 Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments byX-Ray Diffraction-------06.02 Specification for Synthetic Red Iron Oxide Pigment ........... 06.02 Specification for Natural Red and Brown Iron Oxide Pigments .................................................................. 06.02 Test Method for Pigment Content ofWater-Emulsion Paints by Low-Temperature Ashing..................... 06.01 Specification for Synthetic Brown Iron Oxide Pigment... ........... 06.02 Test Method for Semiquantitative Determination of Fish Oil in Drying Oils and Drying Oil Fatty Acids by Gas-Liquid Chromatography.......................... 06.03 Specification for n-Butyl Acetate (99.5 % Grade) (Discontinued 1987t--Replaced by Specification D4615)............................................................................................. 06.03 Specification fob Ethyl Acetate (99.5% Grade) (Discontinued 1987f--Replaced by Specification D4614)........................................................................................... 06.03 Specification for 2-Ethoxyethyl Acetate (99 % Grade).................................................................................... 06.03 Specification for Methyl Ethyl Ketone (99.5 % Grade) (Discontinued 1989t--Replaced by Specification D 740)......................... 06.03 Guide for Testing High-Performance Interior Architectural Wall Coatings ............................................... 06.01 Practice for Reporting Cure Times of Ultraviolet-Cured Coatings................... 06.01 Test Method for Silicon Content of Silicone Polymers and Silicone-Modified Alkyds byAtomic Absorption...................................................................................................................................................... 06.02 Specification for High-Flash Aromatic Naphthas.............................. 06.03 Specification for VM&P Naphthas........... .......................................................................................................06.03 Test Method for Water Content of Water-Reducible Paints by Direct Injection Into a Gas Chromatograph --........................................ 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 Nuclear Power Plants ........... 06.01 Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities....................... 06.01 Specification for Glacial Methacrylic Acid............................................................................................. 06.03 Test Method for Ferrous Iron in Iron Oxides........................................ 06.02 Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography................. 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 Light-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.............. 06.01 Specification 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 ofGloss 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........................... 06.03 Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings. 06.01 Practice for Selection of Coating Specimens for Appearance Measurements.......................... 06.01 Test Method for Zirconium in Paint Driers by EDTA Method.....................................................................06.03 Test Method for Cerium in Paint Driers by Gxidimetric 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.................. 06.03 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 DUP050295657 >8 i. ifr* '^PD4140 -82 (1991)" fflk i 4141 -82 (1987)" >4142 -89 1*4143 -89 >4144 -82 (1987) 14145 -83 (1990)" >4146 -83 (1989)" >4147 -82 (1987) >4206 -89 >4207 -91 IB4209 -82 (1991)" -88 -87 -89 -83 (1989) (1989) -91 -89 -87 |i>4258 -83 (1988) >4259 -88 I>4260 -88 >4261 83 (1988) 13p 4262 - 83 (1988) IP 4263 83(1988)" 104277 -83(1988)" |4285 83(1988) |D 4286 90 : D 4287-88 JD4288-83(1989)" 10 4301 -84(1989)" D 4302 - 90 D 4303 - 91 D4358 - 84 (1990)" 0 4359 90 04360 90 D4361- 89 D 4366 - 91 D 4367 89 04368- 89 04370- 84(1990)" 0 4399- 90 D4400- 89a D4414- 84(1990)" D4415- 91 D4416- 89 D4417- 84 D 4449 - 90 D 4450 - 85(1990)" D4451 - 85(1991)" D4457- 85(1991)" 0 4462 - 85(1989) 0 4487 - 90 D4518-91 D 4537-91 D4538- 90a D4540 - 91 D 4541 -85(1989)" D4563 - 86 (1991)" 04584 - 86(1990" 1 00 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Guide for Determining Volatile and Nonvolatile 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 Zinc-Rich Primer/Chromate 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 u:............ ......................................... ................. ;...................... ............ 06.02 Test Method for Viscosity by Dip-Type Viscosity Cups...:....................................................................... >06.01 Test Method for Wqt Abrasion Resistance oflnterior Paints .....;........ ......................................... 06.01 Test Methods for Evaluating Degree of Chalking of Exterior Paint Films................................................ 06.01. Practice for Qualification ofJourneyman 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 1990f) ............. ...... ...................'............................................ 06.01 Practice for Surface Cleaning Concrete for Coating ......................................................................................06.01 Practice for Abrading Concrete ;:...................-- .............. .............. ................................................. 06.01 Practice for Acid 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 ICI Cone/Plate Viscometer..........................................06.01 Specification for Calcium Borosilicate Pigments......................... .................................................................. 06.02 Test Method for Total Chlorine in Epoxy Resins and Compounds...........................................................06.02 Specification for Artiste' 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 of Lead Chromate Type Pigment Dusts by Atomic Absorption Spectroscopy ................... ........................... ..........................................O6;02 Test Method for Determining Whether a Material is a Liquid or a Solid.................................................. 06.01 Specification for Methyl fl-Amyl 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.......................................... 06.03 Guide for Testing PolyfVinyl Chloride) Resins............................. .................. ....'.................................... 06.02 Test Methods for Acid and Base Milliequivalent Content of Electfocoat Bath............................... ...... 06.01 Test Method for Measuring Electrical Conductivity of Electrocoat Baths. ........................................... 06.01 Test Method for Sag Resistance of Paints Using a Multinoteh Applicator ...................................... .. 06.01 Practice for Measurement of Wet Film Thickness by Notch Gages.......................................................... > 06.01 Test Method for .Determination of Dimer in Acrylic Add................... .................................................. 06.03 Specification for Acrylic Acid ......................................................................................................................: 06.03 Test Methods for Field 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.............06.01 Guide for Testing Interior Latex Semigloss and Gloss Paints .1.................................................................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 xix DUP050295658 D 4585 - 87ei D 4587-91 D 4610 - 86 D 4613 - 86 (1990)el D 4614 - 86 D4615-86*1 D 4618 - 87 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Practice for Testing Water Resistance of Coatings Using Controlled Condensation..................................($.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 Algal) Growth on Paint and f Test Method for Measuring Apparent pH of Water Insoluble Phenol-FormaldehydeResins..................... 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 D 4640 - 86 (1990)el D 4706 - 87 D 4707 - 87 D 4708 - 91 D 4709 - 87 D 4710 - 87 D4712-87a (1991) D 4713 - 87el D 4747 - 87 D 4752 - 87 D 4758 - 87 D 4764 - 88 D 4773 - 89 D 4787 - 88 D 4794 - 88 D 4795 - 88 D 4796 - 88 D4797 - 88 D 4827 - 88 D 4828 - 91 D 4834 - 88 D.4835 - 89 D 4836-90 D 4837 - 89 D 4838 - 88 D 4938 - 89 D 4939 - 89 D 4940 - 89 D 4941 - 89 D 4942 - 89 D 4946 - 89el D 4948 - 89 D4958-91 D 4960 - 89 D 5007 - 89 D 5008-89 D 5009 - 89 D 5010 - 91 D 5031 - 89 D 5043 - 90 D 5062 - 90{l D 5063 - 90 D 5064 - 90 D 5065 - 90 D 5066 - 91 D 5067 - 9061 D 5068 - 90 D 5069 - 90 Test Method for Determining Stroke Cure Time of Thermosetting Phenol-Formaldehyde Resins..... 06.02 Test Method for Determining Qualitatively Methylol Group in Phenolic Resins....................................... 06.02 Test Method for Measuring Paint Spatter Resistance to Roller Application........................................... 06.01 Practice for Preparation of Uniform Free Films of Organic Coatings............................................................ 06.01 Specification for Methyl Acrylate........................ 06.03 Specification for Acetaldehyde............................................................................................................................ 06.03 Guide for Testing Industrie Water-Reducible Coatings................................................................................... 06.01 Test Methods for Nonvolatile Content of Printing Inks, Resin Solutions, and Vehicles.............................06.01 Test Method for Determining Unreacted Monomer Content of Latexes Using Gas Chromatography .. 06.02 Test Method for Measuring MEK Resistance of Ethyl Silicate (Inorganic) Zinc-Rich Primers by Solvent Rub.................................................................................................................................................................06.01 Test Method for Nonvolatile Content of Latexes...................................................................................-- 06.02 Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint ....................................................................................................... .......................................... .. -. 06.01 Test Method for Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene 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 of Latexes Using Capillary Column Gas Chromatography................................. ................ .............................................................................. -- 06.02 Test Method for Practical Washability of Organic Coatings........................... 06.01 Test Method for Detection of Lead in Paint by Direct Aspiration Atomic Absorption Spectroscopy... 06.01 Specification for Propylene Glycol Monomethyl Ether Acetate .................................................................... 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 ...........................................................................................................................................................06.01 Test Method for Conductimetric Analysis of Water Soluble Ionic Contamination ofBlasting 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.................................. 06.01 Test Method for Determination of the Upper Layer Separated from a Viscous Liquid .............................06.01 Test Method for Comparision-of the Brush Drag of Latex Paints ................................................................ 06.01 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 .................................................................................................................... 06.03 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...........................................................................................................06.01 Test Methods for Field Identification of Coatings ........................................................................................... 06.01 Test Method for Resin Solution Dilutability..................................................................................................... 06.01 Guide for Use of Certification of Coating Conformance Form............................ 06.01 Practice for Conducting a Patch Test to Assess Coating Compatibility..........................................................06.01 Guide for Assessing the Condition of Aged Coatings on Steel Surfaces........................................................06.01 Test Method for Determination of the Transfer Efficiency Under Production Conditions for Spray Application of Automotive Paints--Weight Basis............................................. 06.01 Specification for Artists' Watercolor Paints........................................................................................................06.01 Practice for Preparation of Paint Brushes for Evaluation.................................................................................06.01 Practice for Preparation of Paint Roller Covers for Evaluation...................................................................... 06.01 xx DUP050295659 ifWa: i<#5087 - 91 I# 05095-90 ?-90 S -- 90 5107-90 65108-90 JJ|p5125-91 165137-90 >5139-90 65144-91 55145-90 `5146-90 5150-91 5161-91 5162-91 MKD5163-91 f 65164 -91 65166 - 91 D 5178-91 ' ID 5179 -91 tr $ D 5181 -'91 05200-91 65201 -91 E 28-67 (1982)61 " E 97-82(1987) E 259 91 6 430- 91 E 852- 82 (1987)cl O 6- 88 G 8- 90 G 9- 87 G 10- 83(1988) G 11 - 88 G 12 83 (1988) G 13- 89 G 14- 88 G 17- 88 G 18- 88 G 19- 88 G 20- 88 G 23- 90 G 26-90 -t-fii G 42-90 h G 53-88 D 362 - 84 D 835 - 90 D 836 - 84 D 841-90 D 843-90 D 846-84 D 847-91 D 848-81(1989)" D 849-88 D 850-91 c o n t e n t s ; v o l u me s o s .o i, 06.02, a n d 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 13aihts.......................................................................................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 Electrocoat Baths.................................................. 06.01 Guide to Testing Solvent-Borne Architectural Coatings..................... ........... ....................................06.01 Test Method for 'Hiding Power of Architectural Paints Applied by Roller................................................ 06.01. Guide for Specifying Inspection Requirements for Coating and Lining Work (Metal Substrates)____ _ 06.01 Practice for Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates..................... ....................................................... .........:............................................................ 06.01 Guide for Establishing Procedures to Monitor the Performance of Safety Related Coatings1 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) of Solvent Reducible Paints in Aerosol Cans. ................................................................................... ............... ................................06.01 Practice for Calculating Formulation Physical Constants of Paints and Coatings....................................06.01 Test Method for Softening Point by Ring-ahd-Ball Apparatus ................................................................... 06.03 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry ;.................................................................................................................... 06.01 Practice for Preparation of Reference White Reflectance Standards .........................................................06.01 Method for Measurement of Gloss of High-Gloss Surfaces by Goniophotometry ..................................06.01 Test Methods for C4-C]3 Plasticizer Grade Alcohols................... .........................................................06.03 Test Method for Abrasion Resistance of Pipeline Coatings ....................................................................... 06.01 Test Methods for Cathodic Disbonding of Pipeline Coatings........ ............................................................ 06.01 Test Method for Water Penetration Into Pipeline Coatings......................................................................... 06.01 Test Method for Specific Bendability of Pipeline Coatings........................................................................... 06.01 Test Method for Effects of Outdoor Weathering on Pipeline Coatings...................................................... 06.01 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel.......... 06.01 Test Method for Impact Resistance of Pipeline Coatings (Limestone Drop Test)....................... .......... . 06.01 Test Method for Impact Resistance of Pipeline Coatings (Falling Weight Test)'....................................... 06.01 Test Method for Penetration Resistance of Pipeline Coatings (Blunt Rod) ...............................................06.01 Test Method for Joints, Fittings, and Patches in Coated Pipelines.................................................... .. . 06.01 Test Method for Disbonding Characteristics of Pipeline Coatings by Direct Soil Burial......................... 06.01 Test Method for Chemical Resistance of Pipeline Coatings................. ..................................................... .. 06.01 Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials............... ............................... ......................................... .............06.01 Practice for Operating Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials .............................................................................................................06.01 Method for Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures................. 06.01 Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetallic Materials ...................................................................................................... .. 06.01 AROMATIC HYDROCARBONS AND RELATED CHEMICALS (see gray-edged pages 539 to 817 of Volume 06.03) Specification for Industrial Grade Toluene (Discontinued 1991) ............................................................... 06.03 Specification for Refined Benzene-485 .,............ ...................... ............................................................... 06.03 Specification for Industrial Grade Benzene (Discontinued 1991)....................... .................................... 06.03 Specification for Nitration Grade Toluene......................... ...........................................................................06.03 Specification for Nitration Grade Xylene ............................. T................................................................... 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 ................................................. 06.03 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons ........................... ...................06.03 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials .......... :... 06.03 xxi DUP050295660 D 852 -87 (1991) D 853-91 D 1015-84 D 1016-84 D 1492-91 D 1493 - 90 D 1555-91 D 1631 - 85 (1989)*' D 1685 - 86 (1990) D 1686 - 81 (1990) D 2030 - 84 (1989)** D2031 -84(1989)*' D`2119-87 02120-87 02121-90 D 2232-81 (1986)** D 2306-81 (1985) D2323!- 84(1989)*' D 2324 - 81 (1989)*' D 2340-82(1987)*1 02359-90 0 2360 - 82 (1987)*1 0 2403 - 91 is; 0 2439 - 91 Hi 02747-81 02748-82 0 2827 - 88*1 D 2870 - 86 0 2930 - 80 (1989)*1 0 2935 - 91 0 3054-81(1985) 0 3055 - 90 0 3160 - 91 03193 - 91 0 3264-86 0 3366 - 90 8 0 3436 r- 91 03437-89 U 0 3438-89 0 3439 - 89 0 3504-91 0 3505 - 91 0 3626 - 85 (1990)*1 0 3627 - 91 0 3760 - 79(1984) 0 3797 - 88 0 3798 - 89 0 3799 - 89 0 3852-90 0 3961-89 0 3962 - 80(1989)*' 0 4076 - 86(1990) D 4077 - 91 04297-89 0 4471 -85(1989)*' 0 4492 - 85(1989)*' 04493-89 0 4534 - 89 0 4588 - 87 04589-91 0 4590 - 86 D 4734 - 90 D 4735-87 (1991)*' 0 4789 - 88 CONTENTS* V0UJMES6^S0e.Q2r Test Method for Solidification- Point of Benzene ................................. ............ ................................06.03 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons.................................... *................................ ...................................................................... 06.03 Test Method for freezing Point of High-Purity Hydrocarbons .......... .....................................................06.03 Test Method for Purity of Hydrocarbons from Freezing Points .................................................................06.03 Test Method for Bromine Index ofAromatic 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 ................................. ..................................... 06D3:`. Test Method for Aldehydes in Styrene Monomer ................................................ .................................. 06.03; t Test Method for Inhibitor, p-tert-Butylcatechol, in Styrene Monomer ,,...... ........................................... 06.03 Test Method for Polymer Content of Styrene Monomer ................. .........-- ................................... O&fet Test Method for Evaporating Residue of Naphthalene ......................... ...................................... 063)^ Method for Xylene Isomer Analysis by Gas Chromatography ........................... ....................................... 06.03 Specification for Refined Pyridine (1 Degree) .................................................... Test Method for Carbon Disulfide in Benzene ............................................................. Test Method for Peroxides in Styrene Monomer ....................................................... Specification for Refined Benzene-535 ................................................................. Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography .. 06.03 - Specification for Refined Phthalic Anhydride-1308 ................................................ Specification for Refined Phenol ............................................................................................. Test Method. for Trace Quantities of Total Sulfur in Volatile Organic Liquids (Oxy-Hydrogen Combustion Methods) (Discontinued I987f) ----- ...................................................................................0G>03S Test Method for Pyridine Bases in Tar Adds (Discontinued 1987f--Replaced by Test Method 04471) .................................... ................ :..................... .............. ............................ ...........................;... 06.03 Specification for Styreue Monomer 996 ......................................... .................................. 06.03 ; i Test Method for Gel Time of Tar Adds ....................... ...................... ...................................................... 06.03 Test Method for Maleic Add in Maleic Anhydride by Potentiometric Titration .................................... 06.03. Test Method for Apparent Density of Industrial Aromatic Hydrocarbons .,.......................................... 06.03> Test Method for Purity and Benzene Content of Cydohexane by Gas Chromatography....................... 06.03; Spedfication for Cyclohexane 99.5 ............................. .................. ......................................................... 06,03, Test Method for Phenol Content of Isopropylbenzene (Cumene) .............................................................06.03 Spedfication for Ethylbenzene ........ ; ................................. ........................................................... 06.03 Spedfication for Industrial Grade Aniline.................................................. ............ ..................................... 06.03 ; Test Method for Color of Maldc 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 Ctesylate Solutions from Petroleum Sources ................................. 06.03. Spedfication 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 ...................................................06.03 Test Method for Color of Cresylic Adds ("C" Series Standards) ............................................... 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 ofp-Xylene by Gas Chromatography .............................................................. 06.03 Test Method for Purily of Styrene by Freezing Point Method ..................... ............................................. 06.03 Practice for-Sampling and Handling Phenol and Cresylic Acid ................................................................. 06.03 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry ............................................................................................................................................06.03 Test Method for Analysis of Styrene by Gas Chromatography ................................................................... 06.03 Spedfication for o-Xylene 950........................................................................................ Spedfication for Isopropylbenzene (Cumene).................................................................... Practice for Sampling and Handling 4,4'-IsopropyIidenediphenol (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'-lsopropylidenediphenol (Bisphenol A)..................................06.03 Test Method for Benzene Content ofCyclic Products by Gas Chromatography........................................ 06.03 Guide for Analysis ofp-Xylene (Discontinued 1992f--Replaced by Specification D 5136)................... 06.03 Test Method for Nitrobenzene in Aniline............................. ?................................................................ .. 06.03 Test Method for Colorimetric Determination of p-fert-Butylcatechol in Styrene Monomer by Addition of Alcoholic NaOH.................................................................................................... Specification for Refined Benzene-545 ....................................... ................................................. 06.03; Test Method for Determination of Trace Thiopene in Refined Benzene by Gas Chromatography .... 06.03 Test Method for Solution Color of 4,4'-Isopropylidenediphenol (Bisphenol A).......................................... 06.03 06 06.031 l 06.03 0 06. xxn DUP050295661 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 4790 - 89a D 4961-89 D 5060 - 90 D5135 - 90 D 5136 -90 D5194-91 D 5211-91 E 299-90 E 300 - 86 E 691-87 Terminology of Aromatic Hydrocarbons and Related Chemicals.............................................................. 06.03 Test Methods for Gas Chromatographic Analysis of Major Otganic Impurities in Phenol Produced by the Cumene Process................................................................ ................................................................... 06.03 Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography ........ 06.03 Test Methods for Analysis of Styrene by Capillary Gas Chromatography...................................... .... 06.03 Specification for Purity p-Xylene... .......................................................................................................... 06.03 Test Method for Trace Chloride in Liquid Aromatic Hydrocarbons,........................................................ 06.03 Specification for Xylene for p-Xylene feedstock............................. ............................................................06.03 Test Method for Trace Amounts of Peroxides in Organic Solvents.............................................................06.03 Practice for Sampling Industrial Chemicals ............................. .................................................................... 06.03 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method...........06.03 RELATED MATERIAL jlist by Subjects, Volume 06.01 .. |ist by Subjects, Volume 06.02 .. : by Subjects, Volume 06.03 .. jietric Practice (Excerpts) (E 380) >1 Index........................................ index pSTM 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 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. Revision ofStandards: D 1492 - 91 D 3359-91 D4417-91 Slew Standards: D5165 - 91 D 5180- 91 Practice for the Laboratory Preparation of Gelled Vehicles Using a Resin Kettle Test Method for Quantitative Test for Turbidity in Clear Liquids.......... ......... 06.02 06.02 xxiii DUP050295662 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.03 Pa in t --Fa t t y Oil s a n d Ac id s , Na v a l St o r e s , So l v e n t s , Mis c el l a n eo u s ; Ar o ma t ic Hy d r o c a r bo n s Since the standards in this book are arranged in alphanumerical sequence, no page numbers are given in this list. The standards listed in italics are related documents included for information only and do not appear in this volume. . For List by 'Subjects of Volumes 06.01 and 06.02, see pp. S2J and 829 A complete Subject Index begins on p. 861 M FATTY OILS AND ACIDS, DRYING AND NONDRYING Specificationsfor: D 1539 - 60 (1988) D 961-86 D 960-79(1988) D184J -63(1988)" P 1842-63(1988) D 1843-63(1988)" P 1538-60(1988)" D 260 - 86(1990) D 234-82(1991)" D 601-87(1991)" D1392-87 P 1537-60(1988)" D 124-88 P 1462 - 87 D 3169 -89 D 1984-69(1988) D 12-88 Test Methodsfor: D 1950-86 D 1980-87(1991) D 1951-86 D1952-86 D 2090 - 88 01967-86 D}981-86(1990) D 1544-80 (1989)" 01358-86 D 1983 -90 D 3457 -87 (1991)" D 2800-87 D3725 - 78 (1988)" D 93-90 D 3278 -89 0 1966 - 69(1991)" D 1954-86 D 1955-85(1989)" P 1957 -86 02245-90 D 1959-85(1989)" D 1541-86 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 Qiticica Oil (Permanently Liquid) Safflower Oil Soybean Fatty Acids, Distilled Soybean Oil, Degummed Soybean Oil, Refined Sunflower Oil ,, Tall Oil Fatty Acids Tung Oil, Raw Acetone Tolerance of Heat-Bodied Drying Oils Acid Value of Fatty Acids Ash in Drying Oils and Fatty 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 Alim- Heating of Fatty Acids, Measuring Color of Transparent liquids (Gardner Color Scale) Diene Value, Spectrophotometric, of Dehydrated Castor Oil and Its Derivatives Fatty Add Composition by Gas-Liquid Chromatography of Methyl Esters Fatty Add Composition by Gas-Liquid Chromatography, Preparation of Methyl Esters from Fatty Adds for Determination of Fatty Acid Composition by Gas-Liquid Chromatography, Preparation of Methyl Esters from Oils for Determination of Fish Oil in Drying Oils and Drying Oil Fatty 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 (Mis and Fatty Adds Iodine Value, Total, of Drying Oils and Their Derivatives Approved for use by agencies of the Department of Defense, and if indicated on the standard, replaces corresponding Federal or Military document. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. XXIV i DU P050295663 LIST BY SUBJECTS, VOLUME 06.03 jtO- 86 (1990) 'IP-86 (1990) w5-70 (1987) Ip-82 PS-86 p2-85(1989)I p3-85(I989)l fo-82 (1987) p.5-82 Jb-85(1989)fl BS4- 85 (1989)ei P65-87 ()99!)1 P45-89 Loss on Heating of Drying Oils Oiticica Oil, Chloroform Insoluble Matter in Polymerized Fatty Acids Rosin Acids in Fatty Acids " Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes-, and Related Materials " Saponification Value of Drying Oils and Fattv Acids Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials Tall Oil - ' " 1 Tall Oil Rosin, Fatty Acids Content of Titer of Fatty Acids Tung Oil Quality Unsaponifiable Matter in Drying Oils and Fatty Acids Viscosity of Transparent Liquids by Bubble Time Method - p$5-84(1988)l 1467-89 140-82 <199I)eI 'ethodsfor: :076 64 (1987)*' 074 -66(1987)1 lp)|Q73 -66(1987)1 -64(1987) WkM Su' I "-87(1991) En.'iffs--89 **02078--86(1990) [02080 --64(1987) 402082 - 82 (1987) 02079 - 82(1987) d 2081 - 64(1987) ;D2083- 66(1987) 02072 - 66(1987)C| 235 - 87C1 3,3735 - 87 13-82 S'0' 836-84 ' ID 835-85 D 2359-85a D 3055-86 D 3734-91 t D 4077 - 81 (1986)i D 2827 - 881 :D 362-84 D 841-85 D 4076-86 D 843-80(1985)l D 846-84 D 319-90 D 330-89 ! D 304-90 D 1007-85 D 2694 -87 D 2696-87 D 4836-90 D 331-90 Drying Oils, Testing '; Fatty Acids Used in Protective Coatings! Testing, Volatile and Nonvolatile Content of Driers, Drying Oils, Naval Stores, and Solvents, Determining FATTY NITROGEN PRODUCTS Acid Value and Amine Value of Fatty Quaternary Ammonium Chlorides . Amine Values, Total, Primary, Secondary, and Tertiary, ofFatty Amines by Alternative Indicator Method Amine Values, Total, Primary, Secondary, and Tertiary, of Fatty, Amln.es, Amidoamines, and Diamines by Referee Potentiometric Method Ash in Fatty Quaternary Ammonium Chlorides . , Fatty Nitrogen Products Iodine Value of Fatty Amines, Amidoamines, and Diamines Iodine Value ofFatty Quaternary Ammonium Chlorides Molecular Weight, Average, ofFatty Quaternary Ammonium Chlorides . Non-amines, Percent in Fatty Nitrogen Compounds Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides pH of Fatty Quaternary Ammonium Chlorides Primary, Secondary, and Tertiary Amines, Percent in Fatty Amines Water in Fatty Nitrogen Compounds SOLVENT SPECIFICATIONS Petroleum Spirits Petroleum Spirits (Mineral Spirits) VM&P Naphthas Turpentine, Spirits of Terpene Solvents ... Aromatic Hydrocarbons and Related Materials Benzene,'IndustriarGrade (Discontinued 1991) Benzene-485, Refined (Nitration Grade) Benzene-535, Refined Cyclohexane 995 High-Flash Aromatic Naphthas Isopropylbenzene (Cumene)' Styrene Monomer 996 , 7. Toluene, Industrial Grade (0iscop'timied 1991) Toluene, Nitration Grade ' ,.o-Xyl$ne 950 '. Xylene, Nitration Grade Xylene, Ten-Degree (Discontinued 1991) . ' , .: : ... Alcohols and Ether Alcohols Amyl Alcohol (Synthetic) 2-Butoxyethanol -ButyI Alcohol (1-Butanol) jiec-Butyl Alcohol (2-Butanol) Diethylene Glycol Dipropylene Glycol (Discontinued 1992f--Replaced by Specification D 5164) Dipropylene Glycol Monomethyl Ether 2-Ethoxyethanol , XXV DUP050295664 D 2693-87 D 2636-91 D 1719-90 D 770-90 D 3160-91 D 3128 -89 D 1152-89 D 2635 - 91 D 3622-90 D 2695-87 D 4837-89 D 329-90 D 2627-91 D 2916-88 D 4360 - 90 D 740 - 89 D 3729-84 D 2917-91 D 1153-90 D 3540-86 D4615-86*1 D 3728-88 D 4614-86 D5137-90 D 1718-86 D3131-88 D 2634-86 D3130-86 D 4835-89 Test Methods for: D 801-57(1987) D 233 -- 65 (19Sl)el D 268-90 Test Methodsfor: D 1612- 90 D 1613- 91 D 847- 87 D 1614- 91 D 1492- 87 D 2324- 81 (1989)*' D 848- 81 (1989)*' D 849- 88 D 130- 88 D 1617- 90 D 853 - 82(1987)*' P 1363- 88 D 3961- 89 D 1685- 86 D 890- 58 (1987) D 1364- 90 E 203- 75 (1986)*' 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 rt-Propyl Alcohol (1-Propanol) Propylene Glycol (Discontinued 19927--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 19897--Replaced by Specification D 740) Methyl Isoamyl Ketone Methyl Isobutyl Ketone Esters Amyl Acetate, Primary, Synthetic (98 % Grade) K-Butyl Acetate (All Grades) 2-Ethoxyethyl Acetate (99 % Grade) Ethyl Acetate-(All Grades) - Hexyl Acetate Isobutyl Acetate (95 % Grade) Isopropyl Acetate (98 % Grade) Methyl Amyl Acetate n-Propyl Acetate (96 % Grade) Propylene Glycol Monomethyl Ether Acetate SOLVENT TEST METHODS General Methods Dipentene, Sampling and Testing Turpentine, Sampling and Testing Volatile Solvents for Use in Paint and Related Coatings and Materials, Sampling and Testing Chemical Tests Acetone in Methanol (Methyl Alcohol) Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons Alkalinity in Acetone Bromine Index of Aromatic Hydrocarbons by Coulometric Titration Carbon Disulfide in Benzene Color, Add 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. XXvi DUP050295665 LIST BY'SUBJECTS, VOLUME 06.03 t. Methods for: 3257-88 2935-81(1985) 4367-89 1209-84(1988)" 1054-81 (1985) 850-86 86-90 1078-86 5008-89 3539-87 3934 - 90 1310-6(1990)" 93-JO 56 #87 3941 #90 3278# 82" 3893-90 `2804 - 88 ` _ CG P 2360 - 82 (1987)" 1353-90 >4296-84(1988)" >4773-89 fp 852- 87 to-1493- 84(1988) [`iO 4206 - 89 LP4207- 91 ip 3962 - 80(1989)" P 3009 72(1981)" mp1555- 83 95- 83(1990) [p 2306 - 81(1985) P3797- 88 P 3798 - 89 D1217 - 86 D 1015- 84 P1016 - 84 D1218 - 87 Aromatics in Mineral Spirits by Gas Chromatography Apparent Density of Industrial Aromatic Hydrocarbons Benzene in Hydrocarbon Solvents by Gas Chromatography Color of Clear Liquids (Platinum-Cobalt Scale) Cyclohexane, Purity and Benzene Content by Gas Chromatography Distillation of Aromatic Hydrocarbons ;< Distillation of Petroleum Products Distillation Range of Volatile Organic Liquids 2-Ethylhexonal, Ethyl Methyl Pentanol Content and Purity Value by Gas-Chromatography Evaporation Rates of Volatile Liquids (see Vol 06.01) Flash/No-Flash--Equilibrium Method by a Closed-Cup Apparatus , Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus Flash Point by Pensky-Martens Closed Tester Flash Point by Tag Closed Tester Flash Point of Liquids by Equilibrium Method With Closed-Cup Apparatus Flash 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 and Diluents Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene Glycol Monomethyl Ether Acetatq Solidification Point of Benzene Solidification Point of Industrial Organic Chemicals ,. > ., Sustained Burning of Liquid Mixtures by Setaflash Apparatus (Open Cup) Sustained Burning of Low-Viscosity liquid Mixtures by Wick Test Styrene Analysis by Gas Chromatography Turpentine Composition by Gas Chromatography Volume and Weight of Industrial Aromatic Hydrocarbons, Calculation of Water in Petroleum Products and Bituminous Materials by Distillation Xylene Isomer Analysis by Gas Chromatography .. 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) ' Solubility and Miscibility Tests est Methodsfor: D 611-82(1987)" D 1720 - 88 D 1476 - 88 D 1133-90 P 1722-90 i-' l; Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents Dilution Ratio of Active Solvents in pellulose Nitrate Solutions ' Heptane Miscibility of Lacquer Solvents Kauri-Butanol Value of Hydrocarbon Solvents Water Miscibility of Water-Soluble Solvents Liquid Naval Stores Test Methodsfor: ilP'D 801 -57 (1987) . D 86 - 82C2 D 56-87 D 802-82(1987) D 856-49(1987) 01131-53(1981)" D 803 - 82 (1987) D 233-65(1981)" 0 3009 - 72(1981)" D 890-58(1987) Dipentene, Sampling and Testing Distillation of Petroleum Products Flash Point by Tag Closed Tester Pine Oil, Sampling and Testing Pine Tars and Pine-Tar Oils Rosin Oils Tall Oil Turpentine, Sampling and Testing Turpentine Composition by Gas Chromatography Water in Liquid Naval Stores > General Definitions ofTerms Relating to: D 804 - 79 (1987) Naval Stores and Related Products xxvn DU P050295666 LIST BY SUBJECTS, VOLUME 06,03 MISCELLANEOUS RAW MATERIALS Specifications for: D 4710-87 Acetaldehyde D 3620 -90 Acetic Acid, Glacial D 4416-89 Acrylic Acid D 3547 -91 n-Butyl Acrylate D 608-90 Dibutyl Phthalate D 3548-86 Ethyl Acrylate D 3193 - 91 Ethylbenzene D 3541-91 2-Ethylhexyl Acrylate D 1969-91 2-Ethyihexyl (Synthetic) - ' D 2378-84 (1987) Formaldehyde H D 1257 - 90 Glycerin, High-Gravity p D 3504-91 Maleic Anhydride D 3845-89 Methacrylic Acid, Glacial D 4709-87 Methyl Acrylate D 600 - 90 Paint Driers,-Liquid D 2403-68 (1982)*' Phthalic Anhydride-1308, Refined D 363 - 90 Tricresyl Phosphate f D 2190-89 Vinyl Acetate Test Methods for: ` ...... ;i > ; I j j D 3362 - 84 (1987) Acrylate Esters, Purity by Gas Chromatography . D4415-91 i D 2192-89 'I D2119-87 Acrylic Acid, Determination of Dimer in ' Aldehydes and Ketones, Purity of Aldehydes in Styrene Mondmer | 1 D 2613-85 (1990)*' Calcium and Zinc in Paint Driers by EDTA Method I 03970-80(1990)*' Cerium in Paint Driers by Qxidimetric-Determination J D 2373 - 85 (1990)*' Cobalt in Paint Driers by EDTA Method ;; I 0 2379 - 84(1987) Formaldehyde Solutions, Acidity of . 1 D 2194-89 Formaldehyde Solutions, Concentration of I D 2087-89 Formaldehyde Solutions, Iron in D 2380 -84 (1987) Formaldehyde Solutions, Methanol Content of ( D 3546 - 90 Formic Acid in Glacial Acetic Arid D 1258-90 Glycerin, High-Gravity, Testing ' D 1728 - 83 Glycerin, Phthalate Ester Color of High Gravity (Discontinued 199 If) D 3804-86 (1991)*' Iron in Paint Driers by EDTA Method D2374- 85 (1990)*' Lead in Paint Driers by EDTA Method D2375 - 85 (1990)*' Manganese in Paint Driers by EDTA Method ' D 3125-83 (1987) Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid D 2999-85 Monopentaerythritol in Commercial Pentaerythritol by Gas Chromatography (Discontinued 1989f-- Replaced by Test Method D 2195) D 564-87(1991)*' Paint Driers, Liquid . D 2195-84 Pentaerythritol D 3989-81a (1990)*' Rare Earth Metals, Total, in Paint Driers by EDTA Method D 3962 -80(1984)*' Styrene Analysis by Gas Chromatography D 2119-87 Styrene Monomer, Aldehydes in D 2120-87 Styrene Monomer, p-tert-Butylcatechol Inhibitor in D 2340 - 82 (1987)*' Styrene Monomer, Peroxides in D 2121 - 84 Styrene Monomer, Polymer Content of D 1721 -84 (1988)*' Tricresyl Phosphate, Permanganate Time of D 1399-90 TricresylPhcsphate, Unsaponifiable Content of D 1468-84(1988)*' Tricresyl Phosphate, Volatile Matter in D 1638-74*' Urethane Foam Isocyanate Raw Materials (Discontinued 199 If) D 3988-85 (1990)*' Vanadium in Paint Driers by EDTA Method D2191-84 Vinyl Acetate, Acetaldehyde Content of D 2086 -84 Vinyl Acetate and Acetaldehyde, Acidity in D 2193-84 Vinyl Acetate, Hydroquinone in D 1631-85 Water in Phenol and Related Materials by the Iodine Reagent Method D 3969-85 (1990)*' Zirconium in Paint Driers by EDTA Method Terminology Relating to: D 16-91 Paint, Varnish, Lacquer, and Related Products NAVAL STORES Rosin Test Methodsfor: D 465-82(1987)*' Acid Number of Rosin xx'vm i l DUP050295667 ethodsfor. 1063-51(1987) 585 - 82 064-58 (1981) 8-90 1240 - 82 509-70(1987) 464 - 91 i 28-67 (1982)I 269-52(1987)" 065-82 889-58(1987) |! 'itfications for: !'3264 - 86 836-84 835-90 2359 - 90. 14734 - 90 3055-90 4077 - 91 3504-87 2439 - 91 2403 - 91 2323-84(1989)" ,2827-88" 362-84 841 - 90 5211-91 843-90 846-84 4076-86(1990) 5136-90 t Methodsfor: 847- -91 D 848- -81(1989)" ID 2119 87 D 2935 -91 D4492- 85(1989)" D 4534 89 I'D 1492- 91 D 2324 - 81 (1989)" D 5194 -91 D 3627 - -82(1987)" D 4789 -88 D3366- 90 D 1686- 81(1990) D4590- 86 :D 849- 88 D 3439 - 89 D 3505 - 84" D 850- 91 D 2232 - 81 (1986)" D1015 - 89 D 2870 - 86 853- 91 D 5060 - 90 D 4961 - 89 D2120- 87 D 3760 - 79(1984) D 2930 - 80(1989)" D 2360 - 82 (1987)" D 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 Rosin > Softening Point by Ring-and-Ball Apparatus ; .y 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 1991 f) Benzene-485, Refined (Nitration Grade) Benzene-535, Refined Benzene-545, Refined Cyclohexane 995 Isopropylbenzene (Cumene) Maleic Anhydride Phenol, Refined Phthalic Anhydride-1308, Refined Pyridine, Refined Styrene Monomer 996 Toluene, Industrial Grade (Discontinued I991f) Toluene, Nitration Grade r Xylene, Feedstock for p-Xylene Xylene, Nitration Grade' Xylene, Ten-Degree (Discontinued 1991f) o-Xylene 950 p-Xylene, High Purity Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons Acid Wash Color of Industrial Aromatic Hydrocarbons Aldehydes in Styrene Monomer Apparent Density of Industrial Aromatic Hydrocarbons Benzene Analysis by Gas Chromatography Benzene Content of Cyclic Products by Gas Chromatography Bromine Index of Aromatic Hydrocarbons by Coulometric Titration Carbon Disulfide in Benzene Chloride, Trace, in Liquid Aromatic Hydrocarbons Color of Cresylic Acids ("C" Series Standards) Color of 4,4'-Isopropylidenediphenol (Bisphenol A) in Solution Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating Color of Solid Aromatic Hydrocarbons and Related Materials in the Molten State (Platinum-Cobalt Scale) Colorimetric Determination ofp-terf-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-terf-Butylcatechol, in Styrene Monomer Isopropylbenzene (Cumene) by Gas Chromatography Maleic Acid in Maleic Anhydride by Potentiometric Titration Monocyclic Aromatic Hydrocarbons, Trace Impurities in, by Gas Chromatography Nitrobenzene in Aniline Peroxides in Styrene Monomer Polymer Content of Styrene Monomer xxix DU P0502 95668 LIST BY SUBJECTS, VOLUME 06,03 ) Test Methodsfor: D3054- 81 (1985) D 1016-89 D4471 - 85(1989)ei D2031 -84(1989)1 D 852 - 87(1991) D1493-90 D4493-89 D5135-90 D3962-80(1989)1 D 3799-89 D 3961 -89 D3626-85(1990)I D 1685 - 86 (1990) D4735-87 (1991 )e 1 D 1555-91 D 1631 - 85 (1989)ei D 2030 - 84 (1989)1 D2306- 81 (1985) D 3797-88 D 3798 - 89 D1217 -86 D1218 -87 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-Xylene by Gas Chromatography Density and Relative Density (Specific Gravity) ofLiquids by Bingham Pycnometer (see Voi 0S.01) Refractive Index and Refractive Dispersion ofHydrocarbon Liquids (see Voi 05.01) Practices for: D 3436-91 D 4297 - 89 D 3437-89 D 3438-89 D 3852-90 Guidefor: D 4588-87 Terminology of: D 4790 - 89a 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 1992t--Replaced by Specification D 5136) Aromatic Hydrocarbons and Related Chemicals GENERAL STANDARDS Specificationsfor: D1193-91 E 100 - 81(1986) E 1-90 E 133-86 Test Methodsfor: E 299-90 E 70-90 E 200 - 86 Practicesfor: E 300-86 E 691-87 Reagent Water ASTM Hydrometers (see Voi 14.03) ASTM Thermometers (see Voi 14.03} Distillation Equipment (see Voi 14.02) Peroxides in Organic Solvents, Trace Amounts pH ofAqueous Solutions with the Glass Electrode (see Voi 15.05) i Standard Solutionsfor Chemical Analysis, Preparation, Standardization, and Storage of(see Voi 15.05) 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 Practice for: E 380-91 . > Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Material section) xxx DUP050295669 V-. PAINT AND RELATED COATINGS AND MATERIALS DUP050295670 Designation: D 12 - 88 Standard Specification for Raw Tung Oil1 This, standard is issued under the fixed designation D 12; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision dr reapproval. . Scope 1.1 This specification covers raw tung oil derived from Aeuntesfordii Hemsley. 2. Referenced Documents 2.1 ASTM Standards: D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2 D 555 Guide for Testing Drying Oils3 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D1541 Test Method for Total Iodine Value of Drying Oils and Their Derivatives3 D 1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4 D1639 Test Method for Acid Value of Organic Coating Materials5 D1955 Test Method for Gel Time of Drying Oils3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 D1962 Test Method for Saponification Value of Drying. Oils, Fatty Acids, and Polymerized Fatty Acids3 D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 3 D1964 Test Method for Tung Oil Quality3 1 This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of SubcomLmittee D01.32 on Drying Oils. Current edition approved Oct 31, 1988, Published December 1988. Originally published as D 12 -15 T. Last previous edition D 12 - 87. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 5 Annual Book ofASTM Standards, Vol 06.01. TABLE 1 Properties of Raw Tung Oil * Specific gravity, 25/260C Acid value, max Saponification value Unsaponifiable matter, max, % Iodine value (Wifsj, min Total iodine value, min Clarity Color (Gardner), max Rash point, min Gel time, minutes, max Tung oil quality test Refractive index, 25C Requirements 0.933 to 0.938 5.0 189 to 195 0.75 163 220 clear and transparent at 25C 12 203F(95 "C) 250F (121 C) 12 ' pass 1.5160 to 1.5200 ' ASTM Test Method D1963 D1639 D 1962 01965 D1959 D1541 02090 D1544 D3278e D 93 D 1955 D1964 A A relationship between refractive index and tung' oil adulteration with other oils is described in "Paint Testing Manual," Gardner-Swarti-13th Edition, 1972, Chapter 2,1, Section 12.1, p. 62. B Test Methods D 3278 are useful only at temperatures up to 230F, but may be used to test for the presence of volatile solvents as evidenced by a flash point of 230F or lower. D 1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 D2090 Test Method for Clarity and Cleanness of Paint Liquids6 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus3 3. Properties 3.1 Raw tung oil shall conform to the requirements given in Table 1. 4. Test Methods 4.1 Sampling--Sampling shall be conducted in accord ance with Test Method D 1466. 4.2 The significance of the test methods enumerated under properties in this specification is discussed in Guide D 555. 6 Annual Book ofASTM Standards, Vols 06.02 and 06.03. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Vour comments are invited either for revision of-ibis 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, 1978 Race St., Philadelphia, PA 19103. DUP050295671 Designation: D 13 - 82 (Reapproved 1987) Standard Specification for Spirits of Turpentine1 This standard is issued under the fixed designation D 13; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovaL This specification has been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. I. Scope 1.1 This specification covers the following kinds of spirits of turpentine: Gum spirits of turpentine, steam-distilled wood turpen tine, sulfate wood turpentine, and destructively-distilled wood turpentine. 1.2 The purchaser should specify the kind of spirits of turpentine desired. 2. Referenced Document 2.1 ASTM Standard: D233 Methods of Sampling and Testing Turpentine2 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 1.34 on Naval Stores. Current edition approved March 26, 1982. Published June 1982. Originally published as D 13- 14 T. Last previous edition D 13 -65 (1981). 2 Annual Book ofASTM Standards, Vol 06.03. 3. Properties 3.1 Spirits of turpentine shall be pure and shall conform to the requirements prescribed in Table 1. 4. Appearance 4.1 Spirits of turpentine shall be clear and free from suspended matter and water. 5. Color 5.1 The color shall be "standard" or better. 6. Odor 6.1 The odor shall be mild and characteristic of the kind of spirits of turpentine specified. If desired, deliveries shall conform to the odor of the sample agreed upon by the purchaser and the seller. iij | '/ j! 7. Test Methods < 7.1 The materialshall be sampled and the properties / enumerated in this specification determined in accordance with the Methods D 233. TABLE 1 Gum Spirits of Turpentine Physical Requirements max min Specific gravity, 15.5/15.5C Refractive index at 20C, D line Residue after polymerization with 38 W HaS04: Volume,- % Refractive index at 20C'' Initial boiling point at 760-mm Hg pressure, C Distilling below 170C at 760-mm Hg pressure, % ' Distilling below 180C at 760-mm Hg pressure, % 0.875 1.478 2 ... 160 0.860 1.465 1.500 150 90 A This requirement is not necessary when the volume is 2 % and lower. Steam Distilled max 0.875 1.478 min 0.860 1.465 2 1.500 160 150 90 Wood Turpentine Sulfate max 0.875 1.478 ... min 0.860 1.465 160 150 90 Destructively Distilled max min 0.865 1.483 0.850 1.463 2 1.480 157 150 60 90 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 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 views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 4 DUP050295672 Designation: D 16 - 91 Standard Terminology Relating to Paint, Varnis^ 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 the last revision or reapproval. This standard has been approved for use by agencies ofthe Department ofDefense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. abrasion resistance (coatings)--the ability of a coating to resist being worn away and to maintain its original appearance and structure when subjected to tabbing, 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, sccalkyd 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, autadeposition--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 rate of the latex is controlled by the rate ,of surface solubilization. The process does not require any pretreatments such as phosphating, needs no external energy input, and gives rise to deposition wherever the solution wets the substrate. Irregularly shaped parts can be uniformily coated. '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 Decerhber 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 of 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 of the appearance of an object dependent upon the spectral composition of the incident light, the spectral reflectance or transmittance of the DUP050295673 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 ceUulosic lacquer, for appli cation on textiles and leathers, drier--a composition that accelerates the drying of oil, paint, printing ink, .or varnish. Driers are usually metallic com positions and are available in both solid and liquid forms, drying oil--an oil that possesses to a marked degree the property of readily taking up oxygen from the air and changing to a relatively hard, tough, elastic substance when exposed in a thin film to the air. durability--a relative term indicating degree of permanency. It may be applied to individual protective, decorative, or functional properties, for example, "the durability of gloss," but if used in a general way, for example, "the excellent durability of a paint," implies the ability of the described coating to retain, to the indicated degree, all the properties required for the continued service of the coating. edge-tracking (coatings)--a residual, discernible pattern in a roller-applied coating characterized by trails from either or both ends of the roller. emulsion paint--under paint, see emulsion paint. enamel--a paint that is characterized by an ability to form an especially smooth film. erosion resistance (coatings)--the ability of a coating to withstand being worn away by chalking or by the abrasive action of water or 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, blanc fixe, or calcium carbonate). filler--a pigmented composition for filling the pores or irregularities in a surface preparatory to application of other finishes. fire-retardant--a descriptive term which implies that the described product, under accepted methods of test, will significantly: (a) reduce the rate of flame spread on the surface of a material to which it has been applied, or (b) resist ignition when exposed to high temperatures, or (c) insulate a substrate to which it has been applied and prolong the time required to reach its ignition, melting, or structural-weakening temperature, filiform corrosion resistance (coatings)--the ability of a coating to resist that type of corrosion of metal substrates characterized by a definite thread-like structure and direc tional growth that occurs under coatings, fire-retardant coating--a coating that will do one or more of the following: (1) reduce the flame spread on the substrate over which the coating is applied, sometimes at the sacrifice of the coating (see intumescent coating); (2) resist ignition of the substrate when exposed to high tempera ture; or (3) insulate the substrate to which the coating is applied and thereby prolong the time required to reach its ignition, melting or structural-weakening temperature, flaking resistance (coatings)--the ability of a coating to resist the actual detachment of film fragments either from the previously applied coating or the substrate. Flaking is generally preceded by cracking, checking, or blistering and is the result of loss of adhesion. Also known as scaling resistance. flatting agent--a material added to paints, varnishes, and other coating materials to reduce the gloss of the dried film. forced drying temperature--a temperature between room temperature and 150'F (65C). fossil resin--under resin, natural, see fossil resin. gallon, U. S.--a volume equal to 231 in.3 For paint, varnish, lacquer, and related products this is measured at 77F (25Q. glaze--a very thin coating of a paint product usually a semi-transparent coating tinted with Van Dyke brown, burnt sienna, or a similar pigment, applied on a previously painted surface to produce a decorative effect, 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 of square feet over which a gallon of paint, or pound of pigment, as used, can be uniformly spread to produce a specified contrast ratio (see 6 DUP050295674 contrast ratio). The term covering power has no specific |1 Relationship to hiding power, and actually has no precise meaning. hte--under color of an object, see hue. ' 'roxyl number--the number of milligrams of potassium hydroxide (KOH) equivalent to the hydroxyl content of 1 of sample. iustriai talc--a mineral product vatyingX^m composition Lfrom that approaching the theoretical formula of talc, itMg3Si4O10 (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 SyAsbestos. These fibrous minerals may or may not be jl-asbestos. ^industrial talc, nonasbestos type--industrial talc of which % wless than 2 particles per 100 particles (by light microscopy) are asbestos fibers, where "asbestos fiber" is defined as sbeing both a fiber by Definitions D 2946 and one of the asbestiform varieties of serpentine, riebeckite, cummingfionite (which are chrysotile, cfocidolite and amosite, respectively), anthophyllite, tremolite, or actinolite. The rionasbestiform varieties of these same minerals are not ;asbestos. fititumescent coating--a fire-retardant coating (which see) j that when heated forms a foam produced by I nonflammable gases, such as carbon dioxide and aim t monia. This results in a thick, highly insulating layer of j^carbon (about fifty times as thick as the original coating) II that serves to protect the coated substrate from fire, japan---a varnish yielding a hard, glossy, dark-colored film. r .Japans are usually dried by baking at relatively high , temperatures. ipan, a vehicle for japan colors; frequently contains shellac, iapan color--a paste containing pigment arid a grinding g. japan vehicle used for lettering and decoration, japan drier--a resinate-base liquid drier, lacquer--a coating composition that is based on synthetic thermoplastic film-forming material dissolved in organic solvent that dries primarily by solvent evaporation. Typ ical lacquers include those based on nitrocellulose, other cellulose derivatives, vinyl resins, acrylic resins, etc. j; 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 dolor ..and a more or less pronounced translucency when made into an oil paint. Under this term are included two (and perhaps three) types of pigment: (a) the older original type composed of hydrate of alumina dyed with a solution of the natural organic color, (b) the more modem arid 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 ofa 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 lCT' m2 s_I) at 104F (40C) or an equivalent viscosity at agreed upon temperature. (This does not include powdersand granular materials.) Liquids are divided into two classes: Class A, low viscosity--a liquid having a viscosity of 1 x 10~3 to 25.00 St (1 X 10~7 to 25.00 x 10~4 m2 s~') at 104F (40C) or an equivalent viscosity at an agreed upon temperature. Class B, high viscosity--a liquid having a viscosity of 25.01 to 1 X 103 St (25.01 X 10-4 to 1 X 10~` m2 s"`) at 104F (40C) or an equivalent viscosity at an agreed upon temperature. mass color--the color, when viewed by reflected light, of a pigment-vehicle mixture of such thickness as to obscure completely the background. Sometimes called over-tone or mass-tone. mass-tone--see mass color. melamine resin--under resin, synthetic see melamine resin. metal marking resistance--the ability of a coating to with stand streaking or marking when a metal object is rubbed against or dragged across the surface of the coating, mildew (fungus) resistance (coaftags)--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. nondrying oil--an oil that does not of itself possess to a perceptible degree the power to take up oxygen from the air and lose its liquid characteristics, nonvolatile content--the portion of a coating that does not evaporate during drying or curing under specified condi tions, comprising the binder and, if present, the pigment. (The percent volatile content is obtained by subtracting the nonvolatile content from 100.) nonvolatile vehicle--the liquid portion of a paint excepting its volatile thinner and water. oil color--an oil paint containing a high concentration of colored pigment, commonly used for tinting paint. oil paint--under paint, see oil paint, oil varnish--under varnish, see oil varnish. opacity--the degree of obstruction to the transmission of visible fight. 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. DUP0502 95675 D 16 paint vb--to apply a thin layer of a coating to a substrate by brush, spray, roller, immersion, or any other suitable means. paint n, general--a pigmented coating. See coating, paint n, specific--a classification sometimes employed to distinguish pigmented drying oil coatings ("paints") from synthetic enamels and lacquers. emulsion paint--a paint, the vehicle of which is an emulsion of binder in water. The binder may be oil, oleoresinous varnish, resin, or other emulsifiable binder. latex paint--a paint containing a stable aqueous disper sion of synthetic resin, produced by emulsion polymeriza tion, as the principal constituent of the binder. Modifying resins may also be present. oilpaint--a paint that contains drying oil or oil varnish as the basic vehicle ingredient. paste paint--a paint in which the pigment is sufficiently concentrated to permit a substantial reduction with vehicle before use. water paint--a paint, the vehicle of which is a water emulsion, water dispersion, or ingredients that react chem ically with water. paint brush--a paint application tool consisting of a flexible brushing part composed of long filamentary material (brushing material) bound to a handle. 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 of the 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 figment in the nonvolatile portion of a paint or printing ink, as calculated from bulking value and composition data. The letters PV are commonly used as an abbreviation. pinholes--small pore-like flaws in a coating that extend entirely through the applied film and have the general appearance of pin pricks when viewed by reflected light. plasticizer--a substance added to paint, varnish, or lacquer to impart flexibility. primer--the first of two or more coats of a paint, varnish, or lacquer system. printing ink--a colored or pigmented liquid or paste compo sition that dries to a solid film after application as a thin layer by printing machinery. print resistance (coatings)--the ability of a coating to resist taking on the imprint due to the pressure of another surface placed against it. putty--a dough-like material consisting of pigment and vehicle, used for sealing glass in frames, and for filling imperfections in wood or metal surfaces. See glazing compound. resin, natural--a solid organic substance, originating in the secretion of certain plants or insects, which is thermo plastic, flammable, nonconductive of electricity, breaks with a conchoidal fracture (when hard); and dissolves in certain specific organic solvents but not water. fossil resin--a natural resin of ancient origin usually found in the earth. resin, synthetic--a synthetic substance physically similar to natural resin. acrylic resin--a synthetic resin made from derivatives of acrylic add. alkyd resin--a synthetic resin made from polyhydric alcohols and polybasic acids; generally modified with resins, fatty oils or fatty adds. 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 maldc 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 front 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 8 DU P050295676 D 16 exposure to humid atmosphere or chemical attack. See j white rust. st resistance (coatings)--the ability of a coating to protect , the substrate of iron or its alloys from rusting, aturation--under color of an object, see saturation. paling resistance (coatings)--See flaking resistance, jkler--a liquid composition to prevent excessive absorption &f finish coats into porous surfaces; also a composition to prevent bleeding (see size). jiinidryrag 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, hade--a term descriptive of a lightness difference between surface colors, the other attributes of color being essen tially constant. A lighter shade of a color is one that has ishigher lightness but approximately the same hue and I saturation; and a darker shade is one that has a lower P 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 fctoward a darker color. Shade of a color has been defined , by several authorities as the mixture of black with that scolor, thus establishing its opposite character to "tint," but 5 by extension ofits relative sense it has been frequently and widely used to include lighter shades by use of the adjective "lighter" or "paler." Although such expressions apparently involve a contradiction, it is clear that while we may have a shade of a color or darker color of the same sort, it is easy to conceive of another shade not quite so dark and therefore lighter. Iheepskin paint roller cover--a cover in which the paint L applicating material is wool fleece still attached to its tanned natural skin. ize--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. soii (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 1CT1 m2 s-1) at 104F (40C) or an equivalent viscosity at an agreed upon temperature. (This includes powders and granular mate rials.) spreading rate--the area covered by a unit volume of coating material frequently expressed as square feet per gallon. stain--a discoloration, arising from foreign materials, that ..s penetrates into the coating. stem^ra 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 1, 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 of these isocyanate groups with ambient moisture. Type III, one-package heat cured--urethane coatings that dry on cure by thermal release of blocking agents and regeneration of active isocyanate groups that subsequently react with substances containing active hydrogen groups. Type IV, two-package catalyst--urethane coatings that comprise systems wherein one package contains a prepoly mer or adduct having free isocyanate groups capable of forming useful films by combining with a relatively small quantity of catalyst, accelerator, or crosslinking agent such as a monomeric polyol or polyamine contained in a 9 DUP050295677 D 16 second package. This type has limited pot-iife 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 Qr 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. vernonia 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 0C and thus needs only a fraction of the volatile solvents usually used for other drying oils. Thus, it can be used as a reactive diluent for high solids alkyds and epoxy coating formulations. vinyl resin--under resin, synthetic, see vinyl resin, volatile thinner--see thinner. volume percent solids--the portion of a coating that remains as part of the dry film expressed as percent by volume. 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 ifnot revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you 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. 10 DUP050295678 IP Designation: D 56 - 87 An American National Standard Standard Test Method for Flash Point by Taj Closed Tester1 This standard is issued under the fixed designation D56; the number immediately following the designation indicates the year of originai 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 lest method has been adoptedfor use by government agencies to replace Method 1101 ofFederal Test Method Standard No. 791b, and Method 4291 ofFederal Test Method Standard No. 141A. Scope t.l This test method covers the determination of the flash pint, by Tag closed tester, of liquids with a viscosity of glow 5.5 centistokes (cSt) at 104F (40'C), or below 9.5 cSt L-77'F (25`C), and a flash point below 200F (93C) except t-back asphalts, those liquids which tend to form a surface 'm under test conditions, and materials which contain uspended solids. No t e I --For the closed-cup flash point of liquids with a viscosity of .5 cSt or more at 104F (40C), or 9.5 cSt or more at 77*F (25"C), with k flash point of200F (93C) or higher, which tend to form a surface film Sunder test conditions, or suspensions of solids, use Method D 93. For ut-back asphalts refer to Methods D 1310 and D3143. No t e 2--The U. S. Department of Transportation (RSTA)2 and U. ", Department of Labor (OSHA) have established that liquids with a 'ash point under 100F (37.8C) are flammable as determined by this Tnethod for those liquids which have a viscosity less than 5.5 cSt at 104"F |'(40"C), or 9.5 cSt or iess at 77F (25'C), or do not contain suspended jsolids or do not have a tendency to form a surface film while under test jOther classification flash points have been established by these Depart ments for liquids using this test. 1.2 Liquids having viscosities more than 5.5 cSt at 104F ;(40C), or 9.5 cSt or more at 77*F (25C), and contain i suspended solids or have a tendency to form a surface film while under test should be tested in accordance with Test Methods D 93. 1.3 The values stated in inch-pound units are tb be regarded as the standard. Temperatures are in degrees Fahrenheit and viscosity is in Centistokes units. The values in parentheses are for information only. 1.4 This standard should be used to measure and describe the properties of materials, products, or assemblies in re sponse to heat and flame under controlled laboratory condi tions and should not be used to describe or appraise the fire hazard orfire risk ofmaterials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements offire risk assessment which takes into account all ofthefactors which are pertinent to an assessment ofthefire hazard ofa particular end use. 1 This test method is under the joint jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcom mittee D 02.08 on Volatility. Current edition approved Dec. 14, 1987. Published February 1988. Originally published as D 56 -18 T. Last previous edition D 56 - 82. 2 For information on U. S. Department of Transportation's regulations, see Codes of U. S. Regulations 49 CFR Chapter 1 and for information on U. S. Department of Labor's regulations see Code ofU. S. Regulations 29 CFR Chapter XVIL Each of these items are revised annually and may be procured from the Superintendent of Documents, Government Printing Office, Washington, DC 20402. 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 or regulatory limitations prior to use. For specific hazard statements, see Note 5. 1.6 Related Standards are Test Methods D93, D3828 and D 3941. 2. Referenced Documents 2.1 ASTM Standards: D93 Test Methods for Flash Point by Pensky-Martens Closed Tester3 D850 Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials4 D1015 Test Method for Freezing Points of High-Purity Hydrocarbons3 D1078 Test Method for Distillation Range of Volatile Organic Liquids4 D 1310 Test Method for Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus3 D3143 Test Method for Flash Point of Cutback Asphalt with Tag Open-Cup Apparatus5 D 3828 Test Method for Hash Point by Setaflash Closed Tester6 D3941 Test Method for Hash Point by the Equilibrium Method with a Closed-Cup Apparatus4 E 1 Specification for ASTM Thermometers7 3. Definition 3.1 flash point--the lowest temperature corrected to a pressure of 760 mm Hg (101.3 kPa, 1013 m bar) at which application of a test flame causes the vapors of a portion of the sample to ignite under specified conditions of test. 4. Summary of Test Method 4.1 The sample is placed in the cup of the tester and, with the lid closed, heated at a slow constant rate. A small flame of specified size is directed into the cup at regular intervals. The flash point is taken as the lowest temperature at which application of the test flame causes the vapor above the sample to ignite. 3 Annual Book ofASTM Standards, Vol 05.0 1. 4 Annual.Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 04.03. 6 Annual Book ofASTM Standards, Vol 05.03. 7 Annual Book ofASTM Standards, Vols 05.01 and 14.03. II DUP05029567r9 D56 5. Significance and Use 5.1 Flasb point measures tendency of the sample to form a flammable mixture with air under controlled laboratory conditions. It is only one of a number ofproperties that must be considered in assessing the overall flammability hazard of a material. 5.2 Flash point is used in shipping and safety regulations to define "flammable" and "combustible" materials. One should consult the particular regulation involved for precise definitions of these classes. 5.3 Flash point can indicate the possible presence of highly volatile and flammable materials in a relatively nonvolatile or nonflammable material. For example, an abnormally low flash point on a sample of kerosine may indicate gasoline contamination. 6. Apparatus 6.1 Tag Closed Tester--The apparatus is shown in Fig. 1 and described in detail in Annex Al. Refer to Annex A2 for directions for checking the condition and operation of the tester. 6.2 Shield--A shield 18 in. (460 mm) square and 24 in. (610 mm) high, open in front, is recommended. 6.3 Thermometers--For the test cup thermometer, use one as prescribed in Table I. For the bath thermometer, any convenient type that has an adequately open scale covering the required range may be used; it is often convenient to use the same type of thermometer as used in the test cup. No t e 3--Whenever thermometers complying with ASTM require ments are not available, thermometers complying with the requirements for The Institute of Petroleum thermometer IP 15F FM-Low may be used. No t e 4--There are automatic flash point testers available and in use which may be advantageous in that they save testing time, permit the use of small samples, and exhibit other factors which -may merit their use. When automatic testers are used, the user must be sure that all of the manufacturer's instructions for calibrating, adjusting, and operating the instrument are followed. In any case of dispute, the flash point as determined manually shall be considered the referee test. 7. Sample 7.1 Erroneously high flash points can be obtained when precautions are not taken to avoid the loss of volatile material. Containers shall not be opened unnecessarily and transfers shall not be made unless the sample temperature is at least 20"F (11C) below the expected flash point. Samples in leaky containers shall be discarded. 7.2 Samples are not to be stored in plastic (polyethylene, polypropylene, etc.) bottles, since volatile material may diffuse through the walls of the bottle. 8. Preparation of Apparatus 8.1 Support the tester on a level steady table. Unless tests are made in a draft-free room or compartment, surround the tester on three sides by the shield for protection from drafts. Tests are not to be made in a laboratory draft hood or near ventilators. 8.2 Gas is recommended for the test flame. 9. Procedure 9.1 For flash points below 55F (13C) or above 140'F (60C), use as bath liquid a 1 + 1 mixture of water and ethylene glycol (see Warning--see Note 5). For flash points between 55F (13C) and 140F (6(FC), either water or a water-glycol mixture may be used as bath liquid (Note 5). The temperature of the liquid in the bath shall be at least 20F (11C) below the expected flash point at the time of introduction of the sample into the test cup. Do not cool bath liquid by direct contact with dry ice (solid carbon dioxide). Place the test cup in position in the bath. No t e 5: Precaution--Although ethylene glycol is considered low in oral toxicity, nonirritating to the skin, and appears to be no respiratory hazard during normal handling, caution should be exercised when using - TABLE 1 Thermometers For Tests Use ASTM Thermometer* Below 40F (4C> 57F or 57C At 40 to 120F {4 to 49C) 9F or 9C 57F or 57C Above 120F (49C) 9F or 9C A Complete specifications for these thermometers are given in Specification El. DUP050295680 D 56 ^operator must avoid oral ingestion of the liquid, inhalation of Quantities of vapors, and contact of the liquid with the eyes or areas of the skin. 6__ Due to possible difficulty in maintaining the prescribed perature rise and due to the formation of ice on the lid, results method for samples having flash points below 32F (0C) may be at unreliable. Trouble due to ice formation on the slide may be by carefully lubricating the slide shutter with high-vacuuin lubricant. fusing a graduate and taking care to avoid wetting the ove the final liquid level, measure 50 + 0.5 mL of the e into the cup, both the sample and graduate being led, if necessary, so that the sample temperature at the f measurement will be 80 10F (27> 5C) or at least i(ll*C) below the expected flash point, whichever is It is essential that the sample temperature be mainat least 20F (1TC) below the expected flash point the transfers from the sample container to the ate and from the graduate to the test cup. Destroy air lies on the surface of the sample. Wipe the inside of the with a clean cloth or absorbent tissue paper; then ;jh the lid, with the thermometer in place, to the bath r. 1 Light the test flame, adjusting it to the size ofthe small on the cover. Operate the mechanism on the cover in a manner as to introduce the test flame into the vapor ; of the cup, and immediately bring it up again. The consumed for the full operation shall be about 1 s, or time required to pronounce distinctly the words usand and one." Avoid any jerkiness in the operation of ressing and raising the test flame. ;4 Flash Points Below 140F (60C )--When the flash t of the sample is known to be below 140F (60C), apply adjust the heat so that the temperature of the portion rise at a rate of 2F (lC)/min 6 s. When the perature of the portion in the test cup is 10F (5C) below ^expected flash point, apply the test flame in the manner described in 9.3, and repeat the application of the test e after each IT (0.5C) rise in temperature of the rtion. .5 Flash Points at or Above 140F (60C )--If the flash lint of the sample is known to be MOT (60C) or higher, iply and adjust the heat so that the temperature of the rtion will rise at a rate of 5F (3C)/min + 6 s. When the fnperature ofthe portion in the test cup is 10T (5C) below expected flash point, apply the test flame in the manner Iscribed in 9.3 and repeat the application of the test flame ch 2F (TC) rise in temperature of the portion, at each Imperature reading that is a multiple of 2T (PC). >9.6 When the test flame application causes a distinct flash i the interior ofthe cup, observe and record the temperature of the portion as the flash point. Do not confuse the true lash with the bluish halo which sometimes surrounds the st flame during applications immediately preceding the iafetual flash. 9.7 Discontinue the test and remove the source of heat. Lift the lid and wipe the thermometer bulb. Remove the sample cup, empty, and wipe dry. 9.8 If, at any time between the first introduction of the test flame and the observation of the flash point, the rise in temperature of the portion is not within the specified rate or if the actual flash point differs from the expected flash point by an amount greater than 4T (2C), discard the result and repeat the test, adjusting the source of heat to secure the proper rate of temperature rise, or using a modified "ex pected flash point," or both, as required. No t e 7--Never make a repeat test on the same portion of sample; always take a fresh portion of sample for each test. 10. Correction for Barometric Pressure 10.1 Observe and record the ambient barometric pressure (Note 8) at the time of the test. When the pressure differs from 760 mm Hg (101.3 kPa), correct the flash point as follows: (A) Corrected flash point = C + 0.25 (101.3 -- p) (B) Corrected flash point <= F + 0.06 (760 -- P) (Q Corrected flash point = C + 0.033 (760 -- P) where: F = observed flash point, T, C = observed flash point, C, P = ambient barometric pressure, mm Hg, and p = ambient barometric pressure, kPa. No t e 8--The barometric pressure used in this calculation must be the ambient pressure for the laboratory at the time oftest. Many aneroid barometers, such as those used at weather stations and airports, are precorrected to give sea level readings; these must not be used. 10.2 Record the corrected flash point to the nearest 1F (or 0.5C). 11. Precision and Bias8 11.1 Precision--The following criteria should be used for judging the acceptability of results (95 % probability): 11.1.1 Repeatability--The difference between successive test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty: Flash Point, F (*C) Below 140 (60) , 140 (60) to 199(93) Repeatability, "F ("C) 2(1.1) 3 (1.7) 11.1.2 Reproducibility--The difference between two single and independent results, obtained by different opera tors working in different laboratories on identical test mate rial, would in the long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty: Flash Point, "F CC) Below 55 (13) 55 (13) to 139(59) 140 (60) to 199(93) Reproducibility, "F CC) 6(3.3) 4(2.2) 6 (3.3) 11.2 Bias--The procedure in Test Method D 56 for measuring flash point can be defined only in terms of a test method. 8 Supporting data are available from ASTM Headquarters. Request RR: D2-1003. 13 DUP050295681 D 56 ANNEXES (Mandatory Information) Al. APPARATUS A1.1 The Tag closed tester shall consist of the test cup, lid with test flame, and liquid bath conforming to the following requirements: Al.1.1 Test Cup, of brass or other nonrusting metal of equivalent heat conductivity, conforming to dimensional requirements prescribed in Table Al.l. It shall weigh 68 1 gA 1.1.2 Lid: A 1.1.2.1 The lid comprises a circle of nonrusting metal with a rim projecting downward about 5/s in. (15.9 mm), a slide shutter, a device which simultaneously opens the shutter and depresses the tip of the tube which carries fuel through to the test flame, and a slanting collar in which the cup-thermometer ferrule is inserted. Figure Al.l gives a diagram of the upper surface of the lid, showing dimensions and positions of the three holes opened and closed by the shutter, and the size and position of the opening for the cup thermometer. A l. 1.2.2 The rim shall fit the collar of the liquid bath with a clearance not exceeding 0.002 in. (0.05 mm) and shall be slotted in such a manner as to press the lid firmly down on the top of the cup when the latter is in place in the bath. When this requirement is not met, the vertical position of the cup in the bath shall be suitably adjusted, as by placing a thin ring of metal under the flange of the cup. A1.1.2.3 The shutter shall be ofsuch size and shape that it covers the three openings in the lid when in the closed position and uncovers them completely when in the open position. The nozzle of the flame-exposure device shall conform to the dimensions given in Table Al.l. The device shall be designed and constructed so that opening the shutter depresses the tip to a point approximately 0.08 in. (2 mm) to the right of the horizontal center of the middle opening of the lid (Refer to lower part of Fig. A 1.2). This will bring the test flame to the approximate center of the opening. The plane of the underside of the lid shall be between the top and bottom of the opening in the tip ofthe flame-exposure device TABLE Al.l Dimensional Requirements Depth of bath liquid surface below top of test cup Depth of sample surface below top of test cup Depth of bottom of bulb of test thermometer below top of cup when in place Inside diameter of test cup at top Diameter of bead on top of cover Diameter of opening in tip of test flame nozzle Outside diameter of tip of test flame nozzle 1.094 0.016 in. (27.8 + 0.4 mm) 1.156 + 0.031 in. (29.4 + 0.8 mm) 1.77 0.03 in. (45.0 0.8 mm) 2.125 0.005 in. (54.0 + 0.1 mm) 0.156 0.031 in. (4.0 0.8 mm) 0.049 0.010 in. (1.2 0.3 mm) 0.079 in. max (2.0 mm max) A 0.281" B 0.188" C 0.594" D 0.469" E 0.406" Note' All dimensions 10.005 unless otherwise shown. v-- 0.8lt1-- TOP OF LID SHOWING POSITION AND DIMENSIONS OF OPENINGS in. 0.001 0.005 0.188 0.281 0.387 Metric Equivalents mm 0.03 0.13 4.78 7.15 9.84 in. 0.406 0.469 0.594 0.71 0.81 mm 10.32 11.92 15.10 18.0 20.6 No t e--Dimensions relating to the size and position of the thermometer collar are recommended but not mandatory. FIG. Al.l Top of Lid Showing Position and Dimensions of Openings when the latter is fully depressed. A 1.1.2.4 The collar for the cup-thermometer ferrule shall be set at an angle which permits placement of the thermom eter with its bulb approximately in the horizontal center of the cup, at a depth prescribed in Table Al.l. A 1.1.3 Liquid Bath, conforming to the limiting or min imum dimensions shown in Fig. A1.2. It shall be of brass, copper, or other noncorroding metal of substantial construc tion. Sheet metal of about No. 20 B & S gage (0.812 mm) is satisfactory. It may, if desired, be lagged with heat-insulating material to facilitate control of temperature. A 1.1.4 Heater, of any type (electric, gas, alcohol, etc.) capable of controlling temperature as required in Section 8. An external electric heater, controlled by a variable voltage transformer, is recommended-. 14 DUP050295682 # D56 in. 3.76 mm 6.4 62.6 95.3 m FIG. A1.2 Section of Liquid Bath and Cup f Al.1.5 Bath Stand--For electric heating, any type of as illustrated in Fig. 1, to protect the flame from air currents gf stand may be used. For alcohol lamp or gas burner, a stand, (unless tests can be made in a draft-free room) is required. A2. CHECKING CONDITION AND OPERATION OF TAG CLOSED TESTERS V2.1 Material jfr A2.1.1 p-Xylene,9 conforming to the following requiregjjLments: |p Specific gravity (60/60F) (15.6/15.6C), 0.860 min, 0.866 max. Soiling range.... 2C niax from start to dry point, when I tested by Test Method D 850 or Test Method D 1078. The 9 Available as Flash Point Check Fluid (p-xylene) from Special Products Div., Phillips Petroleum Co., Drawer O, Borger, TX 79007. range shall include the boiling point of pure p-xylene, which is 281F (138.4C). Freezing point......... 52.2F (11.23'C), min (95 % molal pu rity) as determined by Method D 1015. A2.2 Procedure A2.2.1 Determine the flash point of the p-xylene, fol lowing the directions in Sections 6 to 9. When the tester is operating properly, a value of 81 1F (27.2 0.6C) will be obtained. 15 DUP0502 95683 7 D56 A2.2.2 When the flash point obtained on ^-xylene is not within the limits stated in A2.2.1, check the condition and operation of the apparatus to ensure conformity with the details listed in Annex Al, especially with regard to tightness of the lid (A 1.1.2.2), the action of the shutter and the position of the test flame (A 1.1.2.3), and the angle and position of the thermometer (A 1.1.2.4). After adjustment, when necessary, repeat the test, with special attention to procedural details prescribed in Section 8. A3. MANUFACTURING STANDARDIZATION A3.1 The cup thermometer, which conforms also to the specifications for the low-range thermometer used in the Pensky-Martens flash tester, Method D93, is frequently supplied by the thermometer manufactufer with a metal or polytetrafluoroethylene ferrule intended to fit the collar on the lid of the flash tester. This ferrule is frequently supple mented by an adapter which is used in the larger-diameter collar of the Pensky-Martens apparatus. Differences in di mensions of these collars, which are immaterial in their effect on the result of tests, are a source of considerable unnecessary trouble to manufacturers and suppliers of in struments, as well as to users. A3.2 Subcommittee 21 on Metalware Laboratory Appa ratus, of ASTM Committee E-l on Methods ofTesting, has studied this problem and has established some dimensional requirements which are shown, suitably identified, in Figs. Al.l, A3.1, and A3.2. Conformity to these requirements is not mandatory but is desirable to users as well as suppliers of Tag closed testers. in. 0.002 0.21 0,28 0.05 5.3 7.1 0.34 0.385 0.68 mm 8.6 9.8 17.3 FIG. A3.1 Dimensions for Thermometer Ferrule (Not Mandatory) in. mm 1.5 7.23 8.40 FIG. A3.2 Dimensions for Thermometer Packing Ring (Not Mandatory) The American Society for Testing anti Materials Jakes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 Race St., Philadelphia, PA 19103. 16 DUP050295684 Designation: D 86 - 901 Standard Test Method for Distillation of Petroleum Products1 This standard is issued under the fixed designation D 86; 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 approved for use by agencies ofthe Department of Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. *'No t e--Paragraph 11,4.6 was corrected editorially in October 1991. ----------------------------------------------------------------------------------------------------~1------------------------------------------------ Scope |; 1.1 This test method covers the distillation of natural olines, motor gasolines, aviation gasolines, aviation tur- |me fuels, special boiling point spirits, naphthas, white spirit, srosines, gas oils, distillate fuel oils, and similar petroleum ducts, utilizing either manual or automated equipment. 1.2 In cases of dispute, the referee test method is the aual test method prepared as directed for the indicated 3UPI;11.3 The values stated in SI units are to be regarded as the adard. The values given in parentheses are provided for , formation purposes only. If 1.4 This standard does not purport to address the safety Iroblems associated with its use. It is the responsibility ofthe Her of this standard to establish appropriate safety and faith practices and determine the applicability ofregulatory mtations prior to use. Referenced Documents 2.1 ASTM Standards: D323 Test Method for Vapor Pressure of Petroleum Products (Reid Method)2 D396 Specification for Fuel Oils2 D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D975 Specification for Diesel Fuel Oils2 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D 2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)4 D4057 Practice for Manual Sampling of Petroleum and Petroleum Products5 D4177 Test Method for Automatic Sampling of Petro leum and Petroleum Products5 E 1 Specification for ASTM Thermometers3 1 This test method is under the jurisdiction of ASTM Committee D-2 on JjPetroleum Products and Lubricants and is the direct responsibility of Subcom mittee D02.08 on Volatility. In the IP, this test method is under the jurisdiction of the Standardization ..Committee. P Current edition approved Sept 28, 1990. Published November 1990. Originally |[published as D 86 - 21. Last previous edition D 86 - 82. 1 Annual Book ofASTM Standards, Vol 05.01. 5 Annual Book ofASTM' Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 05.02. s Annual Book ofASTM Standards, Vol 05.03. E 77 Test Methods of Verification and Calibration of Liquid-in-Glass Thermometers6 E 133 Specification for Distillation Equipment5 E 220 Method for Calibration of Thermocouples by Com parison Techniques6 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 decomposition point--the thermometer reading that coincides with the first indications of thermal decomposition of the liquid in the flask. 3.1.1.1 Discussion--Characteristic indications of thermal decomposition are an evolution of fumes, and erratic ther mometer readings that usually decrease after any attempt is made to adjust the heat. 3.1.2 dry point--the thermometer reading that is observed at the instant the last drop of liquid evaporates from the lowest point in the flask. Any drops or film of liquid on the side of the flask or on the thermometer are disregarded. 3.1.2.1 Discussion--The end point (final boiling point), rather than the dry point, is intended for general use. The dry point can be reported in connection with special purpose naphthas, such as those used in the paint industry. Also, it is substituted for the end point (final boiling point) whenever the sample is of such a nature that the precision of the end point (final boiling point) cannot consistently meet the requirements given in the Precision Section. 3.1.3 end point or final boiling point--the maximum thermometer reading obtained during the test. This usually occurs after the evaporation of all liquid from the bottom of the flask. The term maximum temperature is a frequently used synonym. 3.1.4 initial boiling point--the thermometer reading that is observed at the instant that the first drop of condensate falls from the lower end of the condenser tube. 3.1.5 percent evaporated--the sum of the percent recov ered and the percent loss. 3.1.6 percent loss--one hundred minus the percent total recovery. 3.1.7 percent recovered--the volume in millilitres of con densate observed in the receiving graduate, in connection with a simultaneous thermometer reading. 3.1.8 percent recovery--the maximum percent recovered, 6 Annua! Book ofASTM Standards, Vol 14.03. 17 DU P0502 95685 # D 86 as observed in accordance with 9.10. 3.1.9 percent residue--the volume of residue in millilitres measured in accordance with 9.11. 3.1.10 percent total recovery--the combined percent re covery and residue in the flask, as determined in accordance with 9.12. 3.1.11 thermometer reading--the temperature of the sat urated vapor measured in the neck of the flask below the vapor tube. 4. Summary of Test Method 4.1 A 100 mL sample is distilled under prescribed condi tions that are appropriate to its nature. Systematic observa tions of thermometer readings and volumes of condensate are made, and from these data, the results of the test are calculated and reported. 5. Significance and Use 5.1 The distillation (volatility) characteristics of hydrocar bons often have an important effect on their safety and performance, especially in the case of fuels and solvents. Volatility is the major determinant of the tendency of a hydrocarbon to produce potentially explosive vapors. It is also critically important for both automotive and. aviation gasolines, affecting starting, warmup, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits. 5.2 Volatility, as it affects rate of evaporation, is also an important factor in the application of many solvents, partic ularly those used in paints. 5.3 Petroleum product specifications generally include distillation limits to assure products of suitable volatility performance. 6. Apparatus 6.1 All of the section and figure reference numbers in 6.2 through 6.8 refer to Specification E 133, the specification to which all the items listed shall conform. 6.2 Flask--Flask A (100 mL), as shown in Fig. 3 (of Specification E 133) for natural gasolines. Flask B (125 mL), as shown, in Fig. 3 (of Specification E 133) for all others. 6.3 Condenser and.Cooling Bath--Section 5, and Figs. 1 and 2 of Specification E 133. 6.4 Shield--Section 6, and Figs. 1 and 2 of Specification E 133. 6.5 Heater--Section 7, and Figs. 1 and 2 of Specification E 133. 6.6 Flask Support--Table 2 (of Specification E 133), Boards A 32-mm (1.25-in.) B 38-mm (1.5-in.) or C 50-mm (2-in.) hole. 6.7 Graduated Cylinder--Section 9; Graduate B, 100 mL, as shown in Fig. 4 of Specification E 133. The cylinder must have graduations at the 5 mL level and from 90 to 100 mL in 1-mL increments. For automatic apparatus, the cylinder shall conform to the physical specifications described in this section, with the exception of the graduations. 6.7.1 For automatic apparatus, the level follower/ recording mechanism of the apparatus will have a resolution of 0.1 mL with an accuracy of 1 mL. The calibration of the assembly should be confirmed according to manufacturer's instructions at regular intervals. The typical calibration procedure involves verifying the output with the receiver containing 5 and 100 mL of material respectively. 6.8 Temperature Smsw--Section 10 of Specification E 133, ASTM Thermometers 7C (7F) and 8C (8F) or IP Thermometers 5C (low distillation) and 6C (high distillation) conforming to the IP Specifications for Standard Thermom eters. Under certain test conditions the bulb of'the thermom eter can be 28C (50F) above the temperature indicated, and at an indicated temperature of 37 TC (700F) |he tempera ture of the bulb is approaching a critical rangem the glass. Thermometers that have been exposed to such conditions are not to be reused without checking their ice point, to verify calibration as prescribed in Specification E 1 and Test Method E 77. 6.8.1 Temperature measurement systems using thermo couples or resistance thermometers must exhibit the same temperature lag and accuracy as the equivalent mercury in glass thermometer. Confirmation of the calibration of these temperature sensors is to be made on a regular basis. This can be accomplished as described in Method E220, potentiometrically by the use of standard precision resis tance, depending on the type of probe. Another technique is to distill pure toluene in accordance with Test Method D 850 and compare the temperature indicated with that shown by the above mentioned mercury in glass thermometers when carrying out a manual test under the same conditions. No t e 1--Toluene is shown in reference manuals as boiling at 110.6C under the conditions ofTest Method D 1078 that uses a partial immersion thermometer. Because this test method uses total immersion thermometers the results will be lower and different with each. The approximate figures are Thermometer 7C (7F) or IP SC at 109C (228'F), and Thermometer 8C (8F) or IP 6C at 100"C (230oF). 7. Sampling 7.1 Determine the GROUP characteristics that corre spond to the sample to be tested (see Table 1). Where the procedure is dependent upon the group the section headings will be so marked. 7.2 Sampling shall be done in accordance with Practice D 4057 or Test Method D 4177 and as described in Table 2. 7.2.1 GROUP 0--Collect the sample in a bottle previ ously cooled to 0 to 4.5C (32 to 40F) preferably by immersing the bottle in the liquid, where possible, and discarding the first sample. Where immersion is not possible, the sample shall be drawn off into the previously cooled bottle in such a manner that agitation is kept at a minimum. Close the bottle immediately with a tight-fitting stopper and place the sample in an ice bath or refrigerator to maintain the sample at that temperature. 7.2.2 GROUPS 1 and 2--Collect and maintain the sample as described in 7.2.1 at a temperature of 0 to 10C (32 to 50F). 7.2.3 GROUPS 3 and 4--Maintain the sample at am bient temperature. If sample is not fluid at ambient temper ature, it is to be maintained at a temperature of 11C (20F) above its pour point. 7.3 Samples of materials that visibly contain water are not suitable for testing. 7.3.1 GROUPS 0, 1, and 2--If the sample is not dry, 18 DUP050295686 actertstics: sure at 37,aC, kPa 100F, psi pathod D 323 IP 69 or IP 171) illation, IPB C F EP'C F m D 86 TABLE 1 Group Characteristics Group 0 Group 1 Group 2 Natural Gasoline a 65.5 2:9.5 <65.5 <9.5 250 482 250 482 Group 3 <65,5 <9.5 <100 212 >250 >482 Group 4 <65.5 < 93 >100 >212 >250 >482 jjafrature of Sample Bottle: C - F |$j&!ture of Stored Sample: C Bp. F Rile is wet: SH" ; is*'' : jfer-- Hi Distillation Thermometer Biillation Thermometer llsiipport ffijeter of hole, mm (In.) gfferature at startof Test: Task and thermometer, C 1' F Sask support and shield Graduate and 100 mL charge, C I, . F Group 0 0 to 4.5 32 to 40 : 0 to 4.5 32 to 40 Resample TABLE 2 Sampling Group 1 OtolQ 32 to 50 Oto 10 32 to 50 Resample Group 2 t: 0 to to 32 to 50 Resample Group 3 Group 4 Ambient Ambient 11"C above pour point Ambient Ambient 20F above pour point Dry in accordance Dry in Accordance with 7.3.2 with 7.32 TABLE 3 Group 0 100 7C(7F) 5C A 32(1.25) Preparation of Apparatus Group 1 Group 2 126 70 (7F) 5C B 38 (1.5) 125 7C(7F) 5C B 38(1.5) 0 to 4.5 32 to 40 Not above ambient 0 to 4.5 32 to 40 .. 13 to 18 55 to 65 Not above ambient 13 to 18 5510 65 13 to 18 55 to 65 Not above ambient 13 to 18 55 to 65 Group 3 125 7C(7F) 5C C 50 (2.0) 13 to 18 55 to 65 Not above ambient 13 to 18 55 to 65 Group 4 125 8C (8F) 6C C 50 (2.6) Not above ambient 13 to ambient 55 to ambient ain another sample that is free from suspended water for itest. *|7.3.2 GROUPS 3 and 4--In cases where a water free hple is not practical, the suspended water can be removed * shaking the sample with anhydrous sodium sulfate or her suitable drying agent and separating it from the drying pfent by decanting. p. Preparation of Apparatus 8.1 Refer to Table 3 and prepare the apparatus as directed lifor the indicated group. Bring the temperature of the Igraduate, the flask, the temperature sensor, and the cooling [ bath to the indicated temperature. 8.2 Make any necessary provisions so that the tempera ture of the cooling bath and the graduate will be maintained at their respective temperatures. The cooling bath must have a liquid level above the- highest point of the condenser. If necessary, make suitable provision for circulation, stirring, or air blowing to provide a uniform temperature throughout the bath. The graduate must be in a bath such that either the liquid level is at least as high as the 100 mL mark, or the entire graduate is surrounded by an air circulation chamber. 8.2.1 GROUPS 0, 1, 2, and 3--Suitable media for low temperature baths include chopped ice and water, refriger ated brine, and refrigerated ethylene glycol. 8.2.2 GROUP 4--Suitable media for ambient and higher bath temperatures can include cold water, hot water, or heated ethylene glycol. 8.3 Remove any residual liquid in condenser tube by swabbing with a piece of soft, lint-free cloth attached to a cord or copper wire. 8.4 GROUPS 0,1, 2, and 3--Fit a thermometer 7C (7F), provided with a snug-fitting, well-rolled cork or siliconerubber stopper, tightly into the neck of the sample container and bring the temperature of the sample to the temperature indicated in Table 3. - 8.5 Measure 100 mL of sample in the graduate and transfer as completely as practical the contents of the graduate to the .distillation flask, taking care that none of the liquid flows into the vapor tube. 8.6 Fit the temperature sensor, provided with a snugfitting, well-rolled cork or silicone-rubber stopper, tightly into the neck of the flask. In the case of a thermometer, the bulb is centered in the neck and the lower end of the capillary is level with the highest point on the bottom of the inner wall of the vapor tube (see Fig. 1). Iii the case of thermocouple/resistance thermometer, follow the manufac turer's instructions as to placement. 8.7 Fit the flask vapor tube, provided with a snug-fitting, well-rolled cork or silicone rubber stopper, tightly into the condenser tube. Adjust the flask in a vertical position and so that the vapor tube extends into the condenser tube for a distance of 25 to 50 mm (1 to 2 in). Raise and adjust the 19 DUP050295687 D 86 FIG. 1 Position of Thermometer in Distillation Flask flask support board to fit snugly against the bottom of the flask. 8.8 Place the graduate that was used to measure the charge, without drying, into its bath under the lower end of the condenser tube so that the end of the condenser tube is centered in the graduate and extends therein for a distance of at least 25 mm {1 in), but not below the 100-mL mark. Cover the graduate closely with a piece of blotting paper, or similar material, that has been cut to fit the condenser tube snugly. 8.9 Record the room temperature and prevailing baro metric pressure. Proceed at once with the distillation, as given in the Procedure Section. 9. Procedure 9.1 Apply heat to the distillation flask and contents. The heating at this stage must be so regulated that the time interval between the first application of heat and the initial boiling point is as indicated in Table 4. 9.2 Observe and record the initial boiling point. If a receiver deflector is not being used, immediately move the graduate so that the tip of the condenser touches its inner wall. 9.3 Regulate the heating so that the time from initial boiling point to 5 or 10 % recovered is as indicated in Table 4. u. 9.4 Continue to regulate tjje heating so that the uniform average rate of condensation from 5 or 10 % recovered to 5 mL residue in the flask is 4 to 5 mL per min. 9.5 Repeat any distillation that did not meet the foregoing conditions. 9;6 If a decomposition point is observed, discontinue the heating and proceed as directed in 9.10. 9.7 In the interval between the initial boiling point and the end of the distillation, observe and record data necessary for the calculation and reporting of the results of the test as required by the specification involved, or as previously established for the sample under test. These observed data can include thermometer readings at prescribed percentages recovered, or percentages recovered at prescribed thermom eter readings, or both. Record all volumes in the graduate to the nearest 0.5 or 0.1 mL, and all thermometer readings to the nearest 0.5'C (1.0F) or 0.1C (O.TF) as appropriate to the apparatus being used. 9.7.1 GROUP 0--In cases in which no specific data requirements have been indicated, record the initial boiling point, the end point (final boiling point) and thermometer readings at each 10 % multiple of volume recovered from 10 to 90, inclusive. 9.7.2 GROUP 1, 2, 3, and 4--In cases in which no specific data requirements have been indicated, record the initial boiling point, the end point (final boiling point) or dry point, or both, and thermometer readings at 5, 15, 85 and 95% recovered, and at each 10% multiple of volume recovered from 10 to 90, inclusive. 9.8 When the residual liquid in the flask is approximately 5 mL, make a final adjustment of the heat so that the time from the 5 mL of liquid residue in the flask to the end point (final boiling point) shall be within the limits prescribed in Table 4. If this condition is not satisfied, repeat the test, with appropriate modification of the final heat adjustment 9.9 Observe and record the end point (final boiling point) or dry point, or both, as required, and discontinue the heating. 9.10 While the condenser tube continues to drain into the TABLE 4 Conditions During Test Procedure Temperature of cooling bath'4. C F Temperature of bath around graduate. C op Time from first application of heat to initial boiling point minutes Time from initial boiling point to 5 56 recovered, seconds to 10 56 recovered, minutes Uniform average rate of condensation from 5 5! recovered to 5 mL residue in flask, mL/min Time recorded from 5 mL residue to end point, min Group 0 Oto 1 32 to 34 Oto 4 32 to 40 2 to 5 3 to 4 4 to 5 3 to 5 Group 1 Oto 1 32 to 34 13 to 18 55 to 65 5 to 10 60 to 75 4 to 5 3 to 5 Group 2 0 to 4 32 to 40 13 to 18 55 to 65 5 to 10 60 to 75 4 to 5 3 to 5 ' Group 3 0 to 4 32 to 40 13 to 18 55 to 65 5 to 10 4 to 5 . 5 max Group 4 Oto 60 32 to 140 3 5 of charge temperature 5 to 15 4 to 5 5 max A The proper condenser bath temperature will depend upon the wax content of the sample and of its distillation fractions. The minimum temperature that permits satisfactory operation shall be used. In general, a bath temperature in the 0 to 4C (32 to 40F) range is suitable for karosine and products meeting the specifications for Grade No. 1 fuel oil as prescribed In Specification D'396, and those meeting the specifications for Grade No. 1 -D diesel fuel oil as prescribed in Specification D 975. In some cases involving Grade No.2 fuel oil (see Specification D 396), Grade No. 2-D diesel fuel oil (see Specification D 975), gas oils and similar distillates, it may be necessary to hold the condenser bath temperature at some point in the 38 to 60C (100 to 140F) range, in order to avoid the condensation of solid waxy materials in the condenser tuba 20 DUP050295688 I D 86 .ate, observe the volume of condensate at I. min' vals until two successive observations agree. Md^sure .blume accurately, and record it, to the nearest 0/5 or as appropriate to the apparatus being used, as percent ry. If the distillation was previously, discontinued rihe conditions of a decomposition point, deduct the at recovery from 100, report this difference as percent 'ue and loss, and omit the procedure given in 9.11. . 1 After the flask has cooled, pour its contents into a 5 graduated cylinder, and with the flask suspended over 5 mL graduate, allow the flask to drain until no ciable increase in the volume of liquid in the 5 mL *te is observed. .U.l GROUP 0--Cool the graduate to 0 to 4.5C (32 to . Record the volume in the graduate, to the nearest 0.1 {as percent residue. 11.1 GROUPS 1, 2, 3, and 4--Record the volume in raduate, to the nearest 0.1 mL, as percent residue. f2 The sum of the percent recovery, (see 9.10) and the *int residue (see 9.11) is the percent total recovery, ct the percent total recovery from 100 to obtain the TABLE 5 Appraximata Thermometer Reading Corrections Temperature Range c Correction'1 per 1.3kPa (10 mm) Difference in Pressure c F 10 to 30 30 to 50 50 to 70 70 to 90 90 to 110 110 to 130 130 to 150 150 to 170 170to.190 190 to 210 210 to 230 230 to 250 250 to 270 270 to 290 290 to 310 310 to 330 330 to 350 350 to 370 370 to 390 390 to 410 50 to 86 66 to 122 122 to .158 158 to 194 194 to 230 230 to 266 266 to 302 302 to 338 338 to 374 374 to 410 410 to 446 446 to 482 482 to 518 518 to 554 554 to 590 590 to 626 626 to 662 662 to 698 698 to 734 734 to 770 0.35 0.38 0.40 0.42 0.45 0.47 0.50 0.52 0.54 0.57 0.59 0.62 0.64 0.66 0.69 0.71 0.74 0.76 0.78 0.81 0.63 0.68 0.72 0.76 0.81 0.85 0.90 0.94 0.99 1.03 1.06 1.12 1.15 1.19 1.24 1.28 , 1.33 1.37 1.40 1.46' A To be added when barometric pressure is below 101.3 kPa (760 mm Hg); to be subtracted when barometric pressure is above 101.3 kPa (760 mm Hg). . Calculations and Report Jl For each test, calculate and report whatever data are ed by the specification involved, or as previously tjHshed for the sample under test (see 9.7). Report all entages to the nearest 0.5 or 0.1, and all thermometer M'ngs to the nearest 0.5'C (l.QT) or 0.1C (0.1F) as opriate to the apparatus being used. Report the baroic pressure to the nearest 0.1 kPa (1 mm Hg). 3.2 GROUP 4--When ASTM Thermometer 8C (8F) or i Thermometer 6C is used in testing aviation turbine fiiels * similar products, pertinent thermometer readings can be red by the cork. To provide the desired data, a second filiation according to Group 3 may have to be performed. Such cases, reading from ASTM thermometer 7C (7F) or Thermometer SC can be reported in place ofthe obscured ,,TM Thermometer 8C (8F) or IP Thermometer 6C readings, and the test report shall so indicate. If, by agreement, the obscured readings are waived, the test report shall So indicate. 10.3 Thermometer readings shall be corrected.to 101.3 ipi (760 mm Hg) pressure except when product definitions, Ipepifications, or agreements between the purchaser and the er indicate, specifically, that such correction is not re quired or that correction shall be made to some other base sure. This report shall include the observed pressure and ll,shall state whether corrections have or have not been applied. When the report is based on thermometer readings orrected to 101.3 kPa (760 mm Hg), obtain the correction |(to be applied to each thermometer reading by means of the ydney Young equation as given in Eq. 1, or by the use of r-Table 5. For Celsius temperatures: Cc = 0.0009 (101.3 - Pfc)(273 + tc) (1) Ce - 0.00012 (760 - P)(273 + tc) (2) |For Fahrenheit temperatures: Cf= 0.00012 (760 - P)(460 + tf) .(3) (where: Cc and Cf = corrections to be added algebraically to the observed thermometer readings .or (0 respec tively,- ; Pk = barometric pressure, kPa, prevailing at the time and location of the test, and P = barometric pressure, mm Hg, prevailing at the time and location of the test, After applying the corrections and rounding each result to the nearest 0.5'C (1.0T) or O.TC (0.1-F) as appropriate to the apparatus being used, use the corrected thermometer reading^ in all further calculations and reporting. 10.4 After barometric corrections of the thermometer reading readings have been made, if required (see 10.3), the following data require no further calculation prior to re porting: initial boiling point, dry point, end point (final boiling point), decomposition point, and all pairs of corre sponding values involving percentages recovered and ther mometer readings. 10.5 When thermometer readings are corrected to 101.3 kPa (760 mm Hg) pressure, the actual loss shall be corrected to 101.3 kPa (760 mm Hg) pressure, according to the following equation: LC~AL + B (4) where: L = percent loss as calculated from test data, Lc -- corrected loss, and A and B = numerical constants. 10.5.1 The values of A and B that depend upon the prevailing barometric pressure are listed in Table 6. The following equation can be substituted: Le = {(, - 0.499287)/( 13.65651 - 0.12492914 Pk)} + 0.4997299 1 ' Lc = {(, - 0.499287)/( 13.65651 - 0.01665174 P)} + Q.4997299 w where: L - percent loss as calculated from test data, Lc = corrected loss, 21 DUP050295689 D 86 TABLE 6 Values of Constants A and B Used in Obtaining Corrected Distillation Loss Observed Barometric Pressure kPa mm Hg 74.6 76.0 77.3 78.8 80.0 81.3 82.6 84.0 85.3 86.6 88.0 89.3 90.6 92.0 93.3 94.6 96.0. 97.3 98.6 100.0 101.3 560 570 580 590 600 610 620 630 640 660 660 670 680 690 700 710 720 730 740 750 760 A 0.231 0.240 0.250 0.261 0.273 0.286 0.300 0.316 0.333 0.353 0.375 0.400. 0.426 0.461 0.500 0.545 0.600 0.667 0.750 0.857 1.000 B 0.384 0.380 0.375 0.369 0.363 0.357 0.350 0.342 0.333 0.323 0.312 0.300 0.286 0.269 0.250 0.227 0.200 0.166 0.125 0.071 0.000 Pk = pressure, kPa, and P = pressure, mm Hg. 10.5.2 The corresponding corrected percent recovery is calculated according to the following equation: RC = R + (L-LC) (7) where: L = observed loss, Lc -- corrected loss, R = observed recovery, and . Rc * corrected recovery. 10.5.3 When the thermometer readings have not.been corrected to 101.3 kPa (760 mm Hg) pressure, the percent residue and percent loss are to be reported as observed in accordance with 9.11, and 9.12 respectively. 10.5.4 When reporting data, state whether the corrections have or have not been applied. 10.5.5 The corrected loss shall not be used in the calcula tion of percentages evaporated. 10.6 It is advisable to base the report on relationships between thermometer readings and percentages evaporated in any. case in which the sample is a gasoline, or any other product classed under GROUP 1, or in which the percent loss is greater than 2.0. Otherwise, the report can be based on relationships between thermometer readings and percentages evaporated or recovered. Every report must indicate clearly which basis has been used. 10.7 To report percentages evaporated at prescribed ther mometer readings, add the percent observed loss to each of the observed percentages recovered at the prescribed ther mometer readings, and report these results as the respective percentages evaporated, that is: Pe -- Pr + L (8) where: L = observed loss, Pe = percentage evaporated, and Pr = percentage recovered. 10.8 To report thermometer readings at prescribed per centages evaporated, use either of the two following proce dures, and indicate on the report whether the graphical procedure or the arithmetical procedure has been used. 10.8.1 Arithmetical Procedure--Deduct the observed dis tillation loss from each prescribed percentage evaporated in order to obtain the corresponding percentage recovered. Calculate each required thermometer reading as follows: T-T , {Th ~Tl ){R-Rl) L Rh -Rl (9) where: R = percent recovered corresponding to the prescribed percent evaporated, Rh - percent recovered adjacent to, and higher than R, Rl -- percent recovered adjacent to, and lower than R, T = thermometer reading at the prescribed percent evap- orated. Tu -- thermometer reading recorded at RH and Tl = thermometer reading recorded at Rz- , Values obtained by the arithmetical procedure are affected > by the extent to which the distillation graphs are nonlinear. Intervals between successive data points can, at any stage of' the test, be no wider than the intervals indicated in 9.7. In no, case shall a calculation be made that involves extrapolation. 10.8.2 Graphical Procedure--Using graph paper with uni form subdivisions, plot each thermometer reading corrected for barometric pressure, if required (see 10.3), against its corresponding percent recovered. Plot the initial boiling point at 0 % recovered. Draw a smooth curve connecting the points. For each prescribed percent evaporated, deduct the distillation loss, in order to obtain the corresponding percent ,, ! recovered, and take from the graph the thermometer reading, : which this percent recovered indicates. Values obtained by` : graphical interpolation procedures are affected by the care - with which the plot is made. i No t e 2--See Appendix X1 for numerical examples illustrating these t arithmetical procedures. "* t 11. Precision and Bias ' 11.1 The precision of this test method as determined by the statistical examination of interlaboratory test results is described below. Table Al. 1 lists which tables and figures are to be used for the different fuel groups, distillation methods, and temperature scales. 11.2 Repeatability: 11.2.1 GROUP 0--With proper care and strict attention to details, duplicate results obtained for endpoint should not differ from each other by more than 3.5C (6F). Differences in duplicate temperature readings for each prescribed per centage point should not exceed the amounts equivalent to 2 mL of distillate at each point in question. 11.2.2 GROUP 1--The difference between successive 5 J 1 * TABLE 7 Repeatability and Reproducibility for Group 1 (Manual) Evaporated Point Repeatability4 C CF ReproducibiSty''' C F IBP 5% 10 to 80% 90% 95% FBP ' 3.3 r0 + 0.66 r0 r0 ro 3.9 6 r0 + 1.2 ro r0 ro 7 5.6 ft0 + 1.11 R0 - 1.22 Ro ~ 0.94 7.2 10 R0 + 2.0 *0 Ro - 2-2 Ro- 1.7 13 A Read r,, and R0 from the graph In either Fig. 2 (C) or Fig. 3 (F). 22 DU P050295690 D 86 s No t e-- r0 = 0.864 (*C/V 96) + 1.214 B0 -1.736 (C/V 96) + 1.994 (14) (15) FIG. 2 GROUP 1--Repeatability, r, and Reproducibility, fl07 SJO 2J5 "C/VJi no t e- r0 = 0.673 (G/V %) + 1.131 R0 = 1.998 (C/V %) + 2.617 (18) (19) FiG. 4 GROUP t--Repeatability, r0 and Reproducibility, fl08 Ifere-- ' FIG. 3 r0 -- 0.864 (F/V 56) + 2.186 (16) = 1.736 (F/V%) +3.589 (17) GROUP 1--Repeatability, r,, and Reproducibility, f?07 TABLE 8 Repeatability and Reproducibility for Group 1 (Automatic) {Evaporated Point f IBP 5% 10% 20% 30 to 70% 60% 90% 95% FBP Repeatability* c F 3.9 r,, + 1-0 r0 + 0.56 To to ro r0 + 1-4 4.4 7 r0 + 1.8 r0 + 1-0 70 To To To r0 + 2.5 8 Reproducibility* "C "F 7.2 fli + 1.78 R0 + 0.72 R0 + 0.72 Ro R0 + 0.94 ft0+ 1.9 Bo 8.9 13 R0 + 3.2 R0 + 1.3 fl0 + 1.3 Ro Ro~ 1.7 Ro - 3.5 Bo 16 " Read r,, and R0 from the graph In either Fig. 4 (C) or Fig. 5 (F). i&Pj| results obtained by the same operator with the same appa ll ratus under constant operating conditions on identical test material would, in the long run, in the normal and correct |bperation of this test method, exceed the values indicated in ratable 7 (Manual) or Table 8 (Automatic) in one case in twenty. I 11.2.3 GROUPS 2, 3, and 4--The difference between 22 20 18 16 14 12 "Ro 10 8 6 4 2 0 45 F/V% No t e-- ro ` 0.673 (F/V 95) + 2.036 Bn- = 1.998 (^F/V 96) -1- 4.711 (20) (21) FIG. 5 GROUP 1--Repeatability, r,, and Reproducibility, f?0# successive results obtained by the same operator with the same apparatus under constant operating conditions on identical test materials would in the normal and correct operation of this test method, exceed the values indicated in Fig. 6 (Manual, C) or Fig. 7 (Manual, CF) or Table 9 (Automatic) in 1 case in 20.7 11.3 Reproducibility: 11.3.1 GROUP 1--The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would in the normal and correct operation of this test method, exceed the values indicated in Table 1 (Manual) or Table 8 (Auto matic) in one case in twenty,8 11.3.2 GROUPS 2,3, and 4--The difference between two single and independent results obtained by different opera tors working in different laboratories on identical test mate- 7 Test Method D 86 Manual Method North American and IP Labs. 8 Test Method D 86 Automatic Method North American and IP Labs. 23 DUP050295691 REPEATABILITY REPRODUCIBILITY # D 86 REPEATABILITY REPRODUCIBILITY No t e--I = initial boiling point, C, s end point (final boiling point) or dry point, C, r = thermometer reading at prescribed percent evaporated or recovered, C, and P = percent evaporated or recovered at prescribed thermometer reading, C. PIG. 6 Groups 2,3,4--Manual Method-Celsius Precision of Distillation Test Method D 86 - IP 123 I ETP IET P No t e --I = initial boiling point, F, E = end point (final boiling point) or dry point "F, T = thermometer reading at prescribed percent evaporated or recovered. F, and P = percent evaporated or recovered at prescribed thermometer reading, F. FIG. 7 Groups 2,3, 4--Manual Method-Fahrenheit Precision of Distillation Test Method D 86 - IP 123 rial would in the normal and correct operation of this test method, exceed the values indicated in Fig. 6 (Manual, C) or Fig. 7 (Manual, F) or Table 9 (Automatic) in only one case in twenty. 11.4 To facilitate the use of the tables and figures, the rate of change in thermometer readings in degrees Celsius (Fahrenheit) per the percentage recovered, at any point between the 10 and 90 % point, is assumed to be the same as the average rate between two data points that are equidistant above and below the point in question. The span from the point in question to either of the other data points does not represent more than 10 % recovered in any case, nor more than 5 % if the point in question is the 5 % point. Precision values for typical values of slope for GROUPS 2, 3, and 4 (Automatic) are given in Table 10. T1.4.1 The equations that folio# are used as guidelines in calculating C/V % (F/V %). In the event the distillation end point occurs prior to the 95 % poiht, then appropriate modifications to the use of these equations must be made. 11.4.2 Initial boiling point and end point do not require C/V% {F/V %). TABLE 9 Repeatability and Reproducibility for Groups 2, 3, and 4 (Automatic) % Collected Repeatability* C *F Reproducibility* c f IBP 2% 5% 1056 20 to 70 % 80% 90 to 95 % FBP 3.5 3.5 1.1 + 1.08 S 1.2 +1.42 S 1.2 + 1.42S 1.2 +1.42 S 1.1 + 1.08 S 3.5 6.3 6.3 2.0 + 1.95 S 2.2 +2.25 S 2.2 + 2.55 S 2.2 + 2.55 S 2.0 + 1.95 S 6.3 8.5 2.6+ 1,92 S 2.0 + 2.53 S 3.0 +2.64 S 2.9 +3.97 S 3.0 + 2.64 S 2.0 + 2.53 S 10.5 15.3 4.7 + 3.45 S 3.6 + 4.55 S 5.4 +4.75 S 5.2 + 7.15 S 5.4 + 4.75 S 3.6 + 4.55 S 19.0 * S is the average slope calculated in accordance with 11.4. 11.4.3 5 % recovered is calculated as follows: . C/V%, F/V% = 0.1(7,0 - Tmp) (10 11.4.4 10 to 80 % recovered is calculated as follows: c/v%, F/v% = 0.05(r(r+1O) - v_10)) (11 11.4.5 90 % recovered is calculated as follows: c/v%, F/V% = O.i<r9o - r80) <12 24 DUP050295692 'i.4.6 95 % recovered is calculated as follows: c/v%, f /v '% = o,2(r95 - r90) (13) = rate of change in temperature at the volume percent in question, C, y- = rate of change in temperature, at-mfe volume percent in question, F, and = temperature at the percent volume recovered indicated by the subscript, C or 'F, fcripts: volume percent recovered in question, 10 = 10 % less than volume percent in question, 10 = 10 % more than volume percent in question, and 5, i0, 80, 90, 95 = appropriate volume percent indicated. .5 Bias: .5.1 Absolute Bias--Due to the use of total immersion ometers or temperature sensing systems designed to 'ate them, the distillation temperatures in this .test od are somewhat lower than the true temperature. The unt of absolute bias has not been determined. .5.2 Relative Bias--There exists a bias between the ical results of distillation properties obtained by this I method and the true boiling point distillation curve ned by Method D 2892. The amount of relative bias en the two test methods has not been determined. TABLE 10 Precision Values for Typical Values of Slope Groups 2, 3, and 4 (Automatic) % Collected Slope C/%V "F/S6V Repeatability C F Reproducibility C F 20 to 70 % 10 and 80 % ' : 5, 90. and 95 % 2% IBP FBP 0.5 1.0 1.5 2.0 2.5 0.5 1.0 1.5 2.0 2.5 1.0 2.0 3.0 4.0 2.0 3.0 4.0 5.0 0.9 1.5 2.7 4.5 8.1 1.8 2.5 4.5 6.5 11.7 2.7 3.0 5.4 8.5 15.3 3.6 4.0 7.2 10.5 18.9 4.5 4.5 8.1 12.5 22.5 0.9 1.5 2.7 4.0 7.2 1.8 - 2.5 4.5 5.5 9.9 2.7 3.0 5.4 7.0 12.6 3.6 4.0 7.2 8.0 14.4 4.5 4.5 8.1 9.5 17.1 1.8 2.0 3.6 4.5 8.1 3.6 3.0 5.4 7.0 12.6 5.4 4.0 7.2 9.5 17.1 7.2 5.0 9.0 12.0 21.6 3.6 3JS 6.3 6.0 10.8 5.4 3J5 6.3 8.0 14.4 7.2 3 6.3 10.0 18.0 9.0 3.5 6.3 12.0 25.6 3.5 6.3 8.5 15.5 3.5 6a 10.5 19.0 11.5.2.1 Groups 1, 2, 3, and 4--Refer to Tables A2.1 A2..2, and A2.3 ,for the statement of bias between automatic arid manual apparatus. 12. Keywords 12.1 Distillation; petroleum products; distillates. ANNEX (Mandatory Information) I* l! TABLE A1.1 Summary of Aids for Definition of Repeatability and Reproducibility Group Distillation Method Temperature Scale Table, Section, and Figure to Use 0 1 1 2,3,4 2,3,4 Manual or Automatic Manual Automatic Manual Automatic C or F C F C F C F C F 11.2.1 Table 7 and Fig. 2 Table 7 and Fig. 3 Table 8 and Fig. 4 Table 8 and Fig. 5 Fig. 6 Fig. 7 Tables 9 or 10 Tables 9 or 10 25 DUP050295693 TABLE A1.2 Condensed Summary of Comparative Manual and Automatic Distillation Results r- No t e--All thermometer readings were corrected to 101.3 kPa (760 mm Hg) pressure. The left-hand figures were manually obtained, and the right-hand figures represent corresponding results from the automatic apparatus. _____________ __________________________________________________________________________ __________________ Celsius \ Max Mm Average Max Min Average Gasoline--Twenty six laboratories and fourteen samples (see Table A1.3) Keroslne--Hght tests In four laboratories for manual, and six tests In three laboratories for automatic 176.5.174.5 193.5,193 215.5,215.5 248, 248.5 171.5,172 191, 190.5 213.5,214 245.5,246.5 174.5.173.5 191.5, 191.5 214.5,214.5 246, 247 Diesel Fuel--Ten tests in five laboratories for manual and for automatic 190.5,189 -215, 21B 268.5,269 322,323 179.5.179.5 208.5,208.5 264,264 318,316 185.5,184.4 213, 214 266,266 319.5,318.5 268,. 268.5 264, 265 265.5, 266.5 341.5,343 337, 338.5 340, 340,5 Fahrenheit Max Min Max Min Gasoline--Twenty six laboratories and fourteen samples (See Table A1.4) InitialBciling 10% 50% - 00% Point Evaporated Evaporated Evaporated Keioslne--Eight tests In tour laboratories for manual, and six tests in three laboratories for automatic 350, 346 380, 379 420, 420 478,479 341,342 376,375 416,417 474,476 346,344 377,377 418,418 475,477 Diesel Fuels Ten tests in five laboratories for manual and for automatic 375,372 419,424 515,516 612,613 355, 355 407, 407 507, 507'' 604, 801 366,364 415,417 511,511 607,605 End Point (Final Boiling Point) . 514,515 507,509 510, 512 647,649 639,641 644,645 . TABLE A1.3 Bids Between Methods (ADA-Manual) C (Based on Averages of ASTM and IP Date) Sample IBP 5% 10% 20% 30% 40% 50% 60% 70% 80%' 90% 95% FBP 1 +1.1 +1.9 +2.2 +1.6 +1.4 +0.7 +0.8 +0.7 +0.7 +0.1 +0.4 +0.7 -0.4 2 (+0.9) (0.0) +0.8 +0.5 +0.4 +0.8 +0.2 +0.1 +0.1 +0.4 (+4.7>*8 (+1.3)8 (-12) 3 +0.7 +1.4 +1.6 +1.0 +0.8 +0.6 +Q.3 +0.1 +0.2 +0.9 +0.5 +0.1 -0.8 4 +0.3 +0.6 +0.8 +0.8 +0.3 +0.7 +0.6 +0.8 +1.1 +1.2 +0.8 +0.5 -0.9 5 +0.5 +1.3 +1.3 +1.3 +1.2 +1.0 +0.9 +0.6 +0.8 +1.0 +0.4 +0.4 -0.9 6 +1.2 +12 +1.6 +1.2 +1.2 +1.1 +0.8 +1.1 +1.2 +0.2 -0.1 40.2 -0.3 7 + 0.3 +0.8 +0.8 +0.7 +0.8 +0.8 +1.0 +1.5 +1.6 +1.6 +1.5 +1.7 -0.7 8 +0.3 +0.5 +0.7 +0.6 +0.7 +1.2 +1.2 +1.1 +1.3 +1.9 +1.1 +1.2 --0.8 9 +1.7 +2.0 +1.8 +1.5 + 1.5 +1.5 +1.2 +0.9 +1.3 +0.6 -0.4 +0.4 -1.2 10 +1.5 +1.5 +1.2 *0.7 +0.4 +0.6 +0.9 +1.0 +1.4 +1.9 +0.9 +0.1 -2.1 11 +0.9 +1.1 +1.2 -0.8 +0.7 +0.6 + 1.1 +1.0 +0.4 +0.5 -0.4 +0.1 -0.8 12 +1.0 (+2.4)B +2.3 +1.2 +12 +12 -1.2 +0.9 +1.1 +0.2 -0.7 (-0.8)8 -0.9 13* +0.3 +0.3 +0.4 +0.3 +0.2 +0.9 +1.4 +1.0 +0.1 +1.1 +1.2 +1.0 -1.2 1-4* +0.5 +0.4 +0.7 +0.5 +0.8 +1.1 +1.7 +1.7 +1.0 +0.8 +0.3 0.0 -0.8 * Gasohols. 8 () Points not included in the precision analysis. Sample 1 2 3 4 5 6 7 8 9 10 11 12 13* 14* ( -3 TABLE A1.4 Bias Between Methods (ADA-Manual) F (Based on Averages of ASTM and IP Data) Sample 1 2 3 4 5 6 7 8 9 10 11 12 13* 14* IBP +1.9 (+1.B)8 +1.2 +0.5 +0.9 +2.1 +0.6 +0.6 +3.1 +2.7 +1.6 +1.8 +0.5 +0.9 5% +3.4 (0.0)8 +2.5 +1.1 +2.3 +2.2 +1.4 +0.9 +3.5 +2.7 +2.0 (+4.2)e +0.5 +0.7 10% +4.0 +1.5 +2.8 +1.5 +2.3 +2.8 +1.4 +1.3 +3.2 +2.1 +2.1 +4.1 +0.7 +1.2 20% +2.9 ` +0.9 +1.7 +1.4 +2.3 +2.2 +1.3 +1.0 +2.7 +1.2 +1.4 +2.1 +0.5 +0.9 30% +2.5 +0.7 +1.4 +0.6 +2.1 +2.1 +1.5 +1.2 +2,6 +0,8 +1,2 +2.2 +0.3 +1.4 40% +1.2 +1.1 +1.0 +1.2 +1.7 +2.0 +1.5 +2.1 +2.7 +1.0 +1.0 +2.1 +1.6 +2.0 50% +1.4 +0.4 +0.5 +1.1 +1.6 +1.4 +1.8 +2.1 +2.1 +1.6 +1.9 +2.1 +2.5 +3.0 60% +1.2 +0.2 +0.1 +1.4 +1.0 +2.0 +2.6 +2.0 +1.6 +1.7 +1.7 +1.6 +1.7 +3.0 70% +1.3 +0.1 +0.4 +1.9 +1.4 +2.1 +2.8 +2.4 +2.3 +2.5 +0.8 +1.9 +0.2 +1.8 80% +0.1 +0.7 +1.6 +2.1 +1.8 +0.4 +2.8 +3.4 +i.i +3.4 +0.9 +0.4 +2.0 +1.5 90% +0.8 (+8.4)s +0.9 +1.4 +0.7 -0.1 +2.6 +2.0 -0.7 +1.6 -0.7 -1.2 +2.1 +0.6 95% +1.2 (+2.3)8 +0.1 +0.9 +0.8 +0.4 +3.1 +2.1 +0.8 +0.2 +02 (--1-5) +1.8 0.0 FBP -0.7 (-2.2) -1.4 -1.7 -1.7 -0.5 -1.3 -1.4 -2.1 --3.8 -1.4 -1.7 -2.2 -1.4 * Gasohols. 8 () Points not included In the precision analysis. Sample 1 2 3 4 5 6 7 8 9 10 11 12 13s 14B 26 DUP050295694 D 86 APPENDIX (Nonmandatory Information) XI. EXAMPLES ILLUSTRATING CALCULATIONS FOR REPORTING OF DATA 1.1 Thermometer Readings Corrected to 101.3 kPa (760 Hg) Pressure: 1.1.1 Thermometer Readings Correction to 101.3 kPa 10.3): correction ("C) = 0.0009 (101.3 - 98.6) (273 + Q (Xl.l) correction (F) = 0.00012 (760 - 740) (460,+ tjj. (Xl.2) 1.1.2 Loss Correction to 101.3 kPa (see 10.5): corrected loss = (0.750 x 4.7) + 0.125 = 3.6. (X1.3) 1.1.3 Recovery Correction to 101.3 kPa (see 10.5.2): corrected recovery = 94.2 + (4.7 - 3.6) = 95.3. (XI.4) 1.2 Thermometer Readings at Prescribed Percentages porated: 1.2.1 Thermometer Reading at 10 % Evaporated (5.3 % vered) (see 10.8.1): C) = 33.5 + [(46.5 - 33.S)(5.3 - 5)/(15 - 5)] jr = 34.0'C (Xl,5) hoeCF) = 92 + [(116 - 92)(5.3 - 5)/(15 - 5)] - 93*F (X1.6) XI.2.2 Thermometer Reading at 50% Evaporated (45.3 % Recovered) (See 10.8.1): FjoiCC) - 94 + [(124 - 94X45.3 - 40)/(60 - 40)] = 102.0'C Ts0(F) = 201 + [(255 - 201X45.3 40)/(60 - 40)] = 2151? (XI.7) (X1.8) Xl.2.3 Thermometer Reading at 90 % Evaporated (85.3 % Recovered) (See 10.8.1): MC>= 181.5 . + [(216 - 181.5)(85.3 - 85)/(95.3 - 85)] = 182.5'C ( ) WT) = 359 + (421 - 359X85.3 - 85)/(95.3 - 85) ,V1 - 361"F XI.2.4 Thermometer Reading at 90 % Evaporated (85.3 % Recovered) Not Corrected to 101.3 kPa Pressure (See 10.8.1): TgofiC Q ~ 180.5 .y. ... + [(215 - 180.5X85.3 - 85)/(94.2 - 85)] = 18l.5"C l J rCF) = 357 + [(419 - 357X85.3 - 85)/(94.2 ~ 85)] ,Y1 = 359F TABLE X1.1 Thermometer Readings Corrected to 101.3 kPa (760 mm Hg) Pressure Barometric Pressure Observed 98.6 kPa (740 mm Hg) Corrected 101.3 kPa (760 mm Hg) c F c F Initial BoiBng Point 5 % recovered 10% recovered 15% recovered 20 % recovered 30 % recovered 40% recovered 50 % recovered 60 % recovered 70 % recovered 80% recovered 85% recovered 90 % recovered 95 % recovered End Point Recovery, % Residue, % Loss, % '25.5 33.0 39.5 46.0 ' 54.5 74.0 93.0 108.0 123.0 142.0 168.5 180.5, 200.4 215.0 94.2 1.1 4.7 78 91 103 . 115 130 165 199 226 . 253 288 332 357 392 419 .. 26.0 33.5 40.0 46.5 55.0 75.0 94.0 109.0 124.0 143.5 168.0 181.5 201 :o 216 95.3 1.1 3.6 79 92 104 116 131 167 201 228 255 290 334 359 394 421 The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved dr 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 oI 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. 27 DUP050295695 Designation: D 93 - 90*1 Designation: 34/85 An American National Standard British Standard 2839 American Association Stats Highway Transportation Standard AASHTO No. T73 - 811 ij :i i Standard Test Methods for Flash Point by Pensky-Martens Closed Tester1 This standard is issued under the fixed designation D 93; 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 reapprovai. A superscript epsilon (e) indicates an editorial change since the last revirion or reapproval. These test methods were adopted as a joint ASTM-IP Standard in 1967. These test methods have been adoptedfor use by government agencies to replace Method 1102 ofFederal Test Method Standard No. 79lb, and Method 4293 ofFederal Test Method Standard No. 141A. H No t e--Paragraph 13.1 was corrected editorially in October 1991. INTRODUCTION This flash point test method depends on definite rates of temperature increases to control the precision of the method. It is considered to be a non-equilibrium method. The rate of heating will riot give the precision expected in all cases because of the low thermal conductivity of some materials. To reduce-this effect, Test Method D 3941 was issued in which the heating rate is considered to be an equilibrium method. Due to the slower heating rate, the time required to make a determination is considerably longer. If your specification requires Test Method D 93, do not substitute Test Method D 3941 or any other method without obtaining comparative data and agreement from the specifier. I i 1. Scope 1.1 These test methods cover the determination of the flash point by Pensky-Martens closed-cup tester of fuel oils, lube oils, suspensions of solids, liquids that tend to form a surface film under test conditions, and other liquids of similar viscosities. No t e 1--This test method can be employed for the detection of contamination of lubricating oils by minor amounts of volatile mate rials. No t e 2--The U.S. Department of Transportation (DOT)2 and U.S. Department of Labor (OSHA) have established that liquids with a flash point under lOOT (37.8"C) are flammable as determined by methods for those liquids which have a viscosity of 5.8 cSt or more at 1G0"F (37.8'C) or 9.5 cSt or more at 77F (25C), or that contain suspended solids, or have a tendency to form a surface film while under test. Other classification flash points have been established by these departments for liquids using this test. These regulations are in degrees Fahrenheit. 1.2 Liquids having viscosities less than 5.5 cSt at 40C (104F) do not contain suspended solids or do not have a tendency to form a surface film while under test conditions \ can be tested in accordance with Test Method D 56. 1.3 The values stated in SI units shall be regarded as the standard. The values given in parentheses are for information only. . 1.4 This standard should be used to measure and describe j the properties of materials, products, or assemblies in re sponse to heat andflame under controlled laboratory condilions and should notbe used to describe or appraise thefire hazard orfire risk ofmaterials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a fire risk assessment which takes into account all ofthefactors which are pertinent to an assessment ofthefire hazard ofa particular end use. 1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. For specific hazards statements, see Section 7 and Note 5. 1 These test methods are under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and are the direct responsibility of Subcom mittee D02.08 on Volatility. In the IP, these methods are under the jurisdiction of the Standardization Committee. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as D 93 - 21 T. Last previous edition D 93 - 85. 2 For information concerning regulations of U.S. Department of Transporta tion, see Codes of U.S. Regulations 49 CFR, Chapter I, and of U.S. Department of Labor, see 29 CFR, Chapter XVII. Each ofthese items is revised annually and may be procured from Superintendent of Documents, Government Printing Office, Washington, DC 20402. 2. Referenced Documents 2.1 ASTM Standards: D56 Test Method for Flash Point by Tag Closed Tester3 D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials4 3 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 06.03. 28 DUP050295696 093 {] ! t ? lisCest Method for Freeang Biint of High-Purity rdcarbons3 ^ r Test Method for Purity of Hydrocarbons; from Points3 Test Method for Distillation Range of Volatile ,,'eLiquids4 Safest Method for Flash Point by the Equilibrium f|pd With a Closed Cup Apparatus4 ^jfractice for Manual Sampling of Petroluem and -leum Products5 r__Ecation for ASTM Thermometers6 ; ^Practice for Sampling Industrial Chemicals7 : I./: gfmjnology ' - . ' ; Ascription ofa Term Specific to This Standard: 'WLfldsh point--the lowest, temperature corrected to a pressure of 101.3 kPa (760 mm Hg), at which jlfn of a test flame causes the vapor of a specimen to piaer specified conditions of test _ Discussion--The sample is deemed to have " when a large flame appears and instantaneously s itself over the surface of the sample. ^Discussion--Occasionally, the appEcation of the he will cause a blue halo or an enlarged flame. This y. occurs near the actual flash point but in some ^especially with halogenated hydrocarbons and admix es, can occur at any temperature. These phenomena are Wfo fae considered true flash points. 6. Apparatus 6.1 Pensky-Martens Closed Flash Tester, as described in Annex Al. 6.2 Thermometers--Three standard thermometers shall be used with the ASTM Pensky-Martens tester as follows: 6.2.1 For tests in which the indicated reading falls within the limits of 10 to 60C (50 to 140F), inclusive, an ASTM 9C (9F) Pensky-Martens low range Thermometer having a range from --5 to +110C (20 to 230F) and conforming to the requirements of Specification E 1 shall be used. Equally acceptable is IP thermometer 15C (15F), with specifications as shown in Annexes A2 and A3. 6.2.2 For tests in which the indicated reading falls within the limits 60. to I40C (140 to 284F), inclusive, an ASTM 88C (88F) Vegetable Oil Flash Thermometer having a range of 10 to 200C (50 to 392F) and conforming to the requirements of Specification E 1 shall be used. Equally acceptable is IP thermometer IP 101C. 6.2.3 For the range 60 to 110C (140 to 230"F) either low or medium range thermometer may be used. 6.2.4 For tests in which the indicated reading falls within 130 to 370C (265 to 700`F) an ASTM IOC (10F) PenskyMartens high-range Thermometer having a range from 90 to 370C (200 to 700`F) and conforming to the requirements of Specification E 1 shall be used. Equally acceptable is IP thermometer 16C (16F), with specifications as shown in Annex A3. 6.2.5 For the range 130 to 140C (265 to 285F) either the medium or high-range thermometer may be used. of Test Methods he sample is heated at a slow, constant rate with ual stirring. A small flame is directed into the cup at intervals with simultaneous interruption of stirring, ie flash point is the lowest temperature at which applica nt! the test flame causes the vapor above the sample to ute. ignificance and Use Bash point measures tendency of the sample to form ^Triable mixture with air under controlled laboratory 'tionS. It is only one of a number of properties which "* be considered in assessing the overall flammability lid Of a material. .2:Flash point is used in shipping and safety regulations ^Cfme flammable and combustible materials'. One should iult the particular regulation involved for precise defini, ns of these classes. .3' Flash point can indicate the possible presence of y volatile and flammable materials in a relatively volatile or nonflammable material. For example, an formally low flash point on a sample of kerosine can 'cate gasoline contamination. 3.4 This test method provides the only closed cup flash pcjiint test procedures for temperatures to 370C (698*F). 3Annual Book ofASTM Standards, Vol 05.03. *Annual Book ofASTM Standards, Vols 05.03 and 14.03. ''Annual Book ofASTM Standards, Vols 06.03 and 15.05. No t e 3--There are automatic flash point testers available and in use that may be advantageous in that they save testing time and exhibit other factors which may merit their use. In any cases ofdispute the flash point as determined manually is considered the referee test 7. Hazards 7.1 The operator must exercise and take appropriate safety precautions during the initial application of the test flame, since samples containing low-flash material can give an abnormally strong flash when the test flame is first applied. 8. Sampling 8.1 Erroneously high flash points may be obtained if precautions are not taken to avoid the loss of volatile material. Do not open containers unnecessarily and make a transfer'unless the sample temperature is at least the equiva lent of 8C (18F) below the expected flash point. Do not use samples from leaky containers for these test methods. 8.2 Do not store samples in plastic (polyethylene, polypropylene, etc.) containers, since volatile material may diffuse through the walls of the enclosure. 8.3 Obtain a sample in accordance with instructions given in Practice D 4057 or E 300. 8.4 Samples of very viscous materials may be warmed until they are reasonably fluid before they are tested. However, no sample should be heated more than is abso lutely necessary. It shall never be heated above a temperature of 17'C (30F) below its expected flash point. 8.5 Samples containing dissolved or free water may be dehydrated with calcium chloride or by filtering through a qualitative filter paper or a loose plug of dry absorbent 29 DU P0502 95697 # D 93 cotton. Warming the sample is permitted, but it should not be heated for prolonged periods or above a temperature of 17C (30F) below its expected flash point. No t e 4--If the sample is suspected of containing volatile contami nants, the treatment described in 8.4 and 8.5 should be omitted. 9. Preparation of Apparatus 9.1 Support the tester on a level, steady table. Unless tests are made in a draft-free room or compartment, it is good practice, but not required, to surround the tester on three sides with a shield, each section of which is about 450 mm (18 in.) wide and 600 mm (24 in.) high. No t e 5--Caution--Meticulous attention to all details relating to the flame exposure device, size of test flame, rate of temperature increase, and rate of dipping the flame exposure device into the vapor of the specimen is desirable for good results. 10. Calibration 10.1 Determine the flash point of p-xylene8 (Warning-- See Note 6.), following the directions in Sections 9 through 11. When the tester is operating properly, a value of 27.2 I. rC (81 2F) will be obtained. No t e 6: Warning--P-xylene is extremely flammable. Harmful if inhaled. Keep away from heat, sparks and open flame. Keep container closed. Use with adequate ventilation. Avoid buildup of vapors and eliminate all sources ofignition, especially non-explosion proofelectrical apparatus and heaters. Avoid breathing vapor or spray mist. Avoid prolonged or repeated contact with skin. 10.2 If the flash point obtained on p-xylene is not within the limits stated in 14.1.2, check the condition and operation Of the apparatus to ensure conformity with the details listed in Annex Al, especially with regard to the tightness ofthe lid (A 1.1.2.1), the action of the shutter, and position of the test flame (A 1.1.2.2). After adjustment, if necessary, repeat the test. P-xylene having a flash point of 27.2 1.1 C (81 2F) is not a suitable reference in the high temperature range of the Pensky-Martens Closed Tester which can be as high as 370C (700F). 10.3 P-xylene shall conform to the following require ments: Specific Gravity Boiling Range Purity 15.56/15.56'C 0.860 min., 0.866 max. 2"C from start to dry, point when tested in accordance with Test Method D 850 or D 1078. The range shall include the boiling point of pure p-xylene which is 138.35C (281.03F). 95 % min., (freezing point of 11.23'C), min calculated in accordance with Test Method D 1016, from the experimentally determined freezing point, measured by Test Method D 1015. PROCEDURE A--DETERMINATION OF FLASH POINT OF ORDINARY LIQUIDS II. Procedure 11.1 Thoroughly clean and dry allparts of the cup and its accessories before starting the test, being sure to remove any solvent which had been used to clean the apparatus. Fill the cup with the sample to be tested to the level indicated by the 8 Satisfactory p-xylene may be obtained as Flash Point Check Fluid from the Special Products Div., Chemical Dept., Phillips Petroleum Co., Drawer O, Borger, TX 79007. filling mark. Place the lid on the cup and set the latter in the stove. Be sure to have the locating or locking device properly engaged. Insert the thermometer. Bring the material to be tested and the tester to a temperature of ;15 5C (60 10F) or ire (20F) lower than the estimated flash point, whichever is lower. Light the test flame and adjust it to 4 mm (s/32 in.) in diameter. Supply the heat at such a rate that the temperature as indicated by the thermometer increases 5 to 6C (9 to 1 l0F)/min. Turn the stirrer 90 to 120 rpm, stirring in a downward direction. 11.2 If the sample is known to have a flash point of 110C (230F) or below, apply the test flame when the temperature of the sample is from 17C (30F) to 28C (50F) below the expected flash point and thereafter at a temperature reading that is a multiple of 1C (2F). Apply the test flame by operating the mechanism on the cover which controls the shutter and test flame burner so that the flame is lowered into the vapor space of the cup in: 0.5 s, left in its lowered position for 1 s, and quickly raised to its high position. Do not stir the sample while applying the test flame. 11.3 If the sample is known to have a flash point above 110C (230F) apply the test flame in the manner just described at each temperature that is a multiple of 2'C (5F), beginining at a temperature of 17C (30"F) .to 28'C (50F) below the expected flash point. No t e 7--When testing materials to determine if volatile contami nants are present, it is not necessary to adhere to the temperature limits for initial flame application as stated in 11.2 and 11.3. 11.4 Record as the observed flash point the temperature read on the thermometer at the time the test flame applica tion causes a distinct flash in the interior of the cup. Do not confuse the true flash point with the bluish halo that sometimes surrounds the test flame at applications preceding the one that causes the actual flash. PROCEDURE B--DETERMINATION OF FLASH POINT OF SUSPENSIONS OF SOLIDS AND HIGHLY VISCOUS MATERIALS 12. Procedure 12.1 Bring the material to be tested and the tester to a temperature of 15 5C (60 10F) or 11C (20F) lower than the estimated flash point, whichever is lower. Turn the stirrer 250 10 rpm,.stirring in a downward direction. Raise the temperature throughout the duration of the test at a rate of not less than 1 nor more than 1.5C (2 to 3F)/min. With the exception of these requirements for rates of stirring and heating, proceed as prescribed in Section 11. 13. Calculation and Report 13.1 Observe and record the ambient barometric pressure (Note 8) at the time of the test. When the pressure differs from 101.3 kPa (760 mm Hg), correct the flash point as follows: Corrected flash point - C + 0.25 (101.3 - p) Corrected flash point = F + 0.06 (760 -- P) Corrected flash point = C + 0.033 (760 - P) where: C = observed flash point, C, F = observed flash points, F, P = ambient barometric pressure, mm Hg, and (1) (2) (3) 30 DUP050295698 ambient barometric pressure, kPa. .2 Record the corrected flash-point to the nearest 0.5C m } .3 Report the recorded flash? point as the Pensky- ns Closed Cup Flash Point ASTM D 93 - IP 34, ofthe ie tested. o t e 8--The barometric pressure used in this calculation is the 'ent pressure for the laboratory at the time of test Many aneroid itnetcrs, such as those used at weather stations and airports, are ;ted to give sea level readings and would not give the correct 5 for this test. Precision and Bias 4.1 Precision--The precision of Test Procedure A as iennined by the statistical examination of the laboratory test results is as follows:, .1.1 Repeatability--The difference' between successive lilts obtained by the same operator with the same appaiis under constant operating conditions on identical test erials would, in the long run, in the normal and correct ation ofthe test method, exceed the following values in 1 sin 20. Material Bash Point Range "CCF) Repeatability "CCF) Suspensions of solids All others 35 to 43 (95 to 110) 104 (220) and under Above 104 (220) 2(4) 2(4) 5.5 (10) 14.1.2 Reproducibility--The difference between two ngle and independent results obtained by different operaprs working in different laboratories on identical material ould, in the long run, exceed the following values only in 1 e in 20. Material Flash Point Range "CCF) Reproducibility C("F) Suspensions of solids All others 35 to 43 (95 to 110) 104 (220) and under Above 104(220) ' 3.5 (6) 3.5 (6) 8.5(15) 14.1.3 Bias--The procedure of this test method has no bias because flash point can be defined only in terms of a test method. 14.1.4 The precision data is not known to have been developed in accordance with Research Report D-2-1007. 14.2 Precision--The precision of Test Procedure B as determined by the statistical examination of the interlaboratory test results is as follows: 14.2.1 Repeatability--The difference between successive results obtained by the same operator with the same appa ratus under constant operating conditions on identical test materials would, in the long run, in the normal and correct operation ofthe test method, exceed the following value in 1 case in 20: Repeatability 5C (9"F) 14.2.2 Reproducibility--The difference between 2 single and independent results obtained by different operators working in different laboratories on identical material would, in the long run, exceed the following value only in 1 case in 20. Reproducibility 10'C (18F) 14.2.3 The procedure of this test method has no bias because flash point can be defined only in terms of a test method. 14.2.4 The precision data is not known to have been developed in accordance with Research Report D-2-1007. 14.3 The definition of repeatability and reproducibility given here represents different components ofthe variance of the test methods: those given in 14.1 are derived from standards of ASTM Committee D-2 and the Institute of Petroleum, while those of 14.2 are from ASTM Committee D-2. IS. Keywords 15.1 flash point; flammability; Pensky-Martens closed cup 31 DUP050295699 # D 93 ANNEXES (Mandatory Information) Al. APPARATUS SPECIFICATIONS A 1.1. A typical assembly of the apparatus, gas heated, is shown in Fig. Al. 1. The apparatus shall consist of a test cup. cover, and stove conforming to the following requirements: No t e --Lid assembly may be positioned either right or left-handed. FIG. A1.1 Pensky-Martens Closed Flash Tester 32 DUP0502 95700  Hipbj p D 93 11.1 Cup--The cup shall be of brass, or other fsting metal of equivalent heat conductivity, and shall . to the dimensional requirements in Fig. A 1.2. The shall be equipped with devices for locating the an of the cup in the stove, A handle attached to the of the cup is a desirable accessory. The handle shall : so heavy as to tip over the empty cup. 11.2 Cover: 11-2.1 Cover Proper--Th^ cpver shown in Fig. A 1.3 |be of brass (Al.1.1) and shjfil have a rim projecting Iward almost to the flange of the cup. The rim shall fit Jutside of the cup with a clearance not exceeding 0.36 |(0.014 in.) on the diameter. There shall be a locating or ng device, or both, engaging with a corresponding : on the cup. The four openings in the cover. A, B, C, }, are shown in Fig. A1.3. The upper edge of the cup be in close contact with the inner face of the cover aghout its circumference. 1.1.2.2 Shutter--The cover shall be equipped with a ! (Section 3) shutter (Fig. A 1.4), approximately 2.4 mm 1m.) thick, operating on the plane of the upper surface of lover. The shutter shall be so shaped and mounted that it m # -'I :| f l | % i HAN0LE OPTIONAL 1 ! --*B c 11 rmsssss FILLING MARK-^ SS3D ) D E ,, l Xt. iA IB ;c ID !E !F !6 1H Sl :J ! -------- p-------- G ^..... 1.............. ! ----------- r------------ mm min 79.0 1.0 2.8 21.72 4S.47 50.72 55.75 3.8 53.90 2.29 max 79.8 3.8 21.84 45.72 50.85 56.00 4.0 54.02 2.54 (In.) (min) (3.11) (0.04) (0.11) (0.855) (1.790) (1.997) (2.195) (0.15) (2.122) (0.090) (max) (3.14) (...) (0.14) (0.860) (1.800) (2.002) (2.205) (0.16) (2,127) (0.100) FIG. A1.2 Test Cup min max (min) (max) 0 12.7 13.5 (0.50) (0.53) E 4.8 5.6 (0.19) (0.22) F 13.5 14.3 (0.53) (0.56) 0 23.8 24.6 (0.94) (0.97) K 1.2 2.0 (0.05) (0.08) 1 7.9 (0.31) (...) J 12.27 12.32 (0.483) (0.485) K 16.38 16.64 (0.645) (0.655) L 18.65 19.45 (0.734) (0.766) FIG. A1.3 Cover Proper rotates on the axis of the horizontal center of the cover between two stops, so placed, that when in one extreme position, the openings A, B, and C in the cover are completely closed, and when in the other extreme position, these openings are completely opened. The mechanism operating the shutter should be of the spring type and constructed so that when at rest the shutter shall exactly close the three openings. When operated to the other extreme, the three cover openings shall be exactly open and the tip of the exposure tube shall be fully depressed. A 1.1.2.3 Flame-Exposure Device--The flame-exposure device (Fig. A 1.4) shall have a tip with an opening 0.69 to 0.79 mm (0.027 to 0.031 in.) in diameter. This tip shall be made preferably of stainless steel, although it may be fabricated of other suitable metals. The flame-exposure device shall be equipped with an operating mechanism which, when the shutter is in the open position, depresses the tip so that the center of the orifice is between the planes of the under and upper surfaces of the cover proper at a point on a radius passing through the center of the larger opening A (Fig. A1.3). A1.1.2.4 Pilot Flame--A pilot flame shall be provided for automatic relighting of the exposure flame, A bead 4 mm (V32 in.) in diameter can be mounted on the cover so that the size ofthe test flame can be regulated by comparison. The tip w DUP05029570j D 93 of the pilot flame shall have an opening the Same size as the tip of the flame exposure device (0.69 to 0.79 mm (0.027 to 0.031 in.) in diameter). Al.1.2.5 Stirring Device--The cover shall be equipped with a stirring device (Fig. A1.4) mounted in the center of the cover and carrying two 2-bladed metal propellers. In Fig. A 1.4 lower propeller is designated by the letters L, M, and N. This propeller shall measure approximately 38 mm from tip to tip, with each of its two blades 8 mm in width with a pitch of 45". The upper propeller is designated by the letters A, C, and G. This propeller measures approximately 19 mm, tip to tip, each of its two blades is also 8 mm in width with a pitch of 45. Both propellers are located on the stirrer shaft in such a manner that, when viewed from the bottom of the stirrer, the blades of one propeller are at 0 and 180 while the blades of the other propeller are at 90 and 270. A stirrer shaft may be coupled to the motor by a flexible shaft or a suitable arrangement of pulleys. Al. 1,2.6 Stove--Heat shall be .'supplied to the cup by means of a properly designed stove which is equivalent to an FLAME EXPOSURE DEVICE THERMOMETER SHUTTER STIRRER TEST CUP RIM OF CUP MUST BE IN CONTACT WITH THE INNER FACE OF COVER THROUGHOUT ITS CIRCUMFERENCE mm min max A B' c D E F G H 1* J K L M N: 18.3 2.38 7.6 2.0 . 0.69 2.0 6.4 9.6 43.0 50.0 1.22 31.8 .7.6 19.8 3.18 8.4 2.8 0.79 2.8 10.4 11.2 46.0 51.6 0.36 2.06 44.4 8.4 * Includes tolerance for length of thermometer given in 'Specification E1. -. FIG. A1.4 Test Cup and Cover Assembly (min) (0.72) (0.094) (0.30) (0.08) (0.027) (0.08) (0.25) (0.38) (1.69) (1-97) (...) (0.048) (1.25) (0.30) (in.) 34 (max) (0.78) (0.125) (0.33) (0.11) (0.031) - (0.11) (0.41) (0.44) (1.81) (2.03) (0.014) (0.08) ' (1.75) (0.33) DUP050295702 "The stove shall consist ofan air bath and a top plate itji the flange of the cup rests. " S.7 A& Bath--The air bath shall have a cylindrical and shall conform to the dimensional requirements Vj.l. The air bath may be either a flame or Ily heated metal casting (Al.1.2.8), or an electric\element (Al.1.2.9). In either case,, the air bath suitable for use at the temperatures to which it will "ccted without deformation. 2i8 Heater, Flame or Electric--If the heating eleVa,-flame or an electric heater, it shall be so designed dft that the temperatures of the bottom and the walls loximately the same. In order that'the air bath surfaces should be at a uniform temperature, it iJ.not be less than 6.4 mm (lA in.) in thickness unless the ^element is designed to give equal heat flux densities 11 the wall and bottom surfaces. ; Al. 1.2.9 Heater, Electric Resistance--If the heater is of the electric resistance type, it shall be constructed so that all parts of the interior surface are heated uniformly. The wall and bottom of the air bath shall not be less than 6.4 mm (M in.) in thickness unless the resistance heating elements are distributed over at least 80 % of the wall and all the bottom of the air bath. A heater having such a distribution of the heating elements positioned at least 4.0 mm (%2 in.) away < from the internal surface of the heating unit can be used in -conjunction with a minimum thickness of 1.58 mm (l/ie in.) fbkthe wall and bottom of the air bath. Al.1.2.10 Top Plate--The top plate shall be of metal, and shall be mounted with an air gap between it and the air bath. It may be attached to the air bath by means of three screws and spacing bushings. The bushings should be of proper thickness to define an air gap of 4.8 mm (Vie in.), and they shall be not more than 9.5 mm (3/s in.) in diameter. DUP050295703 D 93 d A2. MANUFACTURING STANDARDIZATION OF THERMOMETER AND FERRULE A2.1 The low-range thermometer, which conforms also to the specification for the cup thermometer in the Tag closed tester (Test Method D 56} and which frequently is fitted with a metal ferrule intended to fit the collar on- the cover of the Tag flash tester, can be supplemented by an adapter (Fig. A2.1) to be used in the larger diameter collar of the i. .: '. Pensky-Martens apparatus. Differences in dimensions of these collars, which do not affect test results, are a source of unnecessary trouble to manufacturers and suppliers of in* struments, as well as to users. A2.2 Dimensional requirements are shown in Fig. A2.1. Conformity to these requirements is not mandatory, but is desirable to users as well as suppliers of Pensky-Martens testers. I I J -if :j j | 1 "I- -t t ?--!--rv'T S ------ ------- ftfeW THREAD T J JL CLAMP NUT-STAINLESS STEEL % UNF THREAD TN M FERRULE STAINLESS STEEL mm min max A 6.20 6.50 B 17.0 18.0 C 9.80 9.85 D 12.19 12.24 E 1.40 1.65 F 8.56 8.61 G 12.4 13.0 H 8.56 8.61 1 8.1 8.6 J 9.9 10.7 K 8.64 8.69 L 5.1 5.6 M 17.0 17.5 N 27.4 28.2 0 7.11 7.16 P 9.73 9.78 (in.) (min) (max) (0.244) (0.67) (0.386) (0.480) (0.055) (0.337) (0.49) (0.337) (0.32) (0.39) (0.340) (0.20) (0.67) (1.08) (0.280) (0.383) (0.256) (0.71) (0.388) (0.482) (0.065) (0.339) (0.57) (0.339) (0.34) (0.42) (0.342) (0.22) (0.69) (1.11) (0.282) (0.385) FIG. A2.1 Dimensions for Thermometer Adapter, Ferrule, and Packing Ring 36 DUP050295704 D 93 A3. THERMOMETER SPEaFICATIONS TABLE A3:1^' IP Thermometer Specifications e--The stem shall be made with an enlargement having a danneterof 1.5 to 2.0 mm greater than the stem and a length of 3 to 5 mm, the bottom of the enlargement gtt I to 66 mm from the bottom of the bulb. These dimensions shall b&measured with the test-gage shown In Fig. A3.1. Name IP15C Pensky-Martens Low IP16C Pensky-Martens High IP 101C Pensky-Martens Medium ge uatton frsion, mm call length 6 mm diameter, mm Ibdiameter, mm i of graduated portion, --5 to +110C 0.5C 57 * 290 6.0 to 7.0, cylindrical 9 to 13 not less than 5.5 and not greater than stem 1*0 to 175 90 to 370C 2C 57 280 10 6.0 to 7.0 cylindrical 7 to 10 not less than 4.5 and not greater than "stem 143 to 180 20 to 150"C T'C 57 290 6.0 to 7.0 cylindrical 9 to 13 not less than 5.5 and not greater than stem 140 to 175 nee bottom of bulb to, :ger lines at each at each Ion chamber .Je error not to exceed r notes 0C 85 to 95 1 and 5C 5C required ring 0.5C 1 and Table A3.3 for emergept stem' temperatures 90C 80'to 90 10 and 20C 20C required ring 1 to 260C 2C above 260C 1 and Table A3.3 for emergent stem temperatures 20C 85 to 95 5C 5C required ring 1C 1 and Table A3.3 for emergent stem temperatures 37 DUP050295705  0 93 FIG. A3.1 Test Gage for Checking Enlargements on Thermometers 38 DUP050295706 TABLE A3.2 Specifications for ASTM Thermometers AB dimensions are in millimetres. See Table A3.3 for Standardization Temperature. L, ,--L. JET " itTij III 39 ASTM No. and Name Range For - Im Test mer at sion 9C-62 PenskyMarlens, Low-Range Tag Closed Tester 9F-62 -5 to +110C (20 to 230F) IOC-62 PenskyMartens, High-Range 10F-62 90 to i 370-C (200 to 700F) 57 57 o3 U. 2 5- i , </> 3 il O w^ m Graduations Expan sion Cham ber Long Lines at Each Num ber at Each Scale Error max Special Inscrip-' tion Permit Heat ing to es ASTM | 9Cor9F 57 mm IMM Bulb Total Length, +5 B 287 Stem OD Length CD 6.0 9.0 to to 7.0 13 8 111 Bot tom of Bulb to Line at * stem OoO u0CcM.o CuM. cm Scale Location OCOl *Q* U3 CO Dis tance F OOor: Bot-, tom of " Bulb to Dis tance Line at G 221 to 237 o li aO h * 10 O o u_ 0 "> o u!- a> COO<03o cSUOp- ffl CO Ooott-~ nu2CM. 0 O u. Oo s8 F o- ASTM IOC or 10F 57 mm IMM 287 6.0 8.0 4.5 to to to 7.0 10.0 6.0 +o-*Oi 227 to 245 8 _X <OcD) . , CD CC Ice Point Scale Contra * Cham .Bot tom of. . Bulb to Ice Point Dis tance, to : Bot tom, min -1 o u- o r *. s* SS- ?Ss " uT "ooQtstt li.' $o> O*. SSI CM " ~ot9!--Q a => u3- gJiPSca *0S3 <CSaO co< e c* &0) & E (o0 (U 3 E | thermometer be heated above the highest temperature reading. The length of the enlargement, and the distance from the bottom of the-enlargement to the bottom of the bulb shall be measured with the test gage shown in Fig. A3.1. DUP050295707 # D 93 TABLE A3.3 Standardization Temperatures No t e__The emergent column temperatures are those attained when using the thermometers In the test equipment for which the thermometers were originally designed. in some cases these temperatures are markedly different from those realized during standardization. Tempera ture Average Tempera ture of Emergent Column Tempera ture Average Tempera ture of Emergent column Tempera ture Average Tempera ture of Emergent Column Tempera ture Average Tempera ture of Emergent Column Thermometer 9C (-5to+100*C) 0C 19*C 35C 28C 70C 40C 105C 50C Thermometer 9F (20 to 230"F) 32F 66F 100F 86'F 160F 106*F 220"F 123"F Thermometer 10C , (90 to 370C) 100C 61 C 200C 71 C 300*0 87*C 370C 104"C Thermometer 10F (200 to 700F) 212F 141"F 390*f 159F 570p 180F 700*F 220F IP 15C (--7 to110*C) IP15F (20 to 230F) IP 16C (90 to 370C) IP 16F (20 to 700"F) 0C 19C 32*F 66F 100'C 61 C 200F 140*F I 20C 200 70*F 70F 150C 65C 300F 149F 40C 31 "C 10OF 86*F 200C 71 C 400*F 160F 70C 40C 150F 104F 250"C 78 "C 500*F 175*F 100C 48C 212F 118F 300C 87C 600F 195F 350*0 99"C 700F 220F TABLE A3.4 Specifications for Medium-Range Pensky-Martens ASTM No. 88F (88C) Vegetable Oil.Flash Thermometer Name Reference Fig. No. Range For test at A Immersion, mm Graduations: Subdivisions Long lines at each Numbers at each Scale error, max Special inscription Expansion chamber: Permit heating to B Total length, mm C Stem OD, mm D Bulb length, mm E Bulb OD, mm Scale location: Bottom of bulb to line at F Distance, mm G Length of graduated portion, mm Ice-point scale: Range H Bottom of bulb to ice-point, mm Contraction chamber: 1 Distance to bottom, min, mm j Distance to top, max, mm Stem enlargement K OD, mm L Length, mm M Distance to bottom, mm * 10-200*C 0.5"C 1Cand5C 5C 0.5*C 205C 20*6 Medium Range Pensky-Martens 5 50-392"F 57 ASTM 88F(88C) 57 mm IMM 1*F 5*F 10F 1F 285 to 295 6.0 to 7.0 8.0 to 12.0 >4.5 and <stenv? 5 - 80 to 90 145 to 180 400*F 68*F 7.5 to 8.5 2.5 to 5.0* 64 to 66 A Bulb OD shall be greater than 4.5 mm and less than the outside diameter of the stem (C). : 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 technicalcommittee and must be reviewed every five years and ifnotrevised, eitherreapproved or withdrawn. Your commentsare invitedeitherforrevision ofthis standard or for additionalstandards and shouldbe addressed to ASTM Headquarters. Your commants will receive careful consideration at a maating 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 ASTMCommittee on Standards, 1916 Race St., Philadelphia, PA 19103. | ] i 1 f40 40 1 DUP050295708 An American National Standard British Standard 4385 American Associationstate Highway Transportation Standard AASHTO No. T55 Standard Test Method for / Water in Petroleum Products and Bituminous Materials by Distillation1 This standard is issued under the fixed designation D 95; the number immediately following the designation indicates,the year of original adoption or, in the case 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. ' This test method has been approved by the sponsoring committees and accepted by the cooperating organizations in accordance with established procedures. This test methodhas been approvedfor use by agencies oftheDepartment ofDefense,andfor listing in the DoD Index ofSpecifications and Standards. el Norn--Paragraphs 1.3 and 11.2 were added editorially in May 1990. .1 This test method covers the determination' of water in " ieum products, tars, and other bituminous materials by distillation method. The specific products considered og the development Of this test method are listed in hie 1. For bituminous emulsions refer to Test Method -44. This test method, along with ASTM Test Method 006 (API Chapter 10.2 and; IP 35), supersedes the vious edition of ASTM Test Method D 95 (API Standard ;0,IP74). Jo t e. 1--With some types ofoil, satisfactoryresults may-be obtained m ASTM Test Method D4007 (API Chapter 1.0.3, IP 358, and. : Method U 1796 API Chapter 10.6). 1.2 This standard may; involve hazardous materialsoper'ons, and equipment. This standard does not purport to 'dress all ofthe safety problems associated with its use. It is responsibility of the . user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For :ecific hazard statements, see 5.1.1.2 and 5.1.1.3. 1.3 The values stated in SI units are to be regarded as the adard. The values in parentheses are for information only. Referenced Documents is 2.1 ASTM Standards: * D86 Method for Distillation of Petroleum Products2 = D244 Test Methods for Emulsified Asphalts3 ' This test method is under the jurisdiction of ASTM Committee -D-2 on I Petroleum Products and Lubricants and API Committee on Petroleum Measure-. !; ment and is the direct responsibility ofSubcommittee D02.02 on Joint ASTM-AP1 Committee on Static Petroleum Measurement I Current edition approved March 2S, 1983. Published January 19S4. Originally published as D 95.21. Last previous edition D 95 - 70 (i960). 2 Annual Book ofASTM Standards. VolsOS.Oi and 06.03. . 3 Annual Book ofASTM Standards, Vol 04.03. D1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)4 D4006 Test Method for Water in Crude Oil by Distillation5 D 40.(17 Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)5 D4057 Practice for Manual Sampling of Petroleum and Petroleum Products5 D4177.Method for Automatic Sampling of Petroleum and. Petroleum, Products5 E 123 Specification, for Apparatus for Determination of Water by Distillation5 2.2 API Manual ofPetroleum Measurements Standards:6 7 Chapter 8.1 Manual Sampling of Petroleum and Petro leum Products.(ASTM Practice D 4057) Chapter 8.2 Automatic Sampling of Petroleum and Petro leum Products (ASTM Test Method D 4177) Chapter 10.2 Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D 4006) Chapter 10.3 Determination of Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Proce dure) (ASTM Test Method D 4007) Chapter 10.6 Determination of Water and Sediment in Fuel Oil by the Centrifuge Method (ASTM Test Method D1796) 2.3 British Standard:1 756 Dean and Stark Apparatus 3. Summary of Test Method 3.1 The material to be tested is heated under reflux with a 4 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 05.03. 6 Available from American Petroleum Institute, 1220 L St., N.W., Washington, DC 20005. 7 Available from American National Standards Institute, 13th Floor, 11 W. 42nd Street, New York, NY 10036. DUP050295709 TABLE 1 Type of Solvent-Carrier Liquid Versus Material to be Tested Type of Solvent-Carrier Liquid Material to be Tested Aromatic Petroleum distillate Volatile spirits asphalt, tar, coal tar, water gas tar, road tar. cutback bltumin, fquid asphalt, tar acid road oil, fuel oil, lubricating oil, petroleum sulfonates lubricating grease water-immiscible solvent, which co-distills with the water in the sample. Condensed solvent and water are continuously separated in a trap, the water settling in the graduated section of the trap and the solvent returning to'the still. 4. Significance and Use 4.1 A knowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products. 4.2 The amount of water as determined by this method (to the nearest 0.05 volume %) shall be used to correct the volume involved in the custody transfer of oil. FIG. 2 Two-millilitre Receiver Showing Alternative Connections to Glass Still 5. Solvent-Carrier Liquid 5.1 A solvent-carrier liquid appropriate to the material being tested (see Table 1) shall be used. 5.1.1 Aromatic Solvent--The following aromatic solvents are acceptable: 5.1.1.1 Industrial Grade Xylene. 5.1.1.2 A blend of 20 volume % industrial grade toluene and 80 volume % industrial grade xylene (Warning--Flam mable. Vapor harmful. See Annex A 1.1.) 5.1.1.3 Petroleum or Coal Tar Naphtha (Warning--Ex tremely flammable. Harmful if inhaled. Vapors may cause fire. See Annex), free of water, yielding not more than 5% distillates at 125C (257F) and not less than 20% at 160C (320F) when tested by Method D 8b and with a relative density (specific gravity) not lower than 0.8545 at 15.56/ 15.56C (60/60F). 5.1.2 Petroleum Distillate Solvent--A petroleum distillate FIG. 1 Typical Assembly with Glass Still (Dean and Stark) solvent, 5% boiling between 90 and 100C (194 and 212F) and 90% distilling below 210C (410F), shall be used. 5.1.3 Volatile Spirits Solvent--The following volatile spirits solvents are acceptable: 5.1.3.1 Petroleum Spirit, with a boiling range of 100 to 120C (212 to 248F). 5.1.3.2 Isooctcme, of 95% purity or better. 6. Apparatus 6.1 General--The apparatus comprises a glass or metal still, a heater, a reflux condenser, and a graduated glass trap. The still, trap, and condenser may be connected by any suitable method that produces a leakproof joint. Preferred connections are ground joints for glass and O-rings for metal to glass. Typical assemblies are illustrated in Figs. 1,2, and 3. The stills and traps should be chosen to cover the range of materials and water contents expected. 6.2 Still--A glass or metal vessel with a short neck and suitable joint for accommodating the reflux tube of the trap shall be used. Vessels of 500, 1000, and 2000-mL nominal capacity have proved satisfactory. 6.3 Heater--A suitable gas burner or electric heater may be used with the glass still. A gas ring burner with ports on the inside circumference shall be used with the metal still. The gas ring burner shall be of sueh dimensions that it may be moved up and down the vessel when testing materials that are likely to form or solidify in the still. 6.4 Glassware--Dimensions and descriptions of typical glassware for use in this method are provided in Specification E 123 and British Standard 756. A straight water-cooled condenser with a length of400 mL is recommended in place of the length of 300 mL specified in British Standard 756. No t e 2--instead of standardizing on a particular apparatus specifi cation with respect to dimensions and style, a given apparatus will be deemed satisfactory when accurate results are obtained by the standard addition technique described in Section 7. 7. Standardization 7.1 A given assembly of apparatus will be considered 42 DUP050295710 s I 0 D 95 , >. 6'r m i 1 'bmM" Im&v. life'- fefl; ill;" m ife r i & IK: Satisfactory when accurate readings are obtained from, the Edition of known amounts of water from a calibrated buret pipet to a clear hydrocarbon oil and tested in accordance with Section 9. 7.2 The readings shall be judged accurate if the permis- TABLE 2 Permissible Limits in Millilitres L Capacity of Kj' Receiver at 20C ' 2 * 10 fi 10 25 Volume of Water Added to Flask at 20C 1 1 5 12 Permissible Limits for Recovered Water at 20C 1 0.05 1 0.1 5 0.2 12 0.2 sible limits given in Table 2 for the various sized graduated traps are not exceeded. 7.3 A reading outside the permissible limits suggests a malfunction resulting from vapor leaks, too rapid boiling, inaccuracies in calibration of the trap, or ingress of extra neous moisture. Eliminate these factors before repeating the standardization. 8. Sampling 8.1 Sampling is defined as all steps required to obtain an aliquot of the contents of any pipe, tank, or other system and to place the sample into the laboratory test container. Only representative samples obtained as specified in Practice D 4057 (API Chapter 8.1) and Method D 4177 (API Chapter 43 DUP050295711 Designation: D 124 - 88 Bf $.fPffj|lJJl rl If Standard Specification for Degummed Soybean Oil1 "| This standard is issued under the fixed designation D124; 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 specification covers degummed soybean oil suit able for use in the paint and varnish industry. 2. Referenced Documents 2.1 ASTM Standards: D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2 D 555 Guide for Testing Drying Oils3 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 D1639 Test Method for Acid Value of Organic Coating Materials4 D1952 Test Method for Quantitative Determination of Break in Drying Oils3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 D1960 Test Method for Loss on Heating of Drying Oils3 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25<'C3 1 This specification is under the jurisdiction of ASTM Commitee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.32 on Drying Oils. Current edition approved Oct. 31, 1988. Published December 1988. Originally published as D 124 - 22. Last previous edition D 124 - 87. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. TABLE 1 Property Specific gravity, 25/25C Acid value, max Saponification value Unsaponification matter, max, % Break, max, % Iodine value (Wijs), min Loss on heating at 105 to 110C, max, % Clarity Color (Gardner 1933), max Color (after heating), max Flash point Physical Properties Requirement 0.917 to 0.924 3.0 189 to 195 1.5 0.10 126 0.3 clear and transparent at 65C 12 12 over 203F (95C) ASTM Test Method D 1963, D 1475 D1639 D1962 D 1965 -D1952 D1959 O1960,D1393 D 2090 D 1544 D 1967 D 93, D 3278 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Adds3 D1967 Test Method for Measuring Color After Heating of Drying Oils3 D2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids6 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus3 3. Properties 3.1 Degummed soybean oil shall conform to the require ments in Table 1. 4. Test Methods 4.1 Sampling--Sampling shall be conducted in accord ance with Test Method D 1466. 4.2 The properties enumerated in this spedfication shall be determined in accordance with the applicable ASTM test methods listed in Table 1. The significance of the methods of testing enumerated under properties in this specification is discussed in Guide D 555. 6 Annual Book ofASTM Standards, Vols 06.02 and 06.03. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either forrevision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 46 DUP050295712 Designation: D 130 - 88 Designation: 154/86 An American National Standard Federation of Societies for Paint Technology Standard No. Dt-28-65 British Standard 4351 Standard Test Method for / Detection of Copper Corrosion/from Petroleum Products by the Copper Strip Tarnish Test1 This standard is issued lander the fixed designation D 130; 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 is also a standard of the Institute of Petroleum issued under the fixed designation IP 134. The final number indicates the year oflast revision. This test method has been approved by the sponsoring committees and accepted by the cooperating societies in accordance with established procedures. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 5325 ofFederal Test Method Standard No. 791b. Consult the DoD Index ofSpecifications andStandardsfor the specific year ofissue which has been adopted by the Department ofDefense. Pe This test method covers the detection of the corrosivej'to copper of aviation gasoline, aviation turbine fuel, "'otive gasoline, natural gasoline or other hydrocarbons a Reid vapor pressure no greater than 18 psi (124 (Caution--see Note 1 and Annex A2.), cleaners `dard) solvent, kerosine, diesel fuel, distillate fuel oil, ing oil, and certain other petroleum products. Ot e 1; Caution--Some products, particularly natural gasoline,, ave a much higher vapor pressure than would normally be eristic of automotive or aviation gasolines. For this reason, ne caution must be exercised to ensure that die test bomb lining natural gasoline or other products of high vapor pressure are jplaced in the 100"C (212'F) bath. Samples having Reid vapor *ures in excess of 18 psi (124 kPa) may develop sufficient pressure at C to cause rupture of the test bomb. For any sample havinga Reid ; pressure above 18 psi (124 kPa), use Test Method f> 1838. 1.2 This standard may involve hazardous materials, operjons, and equipment. This standard does not purport to 'dress ail ofthe safety problems associated with its use. It is f responsibility of the user of this standard to establish fpropriate safety and health practices and determine the iplicabiiity of regulatory {imitations prior to use. For pecific hazard statements, see Notes 1 and 2, and Annex A2. . Referenced Documents 2.1 ASTM Standards: D 396 Specification for Fuel Oils2 D975 Specification for Diesel Fuel Oils2 D1655 Specification for Aviation Turbine Fuels2 1 This test method is under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcom mittee D02.05 on Physical Analysis of Fuels and Light Distillates. In the IP, this method is under the jurisdiction of the Standardization Committee. Current edition approved Oct. 31, 1988. Published December 1988. Originally published as D130 - 22T, replacing' former D89. Last previous edition D 130-83. 2 Annual Book ofASTM Standards, Vol 05.01. D1838 Test Method for Copper Strip Corrosion by Liquefied Petroleum (LP) Gases3 2.2 ASTM Adjunct: Copper Strip Corrosion Standard4 3. Summary of Test Method 3:1 A polished copper strip is immersed in a given quantity of sample and heated at a temperature and for a time characteristic of the material being tested. At the end of this period the copper strip is removed, washed, and com pared with the ASTM Copper Strip Corrosion Standards. 4. Significance and Use 4.1 Crude petroleum contains sulfur compounds, most of which are removed during refining. However, of the sulfur compounds remaining in the petroleum product, some can have a corroding action on various metals and this corrosivity is not necessarily related directly to the total sulfur content. The effect can vary according to the chemical types of sulfur compounds present. The copper strip corro sive test is designed to assess the relative degree ofcorrosivity of a petroleum product. 5. Apparatus 5.1 Test Tubes, 25 by 150-mm. 5.1.1 Provide a bath capable of being maintained at a constant temperature of 50 1C (122 2F) or 100 TC (212 2F ), or both, and having suitable supports to hold the test tubes in a vertical position and immersed to a depth of about 100 mm (4 in.). Either water, oil, or aluminum block baths are suitable. 5.2 Copper Strip Corrosion Test Bomb, constructed of stainless steel according to the dimensions as given in Fig. 1, and capable of withstanding a test pressure of 100 psi (689 kPa). Alternative designs for the bomb cap and synthetic 3 Annual Book ofASTM Standards, Vols 05.01 and 05.05. "Available from ASTM Headquarters, 1916 Race Street, Philadelphia, PA. 19103. Request Adjunct No. 12-401300-00. Names of suppliers in the United Kingdom can be obtained from the Institute of Petroleum. Two master standards are held by the IP for reference. 47 DUP050295713 130 3 2 WIDE GROOVE FOR PRESSURE RELIEF-1 LIFTING CYC KNURLED CAP SYNTHETIC RUB8ER '0' RING FREE FROM FREE SULPHUR -CHAMFER INSIDE CAP TO PROTECT . `O' RU4G WHEN CLOSING BOMB MAX. TEST PRESSURE 100 LBF/IN2 17.03 K9*m2) 1.6 WALL SEAMLESS TUBE Ws*l - * MATERIAL: STAINLESS STEEL WELOED CONSTRUCtlON FIG. 1 Copper Strip Corrosion Test Bomb rubber gasket may be used provided that the internal dimensions of the bomb are the same as those shown in Fig. 1. Provide a 25 by 150-mm test tube as a liner for holding the sample. 5.2.1 Provide liquid baths capable of being maintained at 40 IT (104 2*F) or 100 1G (212 2F) , or both, and having suitable supports to hold the test bomb in a vertical position. The bath must be deep enough so that the entire bomb will be submerged during the test. As the bath medium, use wwter or,.any other liquid which can be satisfactorily controlled at the specified test temperature. 5.3 Thermometers, total immersion, for indicating the required test temperature, with smallest graduations of 1C (2F) or less. No more than 25 mm (1 in.) of the mercury thread should extend above the surface ofthe bath at the test temperature. The ASTM 12C (12F) or IP 64C,(64F) ther mometer, is suitable. 5.4 Polishing Vise, for holding the copper strip firmly without marring the edges while polishing. Any convenient type of holder (see Appendix) may be used provided that the strip is held tightly and that the surface of the strip being polished is supported above the surface of the holder. 5.5 . Viewing Test Tubes* flat, are convenient for protecting corroded strip for close inspection or storage (see Appendix). 6. Materials 6.1 Wash Solvent--Any volatile, sulfur-free hydrocarbon solvent may be used provided that it shows no tarnish at all when tested at 50C (122F). Knock test grade irooctane is a suitable solvent and should be used in case of dispute. No t e 2: Warning--Extremely flammable, see Annex A2.1. 6.2 Polishing Materials--Silicon carbide grit paper of varying degrees of fineness including 65-pm (240-grit) paper or cloth; also a supply of 105-p.m (150-mesh) silicon carbide grain and pharmaceutical grade absorbent cotton (cotton wool). 6.3 Copper Strips: 6.3.1 Specification--Use strips 12.5 mm (`/2 in.) wide, 1.5 to 3.0 mm (`/i6 to Vs in.) thick, cut 75 min (3 in.) long from smooth-surfaced, hard-temper, cold-finished copper of 99.9 + percent purity; electrical bus bar stock is generally suitable (see Appendix). The strips may be used repeatedly but should be discarded when the surfaces become deformed on handling,.., 6.3.2 Surface Preparation--Remove all surface blemishes from, all six Sides of the strip with silicon carbide paper of such degrees of fineness as are needed to accomplish the desired results efficiently. Finish with. 65-pm (240-grit) silicon carbide paper or cloth, removing all marks that may have been made by other grades of paper used previously. Immerse the strip in wash solvent from which it can be withdrawn immediately for final polishing or in which it may be stored for future use. 6.3.2.1 As a practical manual procedure for surface prep aration, place a sheet ofthe paper on a flat surface, moisten it with kerosine or wash solvent, and rub the strip against the paper with a rotary motion, protecting the strip from contact with the fingers with an ashless filter paper. Alternatively, the surface of the strip can be prepared by use of motor-driven machines using appropriate grades of dry paper or cloth. 6.3.3 Final Polishing--Remove a strip from the wash : solvent. Holding it in the fingers protected with ashless filter paper, polish first the ends and then the sides with the 105-p.m (150-mesh) silicon carbide grains picked up from a clean glass plate with a pad of cotton (cotton wool) moist ened with a drop of wash solvent Wipe vigorously with fresh pads of cotton (cotton wool) and subsequently handle only with stainless steel forceps; do not touch with the fingers. Clamp in a vise and polish the main surfaces with siliconcarbide grains on absorbent cotton. Rub in the direction of the long axis of the strip, carrying the stroke beyond the end of the strip before reversing the directioh. Clean all metal dust ffoni the strip by rubbing vigorously with clean pads of absorbent cotton until a fresh pad remains unsoiled. When the. strip is dean, immediately immerse it in the prepared sample. 6.3.3.1 It is important to polish the whole surface of the strip uniformly to obtain a uniformly stained strip. If the edges show wear (surface elliptical) they will likely show more corrosion than the center. The use of a vise (see Appendix) will fadlitate uniform polishing. 7. Corrosion Standards 7.1 ASTM Copper Strip Corrosion Standards4 consist of reproductions in color of typical test strips representing increasing degrees of tarnish and corrosion, the reproduc tions being encased in plastic in the form of a plaque. 7.1.1 Keep the plastic-encased printed ASTM Copper Strip Corrosion Standards protected from light to avoid the possibility of fading. Inspect for fading by comparing two different plaques, one of which has been carefully protected from light (new). Observe both sets in diffused daylight (or equivalent) first from a point directly above and then from an angle of 45. When any evidence of fading is observed, particularly at the left-hand end of the plaque, it is suggested that the one that is the more faded with respect to the other be discarded. 48 DUP050295714 # D 130 I Alternatively, place a 20-mm (3A-m.) opaque strip f tape) across the top of the colored portion of the hen initially purchased. At intervals remove the strip and observe. When there is any evidence of the exposed portion, it is suggested that the be replaced. These plaques are full-color reproductions,,qf typThey have been printed on aluminum sheets by a process and are encased in plastic for protection, for their use are given on the reverse side of each If the surface of the plastic cover shows excessive chins it is suggested that the plaque he replaced. is particularly important that all types of fuel which pass a low-tarnish strip classification, be id in clean, dark glass bottles, plastic bottles, or other i containers that will not affect the corrosive proper'rthe fuel. Av.oid the use of tin plate containers for |on of samples, since, experience has shown that they J|ntribute to the corrosiveness of the sample, pill the containers as completely as possible and close' immediately after taking the sample. Take care, duriftg [ing to protect the samples from exposure to direct ht or even diffused daylight Make the test as soon as file after receipt in the laboratory and immediately after Blhg the container. When suspended water (haze) is observed in the dry by filtering a sufficient volume of sample |gh a medium rapid qualitative filter, into the prescribed I, dry test tube. Carry out this operation in a darkened or under a light-protected shield, j.l Contact of the copper strip with water before, g, or after the completion of the test run, will cause ting, making it difficult to evaluate the strips. rocedure l Those product classes, to which given procedural tions are intended to be applied, are listed below. Some duct classes, being quite broad, may be tested by more 1 one set of conditions; in such cases the copper strip ity requirement for a given product should be limited to iingle set of conditions. The conditions of time and perature given below are those most commonly used and quoted in the ASTM specifications for these products iere such specifications exist. However, other conditions also be used as and when required by specifications or by ement between parties. .1.1 For aviation gasoline, and aviation turbine fuel-- ace 30 mL of sample, completely clear and free of any ispended or entrained water (see 8.3) into a chemically lean, dry 25 by 150-mm test tube, and within 1 min after, ompleting the final polishing, slide the copper strip into the imple tube. Carefully slide the sample tube into the test mb (Fig. 1) and screw the lid on tight. Completely merse the bomb in a boiling water bath at 100 l'C (212 2*F); After 2 h 5 min in the bath, withdraw the bomb 'immerse for a few minutes in tap water. Open the bomb, Withdraw the test tube and examine the strip as described in 9.2. - 9.1.2 For natural gasoline--Carry out the test exactly as described in 9.1.1 but at 40C (104F) and for 3 h 5 min. 9.1.3 For diesel fuel, fuel oil, automotive gasoline--Place 30 mL of sample, completely clear and free of any suspended or entrained water (see 8.3), into a chemically clean, dry 25 by 150-mm test tube and, within 1 min after completing the final polishing, slide the copper strip into the sample tube. Stopper with a vented cork and place in a bath maintained at 50 TC (122 2F) (see 5.1.1). Protect the contents of the test tube from strong light during the test. After 3 h 5 min in the bath, examine the strip as described in 9.2. For tests on fuel oil and diesel fuel; to specifications other than ASTM Specifications D396 and D975, a temperature of 100C (212F) for 3 h is often used as an alternative set of conditions. 9.1.4 For cleaners (Stoddard) solvent and kerosine-- Carry out the test exactly as described in 9.1.3 but at 1Q0 TC (212 2F). 9.1.5 For lubricating oil--Tests can be carried out for varying times and at elevated temperatures other than 1Q0C (212F). For the sake of uniformity, it is suggested that even increments of 50F beginning with 250F (or Celsius equiva lents to the nearest whole degree) be used. 9.2 Strip Examination: 9.2.1 Empty the contents of the test tube into a 150-mL tail-form beaker, letting the strip slide in gently so as to avoid breaking the beaker. Immediately withdraw the strip with stainless steel forceps and immerse in wash solvent. With draw the strip at once, dry with quantitative filter paper (by blotting and not by wiping), and inspect for evidences of tarnishing or corrosion by comparison with the Copper Strip Corrosion Standards. Hold both the test strip and the standard strip plaque in such a manner that light reflected from them at an angle ofapproximately 45 will be observed. 9;2.2 In handling the test strip during the inspection and comparison, the danger of marking or staining can be avoided if it is inserted in a flat tube (see Appendix XI) which can be stoppered with absorbent cotton. 10. Interpretation 10.1 Interpret the corrosiveness of the sample accordingly as the appearance ofthe test strip agrees with one ofthe strips of the ASTM Copper Strip Corrosion Standards. 10.1.1 When a strip is in the obvious transition state between that indicated by any two adjacent standard strips, judge the sample by the more tarnished Standard Strip. Should a strip appear to have a darker orange color than Standard Strip lb, consider the observed strip as still belonging in Classification 1; however, if any evidence of red color is observed, the observed strip belongs in Classification 2. 10.1.2 A claret red strip in Classification 2 can be mis taken for a magenta overcast on brassy strip in Classification 3 ifthe brassy underlay ofthe latter is completely masked by a magenta overtone. To distinguish, immerse the strip in wash solvent; the former will appear as a dark orange strip while the latter will not change. 10.1.3 To distinguish multicolored strips in Classifications 2 and 3, place a test strip in a 20 by 150-mm test tube and bring to a temperature of 315 to 370C (600 to 700F) in 4 to 6 min with the tube lying on a. hot plate. Adjust to 49 DUP050295715 <QP D 130 Classification Freshly polished strip 1 Designation TABLE 1 Copper Strip Classifications B Description'' sight tarnish a. Light orange, almost the same as freshly polished strip b. Dark orange 2. moderate tarnish a. Claret red b. Lavender c. Multicolored with lavender blue or stiver, or both, overlaid on.claret red d. Silvery e. Brassy or gold 3 dark tarnish a. Magenta overcast on brassy strip b. Multicolored with red and green showing (peacock), but no grey 4 corrosidn a. Transparent black, dark gray or brown with peacock green barely showing b. Graphite or lusterless black c. Glossy or jet black A The ASTM Clipper Strip Corrosion Standard is a colored reproduction of strips characteristic of these descriptions. B The freshly polished strip is included in the series only as an indication of the appearance of a properly polished strip before a test run; it is not possible to duplicate this appearance after a test even with a completely noncorrosive sample. temperature by observing a high distillation thermometer inserted into a second test tube. If the strip belongs in Classification 2, it will assume the color of a silver and then a gold strip, if in Classification 3 it will take on the appearance of a transparent black, etc., as described in Classification 4. lb. 1.4 Repeat the test if blemishes due to finger prints are observed, or due to spots from any particles of water droplets that may have touched the test strip during the digestion period. 10.1.5 Repeat the test also if the sharp edges along the flat laces of the strip appear to be in a classification higher than the greater portion of the strip; in this case it is likely that the edges were burnished during polishing. 11. Report 11.1 Report the corrosiveness in accordance with one of the classifications listed in Table 1. State the duration of the test and the test temperature. 12. Precision and Bias 12.1 In the ease of pass/feil data no generally accepted method for determining precision or bias is currently avail able. ANNEXES. (Mandatory Information) Al. COPPER QUALITY A1.1 Copper Quality A1.1.1 Hard-temper, cold-finished type-(ETP) electrolytic tough pitch copper.5 5 Conforming to Copper Development Assn. (CDA), United States of America No. 110, or to British Standard (BS) 1036: 1952, which have proper quality. A2. PRECAUTIONARY STATEMENT A2.1 Isooctane Harmful if inhaled. Vapors may cause flash fire. Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid build-up of vapors and eliminate all sources of ignition, especially nonexplosion proof electrical apparatus and heaters. Avoid prolonged breathing of vapor or spray mist. Avoid prolonged or repeated skin contact. A2.2 Aviation Turbine Fuel (Jet A or A-l, see ASTM D1655) Keep away from heat, sparks, and open flames. Keep container closed. Use with adequate ventilation. Avoid breathing vapor or spray mist. Avoid prolonged or repeated contact with skin., A2.3 Gasoline (Containing Lead) Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid build-up of vapors and eliminate all sources of ignition, especially nonexplosion-proof electrical- apparatus and heaters. Avoid prolonged breathing of vapor or spray mist. 50 DUP050295716 D 130 prolonged or repeated skin contact. oline (White or Unleaded) away from heat, sparks, and open flame. (container closed. |dth adequate ventilation;^'^ build-up of vapors and eliminate all sources of especially nonexplosion-proof electrical apparatus iters. 'd prolonged breathing of vapor or spray mist. Id prolonged or repeated skin contact. A2.S Kerosine Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing vapor or spray mist. Avoid prolonged or repeated contact with skin. A2.6 Stoddard Solvent Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing vapor or spray mist. Avoid prolonged or repeated contact with skin. APPENDIX (Nonmandatory Information) xi. o p t io n a l Us e f u l e q u ip me n t Viewing Tube 1.1 A useful flat glass test tube for holding tarnished er strips for inspection or for storage for later inspection strated and dimensioned in Fig. X1.1. XI .2 Strip Vise X 1.2.1 A useful and convenient vise for holding up to four copper strips during final polishing is illustrated and dimensioned in Fig. X1.2. * MINIMUM DIMENSION TO BE SUCH THAT A COPPER STRIP 3-2 X13 SECTION WILL ENTER B... 1 FIRE POLISH . Q-7S-VOS TUBE TO BE WITHOUT STRIAE OR SIMILAR DEFECTS ALL DIMENSIONS IN MILLIMETRES FIG. X1.1 Flat Glass Test Tube 51 DUP050295717 # D 130 |llW)PIA MCmlplX 5 DIA METRIC THREAD (OR EQUIVALENT) as M psaA) u TOd ia FIG. X1.2 Multistrip Vise The American Society for Testing am/ 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 thne by the responsible technical committee and must be reviewed every five years and tfnotrevised, either reapproved orwithdrawn. Your comments areInvited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 52 DUP050295718 ssignation: D 233 - 65 (Reapproved 1981) Standard Methods of Sampling and Testing Turpentine*1 This standard is issued under the fixed designation D 233; 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 oflast reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. 61 n o t e--Section 2 was added editorially and subsequent sections renumbered in August 1985. liiBse methods cover procedures for sampling and entine and pinene. Hsivnced Documents pp. MSTM Standards: pMethod For Distillation of Petroleum Products2 Test Method for Saybolt Color of Petroleum oducts (Saybolt Chromometer Method)3 Method of Sampling. Petroleum and Petroleum fbducts4 |p>3 Specification for Reagent Water5 ^Specification for ASTM Thermometers6 of Reagents ^Reagent grade chemicals shall be used in all tests. otherwise indicated, it is intended that all reagents fconform to the specifications of the Committee on ical reagents ofthe American Chemical Society,'where ^specifications are available.7 Other grades may be used, sided it is first ascertained that the reagent is of suffilitly high purity to permit its use without lessening the acy of the determination. ;2- Unless otherwise indicated, references to water shall derstood to mean reagent water conforming to Specifim D 1193. SAMPLING JW* Sampling 4.1 The method of sampling specified in 4.2 or 4.3 shall rused, according to the special conditions that obtain, f*4.2 From Loaded Tank Car or Other Large Vessel--The Pmposite sample taken shall be not less than Vi gal (1.9 L) lid should consist of small samples of not more than 1 qt m- 1 These methods are under the jurisdiction of ASTM Committee D-l oo Paint Jaild Related Coatings and Materials and are the direct responsibility of Subcorallnittee DOI.34 on Naval Stores. Current edition approved Oct. 26, 1965. Published December 1965. Originally I [published as D 233 - 26. Last previous edition D 233158. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. i Annual Book ofASTM Standards, Vol 05.01. 4 Discontinued, see 1983 Annual Book ofASTM Standards, Vol 05.01. 5 Annual Book ofASTM Standards, Vols 06.01 and 11.01. 6 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 7 "Reagent Chemicals, American Chemical Society Specifications;" Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by |s 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." (0.9 L) each, taken from near the top and bottom by means of a metal or glass container with removable stopper or top.8 This device, attached to a suitable pole, shall be lowered to the desired depth, the stopper or top removed, and the container allowed to fill. If a sample from close to the bottom of a tank shows a decided difference in color or appearance from samples taken at other depths, an extra bottom sample shall be taken and examined separately from the composite sample. In such case, the composite sample shall not include any portion of such bottom sample. 4.3 From Barrels and Drums--At least 5 % of the pack ages in any shipment shall be represented in the sample. The purchaser may increase the percentage of packages to be sampled at his direction, and it is recommended that every package be sampled in the case of expensive terpene hydro carbons that are bought in small quantity. A portion shall be withdrawn from about the center of each package sampled by means of a "thief" or other sampling device. The composite sample thus obtained shall be not less than 1 qt and shall consist of equal portions of not less than lh pt from each package sampled. DETECTION AND REMOVAL OF SEPARATED WATER 5. Procedure 5.1 Draw a portion by means of a glass or metal container with a removable stopper or top,8 or with a "thief," from the lowest part of the container, or by opening the bottom valve of the perfectly level tank car. If water is found in this sample, draw it all out, record the quantity, and deduct it from the total volume of liquid delivered. APPEARANCE 6. Procedure 6.1 Examine a portion of the sample after agitation to determine whether its appearance conforms to specifications. COLOR 7. Apparatus 7.1 Colorimeter Tube--The colorimeter tube shall be a straight, cylindrical tube of clear, colorless, soda-lime glass. It shall be 230 to 280 mm in length, 21 1 mm in inside diameter, and VA to lVi mm in wall thickness. The bottom may be (/) blown with the tube, ofa uniform thickness of 1.0 8 Detailed description of equipment suitable for such sampling is given in ASTM Method D 270. 53 DUP050295719 # D 233 to 1.5 mm, with the outer surface flat-ground and polished, and showing little or no distortion of the field of view when the tube is filled to a depth of 50 mm with the sample, or it may be (2) a separate colorless glass plate vitreously fused or sealed to the bottom of the cylinder, 1.0 to 1.5 mm in thickness, with the outer surface flat-ground and polished, and having a diameter, not more than 1 mm greater than the outside diameter of the cylinder. Graduation lines shall be ruled or etched on the outside of the cylinder at each 2 mm from the level of the inner surface of the bottom to a height of200 mm, each tenth line being longer and marked to show the distance from the bottom. 8. Reagents 8.1 Cobaltous Chloride (CoCl2 6H20). 8.2 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 8.3 Potassium Dichromate (K2Cr207). 9. Procedure 9.1 Fill one colorimeter tube to. a depth of from 40 to 50. mm with the sample and place over or under it (in a colorimeter, of available) a No. 2.0 yellow Lovibond glass. Place over or under a second colorimeter tube a No. 1.0 yellow Lovibond glass, and then pour the sample into this tube until the colors of the fields of vision or beams of light passing through the tubes and the superimposed glasses are as nearly alike as possible. If the difference in the depths of the columns of sample is 150 mm or more, the material is "Water-white"; ifthis difference is less than 150 mm but not less than 50 mm, the materia:! is "Standard/' 9.2 Alternative Procedure A--Compare the color of the sample in colorimeter tubes or in any other suitable appa ratus (such as ordinary 4-oz (120-mL) oil sample bottles having flat polished bottoms), with the color of an equal depth (at least 100 mm) of freshly prepared solutions containing the following amounts of K2Cr207 and CoCl2 per litre (Note 1): - Test Solution K;.Cr207 C0G2-6H2O For water-white For standard 0.0072 g 0.01 SO g 0.Q7 g 0.15 g No t e 1--These aqueous standard solutions may be conveniently made up by diluting stock solutions, as follows: Solution A--Dissolve 1.80gofcpK2Cr2O7in 1 L ofwater containing 1 tnL of HC1 (sp gr 1.19). Solution B--Dissolve 1.00 g of CoCl2 6H20 in 1 L of water containing 20 mL of HC1 (sp gr 1.19). "Water-white" Test Solution--Add 2.0 mL of Solution A to 35 mL of Solution B and dilute to 500 mL with water. "Standard" Test Solution--Add 5.0 mL of Solution A to 75 mL of Solution B and dilute to 500 mL with water. 9.3 Alternative Procedure B--Compare the color of the sample in the manner described in 7.2 with solutions of K2PtCI6. (Do not use CoCl2 with this reagent for this test.) No t e 2--These aqueous standard solutions may be conveniently made up by diluting a stock solution, as follows: Stock Solution--Dissolve 0.6225 g ofK2PtCl6 in water, add 50 mL of HQ (sp gr 1.19), and dilute to 500 mL. "Water-white" Test Solution--Dilute 22.0 mL ofthe stock solution to 250 mL. "Standard" Test Solution--Dilute 47.5 mL of the stock solution to 250 mL. These diluted solutions are relatively stable, for at least 6 months, and may be preserved for recurrent use by sealing the bottles with clean, new, tightly fitting cork stoppers that have been impregnated and water proofed by immersion in hot melted paraffin wax for 30 min. 9.4 Alternative Procedure C--Determine the color with a Saybolt Chromometer according to Test Method D 156. If the color is equal to Saybolt No. 19 or above, the material is "Water-white." If the color-fa darker than Saybolt No. 19 but not darker than Saybolt Nq: 10, the material is "Standard." ODOR 10. Procedure 10.1 Compare the odor of the sample with an agreedupon water-free reference sample kept in the dark in a completely filled, well-stoppered bottle. In the absence of such a sample, compare with samples of known purity similarily preserved. SPECIFIC GRAVITY 11. Procedure 11.1 Determine the specific gravity at 15.5/15.5CC by any convenient method having a precision of 0.0005. Determina tions made at any other temperature using apparatus stan dardized at 15.5C shall be corrected by adding to or subtracting from the observed reading 0.00082 for each degree Celsius that the temperature of the liquid is above or below 15.5C. If the determination is made with apparatus calibrated for a temperature other than 15.5C, the observed reading shall first be calculated to density at the temperature of observation, then converted to density at 15.5C by applying the above factor, and finally converted to specific gravity by dividing the calculated density by 0.999 (the density of water at 15.5C). REFRACTIVE INDEX 12. Procedure 12.1 Determine the refractive index with an accurate instrument, at 20C if possible. If determined at any other temperature, correct the reading obtained to 20'C by adding or subtracting 0.00045 for each degree Celsius that the temperature at which the determination was made is, respec tively, above or below 20C. DISTILLATION 13. Apparatus 13.1 Use the type of distillation apparatus described in Test Method D 86, with the following exceptions: 13.1.1 For testing turpentine or pinene use an ASTM Turpentine Distillation Thermometer, 76-mm (3-in.) partial Immersion, having a range from 147 to 182C, and con forming to the requirements for Thermometer 27C as prescribed in Specification El, or an ASTM Solvents Distillation Thermometer, 100-mm (3.94-in.) partial immer sion, having a range from 95 to 255C, and conforming to the requirements for Thermometer 42C as prescribed in Specification E 1. 13.1.2 Ice is not necessary in the condenser bath. It is permissible to use a glass Liebig condenser 22 in. (560 mm) 54 DUP050295720 pwith 16 in. (410 mm) in contact with the cooling Hied with an adapter to extend 1 in. (51 mm) into graduate. ure ang the receiving graduate, transfer exactly 100 sample directly into the flask, allowing none to the side tube. If the sample contains dissolved or water it is advisable to add a few small pieces of r broken glass to promote smooth distillation, thermometer, so that the top of the/mercury bulb top of the contraction chamber if the Solvents in Thermometer is used) is level with the bottom of itube. Connect the side tube to the condenser, with im ofthe flask resting securely in the opening in the Aboard. Apply heat cautiously, and regulate it so that drop of condensate falls from the condenser in not _ 5 nor more than 10 min. Record as the initial point the thermometer reading when the first drop 1 the end Ofthe condenser, correcting for barometric as described in Section 15. When the distillation regulate the heat so that the distillate is collected at a not less than 4 nor more than 5 mL/min (apprOxi2 drops/s). Discontinue the distillation-when the iture reaches that specified for the minimum pere requirement (usually 170C for turpentine), after g for barometric pressure. Allow the condenser to read the percentage distilled. .2 The percentages distilled below successive selected tatures and the temperature at which each successive distills may also be determined, if desired, making the correction of the temperature for barometric e. -Barometric Correction 5.1 The distilling temperature ofturpentine (and pinene) ected by 0.052"C for each millimetre) variation of the 'ospheric pressure. Therefore, the distillation temperaobserved or specified shall be corrected to permit ation to be conducted as though the barometer reading, cted to 0C, were exactly 760 m T5.2 When about to begin the distillation, observe and the barometric pressure and the temperature of the ometer.' (No temperature correction is necessary for eroid-type barometers.) From Table 1 determine the proper temperature correction corresponding to these atanospheric conditions, interpolating to the nearest 0.1C. If : the barometric pressure, corrected to CFC, is below 760 mm, the temperature correction must be added to the initial boiling point and subtracted from the minimum percentage requirement temperature; if above 760 mm, the correction must be subtracted from the initial boiling point and added to the minimum percentage requirement temperature. No t e 3: Example--Suppose the observed barometric pressure is 748 mm at 32C, and the initial boiling point is observed to be 155.2C. From Table 1 the temperature correction is seen to be 0.8C. Therefore, the corrected boiling point is 155.2 + 0.8 = 156"C. Furthermore, the temperature observation point at the minimum percentage requirement (170*C at 760 mm) must he altered to the same extent Since the turpentine is distilling 0.8'C below what it would at normal pressure, distillation must be discontinued at 169.2C to determine the percentage distilling below 170"C at 760 mm pressure. TABLE 1 Temperature Corrections for Barometric Pressure4 Observed Mercurial Barometer Barometric Aneroid Temperature of Barometer Pressure, Barometer mm 20C 25C 30C 35C 780 -1.04 -0.91 -0.8B -0.64 -0.81 770 --0.52 -0.39 -0.36 -0.32 -0.29 780 0.00 +0.13 +0.16 +0,19 +0.22 750 +0.52 +0.65 +0.68 +0.71 +0.74 740 +1.04 +1.17 +1.20 +1.23 +1.26 730 +1.56 +1.68 +1.71 +1.75 +1.78 720 +2.08 +2.20 +2.23 +2.26 +2.29 710 +2.62 +2.72 +2.75 +2.78 +2.81 700 +3.16 +3.24 +3.27 +3.30 +3.33 4 These corrections are calculated as follows: The observed barometric pressure Is first corrected to what It would be at 0C, by means of the table In Circular F, Instrument Division, U. S. Weather Bureau. The corrected barometric pressure is then subtracted from 760 mm {or vice versa) and tha difference multiplied by 0.052C to give the temperature correction shown in the above table. The correction factor, C. of 0.052I,C was calculated using the Sydney-Young equation: C = 0.00012 {760 - PK273 + 7) where: P = observed pressure, corrected to 0C, in millimetres, and T = median boiling temperature for turpentine, 160C. POLYMERIZATION 16. Scope 16.1 This test determines the presence of nonterpenic material that is not characteristic of normal turpentine and is not polymerized by fuming sulfuric acid of specified concen tration. The test must be performed under closely controlled conditions if reliable results are to be obtained. The entire procedure should be carefully studied before performing the test. 17. Apparatus 17.1 Pipet, 20-mL, fitted with an acid-resistant pipet bulb (not required when the apparatus shown in Fig. 1 is available). 17.2 Pipet, 5-mL, or buret, 10-mL, funnel-top. 17.3 Babcock Milk Test Bottle, 6'/2-in. (165.1 mm), 18 g, 8 % in 0.1 % divisions. Each small division equals 0.02 mL and is equivalent to 0.4 % for a 5-mL sample of turpentine. 17.4 Cold Water Bath, maintained at 5 to 15"C. 17.5 Hot Water Bath, maintained at 60 to 65"C. 17.6 Centrifuge, to take the Babcock test bottles. 18. Reagent 18.1 Sulfuric Acid (38 N)--In a tared, glass-stoppered 500-mL bottle (a 2V2-L acid bottle may be used for larger quantities) mix concentrated sulfuric acid (H2S04, sp gr 1.84) with fuming sulfuric acid (Note 4). If the concentration of the fuming acid is designated by its content of free sulfur trioxide (S03), the following proportions by weight will ordinarily yield mixtures slightly stronger than 38 N: Free SOj in Fuming Sulfuric Acid, % 50 20 to 30 15 to 20 Parts by Weight of Fuming Sulfuric Acid ioo 100 100 Parts by Weight of H2SOa (spgr 1.84) 150 75 50 After mixing, determine the H2S04 content of the mixed acid by titrating a diluted aliquot with standard alkali, observing all precautions necessary for the accurate analysis 55 DUP050295721 D 233 FIG. 1 Acid Bottle and Pipet of fuming acids. In the same manner determine the per centage of H2S04 in the stock of concentrated H2S04 (sp gr 1.84) . prom these data calculate the quantity ofH2S04 (sp gr 1.84) that must be added to the mixed acid to give a concentration of 100.92 % of H2S04. No t e 4--Fuming sulfuric acid containing oxides of nitrogen should not he used. 18.2 After adjusting the concentration of the mixed acid, thoroughly shake the bottle of mixed acid and again deter mine its H2S04 content (Note 5). The finished acid shall have an H2S04 content of ,100.92 0.15 %. No t e 5--The add should be .checked when made, and periodically thereafter, by running a polymerisation on a turpentine or alpha-pinene ' of known residue content. 18.3 .Special precautions must be taken to prevent absorp tion of moisture by the 38 N H2S04. The design ofa suitable acid storage and delivery bottle and pipet is shown in Fig. 1. With the three-way stopcocks A and B in the position shown, acid is siphoned into the pipet P, the displaced gir passing into the bottle. By turning first A and then B, the pipet empties into the small bottle, air passing in at a. The acid adhering to the walls of the pipet dries the air that passes back into R on the next filling, thus preventing dilution of the acid remaining in R. When not in use, both stopcocks should be closed. If such an arrangement is not available, the acid should be kept in bottle of not more than 500-mL capacity with tight-fitting glass of TFE-fluorocarbon stop pers. The measured portions should be withdrawn with a suitable pipet (see 17.1). 19. Procedure 19.1 Introduce 20 mL of the 38 N H2S04 into the Babcock bottle, stopper lightly (cork or cotton plug), and place in the cold water for 15 min. Swirl the bottle occasionally to cool the acid to uniform temperature. Grasp the bottle with the thumb)and middle finger at the junction of the neck and bottle, supporting the body ofthe bottle with the fourth and little finger,);with the forefinger held against the neck. With the other hjafnd, add 5 mL of the turpentine from a pipet or buret, dropwdse in 0.5-mL portions. After each addition, tilt the bottlg at a 30 to 45 angle (away from the face) and shake vigorously with a rapid sidewise or oscillating motion. To obtain thorough mixing, the bottle; should be: shaken 40-to 50 times .(10 to 15 s) after each addition of turpentine. The- reaction should be allowed to subside between subsequent additions of turpentine. The reaction rate and temperature must be controlled at about 60 to 65C (this temperature is uncomfortable to the hand and can be estimated closely enough by touch). Stop the shaking and return the bottle to the cold water bath if the.reaction becomes violent enough to cause excessive foaming and acid is forced up into the, neck of the bottle. Release of generated sulfur dioxide (S02) gas is facilitated by holding the bottle at an angle. Should any of the contents of the bottle be spewed from the mouth, discard and repeat the test 19.2 When the entire 5-mL sample has been added to the add, without further generation, of foam or heat on shaking, place the bottle in the warm water bath (60 to 65C), so that the water covers the bottle to slightly above the add level. Continue the vigorous, intermittent shaking for an: addi tional 10 min. Each shaking should be for 15 s, with not less than 6 shakings during the period. Observe the same precautions against foaming as before. At the end of the 10-min period, or when all frothing or foaming has subsided, remove the.botde frpm the bath and cool to room tempera ture under tap water or by permitting it to stand a suffident length of time. 19.3 Fill the bottle with H2S04 (sp gr 1.84) to bring unpolymerized residue up into the graduated neck of the bottle, centrifuge for not less than 5 min at 1200 r/min (15 min at 900 r/min, or allow, the bottle to stand, lightly stoppered, for 12 to 16 h. 19.4 Measure the volume of unpolymerized oil or residue in the neck of the test bottle to the nearest half division, reading from the top of the jundion between the acid and residue to the bottom of the upper meniscus at the top ofthe column, and adding one division to the observed reading to correct for the lower obscured meniscus if there is a measurable quantity of unpolymerized residue present. 20. Calculation and Report ' 20.1 Multiply the reading by 0.4 and report as the percentage of unpolymerized residue. Duplicate tests should agree within 0.4 %\ otherwise the test should be repeated. Note the consistency and color of the unpolymerized residue and determine its refractive index at 20C ifgreater than 2 %. If the results exceed 2.0 %, a similar test should be run on a sample of known purity and polymerization residue, in order to check the technique and acid strength. EVAPORATION RESIDUE 21. Procedure 21.1 With a small pipet, deliver approximately 10 g (12 mL) of turpentine into a tared, flat-bottom, straightside 56 DUP050295722 D 233 or glass (milk evaporating) dish 75 to 80 mm in d 18 to 20 mm in depth. Weigh to the nearest % the dish on a boiling water or steam bath for , Remove the dish, wipe off the outside, and oven maintained at 105 2C for an additional ~oVe, cool in a desiccator, and weigh, ffiace the dish in the oven for an additional 15 min "~ol and weigh. If the loss in weight for such an .^eating period does not exceed 0.02 g, record this y as the end point of the test. If the loss in weight ih an additional period exceeds 0.02 g, repeat the heating periods until.the loss in weight for such a '"t not exceed 0.02 g. tion and Report jrtract the tare weight of the dish from the last obtain the Weight of residue. Calculate and report tage of evaporation residue to the nearest 0.1 %, isioa duplicate teste should agree within 0.2 %. ACIDITY -Alcoholic Potassium Hydroxide, Standard Solution Prepare a solution of 6.6 g potassium hydroxide in either 82 %. isopropyl alcphol or 90 % methyl J as follows: Dissolve 6.6 g of KOH in 100 mL of ze water and dilute to 1 L with either 91% panol or 99.5 % methanol; or dissolve 6.6 g of KOH in L of water and dilute to 1 L with 99 % isopropanol. ze to the nearest 0,001 N against primary standard Potassium arid phthalate, or against an 0.1 AT acid ,J:p that has been standardized to the nearest 0.001 N. 6--An 0.1 Absolution of KOH in 95 % ethyl alcohol may also 24.3 Sodium Chloride Solution (100 g/L)--Dissolve 100 g of sodium chloride (NaCl) in 1 L of water. Neutralize to the phenolphthalein end point 24.4 Solvent--Neutral isopropyl alcohol, of either the 99 % (preferred) or 91 % grade. Prepare by adding alcoholic KOH solution dropwise until a pink color is obtained with 25. Procedure 25.1 Measure 100 mL of turpentine in a graduated cylinder and transfer to a 500-mL separatory funnel. Add 100 mL of NaCl solution, stopper, and shake vigorously for about 20 s. Mow to settle and draw off all the salt solution into a 250-mL Erlenmeyer flask. Do not wash the turpen tine. Titrate the salt solution with KOH solution, using 0.5 mL of phenolphthalein indicator solution. 25.2 Draw the turpentine into a 300-mL Erlenmeyer flask and wash the separatory funnel twice with 50-mL portions of isopropyl alcohol solvent, adding these washings to the turpentine. Shake to effect solution of the turpentine in the solvent, add 0.5 mL of phenolphthalein indicator solution, and titrate with KOH solution to a light pink end point that persists for 1 min or more, keeping the flask stoppered. 26. Calculation and Report 26; I Calculate separately the water-soluble add number and the alcohol-soluble add number, in milligrams of KOH per gram of sample, as follows: Acid number = {AN x 56.1)/86 where: A - millilitres of KOH solution required for titration (see 25.1 for water-soluble add number and 25.2 for alcohol-soluble acid number), N = normality of the KOH solution, and 86 = assumed weight in grams of the 100-mL sample used. 26.2 Report the results to the second dedmal place. ,2 Phenolphthalein Indicator Solution' (10 g/L)--Dis1 g ofphenolphthalein in 100 mL ofneutral 95 % ethyl hoi. 27. Precision 27.1 Duplicate results should agree within 0,02 AN, where A and N are defined as in 26.1. The American Society for Testing and Materials takas noposition respecting the validity ot anypatent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, end the risk ot Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and It not revised, either reapproved or withdrawn. Yourcomments areInvitedeitherfor revision otthisstandardorforadditional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful conalderatlon 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. 57 DUP050295723 Designation: D 234 - 82 (Reapproved 1991)' Standard Specification for Raw Linseed Oil1 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 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. {|No t e--Keywords were added editorially in August 1991. 1. Scope 1.1 This specification covers raw linseed oil. 2. Referenced Documents 2.1 ASTM Standards: D93 Test Methods for Hash Point by Pensky-Martens Closed Tester2 , D555 Guide for Testing Drying Oils3 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4 D1639 Test Method for Add Value of Organic Coating Materials5 D1954 Test Method for Foots in Raw Linseed Oil (Volumetric Method)3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 D1960 Test Method for Loss on Heating of Drying Oils3 D1962 Test Method for Saponification Value of Drying Oils, Fatty Adds, and Polymerized Fatty Acids3 D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 3 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 D1966 Test Method for Foots in Raw linseed Oil (Gravimetric Method)3 1 This specification is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of DO 1.32 on Drying Oils. . Current edition approved June 25,1982. Published September 1982. Originally published as D 234 - 26 T. Last previous edition D234 - 72 (1976). 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. TABLE 1 Properties of Raw Linseed Oil Property Requirement Specific gravity, 25/25C Acid value, max Saponifcatiorj value Unsaponifiable matter, max, % Iodine value (Wijs), min Loss on heating at 105 to 110C, max, % Clarity Color (Gardner), max Foots, volumetric, heated oil, max, % Foots, volumetric, chilled oil, max, % Gravimetric foots, max %, Flash point, min, F 0.926 to 0.931 4.0 189.0 to 195.0 1.50 177 0.2 clear and transpar ent at 65"C 13 1.0 4.0 0.25 250 ASTM Method D1963 D1639 D1962 D1965 D1959 ' D1960 D2090 D1544 D1954 D1954 D1965 D93 D2090 Test Method for Clarity and Cleanness of Paint and Ink liquids6 3. Properties 3.1 Linseedjoil shall be the oil obtained from flaxseed and shall conform to the requirements given in Table 1. No t e--It is recognized that raw linseed oil is a natural product and that, in unusual crop years, the color, iodine value and acid value may vary from the stated specification limits. In this case the limits shall be agreed upon between the purchaser and the supplier. 4, Test Methods 4.1 Sampling--Sampling should be conducted in accor dance with Test Method D 1466. 4.2 The properties enumerated in this specification shall be determined in accordance with the applicable ASTM methods listed in Table 1. The significance ofthe methods of testing enumerated under properties in this specification is discussed in Guide D 555. 5. Keywords 5.1 drying oils; linseed oil 6 Annual Book ofASTM Standards, Vols 06.02 and 06.03. 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 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 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. 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. 58 DUP050295724 Designation: D 235 - 87e1 Standard Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)1 This standard is issued under the fixed designation D 235; 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. This specification has been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. fl No t e--Table I was editorially corrected in October 1988. cope *L1 This specification covers four types of hydrocarbon |R'ents, normally petroleum distillates, used primarily in je coatings and dry-cleaning industries. "Mineral spirits" is he most common name for these solvents. ^Referenced Documents ,, ASTM Standards: ,56 Test Method for. Flash Point by Tag Closed Tester2 ;6 Method for Distillation of Petroleum Products2 130 Test Method for Detection of Copper Corrosion I from Petroleum Products by the Copper Strip Tarnish Test2 H 56 Test Method for Saybolt Color of Petroleum ^Products (Saybolt Chromometer Method)3 p268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Materials4 fb 1133 Test Method for Kauri-Butanol Value of Hydro carbon Solvents4 ll'' >1159 Test Method for Bromine Number of Petroleum Distillates and Commercial Aliphatic Olefins by ; Electrometric Titration3 tD 1209 Test Method for Color of Clear Liquids (Platinum- I Cobalt Scale)5 :jD 1296 Test Method for Odor of Volatile Solvents and IV Diluents4 | D 3227 Test Method for Mercaptan Sulfur in Gasoline, Kerosine, Aviation Turbine, and Distillate Fuels (Poten- tiometric Method)6 D3257 Test Method for Aromatics in Mineral Spirits by Gas Chromatography4 D3278 Test Method for Flash Point of .Liquids by Setaflash Closed-Cup Apparatus4 This specification is under the jurisdiction of ASTM Committee D-l on faints and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.35 on Solvents. Plasticizers, and Chemical Intermediates. Current edition approved Nov. 27, 1987. Published January 1988. Originally lublishcd as D 235 - 26. Last previous edition D 235 - 83. 2 Annual Book ofASTM Standards. Vols 05.0 land 06.03. ' Annual Book rtfASTM Standards, Vol 05.01. 1 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards. Vols 06.01 and 06.03. h Annual Book ofASTM Standards. Vol 05.02. E 300 Practice for Sampling Industrial Chemicals4 2.2 U.S. Federal Specification: PPP-C-2020 Chemical, Liquid, Dry, and Paste: Packaging of7 '3. Classification 3.1 Mineral spirits shall be of the following types as specified: 3.1.1 Type I--Regular (Stoddard Solvent). 3.1.2 Type II--High Flash Point. 3.1.3 Type III--Odorless. 3.1.4 Type IV--Low Dry Point. 4. Properties 4.1 The physical and chemical properties of the different types of mineral spirits shall conform to the requirements specified in Table 1.: 5. Sampling 5.1 The material shall be sampled in accordance with' Recommended Practice E 300. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 6.1.1 Bromine Number--Test Method D 1159. 6.1.2 Color--Test Method D 156 or Test Method D 1209. In case of dispute, Test. Method D 156 shall be the referee method. 6.1.3 Corrosion--Method D 130. Perform test under the prescribed conditions for 3 h at 100C. 6.1.4 Distillation--Test Method D 86. 6.1.5 Flash Point--Test Method D 56 or Test Method D 3278. In case of dispute, Test Method D 56 shall be the referee method. 6.1.6 Kauri-Butanol Value--Test Method D 1133. 6.1.7 Odor--Test Method D 1296. Samples of particular types of products being tested, having odor characteristics satisfactory to consumer and producer, are to be used as reference standards for comparison. 6.1.8 Mercaptan Sulfur--Test Method D 3227. 7 Available from Standardization Documents Order Desk, BJdg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 59 DUP050295725 # D 235 TABLE 1 Physical and Chemical Properties of Mineral Spirits A Type 1 Type II Type III Type IV Commercial Reference Appearance Flash point, min, F (C) Color, min Kauri-Butanol value: min max Bromine Number, max Odor Doctor test Distillation, F (C): Initial being point, min 50 % recovered, max Dry point, max Residue from distillation: % max Addity Copper'corrosion, max rating Apparent SpecifioGravlty 60/60F (15.6/15.6C) min max regular mineral spirits (Stoddard solvent) high flash point odorless low dry point dear and free of suspended matter and undissolved water when observed at 60-7SF (15.6-25.6C) 100 (38) 140(60). 100 (38) 100 (38) not darker than +25 on the Saybolt Scale or 25 on the Pt-Co Scale 29 45 S negative 29 45 29 55 characteristic, as agreed between purchaser and supplier negative negative 29 45 5 negative 300(149) 360(182) 415(213) 350(177) 385 (196) 415(213) 300(149) 385(198) 415 (213) 300 (149) 345 (174) 365 (185) 1.5 neutral 2A 1.5 neutral 2A 1.5 neutral 2A 1.5 neutral 2A 0.754 0.820 0.768 0.820 0.775 0.754 0.800 A "Mineral spirits' of all the Types I--IV may be commercially available to meet certain local air pollution regulations (for example, "Rule 66") that limit C8 arid higher aromatics to not more than 8 volume %, olefins to not more than 5 volume %, end total aromatic plus olefins to not more than 20 volume %. : 1 6.1.9 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 15.6C. See Methods D 268. 6.1.10 Doctor Test: 6.1.10.1 Preparation of Doctor (Sodium Plumbite) Solu tion--Dissolve approximately 125 g of sodium hydroxide (NaOH) in 1 L of reagent water. Add 60 g of lead monoxide (PbO) and shake vigorously for 15 min., or let stand with occasional shakings for at least a day. Allow to settle and decant or siphon off the clear liquid. If the solution does not settle clear, filter it through filter paper. Keep the solution in a tightly corked bottle and refilter before use if not perfectly clem". 6.1.10.2 Procedure--Shake vigorously together in a test tube 10 mL of the solvent being tested and 5 mL of sodium plumbite solution for about 15 s. Add a small amount of pure, dry flowers of sulfur so that practically all of its floats on the interface between the solvent and the sodium plumbite solution after shaking. Again shake for 15 s, allow to settle and observe within 2 min. 6.1.10.3 Interpretation ofResults--If the solvent is discol ored or if the yellow color of the sulfur film is noticeably masked, consider the test positive and the solvent as "sour". Ifthe sample remains unchanged in color and the sulfur film is bright yellow or. only slightly discolored with gray or flecked with black, consider the test negative and the solvent as "sweet". 6.1.10.4 If the doctor test result is positive, mercaptan content may be determined using Test Method D 3227 and reported. 6.1.11 Aromatics--Test Method D 3257. 7. Packaging and Package Marking 7.1 Package size shall be agreed upon by the purchaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall' conform to Fed. Spec. PPP-C-2020. The American Society lot 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 standard Is subject to revision af any time by the responsible technical committee and most be reviewed every five years and ifnot revised, either reapproved or withdrawn. Yourcomments are invited either for revislori'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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 60 DUP050295726 Designation: D 260 - 86 (Reapproved 1990} Standard Specification for Boiled Linse&d Oil1 This standard is issued under the fixed designation D 260; 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. ["Scope r! 1 This specification covers two types of boiled linseed Jr IjLl Type I, Regular Boiled, and pZ Type IT; Double Boiled. ieirenced Documents ASTM Standards: 1564 Test Methods for Liquid Paint Driers2 |j|475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products3 1'544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4 '1639 Test Method for Acid Value of Organic Coating Materials3 ir D 1951 Test Method for Ash in Drying Oils and Fatty Acids2 D 1953 Test Method for Drying Properties of Drying Oils5 D 1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 D 1960 Test Method for Loss on Heating of Drying Oils2 D 1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Adds2 D 1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 2 D1965 Test Method for Unsaponifiable Matter in Drying . Oils, Fatty Adds, and Polymerized Fatty Adds2 D2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids6 3. Properties 3.1 Boiled linseed oil shall conform to the requirements shown in Table 1. * This specification is under thejurisdiction ofASTM Committee 0-1 on Paint l Related Coatings and Materials and is the direct responsibility of Subcomllttee DO1.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 260, r 27 T..Last previous edition D 260 - 80. fr 2'Annual Book ofASTM Standards, Vol 06-03., Annual Book ofASTM Standards, Voi 66.01. 14 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 4. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance with the appropriate ASTM methods given in Table 1. 5 Discontinued; see 1980 Annual Book ofASTM Standards, Part 29. 6 Annual Book ofASTM Standards, Vols 06.02 and 06.03. ft- -.rrr---:----------------------------------- :-- Specific gravity, 25/25C Acid value, max Saponification value Unsaponifiable matter, max, % Iodine value (Wijs), min Loss on heating at 105 to 110"C, max, X Appearance at 65C Gardner color, max Set-to-touch time, max, h Ash, max. % TABLE 1 Physical Properties ' Type 1 Type II ' 0.928 to 0.938 7.5 189 to 195 1.5 170 0.4 clear and transparent 15, approximately 16 ' 0.50 0.930 to 0.945 8.0 190 to 198 1.5 165 0.6 dear and transparent 15, approximately 8 0.60 ASTM Methods D 1963, D 1475 D 1639 D1962 D 1965 D 1959 D 1960 D2090 , D1544 D 1953 D 1951, D 564 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 ofInfringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if notrevised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards 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 views known to the ASTM Committee on Standards, 1915 Race St., Philadelphia, PA 19103. 61 DUP050295727 Designation: D 268 - 90 Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material1 This standard is issued under the fined designation D 268; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedforme by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This guide covers procedures for the sampling and testing of volatile solvents used in the manufacture of paint, lacquer, varnish, and related products. The test methods are listed in Table 1. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe User of this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 13 Specification for Spirits of Turpentine2 D 56 Test Method for Flash Point by Tag Closed Tester2 3 D86 Method for Distillation of Petroleum Products2'3 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2'3 D156 Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method)3 D233 Methods of Sampling and Testing Turpentine2 D 235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)2'3 D 329 Specification for Acetone2 D611 Test Method for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents2-3 D847 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons2 D 848 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons2 D 849 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons2 D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials2 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 OOl .35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Sept. 12,1990. Published November 1990, Originally published as D 268 - 27 T. Last previous edition D 268 - 85l. 2 Annual Book ofASTM Standards, Voi 06.03. 3 Annual Book ofASTM Standards, Vol 05.01. D853 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons2 D 891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals4 D1078 Test Method for Distillation Range of Volatile Organic Liquids2 D1133 Test Method for Kauri-Butanol Value of Hydro carbon Solvents2 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)2's D1296 Test Method for Odor of Volatile Solvents and Diluents2 D1310 Test Method for Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus2-5 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D1363 Test Method for Permanganate Time of Acetone .. and Methanol2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1476 Test Method for Heptane Miscibility of Lacquer Solvents2 D1555 Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons2'3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D 1614 Test Method for Alkalinity in Acetone2 D1616 Test Method for Copper Corrosion by Mineral Spirits6 D1617 Test Method for Ester Value of Solvents and Thinners2 D1720 Test Method for Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions2 D1722 Test Method for Water Miscibility of WaterSoluble Solvents2 D 2192 Test Method for Purity ofAldehydes and Ketones2 D 2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography2 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vol 06.01. 6 Discontinued, see 1981 Annua! Book ofASTM Standards, Pari 29. 62 M DUP050295728 # 0 268 TABLE 1 List of Test Methods Test Method Section ASTM Method Hydrocarbons prevents Klor of aromatics Ketones gjimineral spirits iim cobalt scale skm test: hydrocarbons Spirits jgnge: Biydrocarbons prils, turpentine teado liquids jig...: SP' Hlartens dosed cup Usd cup MBFtes*ter prays: Bifand propylene glycols M'i' pics h aromatics pmatter Maromatfcs fanate time for acetone and meth- 11 D847 11 D 1613 23 D 848 18 D 2804, D 3329 12 D 1614 25 D 3257 6 D 1209 14 D 849 14 D 1616 7 P 850 7 D 86 7 D1078 13 D 1617 13 3545 17 D 93 17 0 56 17 D 1310 17 D 3.278 22 E 202 21 E346 24 0 2360 8 D 1353 9 D1296 24 0 2360 16 D1363 ketones ghv 18 D 2192, D 2804, D 3329, D 3893 it . : 4 E 300 Hower evaluation: K'point and mixed aniline point of 19 D 611 Kpleum.products and hydrocarbon Hnntt SKitanol value of hydrocarbon 19 D1133 p/ents Ki ratio in cellulose nitrate solution 19 D1720 pactive solvents, hydrocarbon diluBts, and cellulose nitrates lc gravity jp " 5 D 891, D 2935, D 3505, D 1555 las hydrogen sulfide and sulfur dioxide 15 0953 Iher reagent titration method 10 D1364, E 203 bidtty method 10 D1476 imlscibility of water-soluble solvents20_____________ D1722 H2804 Test Method for Purity of Methyl Ethyl Ketone llEtrsing Gas Chromatography2 . Hp2935 Test Method for Apparent Density of Industrial fifeAromatic Hydrocarbons2 HI 3257 Test Methods for Aromatics in Mineral Spirits by Gas Chromatography2 mb 3278 Test Methods for Flash Point of Liquids by la. Setaflash Closed-Cup Apparatus2 BP 3329 Test Method for Purity of Methyl Isobutyl Ketone fijt by Gas Chromatography2 fc) 3505 Test Method for Density or Relative Density of Sr Pure Liquid Chemicals2 D3545 Test Method for Alcohol Content and Purity of j| Acetate Esters by Gas Chromatography2 p! D3893 Test Method for Purity of Methyl Amyl Ketone s and Methyl Isoamyl Ketone by Gas Chromatography2 >E 12 Terminology Relating to Density and Specific Gravity of Solids, Liquids, and Gases4 E 201 Method for Calculation of Volume and Weight of Industrial Chemical Liquids4 Er202 Test Method for Analysis of Ethylene Glycols and , -.r Propylene Glycols4 E 203 Test Method for Water Using Karl Fischer Reagent4 . E 300 Practice for Sampling Industrial Chemicals2-4 E 346 Method for Analysis of Methanol4 3. Significance and Use 3.1 A brief discussion of each test method is given with the intent of helping the user in the selection of the most applicable procedure where more than one is available. 4. Sampling 4.1 Representative samples are a prerequisite for the evaluation of any product. The directions for obtaining representative samples cannot be made explicit to cover all cases and must be supplemented by judgment, skill, and sampling experience. It is recommended that Practice E 300 be employed in sampling liquid solvents. 5. Specific Gravity 5.1 Specific gravity of liquids is defined in Definitions E 12 as "the ratio of the mass of a unit volume of a material to the mass of the same volume of gas-free distilled water at a stated temperature." When the stated temperature of the water is 4.0C, specific gravity and density are numerically equal. 5.2 The apparent specific gravity of liquid is defined in Definitions E 12 as "the ratio of the weight in air of a unit volume of material at a stated temperature to the weight in air of equal density of an equal volume of gas-free, distilled water at a stated temperature." No t e 1--Specific gravity or density is an intrinsic property of all substances and can to a degree be used to identify them. When such substances are of high purity, specific gravity may be used in support of other properties to define their degree of purity. The use of specific gravity for such purposes, however, is valid only when all components and their relative effects upon the specific gravity of the system are known. 5.3 The choice of test method for determining specific gravity is largely dependent on the degree of accuracy required. In general, when the product specification requires an accuracy to the third decimal place, the hydrometer or specific gravity balance method may be employed. When the product specification requires an accuracy to the fourth decimal place, a pycnometer method should be employed. Test Methods D891 give procedures using all three tech niques. 5.4 With specific reference to the determination of density or specific gravity of a number of aromatic and cyclic hydrocarbon solvents, Test Method D 3505 describes a simplified procedure for this measurement. 5.5 Methods for converting specific gravity data to weight and volume data -at various temperatures are given in Method E 201 for oxygenated and chlorinated compounds, and for aromatic hydrocarbons in Method D 1555. 5.6 The measurement of density of aromatic hydrocar bons at any convenient temperature, and the conversion of the data to an applicable specification or storage temperature are described in Test Method D 2935. DUP050295729 # D 268 6. Color 6.1 The property of color of a solvent will vary in importance with the application for which it is intended, the amount of color that can be tolerated being dependent on the color characteristics of the material in which it is used. The paint, varnish, and lacquer Solvents, or diluents com mercially available on today's market normally have little or no color. The presence or absence of color in such material is an indication of the degree of refinement to which the solvent has been subjected or of the cleanliness of the shipping or storage container in which it is handled, or both (see Test Method D 1709). No t e 2--For a number of years the term "water-white" was consid ered sufficient as a measurement of solvent color. Several expressions for defining "water-white" gradually appeared and it became evident that a more precise color standard was needed. This was accomplished in 1952 with the adoption of Test Method D 1209 using the platinum cobalt scale. This method is similar to the description given in the Standard Methods for the Examination of Water and Waste Water of die American Public Health Assn., 14th Ed;, p. 65 and is referred to by many as "APHA Color," The preparation ofthese platinum-cobaltcolor standards was originally described by Hazen, A., American Chemical Journal, Vol. XIV, 1892, p. 300, in which he assigned the number 5 (parts per ten thousand) to his platinum-cobalt stock solution. Subse quently, in their first edition (1905) of Standard Methods for the Examination of Water, the American Public Health Assn., using exactly the same concentration of reagents, assigned to color designation 500 (parts per million) which is the same ratio. The parts per million nomenclature is not used since color is not referred directly to a weight relationship. It is therefore recommended that the incorrect term "Hazen Color" should not be used. Also, because it refers primarily to water, the term "APHA Color" is undesirable. The recommended nomenclature for referring to the color of organic liquids is "PlatinumCobalt Color, Test Method D 1209." No t e. 3--The petroleum industry uses the Saybolt colorimeter Test Method D 156 for measuring and defining+he color of hydrocarbon solvents; however, this system of color measurement is not commonly employed outside of the petroleum industry. It has been reported by various sources that a Saybolt color Of +25 is equivalent to 25 in the platirium-cobalt system or to colors produced by masses of potassium dichromate ranging between 4.8 and 5.6 mg. dissolved in 1 litre of distilled water. Because of the differences in the spectral characteristics ofthe several color systems being compared and the subjective manner in which the measurements are made, exact equivalencies are difficult to obtain. 7. Distillation Range 7.1 The distillation range of an oiganic solvent is an empirical set of data peculiar to the solvent under study and the apparatus used giving the purchaser an indication of the product quality available to him. No t e 4--The distillation range provides information on the initial boiling point, percent distilled at certain temperatures, and the dry point. These parameters may be affected by improper refining tech niques, impurities inherent in the sample, or contamination. It is absolutely necessary that the purchaser and seller employ the same type ofapparatus, including thermometers, and follow an identical procedure as agreed upon. If these factors are not followed precisely, it is quite possible disagreement will result between the parties. 7.2 Three test methods are available for determining the distillation range of solvents. The major differences among the three methods are the size of distillation flasks and type of thermometers (partial or total immersion) employed. Flask size has little to no effect on the results obtained between laboratories beyond the limits of error noted for each test method. The advantage of the larger size flask is to prevent "boil over" when high-boiling products, processing relatively high coefficients of expansion are being tested. On the other hand, differences between laboratories will be large when one laboratory employs a partial immersion thermom eter and another a total immersion instrument. The spread between results will increase as the boiling range rises above 100C. Partial immersion thermometers are preferred for narrow boiling products since they require no emergent stem temperature correction. The type of heat source may affect the distillation range of products boiling within 1 or 2C. This is especially true for low-boiling solvents such as methyl alcohol or acetone. A large electric heater tends to distort the | dry point due to the heating effect of infrared radiation on j the bulb of the thermometer, while a properly adjusted gas ; burner minimizes this effect. The following test methods are commonly used in determining distillation ranges; 7.2.1 Test Method D1078, using a 200-mL flask, high- I precision partial immersion thermometers, and gas or elec tric heat. The latter may be used only after it has proven to give results comparable to those obtained when using gas heat. The method was designed specifically for determining j the distillation range of volatile solvents used in coating J compositions, but is applicable to any volatile organic liquid ! that boils between 3G and 300C, and is chemically stable during the distillation process. 7.2.2 Test Method D 850, using a 200-mL flask, partial i immersion thermometer, and electric or gas heat. This i method is'applicable to industrial aromatic hydrocarbons 1 and related products. It is particularly suited to narrow 1 boiling hydrocarbons or mixtures of hydrocarbons. 1 7.2.3 Method D86, using a 100-mL flask for products J showing an end point below 250C, a 125-mL flask for products showing an end point above 250C, total immer- | sion thermometers, and electric or gas heat. This method is applicable to mineral spirits conforming to Specification ' D 235, and to spirits of turpentine conforming to Specifica- : tion D 13, using partial immersion thermometers in accord ance with Methods D 233, and to other hydrocarbon mix tures that have wide boiling ranges. 8. Nonvolatile Matter j 8.1 The nonvolatile matter test is run usually on volatile ij solvents capable of evaporating in a reasonable period of 1 time at 1.05C, The finding of a residue significantly higher than 5 mg/100 mL indicates the presence of either contam ination or impurities inherent in the solvent. In certain cases this may adversely affect a product, or coating system into which the solvent is introduced. See Test Method D 1353. 9. Odor 9.1 The evaluation of the characteristic odor of a solvent is a quick and simple means of identifying a material as well , as determining its suitability from an odor point of view for use in a solvent system. Residual odor may be due to " improper refining techniques,- impurities inherent in the solvent, or contamination. Whatever the source, a pro nounced residual odor may find its way into a finished product and thus adversely affect the coating system. See Test Method D 1296. 64 DUP050295730 # D 268 ter Two test methods are available for determining the or water content of a solvent: \ Test Method D1364, covers the determination of concentration in absolute terms. It is not only and accurate for the level of water found in :cially available solvents, but is applicable to a wide || materials including hydrocarbon and oxygenated Srbon solvents. The principles of the procedure are on the use of the Karl Fischer reagent, Test Method 1.2 Test Method D1476 may be used to determine er there is sufficient moisture in a solvent to cause ;ty when the solvent is mixed with n-heptane. This is limited in its usefulness in that it does not cover ement of water in absolute terms and is subject to a -tinge of sensitivity. For example, when applied to esters ier molecular weight ketones (methyl ethyl ketone igher) its. lower limit for detecting water ranges from 0.1 o, depending on the particular solvent being tested, n applied to acetone and most alcohols, its lower limit of 'tivity ranges from 0.5 to 2%, qgain depending on the pillar material. Its main advantage is to detect the gross lination of a solvent by water. Acidity T. 1 Acidity in a solvent may be due to improper refining niques, instability in storage, or contamination. Some cesses are highly sensitive to acidity while others are not. pite the fact that various acids might be involved, two ilations are commonly given for determining acidity, is, weight percent as acetic acid, and acid number is of potassium hydroxide consumed per gram of pie). The purchaser and seller must agree as to which eulation should be used for purchase specifications. See est Methods D 847 and D 1613. 2. Alkalinity No t e 5--Alkalinity is so rarely encountered in commercially avail_b|e solvents that among the solvents under the jurisdiction of Com-[lttee D-l, only Specification D 329 for acetone contains a requirement for alkalinity. 12.1 If alkalinity is suspected as a contaminant in a Solvent, determine the alkalinity in accordance with Test Method t) 1614. This method may be adapted to waterimmiscible solvents by substituting isopropyl, or ethyl al cohol conforming to Formula No. 3A ofthe U. S. Bureau of Internal Revenue, for water in the test procedure. 13. Ester Value 13.1 Test Method D 1617 may be-used to estimate the purity of an ester, the remaining portion of the material usually being the alcohol associated with the original reac tion to produce the ester. The method also may be employed to obtain the total ester content of a lacquer thinner. 13.2 Essentially pure and urethane grade acetate esters may also be analyzed by the gas chromatographic procedure, Test Method D 3545, which provides not only the ester content but also the concentration of the remaining parent alcohol. The alcohol content is of special interest with urethane grade solvents. 14. Copper Corrosion Test V14.1 The copper corrosion test normally is applied to hydrocarbon solvents (aliphatic and aromatic). However, the test also may be used in connection with oxygenated solvents. The test is a visual estimate of the presence of free and combined sulfur and is not a measure of the coiTosiveness of solvent to other metals. See Test Methods D 849 and D 1616. 15. Sulfur 15.1 Test Method D 853 indicates the presence of sulfur dioxide or hydrogen sulfide in aromatic hydrocarbons. No absolute analysis of the sulfur content is obtained. The method is not sensitive to organic sulfur compounds. The presence in a solvent of detectable sulfur compounds using this methoc} indicates the possibility of odor-forming bodies, as well as color-forming agents (color degradation in the final product),, 16. Permanganate Time Test for Acetone and Methanol 16.1 The measurement of permanganate time is a sensi tive means for detecting trace quantities of reducing sub stances such as aldehydes and unsaturates that might be present in acetone and methanol. Determine the permanga nate time of acetone and methanol in accordance with Test Method D1363. No t e 6--The significance of the impurities detected using this test is open to some question; however, the presence of trace quantities of reducing substances may have harmful effects in some chemical reactions, either alone or in combination with other reactants. 17. Flash Point 17.1 The flash point is the lowest temperature, corrected to 101.3 kPa (760 mm Hg) of pressure, of a solvent at which application of ah ignition source causes the vapor of the specimen to ignite under specified conditions of test. 17.2 There are four methods currently used to determine the flash points of volatile solvents. One uses an open cup that allows the solvent vapors to disperse into ambient air during the determination while three'use a closed cup that confines the solvent vapors. Flash point values obtained with the open cup are higher than those measured in closecj'cups. Current United States Department ofTransportation regula tions require the measurement of flash points by the appli cable closed cup procedure to define the characteristics Of a product for labelling and transport purposes. Flash points may be determined by the following methods: 17.2.1 Test Method D1310, Tag Open Cup--A tempera ture range from 0 to 325T (--18 to 168C) is covered by this instrument 17.2.2 Test Method D56, Tag Closed Cup--This appa ratus is applicable to solvents with a viscosity at 100F (38C) below 45 SUS (9.5 cSt or mm2/s at 25C) and which flash below 200*F (93C). 17.2.3 Test Methods D 93, Pensky-Martens Closed Cup-- With a range from 20 to 700F (--7 to 370C), this unit is applicable to products with flash points higher than those obtainable with either the Tag Closed Tester or the Setaflash Tester. In addition, with its stirrer it is applicable to liquids having a viscosity greater than 9.5 cSt (mm2/s) at 25C, 65 DUP050295731 D 268 having a tendency to skin over, or containing suspended solids. 17.2.4 Test Methods D3278, Setaflash Closed Tester-- The construction of this instrument permits the use of a small, 2-mL, specimen and is applicable in the range from 32 to 230F (0 to 110C) to liquids with viscosities below 150 St (1.50 mm2/s) at 77F (25C). One may determine the finite flash point of a liquid or whether the liquid will or will not flash at a certain temperature. 18. Purity of Ketones 18.1 Methyl ethyl ketone and methyl isobutyl ketone may contain small quantities of alcohols and other impurities, depending upon the process by which they were manufac tured. Test Method D 2804 may be used to determine the impurities in methyl ethyl ketone by gas chromatography and Method D 3329 is applicable to methyl isobutyl ketone. An equivalent procedure for the analysis of methyl amyl ketone and methyl isoamyl ketone Test Method D3893. 18.2 Hydroxylamine will react quantitatively with ke tones to provide a wefchemical test for assay. This procedure may be found in Test Method D 2192. 19. Solvent . Power Evaluation . . 19.1 The following three methods may be used singly, or in combination with each other; to characterize the solvency power ofhydrocarbon solvents. The test method described in 18.4 also gives a procedure for evaluating the solvency of oxygenated hydrocarbons. 19.2 Aniline Point and Mixed Aniline Point of Hydro carbon Solvents--Determine the aniline point and mixed aniline point in accordance with Test Method D 611. This method covers the determination of solvent power in terms of miscibility temperatures in the presence of aniline. High aniline points indicate the presence pf saturated hydrocar bons in major proportions. Aromatics produce low aniline points and, when present in major quantities, low mixed aniline points. 19.3 Kauri-Butanol Value ofHydrocarbon Solvents^De termine the kauri-butanol value in accordance with Test Method D 1133.. Numbers obtained by means of the kauributanol value determination represent relative solvent power of hydrocarbon solvents used in coating formulations. Re sults, however, cannot necessarily be translated into terms derived by other test methods, since hydrocarbon solvents vary in composition (ratio of aromatics to paraffins to naphthenes). Solvents from different suppliers may show identical kauri-butanol values but quite different resin solu tion viscosities. The method, therefore, is suitable for routine testing of solvents from a particular source. It also may be used as a guide in determining whether a solvent from a new source should be considered. 19.4 Dilution Ratio in Cellulose Nitrate Solutions for Active Solvents, Hydrocarbon Diluents, and Cellulose Ni trate--Determine the dilution ratio in accordance with Test Method D 1720. This method covets (a) the amount of standard toluene that can be added to a standard solution of nitrocellulose in a given oxygenated solvent, (b) the amount of a given diluent that can be added to a standard solution of nitrocellulose in standard n-butyl acetate, and (c) the amount of standard toluene that can be added to standard n-butyl acetate in a prescribed solution of nitrocellulose of varying solubility characteristics. 19.4.1 Item (a) supplies information dealing with the ability of the oxygenated solvent to withstand dilution by a standard diluent. Superior solvent power is characterized by a high dilution ratio. 19.4.2 Item (b) refers to the ability of the diluent (or nonsolvent) to dilute a standard oxygenated solvent in a standard nitrocellulose solution. Superior solvent power i& characterized by a high dilution ratio. 19.4.3 Item (c) deals with the nitrocellulose itself and its ability to withstand dilution by a standard diluent in '& standard solvent. 20. Water Miscibility of Water-Soluble Solvents 20.1 Determine water miscibility of these materials it accordance with Test Method D 1722. This method .is designed to detect the presence of trace amounts of a hydrocarbon impurity, or other water-insoluble contami nants. No t h 7--Because of modern refining techniques, there is link likelihood of any'commercially available acetone, isopropyl alcohol Si other water-soluble solvents containing even a trace ofa water-insoluble impurity. However, this method is of value in detecting such contami nation that might occur as a result ofan improperly cleaned shipping co storage container, or both. 21. Analysis of Methanol 21.1 A compilation of analytical methods, both genera and specific to methanol is presented in Method E 346. 22. Analysis of Ethylene and Propylene Glycols 22.1 A survey of analytical methods for the specificatioi testing of mono-, di-, and triethylene glycol, and mono- am dipropylene glycol is presented in Test Method E 202. 23. Acid Wash Color of Aromatic Hydrocarbons 23.1 Chemically reactive impurities in aromatic hydrocai bons may impart color to a final product. An estimate of th quantity of these compounds in aromatic hydrocarbons ma be obtained by Test Method D 848. 24. Paraffins and Other Nonaromatic Hydrocarbohs in Art nrntics 24.1 For the determination of less than 1 % nonaromati hydrocarbons in monocyclic aromatics, the applicable proci dure is Test Method D 2360. 25. Aromatics in Mineral Spirits 25.1 Determine the aromatics in mineral spirits in accor< ance with Test Method D 3257. Part A of this gas chromati graphic procedure permits the identification and calculatic of concentrations of aromatic components in accordant with the scope of the method. Part B measures only the eth benzene content by a rapid procedure. 26. Keywords 26.1 solvents; volatile solvents 66 DUP050295732 D 268 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 infrlngemeptof such rights, are entirely their own responsibility. This standard is subject to revisioli 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 of this standard or foradditional standards and should be addressed tp 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, 1915 Race St-, Philadelphia, PA 1S103. 67 DUP050295733 Designation: D 269 - 52 (Reapproved 1987)'1 Standard test Method for Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark)41 1 This standard is issued under the fixed designation D 269; the number immediately following the designation indicates the year of original adoption or, in the case ofrevirion, 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. 41 Nora--Editorial changes were made throughout in October 1987. 1. Scope 1.1 This test method covers the determination of the amount of solid matter (chiefly sand, chips, dirt, and bark) in rosin insoluble in toluene. 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: E 11 Specification for Wire-Cloth Sieves for Testing Purposes2 3. Treatment of Specimen 3.1 If the specimen is less than 200 g, immediately before making the determination, powder it to pass a No. 10 (2.00-mm) sieve, (Note) mix thoroughly, and place in a 1 This test method is under thejurisdiction ofASTM Committee D-l on Faint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO1.34 on Naval Stores. Current edition approved Sept. 30,1952. Published November 1952. Originally published'as D 269 - 27. Last previous edition D 269 - 30. 2 Annual Book ofASTM Standards, Vol 14.02. wide-mouth bottle to completely fill. No t e--Detailed requirements for this sieve are given in Specification Ell. 3.2 If the specimen is more than 200 g, immediately before the determination is made, crush it, to pass a Vz-in. (13-mm) sieve, (Note) mix, divide by quartering to about 200 g, and treat as described in 3.1. 4. Procedure 4.1 Prepare a 25-mL porcelain Gooch crucible with a mat of pure well-washed asbestos (such as is used for the determination of barium sulfate), wash thoroughly with toluene, dry at 105 to 110C for 30 min, cool in a desiccator, and weigh. 4.2 Place 50 g of the freshly powdered specimen in a 300-mL beaker, add 150 mL of toluene, free of water and nonvolatile residue, and dissolve the specimen with the aid of heat and occasional shaking. When solution is apparently complete (no particles of rosin visible), filter at once through the Gooch crucible. If the rosin filtrate is not clear, return it through the Gooch crucible until it is clear, finally washing the residue and the outside of the crucible free of rosin with additional hot toluene. 4.3 Dry the crucible and contents to constant weight at 105 to 110C (1 h usually suffices), cool in a desiccator, weigh, and calculate the percent of solid matter insoluble in toluene. 5. Report 5.1 Calculate and report the percent toluene-insoluble solid matter in rosin to the second decimal place. TheAmerican 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 ofthe validity ofany such patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdmvn. Your comments ere invited either for revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you ahould make your views known to the ASTM Committee on Standarda, ISIS Race St., Philadelphia, PA 19103. 68 DUP050295734 Designation: D 304 - 90 $ Standard Specification for n-Butyl Alcohol (Butanol)1 This standard is issued under the fixed designation D 304; the number immediately following the designation indicates the yeaT of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies cfthe Department ofDefense. Consult the DoD Index of Specifications and Standardsfor.the specific year ofissue which has been adopted by the Department ofDefense. cope This specification covers n-butyl alcohol (butanol). This standard does not purport to address all of the problems associated with its use. It is the responsibility user ofthis standard to establish appropriate safety and h practices and determine the applicability ofregulatory dtions prior to use. For specific hazard statements, see on 4. For hazard information and guidance, see the sup 's Material Safety Data Sheets. referenced Documents 1 ASTM Standards: 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D 891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals3 to 1078 Test Method for Distillation Range of Volatile Organic Liquids2 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)2 ID 1296 Test Method for Odor of Volatile Solvents and Diluents2 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1476-Test Method for Heptane Miscibility of Lacquer Solvents2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals2,3 2.2 U.S. Federal Specification: 1 This specification is under the jurisdiction of the ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 304 - 29 T. Last previous edition D 304 - 85. 2 Annua/ Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 15.05. 4 Annual Book ofASTM Standards, Vol 05.03. 5 Annua! Book ofASTM Standards, Vol 14.03. PPP-C-2020 ..Chemicals, Liquid, Dry, and Paste: Pack aging of6 3. Properties 3.1 n-butyl alcohol (butanol) shall conform to the fol lowing requirements: Apparent specific gravity: 20/20*C 25/25'C Color, Pt-Co scale, max Distillation range, 760 mmHg Nonvolatile matter, max, mg/100 mL Odor Water, max, weight % Acidity, as acetic arid, max, weight % 0.810 to 0.813 0.807 to 0.810 10 nonresidual 0.1 * 0.005 c A Shall distill entirely within a 1.5"C range which shall include 117.7'C. B This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of99 % heptane at 20"C. c Equivalent to 0.047 mg of KOH per gram of sample. 4. Hazards 4.1 /j-Butyl alcohol is a flammable liquid. Its vapors can form explosive mixtures with air. Repeated or prolonged contact may cause drying of the skin. 5. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 6.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20 or 25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Methods D 891 or D 4052. 6.1.2 Color--Test Method D 1209. 6.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 40C having a range from 72 to 126C and conforming to the requirements of Specification E 1. 6.1.4 Nonvolatile Matter--Test Method D 1353. 6.1.5 Odor--Test Method D 1296. 6.1.6 Water--Test Methods D 1364 and D 1476. 6.1.7 Acidity--Test Method D 1613. 6 Available from Standardization Documents Order Desk, Bldg 4 Section D, 700 Robbins Ave., Philadelphia, PA 191 11-5094, Attn: NPODS. 69 DUP050295735 D 304 7. Packaging and Package Marking 7.1 Package size shall be agreed upon between the pur chaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed Spec. PPP-C-2020. 8. Keyword 8,1 m-butyl alcohol 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, rind 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 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 views known to the ASTM Committee on Standards, 1918 Race St,, Philadelphia, PA 19103. ' fi 70 DUP050295736 Designation: D 319 - 90 Standard Specification for Amyl Alcohol (Synthetic)1'2 This standard is issued under the fixed designation D 319; 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. ope This specification covers synthetic amyl alcohol. This standard does not purport to address all of the problems associated with its use. It is the responsibility user ofthis standard to establish appropriate safety and practices and determine the applicability ofregulatory tions prior to use. For specific hazard statements, see on 4. For hazard information and guidance, see the sup 's Material Safety Data Sheet. .eferenced Documents ,1 ASTM Standards: ' 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Re lated Coatings and Material3 891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals4 1078 Test Method for Distillation Range of Volatile Organic Liquids3 11209 Test Method for Color of dear Liquids (PlatinumCobalt Scale)3 > 1296 Test Method for Odor of Volatile Solvents and Diluents3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1476 Test Method for Heptane Miscibility of Lacquer Solvents3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer and Related Products3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals3'4 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 1 This specification is under thejurisdiction ofASTM Committee D-l on Paint 1 Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 319 - 30. Last previous edition D 319 - 85. 2 Amyl alcohol is also known as penianol. This material is a mixture of the jisomers of amy] alcohol. 3 Annual Book ofASTM Standards, Vol 06.03. " Annual Book ofASTM Standards, Vol 15.05. s Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vol 14,03. 7 Available from Standardization Documents Order Desk, Bldg 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 Amyl alcohol (synthetic) shall conform to the fol lowing requirements: Apparent specific gravity 20/20X1 25/25'C Color, Pt-Co scale, max Distillation range, 760 mmHg, `C as: Initial boiling point, min Dry point, max Odor Water, max, weights Acidity, as acetic acid, max, weight % 0.812-0.820 0.809-0.817 15 127.5 139.0 nonresidual 0.3-4 0.0 lB A This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20"C. B Equivalent to 0.093 mg of KOH per gram of sample. 4. Hazards 4.1 Amyl alcohol is a flammable liquid. Its vapors can form explosive mixtures with air. Repeated or prolonged contact may cause drying of the skin. 5. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 6.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20 or 25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Methods D 891 or D 4052. 6.1.2 Color--Test Method D 1209. 6.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 41C having a range from 98 to 152C and conforming to the requirements in Specification E 1. 6.1.4 Odor--Test Method D 1296. 6.1.5 Water--Test Methods D 1364 and D 1476. 6.1.6 Acidity--Test Method D 1613. 7. Packaging and Package Marking 7.1 Package size shall be agreed upon between the pur chaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 8. Keywords 8.1 amyl alcohol 71 DUP050295737 4D D 319 The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any siuch 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 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 /nay 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., Philedelphia, PA 19103. J 72 DUP050295738 D 329 - 90 Standard Specification for Acetone1'2 This standard is issued under the fixed designation D 329; 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. This standard has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adoptedby the Department ifDefense. fThis specification covers acetone (99.5 % grade). Wrhis standard does not purport to address the safety %ns associated with its use. It is the responsibility ofthe |iff this standard to establish appropriate safety and i practices and determine the applicability ofregulatory i This specification specifies the use of a U.S. OccupaSafety and Health Administration (OSHA)-designated lous chemical, acetone. For hazard information and ice see the supplier's Material Safety Data Sheet. Referenced Documents 1 ASTM Standards: 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 ID 1078 Test Method for Distillation Range of Volatile I - Organic Liquids3 D 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 D1296 Test Method for Odor of Volatile Solvents and Diluents3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1363 Test Method for Permanganate Time of Acetone and Methanol3 D1364' Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1476 Test Method for Heptane Miscibility of Lacquer Solvents3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D1614 Test Method for Alkalinity in Acetone3 D1722 Test Method for Water Miscibility of WaterSoluble Solvents3 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct 26, 1990. Published December 1990. Originally published as D 329 - 31 T. Last previous edition D 329 - 86. 2 The compound is also known under the names dimethyl ketone and 2-propanone. 3 Annual Book ofASTM Standards, Vol 06.03. D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Specification:1 PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of O-A-51 Acetone, Technical 3. Properties 3.1 -Acetone (99.5 % grade) shall conform to the following requirements: Acidity (free,arid as acetic) wt %, max. Aldehydes (Note 1) Alkalinity (as ammonia) wt %, max Apparent specific gravity: 20/20"C 25/25'C Assay wt %, min Color Pt-Co, max Distillation range 760 mmHg Nonvolatile matter mg/100 mL, max Odor Permanganate time Water wt 96, max Water miscibility 0.002 (equivalent to 0.Q19 mg of KOH/g of sample) passes test 0.001 0.7910 to 0.7930 0.7865 to 0.7885 99.5 5 shall distill entirely within a I.0C range which shall include 56.tC 5 nonresidual color ofadded KMn04 must be retained for at least 30 minutes at 25"C in the dark 0.5 (Note 2) No t e 1--Aldehydes test is a requirement ofFederal Specification O-A-51. No t e 2-- This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20C. 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. No t e 3: Warning--Acetone is highly flammable. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Acidity--Test Method D 1613. 5.1.2 Aldehydes--Dilute 2.5 mL of the specimen with water to 10 mL.. Prepare a control containing 0.04 mg of * Annual Book ofASTM Standards, Vol 05.03. s Annual Book ofASTM Standards, Vols 05.03 and 14.03. 6Annual Book ofASTM Standards, Vols 06.03 and 15.05. 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 73 DU P050295739 D 329 formaldehyde in 10 mL of water. To both the specimen solution and the control, add 0.15 mL of a 5 % solution of 5,5-dimethyl-1-1,3-cyclohexanedione in alcohol. Evaporate each on a steam bath until the acetone is volatilized (no odor of acetone remains). Dilute each to 10 mL and cool quickly in an ice bath with vigorous stirring. Any turbidity produced in the specimen solution shall be no greater than that produced in the control. 5.1.3 Alkalinity--Test Method D 1614. 5.1.4 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the fourth decimal place, the temperature of. both specimen and water being 20 or.25C. See Methods D 268 and Test Method D 4052. 5.1.5 Assay---Assay is determined by difference; 100% minus (% water -1- % acidity), assuming that no, other impurities are present. . 5.1.6 Color--Test Method D 1209. 5.1.7 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 39C having a range from 48 to 102C and conforming to the requirements in Specification El. 5.1.8 Nonvolatile Matter--Test Method D 1353. 5.1.9 Odor--Test Method D 1296. 5.1.10 Permanganate Time--Test Method D 1363. 5.1.11 Water--Test Methods D 1364 for quantitative de termination and D 1476 for qualitative determination. . 5.1.12 Water Miscibility--Test Method D 1722. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shaU conform to applicable carrier rules and regulations or when specified shall conform to Federal Specification PPP-C-2020. 7. Keywords 7.1 acetone; solvents 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 ct 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 if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7916 Race St., Philadelphia, PA 19103. 8 M 1 i 74 DUP050295740 IP Designation: D 330' - 89 Standard Specification for 2-Butoxyethanol1,2 This standard is issued under the fixed designation D 330; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. I Scope 1.1 This specification covers 2-butoxyethanol. ; 1.2 For specific hazard information and guidance, see the pplier's Material Safety Data Sheet for materials listed in Is specification. Referenced Documents %. 2.1 ASTM Standards: ' D268 Methods of Sampling and Testing Volatile Solvents [ and Chemical Intermediates for Use in Paint and I Related Coatings and Material13 2 `D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Cplor of Clear Liquids (Platinum- Cobalt Scale)4 :D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D 1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D4052 Test Method for Density and Relative Density of f ' Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Standard: PPP-C-2020 Specification for Packaging of Chemicals, Liquid, Dry, and Paste8 1 This' specification is under thejurisdiction ofASTM Committee D-1 on Paint jand Related Coatings and-Materials and is the direct responsibility of Subcom`nrittee DOI .35 on Solvents, Plasticizers, and Chemical Intermediates. Curient edition approved March 3:1, 1989. Published May 1989. Originally published as D 330 - 35 T. Last previous edition D 330 - 84. 2 This compound is also known under the name ethylene glycol monobutyl ether.. 2 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. s Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. * Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Properties 3.1 2-Butoxyethanol shall conform to the following re quirements: Apparent specific gravity 20/20"C 25/25'C, Color, Pt-Co scale, max Distillation range Below 168C Above 173"C Water, weight %, max Acidity (free acid as acetic acid), weight %, max 0.901 to 0.904 0.898 to 0.901 15 none none 0.1 0.01 equivalent to 0.093 mg KOH per gram of material 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 ` Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25C (See Methods D 268 or Test Methods D 4052.) 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 103C having a range from 148 to 202C and conforming to the require ments hr Specification El. 5.1.4 Water--Test Method D. 1364. 5.1.5 Acidity--Test Method D 1613, 6. Packaging and Package Marking 6.1 Package size to be agreed upon between the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to PPPC-2020. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreepprovedor withdrawn. Your comments are Invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 75 DUP050295741 Designation: D 331 - 90 Standard Specification for 2-Ethoxyethanol1,2 This standard-is issued under the fixed designation D331; 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 reapprovai. 1. Scope 1.1 This specification covers 2-ethoxyethanol. 1.2 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 specific hazard statements, see Section 4. 1.3 For hazard information and guidance, see the sup plier's. Material Safety Data Sheets. 2. Referenced Documents 2.1 ASTMStandards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color ofClear Liquids (PlatinumCohalt Scale)4 D I296 Test Method for Odor of Vplatile Solvents and Diluents3 D 1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1364 Test Method for Water in- Volatile Solvents (Fischer Reagent Titration Method)3 J D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates. Used in Paint, Varnish, Lac quer and Related Products3! D 4052 Test Method fqr Density and Relative Density of Liquids by Digital Density Meter5 E l Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals7 2.2 U. S. Federal Specification:' PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of*1 2 3 4 5 6 * 8 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 DO1.35 on Solvents, Plasticizers!, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally ` published as D 331 - 32 T. Last previous edition D 331 - 86. 2 This compound is also known under the name ethylene glycol monoethyl ether. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vol 14.03. 1 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 8Available from Standardization Documents Order Desk, Bldg,4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 2-Ethoxyethanol shall conform to the following re quirements: Apparent specific gravity: 20/20"C 25/25C Color, Pt-Co scale, max Distillation range, 760 mm Hg, C as: Initial boiling point, min Dry point, max Nonvolatile-matter, max, mg/100 ml, Odor Water, max, weight % Acidity (free add as acetic acid), max, weight % 0.929 to 0.932 0.926 to 0.929 15 134.0 136.0 5 nonresidual 0.5A 0.01a A This quantitative water limit ensures that the material is tniscible without turbidity with 19 volumes'af 99 % heptane at 20C. B Equivalent to 0.1 mg of KOH per gram of material. 4. Hazards 4.1 This material has been shown to be a teratogen with test animals. 5. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 6. Test Methods 6.1 Jhe properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 6.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20C or 25C. See Methods D268 or Test Method D 4052. 6.1.2 Color--Test Method D 1209. 6.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 102C having a range from 123 to 177C and conforming to the require ments of Specification E 1. 6.1.4 Nonvolatile Matter--Test Method D 1353. 6.1.5 Odor--Test Method D 1296. 6.1.6 Water--Test Method D 1364. 6.1.7 Acidity--Test Method D 1613. 7. Packaging and Package Marking 7.1 Package size to be agreed upon between the purchaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 8. Keywords 8.1 2-ethoxyethanol 76 DUP050295742 # D 331 The American Society for Testing an<3 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 truest be reviewed every five years end if not revised, eitherreapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should mate your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103.77 77 DUP050295743 Designation: D 363 - 90 Standard Specification for Tricresyl Phosphate1 This standard is issued under the fixed designation D 363; 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 specification covers tricresyl phosphate (99.0 % grade) prepared from commercial cresylic acid. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheets for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1399 Test Method for Unsaponifiable Contents of Tricresyl Phosphate2 D1468 Test Method for Volatile Matter in Tricresyl Phosphate2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer and Related Products2 D1721 Test Method for Permanganate Time of Tricresyl Phosphate2 D4052 Test Method for Density and Realtive Density of Liquids by Digital Density Meter3 E 300 Practice for Sampling Industrial Chemicals4 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of5 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 mittee DO1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 363 - 33. Last previous edition D 363 - 85. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. 4 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 3Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 Tricresyl phosphate shall conform to the following requirements: Apparent specific gravity: 20/20"C 25/25'C Color, Pt-Co scale, max Volatile matter, max, weight % Potassium permanganate test Unsaponifiable matter, max, weight % Water content, max, weight % Acidity, mg of KOH per gram of sample, max 1.150 to 1.180 1.147 to 1.177 100 0.20 A 0.5 0.1 0.1 A Color of added KMn04 to be retained at least 30 min. 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20C or 25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Volatile Matter--Test Method D 1468. 5.1.4 Potassium Permanganate Test--Test Method D 1721. 5.1.5 Unsaponifiable Matter--Test Method D 1399. 5.1.6 Water--Test Method D 1364. 5.1.7 Acidity--Test Method D 1613. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 tricresyl phosphate 78 DUP050295744 0 363 The American Society for Testing and Materials takes no position respecting the validity oi any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision af any time by the responsible technical committee andmustbe reviewed everyfive years and ifnotrevised, eitherreapprovedor withdrawn. Your comments are invitedeither for revision ofthisstandard or for additional standards and should be addressed to ASTM Headquarters Your comments will receive careful consideration at a meeting ot the responsible technical committee, which you may attend, if you feat 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. 79 DUP050295745 Designation: D464 - 91 SfiMardTest Methods for Saponification Number of NavalStore Products Including Tail Oil and Other Related Products1 This standard is issued under the find designauon D 464; 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 (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the determination of the saponification number of tall oil and products obtained by the fractionation of tall oil such as rosin, fatty acids and distilled tall oil. These test methods are also applicable to gum and wood rosin. Two test methods are covered as follows: 1.1.1 Test method using a potentiometric method, and 1.1.2 Test method using an internal indicator method. 1.2 The potentiometric method is suitable for use with both light- and dark-colored test samples. It should be considered the referee method. The internal indicator method is suitable for use only with light- and mediumcolored test samples. It should be considered the alternate method. 1.3 This standard does not purport to address all of the safety problenis, if any, associated with its use. It is the responsibility ofthe user ofthis standard to establish appro priate safety and hecdth practices and determine the applica bility ofregulatory limitations pridr to use. 2. Referenced Documents 2.1 ASTM Standards: D803 Standard Methods of Testing Tall Oil2 D804 Terminology Relating to Naval Stores, including Tall Oil and Other Related Products2 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode3 3. Significance and Use 3.1 These test methods axe designed to broaden the scope ofthe previous edition of the test method by the inclusion of tall oil and tall oil derived products as test materials. Test Methods, D 803, currently includes a method for the deter mination of saponification number. The details of that procedure will be deleted when test methods D803 are revised. Test Methods D803 will reference these test methods. 3.2 The saponification number is an important property of tall oil and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.34 on Naval Stores. Current edition approved Oct. 15, 1991. Published December 1991. Originally published as D 464 - 37 T. Last previous edition D 464 - 59 (1987).ei 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 15.05. total acid content, both free and combined, of these prod ucts. 3.3 The potentiometric test method should be used when ] the most reproducible results are required. 4. Preparation of Sample 4.1 If the sample for analysis is rosin, it shall consist of 1 small pieces ofrosin chipped from a freshly exposed part ofa lump or lumps, and thereafter crushed to facilitate weighing and dissolution. Prepare the sample the same day on which the test is begun in order to avoid changes in properties due to surface oxidation. Changes are very pronounced on ground rosin that has a large surface area exposed to air. Existing roan dust and powdered rosin must not be used. 4.2 If the sample rs a nonhomogeneous liquid, heat the;ii>` entire sample in a closed container fitted with a capillary vent or the equivalent. Some kind of agitation, even if done occasionally by hand, saves much time. Heat by immersion in open steam or hot water bath to avoid overheating. When dealing with crystallized rosin, a higher temperature of approximately 160"C may be needed. Remove samples for 5 testing only when the entire sample is homogeneous and has been well stirred. 5. Purity of Reagents and Water 5.1 Unless otherwise indicated, it is intended that all reagents shall conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Society,4 where such specifications are available. References to water shall be understood to mean distilled or deionized water. POTENTIOMETRIC TEST METHOD (Referee Method) 6. Apparatus 6.1 Erlenmeyer Flask, 250-mL, of chemically resistant glass3 with standard-taper glass joint. 6.2 Hot Plates. 6.3 Water-Cooled Reflux Condenser, with standard-taper joint to fit the Erlenmeyer flask. 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." 3 Coming or Kimble alkali-resistant glasses, or equivalent, are suitable for this purpose. Borosilieate flasks may be used, but they should either be new or be cleaned by rinsing with a hot solution of HF (2 or 3 %). This removes from the flasks the adhering partially disintegrated silicates that would interfere with the determination. 80 DUP050295746 po . iese prod- ised when insist of if |)part ofa; weighing ifflj la which * ties due on i I to air. -p lijused. j at the ' |apillary j fif done .j aersion Nvhenfl of pies for l has : at aU lPtteeidan-c'bany'.'.ui able. Bed or at I [-taper hem. /the [Joseph H&tate$ r this 8 or be i the &th the ^wifti Ojl ppiL divisions. r ,.ir avoid highly variable results,,make sure that the temperature variable-speed, with a polytetrafluoroethylene of the samples is approximately 60 to 70C when titrated. atedrip^hgtie stir bars ; ! . n - 8.4 Titrgte,w(th, 0.5,2V add, recording the buret and pH Wpiery or Volumetric Pipet, 50-mL constant. meter readings. Sufficient acid may, be added initially tp Boiling Stones, or glass b'ebdii.f: 1 bring the pH of the solution to about 12.. Mow sufficient e/y 400-raL tail-form. ' "> ' - -':: time for the electrode system to regch equilibrium, Add acid ss Electrode pH Meter, conforming to the require* in 1.0-mL portions until the change in pH per addition J of Test Method E70. Use either standard or. alkali- exceeds 0.3 pH units. Reduce the additions ofacid to 0,1 mL tant. electrodes for this test. Alternatively, an automatic or smaller until the end point, has been passed, as indicated aitric'tifrator ntay fee used; . V. by d !significant decrease in pH units per 0.1 !mL of add added. Continue the titration with 1.0-niL portions until it becomes apparent that the inflection point has beeti vrell ^,r_T..v.-v I*0* _JTbftWX^V^iBpreat|.pt^^^m^,^S^veriueV6 defined, -v " :>- 8.5 'Determine the inflection point (point of maximum 1 In propyl Alcohol, Reagent grade. .- .,... - change in pH per millilitre of acid) to the nearest 0.05 mL. Wdluene; Reagent grade. Thismay be found by inspection of a plot of pH against IIUkali Solution, Standard Alcoholic (0.5 JgMQissolv^ millilitres of acid added. For greater accuracy, a plot may be KpbtasSittm hydroxide (KDH), preferably & pellet made ofthe changein pHperiplllilitre ofapid added, against ps s ' ethyl alcohol conforming to 7.1 and dilute to 1 L t&p,pH. The jr^iection point is considered as the end point of [ i ethyl alcohol. Standardize to 0.001 Nby dissolving tie titratioul Alternatively if an automatic titrator is used, pum add. phthalate (GeH* CooKCooH), in 60 mL of the endpoint iseitherthe- inflection point from the plotted followed-by the addition of 40 mfc of isopropyl curve m the pH determined to coindde with the inflection bL Once the potassium add phthalate has dissolved, * point in the laboratory performing the analysis. The value of s' g of potassium acid phthalate will be neutralized by 10.8 is the average pH encountered at the inflection point by vdL of 0.5 N !OH solution. Protect the'Stahdardized ` this;procedure. - [ ,f:- ' , &h against evaporation and absorption of carbon di- M 8lg r^/qafc~Makp. duplicate blank determinations using ffCOj) from tile air: The solution should b^standard- 50.b mL of ,the aikali solution: .If 10 mL of isopropyl jffrequently, either potentiometrically or colorimetrically ' alcohol-toluene solution (1:1) is used as a solvent in 8.1, then ; either phenolphthalein or thymol blue as the indicator. use the same amount in the blank determination. ndardization should use the same equipment and liques as used in the actual saponification number 9. Calculation and Report mination. 9.1 Calculate the saponification number, expressed as |S Acid, Standard (0.5 N)--Standardize a 0.5 AT solution milligrams of KOH per gram of sample as follows: l td 0.001 Nby any accepted procedure. Saponification number -- [(B --A) Nx 56.1]/C |6 Borax Buffer, Standard Solution (0.01 M, pH 9.18 at C)--Dissolve 3.81 0.01 g of disodium tetraborate 2B407 10 HaO) in water and dilute to 1 L in a volumetric . Use the special grade7 ofborax prepared spetifically for as a pH standard. As an alternative, commercially able buffer with a pH between 9 and 11 may be used. where: B = add required for titration of the blank, mL, A = add required for titration of the sample, mL, N -- normality of the add, and C = sample weight, g. Report the saponification number to the nearest whole | Procedure number. 3.1 Transfer 2.95 to 3.05 g of the sample, weighed to the est 0.001 g, to the Erlenmeyer flask. If necessary, 10 mL |isopropyl alcohol-toluene solution (hi) can be added to "! flask to predissolve the sample. Using a constant delivery ; or volumetric pipet add 50.0 mL of the alkali solution. I several PTFE boiling stones or glass beads and connect : flask to the condenser. 1,8.3 Place the flask on a hot plate and maintain the llution at reflux for 1 h. At the end of the reflux time, while |e sample is still warm, transfer the contents of the Irlenmeyer flask into a 400-raL tail-form beaker rinsing with |D0 mL of isopropyl alcohol in three washings. Place samples a heated surface until they can be titrated. In order to INTERNAL INDICATOR TEST METHOD (Alternative Method) 10. Apparatus 10.1 Same apparatus as 6.1 through 6.7. 11. Reagents 11.1 Phenolphthalein Indicator Solution--Dissolve 1 gof phenolphthalein in 100 mL of methanol. 11.2 Thymol Blue Indicator Solution--Dissolve 0.1 g of -thymol bluein 100 mL of methanol. 11.3 Same as 7.1 through 7.5. 12. Procedure 6 Available from the U.S. Bureau ofAlcohol, Tobacco, and Firearms, Distilled Spirits and Tobacco Branch, 1200 Pennsylvania Ave., NW, Washington DC 26. 7 The National Institute ofStandards and Technology standard sample ofborax No. 187 is satisfactory for this purpose. 12.1 Transfer 2.95 to 3.05 g of the sample, weighed to the nearest 0.001 g to the Erlenmeyer flask. If necessary, 10 mL ofisopropyl alcohol-toluene (1:1) can be added to the flask to predissolve the sample. Using a constant delivery pipet or volumetric pipet, add 50.0 mL of the alkali solution. Add 81 DUP050295747 ID* D 464 several PTFE boiling stones or glass beads, and connect the flask to the condenser. 12.2 Place the flask on a hot plate and maintain the solution at reflux for 1 h. At the end of the reflux time, place samples on a heated surface until they can be titrated. In order to avoid highly variable results, make sure that the temperature of the samples is approximately 60 to 70C when titrated. . 12.3 Titrate with 0 5 N HC1 using either 4 to 5 drops of phenolphthalein indicator to a clear endpoint or 4 to 5 drops of thymol blue indicator. With thymol blue, the end point is indicated when the color undergoes the first change from a distinct blue to a blue-green, just short of clear yellow. If needed, more indicator may be used. Read the buret to 0.05-mL titrant. If less than 20 mL of titrant is consumed, decrease the sample size. 12.4 Blank--Make duplicate blank determinations using 50.0 mL of the alkali solution and following the same procedure as for the sample. If 10 mL of isopropyl alcohol- toluene solution (1:1) was used as a solvent in 12.1, then use | the same amount in the blank determinations. , 13. Calculation and Report i ' 13.1 Calculate the saponification number as described in i Section 9. Report the results to the nearest whole number. 14. Precision and Bias 14.1 Precision--The precision of these, test methods for measuring the saponification number of tall oil and tall oil products is being determined. 14.2 Bias--The procedure in these test methods for measuring Saponification number has no bias because the value of the saponification number is defined only in terms of these test methods. 15. Keywords 15.1 Rosin; saponification number; tall oil; tall oil fatty acids \ I I I The American Society for Testing anti Materials lakes 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 . if not revised, eitherreapproVed or withdrawn. Your comments areinvited eitherforfevlsion 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 tin Standards, 1916 Race St., Philadelphia, PA 19103. | :j | 1 I 3 | j 1 11 | j 82 DUP050295748 -Designation: D 465 - 82i[Reapproved 1987)f1 Standard Test Methods for Acid Number of Rosin1 This standard is issued under the fixed designation D 465; 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. {1No t e--Section 7 was changed editorially in November 1987. ippe These test methods are intended for determining the Inumber of rosin. Two methods are covered, as follows: Internal indicator method, and Potentiometric method. ! The internal indicator method is suitable for use only ! light- and medium-colored rosin. The potentiometric [iod is suitable for use with both light- and dark-colored This standard may involve hazardous materials, operns, and equipment. This standard does not purport to ttress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish vropriale safety and health practices and determine the vlicability of regulatory limitations prior to use. ^Referenced Document p.l ASTMStandard: fife.70 Test Method for pH of Aqueous Solutions with the ; ' Glass Electrode2 i Preparation of Specimen 3.1 The specimen taken for analysis shall consist of small es ofrosin chipped from a freshly exposed part of a lump lumps, and thereafter crushed.,lo facilitate weighing and (solution. The specimen shall be so prepared the same day on yhich the test is begun, in order to avoid changes in properties due to surface oxidation, which is very pro nounced pn ground rosin having a large surface area exposed > the air. ||t. Purity of Reagents and Water 4.1 Unless otherwise indicated, it is intended that all p teagents shall conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.3 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 1.34 on Naval Stores. Current edition approved March 26, 1982. Published June 1982. Originally published as D 465 - 37 T. Last previous edition D 465 - 59 (1981). 2 Annual Book ofASTMStandards, Vol 15.05. 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," References to water shall be understood to mean, distilled water, INTERNAL, INDICATOR METHOD 5. Reagents 5.1 Alkali, Standard Solution (0.5 N)--Dissolve either 22 g of sodium hydroxide (NaOH) or 33 g of potassium hydroxide (KOH) (pellets or sticks) in water or in alcohol conforming to 5.2, and dilute to l L with the same solvent; Standardize to 0.001 N. 5.2 Ethyl Alcohol--Neutral methanol, neutral isopro panol (91 to 99 %), neutral 95 % ethanol or neutral dena tured alcohol conforming to Formula No. 30 or No. 3A of the U. S. Bureau of Internal Revenue. No t e 1--In case of disagreement between purchaser and seller, aqueous alkali solution shall be used. 5.3 Phenolphthalein Indicator Solution--Dissolve 1 g of phenolphthalein in 100 mL of methanol. 5.4 Thymol Blue Indicator Solution--Dissolve 0.1 g of thymol blue in 100 mL of methanol. 6. Procedure 6.1 Transfer 3.95 to 4.05 g of the sample, weighed to the nearest 0.001 g, to a 250-mL Erlemrieyer flask, and add 100 mL of neutral alcohol. 6.2 Heat, if necessary, to dissolve the rosin, cool to room temperature (Note 2), and titrate the solution with the standard alkali solution using 1 mL of either phenol phthalein or thymol blue indicator solution. With phenol phthalein, titrate to the first persistent faint pink color; with thymol blue, titrate to a distinct blue. No t e 2--If the rosin does not remain in solution when it cools, use 200 mL of alcohol instead of 100 mL. 7. Calculation and Report 7,1 Calculate the acid number of the rosin, expressed as milligrams of KOH per gram of sample, as follows, and report to the nearest whole number: Acid number = (AN x 56.1 )/B where: A -- alkali solution required for titration of the specimen, mL, N = normality of the alkali solution, and B = specimen weight, g. 83 DUP050295749 # D .465 POTENTIOMETRIC METHOD 8. Apparatus 8.1 Glass-Electrode pH Meter conforming to the require ments of Test Method E 70. Use either standard or alkaliresistant electrodes for this test. Alternatively, an automatic potentiometric titrator may be used. 8.2 Stirrer, variable-speed with a glass propeller-type stir ring paddle. 9. Reagents 9.1 Prepare the reagents described in 4.1 and 4.2. . 9.2 Borax Buffer, Standard Solution (0.01 M, pH 9..18 at 25C) --Dissolve 3.81 0.01 g of disodium tetraborate (Na2B407 10H2O) in water an4 dilute to 1 L in a volumetric flask. Use the special grade4 ofborax prepared specifically for use as a pH standard. 10. Standardisation of Apparatus 10.1 Adjust the pH meter with the standard borax buffer solution, following essentially the same procedure as de scribed in Test Method E 70. 11. Procedure 11.1 Transfer 3.95 to 4.05 g of the sample, weighed to the nearest 0.001 g, to a 400-mL tail-form beaker and add 200 mL of neutral alcohol. Heat, if necessary, to dissolve the rosin and cool to room temperature. 4 The National Bureau of Standards standard sample of borax No. 187 is satisfactory for this purpose. 11.2 Adjust the beaker so the lower half of each electrode ofthe pH meter is immersed in the specimen. Start the stirrer and adjust the speed so that there is vigorous stirring without spattering. 11.3 Titrate with the standard alkali solution, recording the buret and pH meter readings. Sufficient alkali may be added initially to bring the pH of the solution to about 8.0. Allow sufficient time, for the electrode system to reach equilibrium. Add alkali in 1.0-mL portions until the change in pH per increment added amounts to about 0.3 pH unit. Reduce the additions ofalkali to 0.1 mL until the end point has been passed, as indicated by a significant decrease in pH per 0.1 mL added. Continue the titration with 1.0-mL portions until it becomes apparent that the inflection point has been well defined. 11.4 Determine the inflection point (point of maximum change in pH per millilitre of alkali solution) to the nearest 0.1 mL by plotting the pH readings against the millilitres of alkali used. For greater accuracy, a plot may be made of the change in. pH per millilitre of alkali, against the pH. The peak ofthis curve will indicate the exact inflection point. The inflection point shall be taken as the end point of the titration. Alternatively, if an automatic titrator is used, the end point shall be taken either as the inflection point from the plotted curve or. pH 10.8 (Note 3) with instruments which titrate to a preset value. No t e 3--The value of 10.8 is the average pH encountered at theinflection point by the above procedure using closely controlled condi tions, solvent, water ratio, eta Glass electrodes tend to dehydrate in nearly anhydrous solvent medium. Condition the electrode in water between tests and check with known pH buffers frequently. 12. Calculation and Report 12.1 Calculate the acid number as described iri Section 7, and report to the nearest whole number. TheAmerican Society for Testing and Materials takes noposition respecting the validity ofany patent rights asserted In connection with any item mentioned In this standard. Users of this standard 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 commentsare Invitedeither forrevision ofthis-standard or tot 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 Baca St., Philadelphia, PA 19103. 84 J DUP0502 95750 Designation: D 509 - 70 {Reapproved 1987) Standard Te^t Methods of Sampling an grading Rosin1 This standard is issued under,the fixed designation D 509; the number irbmediately following the designation indicates the year of original adoption or, in the case ofrevision, the yearoflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision orieapprovaL scope 1.1 These test methods cover procedures for sampling and ermining the grade of rosin delivered.in commercial bags, :1s, or drums. pOTE 1--All rosin sold in interstate commerce must be described by hence to the U. S. Standards for rosin, and is therefor? subject to ng prior to such sale. The grading procedure described in these test |fcods is used for checking grades of'regrading after the rosin has ed from the primary markets to distributing or consuming points. gl.2 This standard may involve hazardous materials, operons, and equipment. This standard does not purport to |dress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish %propriaie safety and health practices and determine the * plicability ofregulatory limitations prior to use. Apparatus 2.1 The apparatus (Fig. 1) for sampling and grading rosin tall consist of the following: 2.1.1 Steel Spike--A portable steel spike (A, Fig. 1) with ^movable wooden handle, for obtaining a sample lump. The like shall have the following approximate dimensions: 30 ' (760 mm) in over-all length, 18Vj in. (47.0 mm) in length steel shank, and 2 in. in outside diameter at handle end. e total weight (Note 2) of the spike shall be 4W lb (20 kg) the weight of the steel shank 3`A lb (1.9 kg). A suitable s may also be made by sharpening one end of the drive jaft of an old automobile. The sharpened point shall be off pter, and, in order to lessen the chances of breaking or Mapping, off at the tip, should not be extremely hard. 2.2 Sampling Adz--A sampling adz (D, Fig.-1) specially igned for cutting the "type" or grading sample from the |osin lump. A lather's hatchet with a narrow blade (C, Fig. 1) jmay also be used. The cutting edge shall be kept razor sharp or best results. 2.3 Heating Device--An electrically heated device for shaping and smoothing the surfaces of the sample to the Ireguired dimension for grading % in. (22.2 mm) thirik in the Iviewing direction). The device shown (E, Fig. I) was con structed from a 3-in. (76.2-mm) length of I'A-in. (38.1-mm) copper T-bar, 'A in. (6.4 mm) thick, which was nickel-plated. One section or fin, opposite those forming the 90 polished ; faces, is clamped between two heating elements. The temper ature must be regulated by means of a variable-voltage transformer, to prevent overheating and too rapid melting or scorching of the sample faces. An electric flat iron, mounted 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!.34 on Naval Stores. Current edition approved Jan. 14, 1970. Published March 1970. Originally issued as D 509 - 38. Last previous edition D 509 - 55. in-a nearly vertical position, point down, with similar heat control, also serves die purpose. 2.4 Grading Box--A comparison or grading box (B, Fig. 1) which is not always necessary but may be helpful in grading samples that are doubtful- or "close to type," that is, almost but perhaps not quite as good as the standard, or which may be difficult tb grade because of some unusual condition such as a reduced brightness or light transmission value caused by cloudiness or the presence of finely divided foreign matter suspended in the rosin. Such a box may be made of `A-in. (6.4-mm) wood stock, with the following approximate dimensions: 21 in. (533 mm) in over-all length at the bottom, 193A* *in*. (502 mm) in length on top, 47/g in. (124 mm) in width at the wide (eye) end, 2% in. (66.7 mm) in width at the small (sample) end of the top, l`A in. (38.1 mm) in width of side member, and 1% in. (44.4 mm) in over-all height (top, bottom, and side). The large end' shall be cut out as Mown in Fig. 1 to fit the face of the grader while the small end shall be fitted with two fiat springs made of %-in. (9.5-mm) clock-spring steel, which serve to hold the sample and the standard in place on the extended end or lip ofthe lower member, in front oftwo Vs-in. (12.7-mm) square holes cut 7/s in. (22.2 mm) apart, center to center in a piece of sheet metal forming the small end of the box. A piece of sheet rubber fastened to the lip, acts as a cushion for the samples to rest on. An eye-piece, in the form of a transverse vertical partition having a centrally cut opening or slit 3/s in. (9.5 mm) in width by 3 in, (76.2 mm) in length, shall be fastened inside the larger end, about 4 in. (102 mm) in from the end. The box shall have an interior finish of dull black, which may be obtained by gluing pieces of black felt, cut to fit the interior, to the inner side of the several pieces of board from which the box is made. 2.5 Official Rosin Standards--The official standards for use in grading rosin (<?, Fig. 1, plus three standards lighter than "X") consist of assemblies of: colored glass plates, cemented together, as issued on loan by the U. S. Depart ment of Agriculture,2 or the similar combinations of Lovibond glasses that have been certified by the Department 3 The U. S. Rosin Standards are issued only on security loan ($ 100 deposit) by the Naval Stores Branch, Tobacco Division, Agricultural Marketing Service. U. S. Department of Agriculture, Washington, DC, under Regulations for Enforcement of the Naval Stores Act. Ifan applicant is unable to borrow a set of the U. S. Rosin Standards, because of the limited number ofsets in existence, secondary sets are available. Lovibond "U. S." rosin standards are manufactured by Tintometer, Ltd., Salisbury, England. The United States'agent for Tintometer, Ltd. is Tintometer U.S.A., Berkshire Valley Rd., Oak Ridge, NJ 07438. These standards are excellent duplicates ofthe U. S. Rosin Standards but could not be classified as identical. The Lovibond standards do not have official recognition by the U. S. Department ofAgriculture. A certificate may be obtained, however, at a cost of $10 from the Nava] Stores Branch, Agricultural Marketing Service, attesting to the degree with which a set compares visually with the master set ofthe Official U. S. Rosin Color Standards. 85 DUP050295751 D 509 A--Rosin spike. B--Comparison box. C--Sampling hatchet D--Sampling adz. E--Smoothing device. F--Rosin type samples. S--Official rosin standards. H--Spiked lump sample. I--Sample for grading, FIG. 1 Apparatus for Sampling and Grading Hosin for use in grading. The grades and standards are designated as follows: XC, XB, XA, X, WW, WG, N, M, K, I, H, G, F, E, D. A special grade, FF, is used for dark wood rosins. Grades XA, XB, and XC are not available from the U. S. Department of Agriculture on security loan but may be purchased commercially.3 The U. S. Department of Agricul ture will certify the purchased standards for a nominal fee. The standards issued by, the Department of Agriculture (except FF), consist of combinations of plates cut, ground, and polished to specified thicknesses from selected melts of Coming and Jena colored glass. The spectral transmission data, for the various assembled standards comprising the Master Set No. 200, for light of different wavelengths, are given in Table 1. The colorimetric specifications of the standards, based on the 1931 CIE Coordinate System, for a standard observer using standard Illuminant C, are given in Table 2. The colorimetric specifications for the U. S. Rosin Standards, Master Cubes XA, XB, and XC, are given in Table 3. 2.6 Secondary standards or "type samples" are sometimes used for approximate grading, in the absence of permanent official standards ofglass. Such samples may consist ofcubes of specially selected rosin or other colored transparent medium; solutions are also sometimes used (Note 2). Sec ondary standards or "types" are usually not permanent in 3 The Standards XA, XB, and XC may be purchased directly from Tintometer, Ltd., Salisbury, England, or from their United States representative Lovibond of America, Inc., 870 Willis Ave., Albertson, Long Island, NY 11507, color and must be protected from excessive exposure to sunlight or heat. Wrapping and storage in a cool dark place when not in use is recommended. To ensure correctness of grading therewith, they should be tested periodically by comparison with permanent glass standards.4 No t e 2--It is riot possible to dissolve a specified quantity of rosin in a solvent and use such solution as a standard for grading the rosin, because there is no constant relationship between the color of the original solid rosin and the color of the rosin after being put in solution. Consequently, the color ofsuch solution is not a criterion ofthe color of the rosin itself. 3. Sampling 3.1 Number of Packages to Be Sampled--A preliminary sampling of20 % ofthe entire lot or shipment shall be made. If the grade of 85 % or more of the number of such preliminary samples agrees with the grade indicated on the package or invoice, with none of the samples disagreeing by more than one grade, the original grading shall be considered confirmed and the shipment accepted as a good delivery. If the grades of more than 15 % of the preliminary samples are in disagreement, or if any appreciable number are under grade by more than one grade, additional packages in the lot 4 The Department ofAgriculture will examine and report on the suitability of any secondary standards for rosin, after suitable arrangements have been made with the Naval Stores Branch. There is a fee for such service. Information on sources of supply of secondary standards may be obtained from the Naval Stores Branch. 86 DUP050295752 D 509 TABLE 1 Spectral Transmission Factors for U.S. Rosin Standards (Master Set No. 200) 1 Grade X WW WG N M K 1 H G F E D 0:005 . 0.001 0.006 0.0022 0.0092 0.0037 0.0008 . 0.0015 0.0152 0.0311 0.0064 0.0139 0.0026 0.0059 0.0008 Q.0020 0.0005 0.0595 0.106 0.166 0.234 0.305 0.0284 0.0549 0.0926 0.143 0.199 0.0131 0.0280 0.0512 0.08S3 0.1305 0.0048 0.0114 0.0232 0.0437 0.0734 0.0013 0.0035 0.0083 0.0181 0.0346 0.0002 0.0007 0.0020 0.0053 0.0119 0.0003 0.0009 0.0027 0.0003 0.373 0.440 0.502 0556 0.604 .0.260 0.324 0.387 0.450 0.506 0.181 0.237 0.299 0.363 0.422 0,1114 0,1587 6.213 0.273 0.333 0.0569 0.0932 0.1372 0.190 0.246 0.0239 0.0434 0.0730 0.1130 0.158 0.0074 0.0159 0.0316 0.0566 0.0896 0.0011 0.0033 0.0089 0.0200 0.0373 0.0001 0.0006 0.0020 0.0060 0.0136 0.643 0.673 . 0.698 0.713 0.724 0555 0.595 0.628 0.651 0.668 : 0.477 0.526 0.567 0.597 0.620 0.394 0.447 0.495 0.533 0.562 0.302 0.358 0.411 0.454 0.489 0.210 0.264 0.316 0.363 0.400 0.1320 0.178 0227 0.272 0.312 0.0635 0.0972 0.1357 0.174 0.210 0.0275 0.0482 0.0760 0.1070 0.1414 0.0004 0.0099 0.0417 0.0655 0.0840 0.0006 0.0034 0.0149 0.0260 0.00015 0.0015 0.730 0.729 0.727 0.724 0.722 0.678 0.683 0.684 0.682 0.682 0.635 0.642 0.645 . 0.646 0.647 0.582 0.594 0.600 0,603 0.606 ' 0.514 0.530 0.540 0.545 0.550 0.430 0.449 0.482 0.469 0.475 . 0.345 0.368 0.384 0.393 0.401 0.242 0.265 0.281 0.292 0.302 0.174. 0.200 0.219 0.233 0.244 0.1015 0.1190 0.1358 0.152 0.167 0.0354 0.0450 0.0549 0.0652 0.0750 0.0046 0.0078 0.0109 0.0142 0.0177 0.723 0.724 0.729 0.738 0.738 ' 0.683 0.684 0.688 0.698 0.699 0.650 0.652 0.659 0.667 0.668 0.610 0.612 0.618 0.628 0.629 0.555 0.558 0.5S4 0.573 0.574 0.482 0.485 0.494 0.504 0.505 0.408 0.413 0.419 0.428 0.429 0.309 0.314 0.322 0.331 0.331 0.253 0.259 0.266 0.270 0.270 0.181 0.197 0.214 0.234 0.253 0.0854 0.0969 0.1099 0.1236 0.139 0.0216 0.0266 0.0322 0.0389 0.0472 if 0 0 30 0.741 0.749 0.756 0.763 0.704 0.710 0.717 0.723 0.673 0.678 0.685 0.691 0.633 0.639 0.644 0.648 0.577 0.584 0.688 0.590 0.509 0.515 0.518 0.519 0.431 0.435 0.436 0.435 0.334 0.336 0.336 0.335 0.269 0.267 0264 0.25B 0.273 0294 0.316 0.340 0.155 0.173 0.191 0212 40 0.769 0.727 0.694 0.650 0.591 0.519 0.433 0.330 0.250 0.365 0235 0.0568 0.0683 0.0821 0.0990 0.117 0.773 0.778 , 0.731 0.734 0.696 0.698 0.651 0.651 0.590 .0.587 0.516 0.512 0.428 0.421 0.324 0.317 0.240 0.229 0.390 0.416 0.258 0.283 0.139 0.162 J'jflce up a total equal to not less than 50 % of the entire ment (preferably the entire shipment if accessible and tho great) shall be sampled. The findings on such larger tity shall be accepted as the basis for settlement between purchaser and the seller. 3--Gum rosin, from the oleoresin or "gum" obtained from i pine trees, is made by distilling individual batches or charges of r m, the size ofwhich depends on the capacity ofthe still. At the end distillation, the'rosin is drawn either into steel drums having a tare Jit of 17 lb (7.7 kg), and uniformly filled to contain 517 net lb (234.5 ofrosin, or into multiwall paper bags containing 100 net lb (45.4 kg). atch or charge may consist of from 8 to 15 drums, or the equivalent ' ber of bags. Two samples of the hot molten rosin are taken from _ batch, from the first and last filled containers, and poured into Ids for grading. The color of the rosin may vary slightly between bsequent batches or between the first and last container filled from a tch. After cooling, the drugs and bags are often transferred to a storage or shed to await shipment Consequently, in every carload nent, the drums or bags will represent a number of batches and itions. Shipments of drum rosin moving in commerce from a ntral storage point usually represent the output of more than one teducer. The rosin may have been made from gum collected at fferent seasons of the year. It will be seen from the above that it correct of the over-all grade of a commercial lot of rosin cannot be ned from just a limited number of samples. 3.2 Method ofSampling--After removing the friction cap m the filler opening in the top ofthe drum, spike into the rosin and remove enough broken material to permit access to the rosin several inches below the surface. Then spike out a solid lump as large as possible (H, Fig. 1) from which an approximate 7/g-in. (22.2 mm) cube can be cut. No part of the lump should have been less than 2 in. (50.8 mm) below the original surface. In the case of the usual 100-lb (45-kg) bags, the sample may come from any convenient location. By means of the sampling adz or hatchet, a grading sample shall be cut or cleaved from the lump as nearly cubical in shape as possible, 7/s-in. on the side. Ifdesired or indicated as necessary by the results of the cutting, the sample shall be shaped to exact size by quick, intermittent, light applications against the heated smoothing device, removing any melted rosin from the surface with cotton waste or a soft cloth between each application. The final specimen for grading shall be an approximate cube having a thickness ofexactly Vs in. (/, Fig. 1), between smooth, parallel faces in the direction or dimension through which it is viewed or compared with the grade standard. 4. Grading 4.1 The sample or "type" shall be compared with the appropriate standard, preferably against an open direct north sky light, or in a direction which excludes direct rays from the sun from passing through the rosin to the eye. The grade 87 DUP050295753 TABLE 2 Colorimetric Specifications for U.S. Rosin Standards ________ (Master Set No. 200)4_______________ ___ Grade X y TXP X 0.4339 0.4863 0.609 575.0 0.755 WW 0.4579 0.4732 0.531 576.8 0.851 WG . 0.4785 0.4741 0.466 578.5 0.905 N 0.5001 0.4704 0.396 580.5 0.944 M 0.5212 0.4619 0.322 582.8 0.969 K 0.5430 0.4483 0.245 585.5 0.985 1 0.5649 0.4310 0.178 588.7 0.993 H 0.5879 0.4102 0.1114 592.4 0.997 G 0.8116 0.3874 0.0723 596.8 0.999 F 0.6364 0.3632 0.0398 602.1 1.000 E 0.8640 0.3358 0.0131 609.4 1.000 D 0.6943 0.3057 0.0021 621.4 1.000 . A x and y are CJE trilinear coordinates; T is the luminous transmission factor; X is the dominant wavelength, in nanometers; p is the eolorimetjric purity.. ' assigned to the rosin shall be considered that ofthe highest or lightest colored standard which the sample equals or expels (is lighter than) in color (Note 4). Should the color or appearance ofthe rosin be such that there is a doubt whether the rosin is as light or bright as the standard, the sample and the standard shall be viewed through the grading box or other suitable colorimeter. Then in case of uncertainty the rosin,shall be given the benefit of the doubt. For example, if a rosin sample is definitely darker than the WW standard, but lighter than the WG standard, it is WG grade. If however, the grader is undecided whether the total color of the rosin is "as good as" or equals, or is darker than that of the WW standard, the grade is WW; No t e 4--The "color" of a' sample of rosin is made up of three attributes; hue, saturation, and brightness. "Hue" alludes to the: charac teristic described by the words "yellow" or "red." "Saturation" describes the purity or strength of the .yellowness or redness of the color. "Brightness" depends on the relative amount oflight transmitted by the rosin. The cleanliness of the rosin affects its transparency and therefore its brightness. The terms "lighter than" and its inverse, "darker than" are convenient to describe the difference between a sample and a standard. The rosin may be . darker than the standard in one or more of the TABLE 3 Colorimetric Specifications for U-. S. Rosin Standards (Master Cubes XA, XB, and XC)A Grade . XA XB XC =X 0.4048 0.3724 0.3406 y 0.4443 0.4117 0.3696 T, 0.708 0.788 0.848 A x and y are C1E trilinear coordinates; T is the luminous transmission factor. following ways: (i) a redder hue, (2) a more saturated hue, and (3) a lower brightness. 4.2 A sample showing two distinct colors, usually evi denced by darker streaks through ihe rosin, indicates a mixture of rosins in the package, intyhich case the darkest part ofthe sample or darkest rosin to. be found in the package shall determine the grade. 4.3 A check sample taken from close to the bottom of a barrel or drum shall not be considered representative, because cif a natural variation in color sometimes found between the top . and bottom rosin as well as a reduced brightness of the bottom rosin due to a settling of finely divided suspended matter usually present in normal gum rosin. Should such bottom sample show not more than one grade lower than the top sample, the latter shall determine the grade of the rosin in the barrel. If, however, the bottom-head sample is more than one grade lower than the top sample, double filling or "mixed-packing" is indicated, and the bottom-head sample shall determine the grade of the rosin in the package. 4.4 Rosin that is.only slightly cloudy or opaque (caused by occluded moisture or separation of crystals in the solid mass) shall be graded in the usual way if the condition is not such as to prevent an accurate evaluation of the color in compar ison with the standards. If, however, the opaqueness is of such a degree that the grade cannot be definitely determined in comparison with the standards, the rosin shall be desig nated "OPAQUE" and graded "QP," in which case its acceptance and value shall be a matter for settlement between the purchaser and the seller without reference to grade. Such opaque rosin may be further, identified or described as pale^medium, or dark opaque. 5. Tolerance 5.1 The tolerance or allowance of 15 % variation (Note 5) described in Section 3 is necessary because careful competent graders rarely get exact duplicate results on all individual, samples when regrading a large number of rosin samples. Moreover, a regrade sample, coming from a different .posi tion in the package, and after storage and weathering for an indefinite period, may be slightly darker than the original sample on which the grade was based. An allowance for such slight variation must therefore be made. No t e 5--This tolerance is that recognized by. the Federal; Govern ment in the administration of the U. S. Naval Stores Act. 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 of infringement ofSuch 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 Ifnekrevised, eitherreapprovedor withdrawn. Yourcomments are invitedeither forrevision of this standard or tor additional standards and should be addressed to fiSTM 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 Wlews known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.. 88 DUP0502 95754 Designation: D 555 - 84 (Reapproved 1988)'1 i*nr- Standard Guide for Testing Drying Oils'1 This standard is issued under the fixed designation D 555; the number'immediately following the designation indicates the year of original adoption or, the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (Vindicates an editorial change since the last revision or reapprovai. < This standard has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 61 No t e--Editorial changes were made throughout, including the title, in October 1988. isThis guide covers the selection anduse of procedures dug; di rying oils commonly "used in paints, varnishes, i products. The test methods included are as follows: address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. 2. Referenced Documents Test Method Section ASTM test Method Pile Tolerance KHaliie mu?' Bfafter Heating of Drying Oils Kg Properties SiPoint K Volumetric KGravimetric Eppie SSroxyi Value H on Heating ntor Insoluble in Chloroform paration of Sample motive Index Ppling bonification Value ecific Gravity ing Oil Quality'Test fasaponifiabfe Matter Jnsaturation: 5 Diene Value: Spectrophotometric Method fVlodine Value: Rosenmund-Kuhnhenn Method Wys Method Viscosity 13 D 1950 6 D 1639 10 D. 1951, D 564 12 D 1952 5 D 2090 19 D 1544, D 1209 25 D 1967 23 D 1640 24 D 93, D 1310, D 56 11 D 1954 11 D 1966 14 D 1955. 16 D 1957 17 D 1960, D 93 18 D 1958 4 21 3 D 1466 8 D 1962 20 D 1963, . D 1475 15 D 1964 D 1965 D 1358 D 1541 7 D 1959 22 D 1545, D 445 i * 1.3 ations, This standard may involve hazardous materials, oper and equipment. This standard does not purport to iff! 1 ` This Guide is under the jurisdiction of ASTM Committee D-J on Faint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.32 on Drying Oils. ' Current edition approved April 27, 1984. Published August 1984. Originally published as D 555 - 39,. replacing methods appearing in D 12, D 124, D 125, D 234, and D 260. Last previous edition D 555 - 78. 2.1 ASTM Standards: D 56 Test Method for Flash Point by Tag Closed Tester2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2 D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)3 D 564 Test Methods for Liquid Paint Driers'* D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)5 D1259 Test Methods for Nonvolatile Content of Resin Solutions6 D1310 Test Method for Flash Point and Fire Points of . Liquids by Tag Open-Cup Apparatus5 D1358 Test Method for Spectrophotometric Diene Value of Dehydrated Castor Oil and Its Derivatives4 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials4; D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products7 D1541 Test Method for Total Iodine Value ofDrying Oils and Their Derivatives4 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)8 D1545 Test Method for Viscosity of Transparent Liquids by Bubble-Time Method8 D1639 Test Method for Acid Value of Organic Coating Materials7 D 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature7 D1644 Test Methods for Nonvolatile Content of Varnishes7 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTMStandards, Vol 05.01. * Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 6 Annual Book ofASTM Standards, Vol 06.02. 7 Annual Book ofASTM Standards, Vol 06.01. 8 Annual Book ofASTM Standards, Vols 06.01,06.02 and 06.03. I; 89 L DUP050295755 # D 555 D 1950 Test Method for Acetone Tolerance of Heat- samples from cars that contain considerable quantities of Bodied Drying Oils4 settled solid material. If it is known that there is no settled D1951 Test Method for Ash in Drying Oils and Fatty material in a tank car, any one of a number of established Acids4 liquid samplers may be used with good results. D1952 Test Method for Quantitative Determination of Break in Drying Oils4 4. Preparation of Sample ,v,. / D1954 Test Method for Foots in Raw Linseed Oil 4.1 Melt the sample; if it is not already completely liquid. (Volumetric Method}4 The temperature during melting should not exceed 10 to D 1955 Test Method for Gel Time of Drying Oils4 15C above the melting point of the sample. D 1957 Test Method for Hydroxyl Value ofFatty Oils and 4.2 Mix the laboratory sample thoroughly by shaking, Acids4 stirring, or pouring from one vessel to another. Take the D1958 Test Method for Chloroform-Insoluble Matter in specimens for the individual tests from this thoroughly Oiticica Oil4 mixed sample, D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids4 5. Clarity D 1960 Test Method for Loss on Heating of Drying Oils4 5.1 This requirement provides for the quick rejection of D1962 Test Method for Saponification Value of Drying natural oils that are obviously contaminated by solid matter, Oils, Fatty Acids and Polymerized Fatty Acids4 such as dirt, or. water in excess of the solubility limit. D1963 Test Method for Specific Gravity of Drying Oils, 5.2 Most natural oils contain some saturated glycerides, Varnishes, Resins, and Related Materials at 25/25C 4 which may crystallize out at low temperatures giving a D1964 Test Method for Tung Oil Quality4 cloudy appearance. Ifthe cloudiness disappears on warming, D 1965 Test Method for Unsaponifiable Matter in Drying it is probably due to these saturated glycerides and should be J Oils, Fatty Acids and Polymerized Fatty Acids4 disregarded. D1966 Test Method for Foots in Raw Linseed Oil 5.3 Some processed oils are naturally hazy, as a result of (Gravimetric Method)4 the processing methods used, and a clarity requirement D1967 Test Method for Measuring Color After Heating of should not be included in specifications for processed oils Drying Oils4 unless it is known that properly processed oils of the type D1983 Test Method for Fatty Acid Composition by desired will meet the requirements. Gas-Liquid Chromatography of Methyl Esters4 5.4 Determine the clarity in accordance with Test Method D2090 Test Method for. Clarity and Cleanness of Paint D 2090. and Ink Liquids9 D2245 Method for Identification of Oils and Oil Adds in 6. Acid Value Solvent-Reducible Paints4 D2800 Test Method for Preparation of Methyl Esters 6.1 The acid value of an oil is an indication of the condition of the seed from which the oil has been extracted from Oils for Determination of Fatty Add Composition and of the refining to which it has been subjected. It is not by Gas Chromatography4 useful for the identification of the type of oil. D3457 Test Method for Preparation of Methyl Esters 6.2 Test Method D 1639 is generally most satisfactory as from Fatty Acids for Determination of Fatty Acid to precision. There is no choice between sodium and Composition by Gas-Liquid Chromatography4 potassium hydroxides except personal preference. D 3725 Test Method for Semiquantitative Determination of Fish Oil in Drying Oils and Drying Oil Fatty Adds by 6.3 If the percent of free fatty acids calculated as oleic is required, the following equation may be used for the Gas-Liquid Chromatography4 transformation: 3. Sampling 3.1 Sample the material in accordance with Test Method D 1466. This test method covers in considerable detail a procedure for obtaining representative samples of liquid oils and fatty materials from drums, barrels, casks, and tank cars. The test method gives instructions on obtaining representa tive samples from 4000, 6000, 8000, 10 000 and 12 000-gal (15, 23, 30, 38, and 45-m3) cars. Additional directions must be obtained for sampling cars of other capacities. 3.2 Test Method D 1466 takes into consideration the possible presence of settled solid or "footy" materials that may exist in the container. The test method requires that drums or casks be thoroughly mixed by rolling before a sample is taken. However, with regard to tank cars, the procedure, if followed carefully, will yield representative 9 Annual Book ofASTM Standards, Vols 06.02 and 06.03. Free fatty acids, % = 0.503 x acid value 7. Unsaturation 7.1 The drying properties of fats and oils are indicated by the amount and nature of unsaturation they contain. The amount is conventionally expressed as the iodine value, that is, centigrams of iodine absorbed per gram of sample (weight percent of iodine absorbed). The iodine value is a fairly satisfactory measure of the relative drying time and speed of heat-polymerization among a group of oils of the same type. However, because both drying time and heat-polymerization are affected by the kind and distribution of fatty acids in the oil, these methods are not so useful in comparing oils of different types. The measurement of unsaturation is an alternative to the determination of the individual fatty acids for the identification of natural oils, since each natural oil has its own range of unsaturation values. 7.2 Determine the unsaturation of natural drying oils that do not contain conjugated double bonds by the Wijs method i 90 m DU P050295756 l` a. D 555 jibed in Test Method D 1959, which gives fairly good |y and precision. It has largely superseded the Hanus fer methods that tend to give high results. When the fethod is applied to oils containing conjugated double jjSsuch as tung oil and dehydrated castor oil, an pal figure is obtained that is indicative of the relative t of unsaturation present, but is not a measure of the insaturation. With careful control of the reaction Sons, however, reproducible, and useful results may be . |edi Where the total unsaturation is required, make,the' Snation using a modification of the Rosenmund-, ignn method as described in Test Method D 154L ethod gives an accurate measure of total unsaturation jugated oils and is also satisfactory for nonconjugated Hiough somewhat more difficult to. run than the Wijs ad. Quantitative hydrogenation will also yield an accu- asure of the total unsaturation. There is no standard iure for this method. It is the only satisfactory method i containing acetylenic bonds, such as isano oil. . The iodine value is useful for the identification of |i3, soybean, safflower, and similar natural oils. The ant of conjugated diene (or triene) is useful for identiI tung and otticica oils, as well as dehydrated castbr oil. ligated diene is a measure of the quality of dehydrated r oil, although it is not the only measure that should he Determine the amount of conjugated diene by tophotometriC measurement using Test Methods fk with nonglyceride matter, such as mineral oil, hydrocarbon resins, etc. 9.2 Determine the unsaponifiable matter in accordance with Test Method D 1965, which is the referee method. Since the exact amount of unsaponifiable matter obtained is governed by the partition coefficient of the matter between the soap solution and the solvent, different results may be expected if some other solvent such as ethyl ether is used. A rapid, qualitative test for excessive unsaponifiable matter consists in saponifying a small quantity of the oil and diluting with water. A milky emulsion indicates excess unsaponifiable matter. 10. Ash 10.1 Ash is determined by igniting the oil, under specified conditions, and weighing the noncombustible material. Most natural and processed oils contain small amounts of ash, but the amount is insignificant. Certain, synthetic drying oils may contain residual catalyst or other materials, thus giving larger amounts of ash. Although the ash and metal content of boiled ops may, be specified, the trend with, new and improved driers is toward the specification of drying time, allowing the manufacturer to obtain this in any way desired. 10.2 Determine the ash in accordance with Test Method D 1951. Determine the drier metal content of the ash in accordance with Test Methods D 564. Wet ashing or extrac tion methods may give more accurate results. 11. Foots Saponification Value ,1 The saponification value is, essentially, a measure of molecular weight of the latty acid ^portion of the ride, varying inversely with the weight, except for jdn modified oils. It is not a measure of the quality or atity of the oil. The value is useful for certain calculations he use of the oil, such as in the manufacture,of alkyd |,2 Determine the saponification value in accordance Test Method D 1962, which is satisfactory for all armal oils and for many special and synthetic products. As |dicated in the test method, longer saponification times are quired for certain synthetic oils, and some special products toy require the use of a higher-boiling solvent, such as hylene glycol, for complete saponification. ! 8.3 Saponification value is not changed significantly by hlymerization but increases rapidly with oxidation. A pponification value significantly higher than normal indifates the presence of oxidized or blown oils or else modificapn with chemicals such as maleic or fumaric acids. ! 9. Unsaponifiable Matter 9.1 The unsaponifiable matter is a measure of the mate- . trials present in the oil that are oil-soluble and are not rconverted to water-soluble soaps by the saponification con ditions used. A small amount of unsaponifiable matter is 'characteristic of all natural oils, varying with the extraction and refining conditions. Within the limits of the individual oil specifications, the amount of unsaponifiable matter is no measure of the quality or identity of the oil, An excessive amount of unsaponifiable matter indicates contamination 11.1 "Foots" is the term applied to nonoil material that will settle out of natural oils on storage. Since the material measured as foots is usually suspended rather than dissolved in the oil, extreme care in sampling is necessary to get a representative sample for measurement. This applies not only to the sampling of the bulk oil but also to the taking of specimens for running the test. Careful agitation to ensure thorough mixing before sampling is absolutely essential. 11.2 Some of the materials included in the foots hydrate readily in the presence of moisture, particularly at low temperatures, and these hydrated materials have a much larger volume than they had originally. Therefore, oils exposed to moisture for periods of time, particularly with chilling, may be expected to show a substantial increase in volumetric foots with time. 11.3 Determine volumetric foots in accordance with Test Method D 1954. Very careful control of all variables in the test is absolutely necessary, as the test is empirical. Even Under the best conditions, the reproducibility is. not good. The test is usually used for raw linseed oil. It has no, meaning when applied to oils that have been processed to any marked degree. 11.4 Determine gravimetric foots in accordance with Test Method D 1966. The precision of this procedure is much better than the older volumetric method. Internationally the procedure is known as the P.A.T. test and its use is increasing in oil trading. 12. Break 12.1 "Break" is the nonoil material that separates from natural oil on heating. It is usually reported by weight. Break is not significant except in oils that are to be heated, as in the 91 DUP0502 95757 D 555 manufacture of varnishes or alkyd resins, and this require ment should not be included in a specification unless necessary for the proposed end use. 12,2 Determine break in accordance with Test Method D 1952; Test Method D 1952 is empirical, and the condi tions prescribed must be carefully followed, but results correlate well with practical performance. 13. Acetone Tolerance 13.1 The acetone tolerance is a measure of the amount of high polymer in a heat-bodied oil when no nonfatty material is present. It is only applicable to heat-bodied oils and should only be used to assure uniformity of deliveries. There is no correlation between the acetone tolerance and the usefulness of an oil, but, if acetone tolerance and other properties of an oil are the same as those of an accepted sample, the two probably have been produced by the same technique. 13.2 Determine the acetone tolerance in accordance with Test Method D 1950. The test method consists of adding acetone until a cloudy dispersion persists. Temperature is extremely important and must be controlled very closely. This determination may be made as a "cloud point," measuring the'temperature at which cloudiness appears for a given acetone concentration, but this is a more difficult technique, experimentally, for this particular solvent-solute combination. Quantities greater than the smallest traces of water in the acetone also affect the result significantly, and the amount must be kept within the prescribed limits. 14. Gel Time 14.1 Gel time is a measure of the tendency of oils to solidify under certain specified conditions. The test is de signed primarily for the detection of adulteration in tung and oiticica oils. The method, usually at a higher temperature, may also be used to,evaluate oils treated to produce rapid polymerization as well as dehydrated castor oil. The method is not applicable to natural oils such as linseed and soybean that do not show a sharp end point at practicable tempera tures. Other natural oils such as tung and oiticica are subject to some variation, depending upon many factors. Slight variations from the standard values should not at first glance be taken as sufficient evidence of adulteration. 14.2 Determine the gel time in accordance with Test Method D 1955. In this test method, since the volume of the oil bath is relatively small, the bath is chilled by the introduction of the specimens, and must be raised above the operating temperature in order to be correct after insertion of the tubes. Since the control of temperature is very important and is difficult to maintain accurately by manual means over a long period of time, oils that gel slowly should be tested at higher (but accurately defined) temperatures, in order that gelation may take place in.a reasonable time. . 15. Tung Oil Quality Test 15.1 Determine the quality of tung oil in accordance with Test Method D 1964, which is designed to detect adultera tion of tung oil with nonconjugated oils. It is not intended for use with any other oil. Temperature is extremely impor tant, and the correct thermometer, used in the correct way, is essential. 16. Hydroxyl Value 16.1 The hydroxyl value is a measure of hydroxyl content i of an oil, expressed as milligrams of potassium hydroxide 1 equivalent to the hydroxyl content of 1 g of oil. It is used to ' determine the efficiency of the dehydration of dehydrated J castor oil. It is also a measure ofthe residual hydroxyl groups | of processed oils, when other interfering groups are not present. 16.2 Determine the hydroxyl value in accordance With Test Method D 1957. This test method involves the acetylation of hydroxyl-containing fatty oils and adds using pyridine as solvent. Other groups that-Wilfreact with acetic anhydride under the conditions of the telt method will be reported as hydroxyl. A correction is applied for acid groups present and, if necessary, similar corrections may be applied for other interfering groups. 17. Loss on Heating 17.1 Determine the loss on heating in accordance with : Test Method D 1960, which is a quick method for detecting contamination or adulteration of natural oils with volatile solvents. It is not a true loss measure since small amounts of | oxygen, if any, in the inert gas used will be absorbed by the ' oil, resulting in a small gain in weight, that may more than 1 offset small losses. This method should be used only for gross ! contamination. When small amounts of flammable volatile : solvent are to be qualitatively detected, as in solvent- ; extracted oil, use Test Method D 93. For oils containing larger amounts of volatile matter where an accurate determi nation is required, use Test Methods D 1259 or D 1644. 18. Matter Insoluble in Chloroform 18.1 The matter insoluble in chloroform, in a drying oil,' represents mineral contamination, since all materials natu rally occurring in such oils are soluble under the conditions , outlined in this test method. 18.2 Determine insoluble matter in accordance with Test s Method D 1958. This test method is rarely applied to drying oils other than oiticica oil which, because of the production ; process, may be contaminated with mineral matter. 19. Color 19.1 The color of an oil, in bulk, is usually relatively useful in predicting how it will behave in use in comparison ? with other similar oils. However, since some oils darken on heating or oxidation and others bleach, the color in bulk is rarely helpful in comparing oils of different types. 19.2 Determine the color by comparison with standards, < either liquid or glass, as described in Test Method D 1544 which is the fastest method and, in general, is sufficiently accurate. For extremely light-colored oils (Gardner color No. 3 or lower) use the APHA or Hazen method as described in j Test Method D 1209. Since this test method uses a much ; thicker layer of oil than Test Method D 1544, light colors ' may be judged more precisely. However, because of this thickness difference, there is no precise correlation between the two methods and the method specified must be used. No t e 1--For edible oils, methods based on Lovibond glasses (American Oil Chemists' Society Method Cc 13b) or, rarely, on spectrophotometric measurements (AOCS Method Cc 13c) are used. 92 2 DUP050295758 Dws and certain other inedible oils, the. FAC Method {AOCS ; Cc 13a) is commonly specified. These methods should not be for drying oils. In making visual comparisons of the color of spec- and standard, careful control of the conditions of illu- ation and view are necessary if high precision is called Care must be taken that the observer has normal color ption. ,4 Standards darker than Gardner color No. 18 are not useful, since comparison of specimen and standard the conditions specified is difficult. When it is neces- >to specify the color of very dark oils, it is usually more factory to specify the color of the oil diluted with a amount of solvent sufficient''! bring the color into range of the standard color-measuring methods. The of the solvent and the dilution must be specified ctiy. . : Specific Gravity 0.1''Specific gravity of an oil is, a useful measure, since ation from volume to weight, or vice versa, is often jtired. For this reason. it should be determined with care, cific gravity is not a measure of the quality ofthe cal, and 011 that deviates slightly from the specified limits,, but erwise conformsj is usually completely satisfactory. Spe- 'c gravity,, increases with polymerization or oxidation in a "ar manner, and for every bodied or blown oil of a given eosity there is an appropriate specific gravity: 12 Determine the specific gravity,in, accordance with st Method D 1963, which is capable,of high precision and the referee method. If less accurate results (3 significant res) are adequate, "weight-per-gallon" cups as described Test Method D 1475 may.be used. Specific gravity is very ensitive to temperature, and the temperature of measure ment must be controlled, or at least known, with high ^precision. If measurements are made at other than the Standard temperature, or if the value of the specific gravity is Inquired at some temperature other than the standard, the Approximate value may be calculated as described in Test Method D 1963. 21. Refractive Index 21.1 Refractive index is a scientifically defined property Add numerous accurate instruments are available for its determination. Since the method used depends upon' the instrument, no method for its determination is given. Any one of a large number of instruments operated according to the manufacturer's instructions will give satisfactory results. 21.2 Refractive index is riot a very useful means of specifying drying 6ils. It is useful in detecting adulteration in oils containing substantial amounts of conjugation, such as tung, oiticica, and dehydrated castor oils. Since refractive index varies with iodine value, it can be used as a quick approximation of iodine value. 22. Viscosity 22.1 Viscosity is the resistance experienced by one portion of a liquid flowing over another portion. It is expressed in poises, the absolute unit, or in stokes, equivalent to poises divided by density. 22.2 The viscosity of most natural oils is very low and its specification serves no useful purpose. Tung, oiticica, castor, and many processed oils have measurable (by the tube method) viscosities, but in the case of processed oils the viscosity is a result of the method of processing and is in no way related to the merit of the oil. 22.3 Determine the viscosity of drying oils in accordance with Test ,Method D 1545. This test method describes a means for measuring the travel of an air bubble in a cylindrical tube either by timing or by comparison with standard tubes of known viscosity. The results are very close to the true viscosity in stpkes, but are not exactly correct, so that viscosity determined by this test, method should be reported in "approximate stokes" or "bubble seconds." More precise results may be obtained for viscosities of less than 4,s by comparison with standards, and for more ,viscous oils by timing, If higher- precision is required, use capillary viscometers, such as those described in Test Method D 445. Results obtained ,in poises should be divided by the density to give stokes. ,, 22.4 When tube methods,are used, results are affected by the size and shape of the air bubble. Therefore, if precise results are required, tubes conforming exactly to the standard must be used, and the air bubble must be adjusted to the correct size. A difference in tube diameter of 0.05 mm will result in an error of approximately 2%. All viscosity measurements are very sensitive to temperature and ex tremely close temperature control (0.lC) is necessary for precise results. 23; Drying Properties 23.1 Since drying oils, by definition, set to a solid film, the time required for this to take place is an important property of all such oils. Unfortunately, the time required is greatly affected by a number of variables including temperature, drier content, light, humidity, film thickness, air circulation, etp. All these must be controlled with great care to assure reproducible results. Furthermore, results obtained under one set of conditions do not necessarily allow prediction of results that might be obtained under other conditions. 23.2 Empirical measures of drying properties are useful in comparing one oil with others of the same general type, but must be used cautiously otherwise. Because of the effect of pigmentation and other variables, it is difficult to predict the drying time of a paint ,from the drying time of the oil used in its manufacture. 23.3 Select from Test Methods D 1640 one Set of gener ally acceptable conditions (except for drier content, which must be specified). These conditions may, of course, be varied as required, but any variation must be outlined care fully ifagreement is to be obtained. Numerous other methods of measuring drying time have been proposed. Most of these use some mechanical device to determine the end point. However, many of these devices interfere, in an unpredict able inanner, with the circulation of air, the amount of oXygen, and the amount of light available to the film so that results are likely to be erratic. The most widely used device, the Sanderson machine which drops sand on the film, gives results between the "set-to-touch" and "diy" times. 23.4 Since the drying of oils is a continuing process that goes on indefinitely, it is difficult to select sharp end points that may be measured precisely. The "set-to-touch" point, 93 DUP050295759 D 555 where the internal cohesion of the film exceeds its adhesion to the finger, is probably the sharpest. This point coincides very closely with the point where the film changes from a liquid to a gel. The "dry time" is more subjective, and it is difficult to get close agreement between laboratories, espe cially for oils with relatively long drying times. Agreement, however, is better as to whether or not a film is dry at a specified time. 24. Flash Point 24.1 The flash point of a liquid is defined as the lowest temperature, corrected to 101.3 kPa (760 mmHg) of pres sure, of the material under test at which application of an ignition source causes its vapor to ignite under specified conditions of test. 24.2 Most natural and synthetic drying oils have very high flash points of about 500F (260C), unless they contain traces of volatile, flammable materials. If the contaminating solvent is known, it is possible to set up a relationship between the solvent content and the flash point. 24.3 Flash point of vegetable oils is helpful in determining that nd hazardous amounts of solvents have been left in solvent-extracted oils, or that the oils have been contami nated with such solvents. If flammable solvents are not present, the flash point of natural oils is meaningless as far as specifications are concerned. 24.4 Determine the flash point in accordance with Test Method D 93 which uses the Pensky-Martens Closed Cup. Use Method B for Testing flash point of highly viscous materials. The exact flash point obtained is empirical, depending upon the rate of heating and other factors set forth in the test method. These must be followed carefully if reasonable precision is to be obtained. No t e 2--If open-cup methods, such as Test Method D1310 are used, traces of flammable solvents may evaporate and be lost without ever igniting and an unduly high result may be obtained. Since many oils are fairly viscous liquids, the use oftest methods that do not provide for stirring, such as Test Method D 56, may give anomalous results. 25. Color After Heating of Drying Oils 25.1 Some drying oils darken on heating to polymeriza tion temperatures while others may lighten^ in color. The procedure in Test Method D 1967 gives an indication of this color change. ^ 26. Composition of Drying Oils and Fatty Acids by GasLiquid Chromatography 26.1 Gas-liquid chromatography has proven to be a very effective tool for the determination of the fatty acid compo sition offats and oils. It is often beneficial to'know the actual chemical composition of a fatty mixture. This can be ob tained by the use of several applicable related ASTM test methods. 26.2 The oil or fatty add to be tested must first be con verted to the methyl ester for the gas-liquid chromatographic determination. This is accomplished using Test Method D 2800 in the case of oils and Test Method D 3457 for fatty adds. 26.3 Test Method D 1983 is the general method for the determination of composition by gas chromatography. Test Method D3725 shows the modifications to Test Method D 1983 needed to determine fish oil present in other drying oils. This gas-liquid chromatography method is more reliable than the old bromination procedures referred to in Appendix X1.3. 26.4 Typical composition of oils used in paint products are shown in Table 1 of Method D 2245. APPENDIX (Nonmandatory Information) XI. REFERENCES TO DELETED METHODS XI. 1 ASTM Method D 1956, Test for Heat Bodying Rate of Drying Oils, last appeared in Part 29 of the 1974 Annual Book of ASTM Standards. Last approved in 1969. With drawn in April 1975. X1.2 ASTM Method D 1961, Test for Maleic Diene Value of Drying Oils, last appeared in Part 29 of the 1974 Annual Book ofASTM Standards. Last approved in 1969. Withdrawn in April 1975. X1.3 ASTM Method D 1724, Qualitative Determination of Fish Qil in Drying Oils and Drying Oil Fatty Adds, last appeared in Part 29 of the 1978 Annual Book of ASTM Standards. Last approved in 1974. Withdrawn in 1978. This method is still used in ISO 150, Specification for Raw, Boiled, and Refined Linseed Oil. XI.4 The preceding methods have been deleted due to nonuse or due to replacement by other more reproducible methods. Ifthe instrumentation or equipment needed for the new methods is not available then by mutual agreement be tween concerned parties the older methods, copies of which may be obtained from ASTM Headquarters, may be used. The American Society for Testing amiMaterials 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 the risk oi infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee arid must be reviewed every five years and ifnot revised, either reapproved or withdrawn Your comments are Invited e/Wer forrevision oi this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technics 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. 94 DUP050295760 Designation: D 564 - 87 (Reapproved 1991),'61 Standard Test Methods for Liquid Paint Driers1 This standard is issued under the fixed designation D 564; 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, tf' ! These test methods have been approvedfor use by agencies ofthe Department ofDefense to replace Method 7231 cfFederal Test Method Standard No. Mia. Consult the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department-^Defense. c 1No t e--Keywords were added editorially in June 1991. Scope ftl These test methods cover the test procedures to be fifed to liquid paint driers used in paints and related fings. Typical paint driers, listed in Specification D 600, carboxylates of lead, cobalt, manganese, zinc, iron, and zirconium. |2 This standard does not purport to address all of the problems, if any, associated with its use. It is the onsibility ofthe user ofthis standard to establish appro ve safety and health practices and determine the applica- jjfy cfregulatory limitations prior to use. t >. Referenced Documents jjl.l ASTM Standards: |p234 Specification for Raw Linseed Oil2 |P 235 Specification for Mineral Spirits (Petroleum Spirits) I (Hydrocarbon Dry Cleaning Solvent)2 p>600 Specification for Liquid Paint Driers2 ft) 1544 Test Method for Color of Transparent Liquids I; (Gardner Color Scale)3 ll> 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature4 IfD1644 Test Methods for Nonvolatile Content of Var nishes4 |ID 2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids5 I 2373 Test Method for Determination of Cobalt in Faint Driers by EDTA Method2 |T :D2374 Test Method for Lead in Paint Driers by EDTA Method2 D2375 Test Method for Manganese in Paint Driers by EDTA Method2 D26I3 Test Method for Calcium or Zinc in Paint Driers by EDTA Method2 D 3804 Test Method for Iron in Paint Driers by EDTA Method2 ! 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 Nov. 27, 1987. Published January 1988. Originally published as D 564 - 40. Last previous edition D 564 - 81. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. ` 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.02 and 06.03. D 3924 Specifications for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer, and Related Material4 D3969 Test Method for Zirconium in Paint Driers by . EDTA Method2 , D3970 Test Method for Cerium in Paint Driers by Oxidimetric Determination2 D3980 Practice for Interlaboratory Testing of Paint and Related Materials4 . D3988 Test Method for Vanadium in Paint Driers by EDTA Method2 D 3989 Test Method for Total Rare Earth Metals in Paint Driers by EDTA Method2 3. Significance and Use 3.1 Driers accelerate the drying of oil, paint, printing ink, and varnish. 3.2 These test methods are applicable to liquid driers manufactured for use in paints and related coatings. 3.3 The tests for metallic content using EDTA are in tended for concentrated solutions of single metals; two or more metals may cause interference. 4. Physical Tests 4.1 Sampling--Sample in accordance with Practice D 3980. 4.2 Conditioning---Follow. Specification D3924 except where other temperatures are specified. 4.3 Appearance--After conditioning overnight at room temperature (see Specification. D 3924) examine the drier without aid of magnification for clarity and cleanness and for presen9e of foreign matter, sediment, skins, turbidity or haziness, in accordance with Test Method D 2090. 4.4 Sediment or Suspended Matter--If sediment or sus pended matter is observed, proceed as follows: 4.4.1 Weigh to 1 mg, by difference, 1 to 5 g of drier into a tared 10 to 15-pm fritted-glass crucible. After most of the drier has passed through wash with mineral spirits con forming to Specification D 235 and dry at 50C until the weight is coiistant to 1 mg. Calculate the difference in weight and report as percent sediment in the drier. 4.5 Color--Determine color in accordance with Test Method D 1544. No t e 1--This scale is useful for yellow and brown organic chromophores, but not with the reds or purple of cobalt and certain other metal compounds. 95 DUP050295761 4ft D564 4.6 Nonvolatile Matter--Determine the nonvolatile con tent in accordance with Test Methods D 1644 using either Method A or B as mutually agreed upon between the supplier and the user. 4.7 Miscibility with Oil--Mix 1 volume of the sample with 19 volumes of raw linseed oil under room temperature conditions. Record any signs of separation or clouding. Observe the mixture at 1-h intervals for 3 h and again after 24 h. For the reference use the raw linseed oil kept in a container similar to the one with the test specimens. No t e 2--In case of disagreement between the supplier and the user, make the test for miscibility with oil at 25 1C. No t e 3--The linseed oil specified in Specification D 234 may vary in clarity from one commercial source or linseed crop year to another and in content ofsmall amounts of moisture. Aging from one to six months in a closed container at 23C or (or even 10Q and then decanting supernatant'oil from sediment may yield a more Uniform linseed oil for miscibility testing. *4.8 Stability--Each drier shall show no clotting or gela tion or evidence of precipitation after standing for 7 days at 25C, --20G, r 50*C. If there is evidence* of clotting, gelation, or precipitation after 7 days at* --20C or 50C, the* drier is still consideredsatisfactory ifall signs ofclotting, gelation, or precipitation disappear after it is permitted to stand over night at room temperature. 4.9 Drying Power--Determine the drying power in accor dance with Test Methods D 1640. It is useful to test a previously evaluated standard of known drying power for comparative purposes. No t e 4--The drying powers or efficiencies ofindividual metal driers may be a function of: (1) the class of carboxylic acids, for example, octoate versus naphthenate, etc., (2) additives in drier solutions, for example, stabilizers, etc., (3) chemical unsaturation ofthe drying oil, (4) other metals used in conjunction with the subject drier, and (5) the other components (for example, pigments, etc.) in the formulated paint. 5. Chemical Analysis , 5.1 Cobalt--Determine in accordance with Test Method D 2373. 5.2 Lead--Determine in accordance with Test Method D 2374. 5.3 Manganese--Determine in accordance with Test Method D 2375. 5.4 Calcium--Determine in accordant with Test Method D 2613. .- * 5.5 Zinc--Determine in accordance with Test Method D2613. 5.6 Iron--Determine in accordance with Test Method D 3804. 5.7 Zirconium--Determine in accordance with Test Method D 3969. 5.8 Cerium--Determine in accordance with Test Method D 3970. 5.9 Vanadium--Determine in accordance with Test Method D 3988. 5.10 Rate Earth--Determine in accordance with Test, Method D 3989. ' 6. Keywords 6.1 driers, standard tests; liquid paint driers APPENDIX (Nonmandatory Information) XI. HISTORICAL INFORMATION XI.1 Historic methods for testing lead, cobalt, calcium, zinc, manganese, and iron can be found in the 1979 Annual Book ofASTM Standards, Part 29, Method D 564. XI . 1.1 These methods were ofprimary interest before the introduction (about 1930) of commercial naphthenate driers that enabled higher concentrations of drier metals in solutioti, than in much earlier practice when the oxides and salts of lead, manganese, and cobalt were saponifiedwhile heating with linseed oil, resin, and other naturally occurring organic acids or esters. Metal concentrations were then as low as 10 % lead, 1 % manganese, or 0.5 % cobalt. X1.2 Methods for testing cerium (Test Method D 3970), rare earth metals (Test Method D 3989), zirconium (Test Method D 3969), and vanadium (Test Method D 3988) are being developed. Each is suitable for the determination ofthe metal content ofthe drier which does not contain other drier elements. Each method is not applicable to drier blends. XI.3 An atomic absorption method is being developed that will be suitable for singular driers as well as drier blends. .The American Society,for Testing and Materials takes no position respecting the validity of any patent rights asserteo in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved orwlthdrawn. Your comments are invited either tor revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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. 96 DU P0502 95762 ; Designation: D 600 - 90 Standard Specification for Liquid Paint Driers1 This standard is issued under the fixed designation D 600; 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. This specification covers liquids for, use in paints, es, enamels, and similar organic coatings and are ns of metallic salts of: / ; lil Class A--2-Ethyl jSexanoic acids in petroleum V'' ' V > ,2 Class B--Naphthenicacids in petroleum spirits. |3 Class C--Neodecanoic acids in petroleum spirits. .4 Class D--Tall oil fatty adds irn petroleum spirits. .5 Class E--Any of the above adds or acid blends, but 'Some other driers may also contain complexing agents. .6, Class F--Other acids and add blends unidentified eir producers. For spedfic hazard information and guidance, see the lier's Material Safety Data Sheets for materials listed in specification. .eferenced Documents .1 ASTM Standards: ) 564 Test Methods for Liquid Paint Driers2 >1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)2 ) 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method2 ,;2.2 V.S. Federal Specification; ! 1 This specification is under the jurisdiction ofASTM Committee P-1 on Paint d Related Coatings and Materials and is the direct responsibility of Subcom- ittee D01.3S on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally Wished as D 600 - 73 (1978). Last previous edition D 600 - 85. 2 Annual Book ofASTM Standards, Vol 06.03. PPP-C-2020 Chemicals, Liquid, Dry, andFaster Packaging of3 3. Significance and Use 3.1 This specification covers the general requirements for liquid paint driers used in paints, varnishes, enamels, and similar organic coatings. 3.2 The values listed should be considered as general guides to the character ofthe products, rather than reproduc ible constants. 4. Chemical and Physical Requirements 4.1 Quantitative Requirements--The drier shall conform to the quantitative requirements as specified in Table 1 for metallic content, color, and viscosity. 4-2 Physical Appearance--Each type of drier shall be a mobile liquid free of sediment and suspended matter and shall be stable and miscible with oil as listed in Test Methods D564. 5. Test Methods , 5.1 The properties enumerated in this specification shall be determined in accordance with Test Methods D564, except as otherwise provided in this specification. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 liquid paint driers 5 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 97 DU P0502 95763 - n - n m D 0 3 0 J > > O C D > > > -n - m i m m a o a j> * n n m o o o J > * n * n ,'ii3 J > -n '*i m m o o a J > > 0 5 > - n - n - n - n m m m o o o j a i > > Metal Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Calcium Cerium Cerium Cobalt Cobalt Cobalt Cbbalt Cobalt Cobalt Cobalt Cobalt Cobalt Iron Iron . Iron Iron Iron Lead : Lead Lead Lead Lead Lead Lead , Manganese Manganese Manganese Manganese Manganese Manganese Manganese Manganese Manganese Nickel Rare earth0 Rare earth Rare earth Rare earth Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc (ft* D 600 TABLE 1 Typical Requirements of Liquid Paint DriersA Metal Concentration, * Nonvolative Matter, % Typical Specific Gravity 25/25C min max max min max 3.9 4.9 3.9 4.9 4.9 3.9 3.9 5.9 3.9 4.9 5.9 7.9 9.9 5.9 5.9 5.9 11.8 ' 5.9 11.8 5.9 4.9 5.9 5.9 11.8 5.95.9 . 5.9 . 8.9 1 '11.8 ' 23.8 23.8 23.8 23.8 23.8 23.8 35.8. 5.9 , '5.9 5.9 5.9 4.9 5.9 5.9 8.9 11.8 9.9 5.9 11.8 3.9 5.9 7.9 17.8 7.9 . 9.9 7.9 7.9 7.9 15.8 4.1 5.1 4.1 5.1 5.1 4.1 4.1 6.1 4.1 5.1 6.1 8.1' 10,1 6.r 6.1 6,1 12.2 6.1 12.2 ; 6.1 5.1 6.1 ' . 6.1 12.2 6.1 6.1 6.1 9.1 12.2 ' 24:2 24.2 24.2 24.2 24.2 24.2 36,2 . 6.1 . 6.1 ' 6.1 6.1 5.t 6.1 6.1 9.1 12.2 10.1 6.1 12.2 4.1 6.1 8.1 18.2 8.1 10.1 8.1 8.1 8.1 16.2 50 60 70 85 46 66 63 76 50 60 74 70 65 30 57 45 90 67 65 72 60 71 70 80 50 67 50 . 78 75 65 67 61 66 71 67 81 . 50 66 .50 72 -42 69 65 80 75 70 30 55 35 35 50 90 70 75 70 42 60 80 0.884 0.894 0.9Q2 0.932 0.888 0.890 0.905 0.922 0.850 0.900 0.873 0.958 1.000 0.856 0.925 0.875 1.008 0.918 0.984 0.912 0.926 0.945 0.870 1.014.' 0.900 . 0.960 0.905 0.950 1.068 1.090 1.125 1.100 1.100 1.125 1.080 1.350 0.888 0.930 0.870 0.942 0.911 0.942 0.870 0.950 1.044 1.032 0.630 0.977 0.840 0.876 0.880 1.068 0.915 0.980 1.008 0.946 0.855 1.020 0.912 0.937 0.970 --0.918 0.930 0.S60 0.884 0.936 0.948 --- ' 1.030 --- -- 0.900 1.060 0.970 -- 0.956 -- 0.960 0.958 1.040 0.930 0.990 0.930 0.985 , -- 1.110 1.--160 1.125 1.150 1.140 1.393 0.920 0.965 -- . 0.972 -- 0.955 1.020 1.020 -- -- 0.880 -- 0.855 -- 0.906 1.130 0.960 1.044 -- -- 0.963 1.100 Color, Gardner (Test Method D1544) 3 5 10 11 2 9 8 5 3 .4 6 .5 , 7-8 B 17 ' blue/purple 1 blue/purple blue/purple blue purple red/purple blue/purple blue/violet blue/violet dark brown dark brown brown brown brown 3 11 2 10 7 10 8 red/brown 17 '10 brown brown brown 18 18 16 sh. green 6 yel.-green 10 e 6 7 9 8 11 2 7 3 G-H Viscosity (Test Method D 1545) A c D T A B G N A B N B K A A1 A J B A c A 1 A J AM A A A A B A2 A A A H A D A E A E A H C A E C A A5 G Z A L D A C B 98 DUP050295764 D 600 TABLE 1 Continued Metal Metal Concentration, min max Nonvolative Matter, % max Typical Specific Gravity 25/25C min max Color,8 Gardner D1544) G-H Viscosity D1545) Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium Zirconium 5.9 s:i 11.8 12.2 17.8 18.2 23.8 24.2 5.9 6.1 11.8 12.2 5.9 6.1 11.8 12.2 5.9 6.1 11.8 12.2 17.8 18.2 23.8 24.2 30 56 55 77 23 46 31 55 28 55 80 93 0.860 0.960 1.070 1.240 0.864 0.976 0.864 0.975 0.855 -- 1.090 1.240 0.864 0.992 1.074 ---' -- -- -- 1.020 0.870 -- 1.130 1.260 2 4 3 2 2 2 4 4 2 -- 4 6 A A A J A5 A A A A5 -- Z J ource: `Raw Material Index," National Paint and Coatings Association Guide, Chemical Specialties Section, April 1978. Available from National Paint and Coatings <1500 Rhode Island Ave. NW, Washington, DC 20005. er Gardner Test Method D1544. If off the scale, as observed by the unaided eye. n|y one drier was listed in this category. le metal content represents total rare earth metals calculated as cerium, but the drier contains cerium and lanthanum, as well as minor amounts of other rare earth ;, -4 ;- 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 ofthis standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard 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. 99 DUP0502 95765 I Designation: D 601-87 (Reapproved 1991)1 Standard Specification for Oiticica Oil (Permanently Liquid)1 This standard is issued under the fixed designation D 601; 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 (c) indicates an editorial change since the last revision or reapproval. u S r;- "No t e--Keywords were added editorially in August 1991. |: 1. Scope 1.1 This specification covers oiticica oil that has been treated to render it permanently liquid. m ! D 1958 Test Method for Chloroform Insoluble Matter in Oiticica Oil3 D 1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25 C3 - 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)2 , D555 Guide for Testing Drying Oils3 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method5 D1639 Test Method for Acid Value of Organic Coating Materials4 D1955 Test Method for Gel Time of Drying Oils3 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 D 01.32 on Drying Oils. Current'edition approved Oct. 30, 1987. Published December 1987. Originally published as D 601 - 41. Last previous edition D 601 - 55 (1981)". 2 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. s Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3. Properties A 3.1 Oiticica oil (pcrmanchtfy liquid) shall conform to the requirements in Table 1. > 4. Test Methods 4.1 Sampling--Sampling shall be conducted in accor dance:with Test Method D 1466. 4.2 The properties enumerated in this specification shall be determined in accordance with the applicable ASTM test methods listed in Table 1. The significance of these test methods enumerated under properties in this specification is discussed in Methods D 555. 5. Keywords 5.1 drying oils; oiticica oil TABLE 1 Physical Properties Property Requirement' Specific gravity, 25/25C, min Viscosity at 25I'C, approximate Stokes Acid value, max Iodine value (Wijs), min Color (Gardner 1933 Standards), max Gel time, minutes, max Refractive index at 25C, min Matter insoluble in chloroform, max, % 0.972 11 to 23 8.0 135 11 17 1.5100 0.1 ASTM Method D1963,D1475 D1545, D 445 D1639 D1959 01544 D 1955 D 1958 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 the! determination of the validity of any such patent rights, and the risk of tntrlngement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you 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. 100 DUP050295766 Designation: D 608 - 90 Standard Specification for Dibutyl Phthalate1 This standard is issued under the fixed designation D 608; 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. fjjpcope p.1 This specification covers dibutyl phthalate (99 % lade). ft 1.2 For specific hazard information and guidance, see the Supplier's Material Safety Data Sheet for materials listed in fjiis specification. Referenced Documents wM D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 |!D 1209 Test Method for Color of Clear Liquids (Platinum- |; Cobalt Scale)3^ j '1 |p 1296 Test Method for Odor of Volatile Solvents and p `Diluents2 pD 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 I' D 1476 Test Method for Heptane Miscibility of Lacquer Solvents2 FD1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 FD1617 Test Method for Ester Value of Solvents and Thiriners2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 300 Practice for Sampling Industrial Chemicals3 j-: 2.2 ' U.S. Federal Specification: *1 PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of6 t- * * 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 D01.35 on Solvents, Plasticizers, and Chemical. Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 608 - 41 T. Previous edition D 608 - 85. ' 2 Annual. Book ofASTM Standards, Vo! 06.03. s 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. * Annual Book ofASTM Standards, Voi 05.03. k 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. . 6 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 Dibutyl phthalate (99 % grade) shall conform to the following requirements: Apparent specific gravity: 20/20C 25/2JC Color, Pt-Co scale, max Odor Water, max, weight % Acidity (free acid as phthalic acid), max, weight % Ester value, max, weight % 1.046 to 1.050 1.043 to 1.047 20 nonresidual 0.2 ^ 0.01B not less than 99.0 A This quantitative limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20"C. * Equivalent to 0.067 mg of K.OH per gram of sample. 4. Sampling 4.1 The material shall be sampled in accordance with Piactice E 300. 5. Test Methods 5.1, The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20 or-25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Odor--Test Method D 1296. 5.1:4 Water--Test Methods D 1364 and D 1476. 5.1.5. Acidity--Test Method D 1613. 5.1.6 Ester Value--Test Method D 1617. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 dibutyl phthalate The American Society lor Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility.- This standard Is subject to revision at:any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Yourcomments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive cereful consideration at a meeting ot the responalble 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, 191B Race St, Philadelphia, PA 19103.101 101 DUP050295767 Designation: D 611 -82 (1987)*2 Designation: 2/84 An American Naiiona) Standard Standard Test Methods for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents1 This standard is issued under the fixed designation D 611; 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. . These lest methods were adopted as ajoint ASTM-IP standard in 1964. These test methods have been approved for use by agencies of the Department of Defense and for listing in the DoD Index of Specifications and Standards. (l No t e--Editorial changes were made throughout in October 1987. "No t e--Table 1 was corrected editorially in December 1989. 1. Scope 1.1 These test methods cover the determination of the aniline point of petroleum products and hydrocarbon sol vents. Method A is suitable for transparent samples with an initial boiling point above room temperature and where the aniline point is below the bubble point and above the solidification point of the aniline-sample mixture. Method B, a thin-film method, is suitable for samples too dark for testing by Method A. Methods C and D are for samples that may vaporize appreciably at the aniline point. Method D is particularly suitable where only small quantities of sample are available. Method E describes a procedure using an automatic apparatus suitable for the range covered by Methods A and B. 1.2 These test methods also cover the determination of the mixed aniline point of petroleum products and hydro carbon solvents having aniline points below the temperature at which aniline will crystallize from the aniline-sample mixture. 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 precautionary statements are given in Sections 7.1 and 7.3. 2. Referenced Documents 2.1 ASTM Standards: D 1015 Test Method for Freezing Points of High-Purity Hydrocarbons2 D 1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham Pycnometer2 1 These test methods are under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and are^the direct responsibility of D02.04 on Hydrocarbon Analysis, Current edition approved Aug. 27, 1982. Published January 1983. Originally published as D 6 H - 41 T. Last previous edition D 611 - 77. 2 Annual Book ofASTM Standards, Vol 05.01. D 1218 Test Method for Refractive Index and-Refractive Dispersion of Hydrocarbon Liquids2 D 1500 Test Method for ASTM Color of Petroleum Products (ASTM Color Scale)2 D 2700 Test Method for Knock Characteristics of Motor and Aviation Fuels by the Motor Method3 E 1 Specification for ASTM Thermometers4 3. Definitions 3.1 aniline point--the minimum equilibrium solution temperature for equal volumes of aniline and sample. 3.2 mixed aniline point--the minimum equilibrium solu tion temperature of a mixture of two volumes of aniline, one volume of sample, and one volume of n-heptanc of specified purity. 4. Summary of Test Methods 4.1 Specified volumes of aniline and sample, or aniline and sample plus n-heptane, are placed in a tube and mixed mechanically. The mixture is heated at a controlled rate until the two phases become miscible. The mixture is then cooled at a controlled rate and the temperature at which two phases separate is recorded as the aniline point or mixed aniline point. 5. Significance and Use 5.1 The aniline point (or mixed aniline point) is useful as an aid in the characterization of pure hydrocarbons and in the analysis of hydrocarbon mixtures. Aromatic hydrocar bons exhibit the lowest, and paraffins the highest values. Cycloparaffins and olefins exhibit values that lie between those for paraffins and aromatics. In homologous series the aniline points increase with increasing molecular weight. Although it occasionally is used in combination with other physical properties in correlative methods for hydrocarbon analysis, the aniline point is most often used to provide an 3 Annual Book ofASTM Standards. Vol 05.04. 4 Annual Book ofASTM Standards, Vol 05.03. 102 DU P050295768 D 611 TABLE 1 Requirements tor n-Heptane ASTM Method i,Octane Number C, g/mL 'fex.no2000 f, c 50% recovered at | (760 mm Hg), C )% recovered minus ,C 0.0 0.2 0.S8380 0.00015 1.38770 0.00015 --90.710 min 98.427 0.025 0.020 max D 2700 D 1217 D 1218 D 1015 A equipment and method used, see Journal of HRersearch, Nat. Bureau . %l 44, No. 3.1950, pp. 309 arid 310 (RP2079). I corrected. i^te of the aromatic hydrocarbon content of mixtures, aratus 'For details of the aniline point apparatus required for ethod see: ' " , Annex A1 for Method A Annex A2 for Method-B Annex A3 for Method C Annex A4 for Method D Annex A5 for Method E -Alternative apparatus may be used, such as the U-tube for dark oils, provided it has been shown to give results of the ecjsion and accuracy as those described in the Annexes. Heating and Cooling Bath--A suitable air bath, a olatile, transparent liquid bath, or an infrared lamp `q 375 W), provided with means for controlling the rate *$ng. t e 2--Water should not be used as either a heating or cooling since aniline is hygroscopic and moist aniline will give eous test results. For example, the aniline point of the n-heptane :nt .as measured with aniline containing 0.1 volume % water is dximately 0.5C (0.9F) higher than that measured with dry aniline, ie aniline point is below the dew point ofthe atmosphere, pass a slow of dry inert gas into the aniline point tube to blanket the ine-sample mixture. \3 Thermometers, having the following ranges and con ning to the requirements of the designated ASTM or IP cification: Range ASTM (Specification E 1) IP .98 to +42"C (-36.5 to +107.5'F) 25 to 105*C (77 to 22 ("F) j|90 to 170"C (194 to 338"F) 33C, 33F 34C, 34F 35C, 35F 20C 21C 59C 6.4 Pipets, with capacities of 10 0.04 mL, 5 0.02 mL, _e latter equipped with a long, fine tip. Provide a rubber section bulb for use with pipets when measuring aniline. 6.5 Balance--A laboratory balance sensitive to 0.01 g, suitable for weighing the tube and sample when the sample cannot be pipetted conveniently. 6.6 Safety Goggles. 6.7 Plastic Gloves, impervious to aniline. 7. Reagents 7.1 Aniline (Warning--See Note 3.) Dry chemically pure aniline over potassium hydroxide pellets, decant, and distill fresh on the day of use, discarding the first and last 10 %. Aniline thus prepared when tested with n-heptane according to Section 9 shall give an aniline point of 69.3 0.2C (I56.7 0,4F) as determined from the average of two independent tests having a difference of not more than 0.1C (0.2T). No t e 3: Warning:Aniline should not be pipetted directly by mouth because of its extreme toxicity. Aniline is also toxic by absorption through the skin even in very small quantities, and should be handled with great caution. No t e 4--For routine purposes the distillation process is not manda tory provided the aniline meets the requirements of the test with n-heptane. No t e 5--The aniline point of aniline and n-heptane determined with automatic apparatus (Method E) shall be 69.3 0.2C (156.7F 0.4F) when corrected in accordance with the equation in Section A5.2.1. No t e 6--As an alternative to distilling the aniline on the day of use, the aniline may be distilled as described in 7.1, collecting the distillate in ampoules, sealing the ampoules under vacuum or dry nitrogen, and storing in a cool dark place for future use. lii either case, rigid precaution must be taken to avoid contamination from atmospheric moisture (Note 2). It is believed that under these conditions the aniline will remain unchanged for a period exceeding 6 months. 7.2 Calcium Sulfate, anhydrous. 7.3 n-Heptane (Warning--See Note 7.), conforming to the requirements listed in Table 1.5 No t e 7--Warning--Flammable. Harmful if inhaled. See Annex A6.1. 8. Sample 8.1 Dry the sample by shaking vigorously for 3 to 5 min with about 10 volume % of a suitable drying agent such as anhydrous calcium sulfate or anhydrous sodium sulfate. Reduce the viscosity of viscous samples by warming to a temperature below that which would cause the loss of light ends or the dehydration of the drying agent. Remove any suspended drying agent by use ofa centrifuge or by filtration. Heat samples containing separated wax until they are homogeneous and keep heated during filtration or centrifu gation to ensure against separation of wax. When suspended water is visibly present and the sample material is known to dissolve less than 0.03 mass % of water, the use of a centrifuge for the removal of suspended water is an accept able procedure. 9. Procedure for Aniline Point 9.1 The following methods, to be used as applicable, are covered as follows: 9.1.1 Method A, described in detail in Annex Al, is applicable to clear samples or to samples not darker than No. 6.5 ASTM color, as determined by Test Method D 1500, having initial boiling points well above the expected aniline point. 9.1.2 Method B, described in detail in Annex A2, is applicable to light-colored samples, moderately dark sam ples, and to very dark samples. It is suitable for samples that are too dark to be tested by Method A. 9.1.3 Method C, described in detail in Annex A3, is applicable to clear samples or to samples not darker than No. 6.5 ASTM color, as determined by Test Method D 1500, having initial boiling points sufficiently low as to give incorrect aniline point readings by Method A, for example, aviation gasoline. 5 These requirements for n-heptane are identical, except for tetraethyl lead, with those prescribed in the 1987 Annual Book ofASTM Standards, Vol 05.04. 103 DUP050295769 D 611 9.1.4 Method D, described in detail in Annex A4, is applicable to the same type of sample as Method C. It is particularly useful when only limited quantities of sample are available. 9.1.5 Method E is applicable when using automatic appa ratus in accordance with the instructions in Annex A5. 10. Procedure for Mixed Aniline Point 10.1 This procedure is applicable to samples having aniline points below the temperature at which aniline crystallizes from the mixture. Pipet 10 mL of aniline (Warning: See Note 3), 5 mL of sample, and 5 mL of -heptane into a clean, dry apparatus. Determine the aniline point of the mixture by Method A or B as described in Annex A1 or A2. 11. Report 11.1 If the range of three successive observations of the aniline point temperature is not greater than 0.1 C (0.2F) for light-colored samples or 0.2C (0.4'F) for dark samples, report the average temperature of these observations, cor rected for thermometer calibration errors, to the nearest 0.05C (0.1F) as the aniline point. 11.2 Ifsuch a range is not obtained after five observations, repeat the test using fresh quantities of aniline and sample in a clean, dry apparatus, and if consecutive temperature observations show a progressive change, or if the range of observations is greater than the repeatability given in 12.1, report the method as being inapplicable. 12. Precision and Bias 12.1 The precision of these test methods as obtained by statistical examination of interlaboratory test results is as follows: 12.1.1 Repeatability--The difference between successive test results (two average temperatures obtained in a series of observations as described in Section 11) obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty: Repeatability Aniline point of: ear, light-colored samples Moderately dark to very dark samples Mixed aniline point of ear, light-colored samples Moderately dark to very dark samples O.I6C <0.3F) 0.3C (0.6'F)'1 0.16C (0.3',F)'f 0.3"C (0.6`F)'* A Not determined from recent cooperative tests; however, the ratios with those given in the 1953 version are believed to apply. 12.1.2 Reproducibility--The difference between two single and independent results; obtained by different opera tors, working in different laboratories on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty: 12.2 Bias--A statement of bias is now being developed by the subcommittee. Reproducibility Aniline point of: ear. light-colored samples Moderately dark to very dark samples Mixed aniline point of: ear, light-colored samples Moderately dark to very dark samples 0.5"C (0.9F) 1.0C (1.8'F)" 0.7C (l,W 1.0C(1.8"F)- ' A Not determined from recent cooperative tests; however, the ratios with those given in the 1953 .version are believed to apply. 12.3 The precision of this test was not obtained in accordance with Committee D-2 Research Report RR:D021007, "Manual on Determining Precision Data for ASTM Methods on Petroleum Products and Lubricants."4 ANNEXES (Mandatory Information) Al. METHOD A Al.I Apparatus A 1.1.1 The apparatus shown in Fig. A 1.1 shall consist of the following: Al.1.1.1 Test Tube, approximately 25 mm in diameter and 150 mm in length, made of heat-resistant glass. A 1.1.1.2 Jacket, approximately 37 to 42 mm in diameter and 175 mm in length, made of heat-resistant glass. A 1.1.1.3 Stirrer, manually operated, metal, approxi mately 2 mm in diameter (14 B&S gage) metal wire as shown in Fig. A1.1. A concentric ring shallbe at the bottom, having a diameter ofapproximately 19 mm. The length ofthe stirrer to a right-angle bend shall be approximately 200 mm. The right-angle bend shall be approximately 55 mm long. A glass sleeve approximately 65 mm in length of 3-mm inside diameter shall be used as a guide for the stirrer. Any suitable mechanical device for operating the stirrer as specified is an approved alternative for the manual operation. A1.2 Procedure Al.2.1 Clean and dry the apparatus. Pipet 10 mL ol aniline (Warning--see 7.1) and 10 mL of the dried sample (8.1) into the test tube fitted with stirrer and thermometer. If the material is too viscous for pipetting, weigh to the nearest 0.01 g a quantity of the sample corresponding to 10 mL al room temperature. Center the thermometer in the test tube so that the immersion mark is at the liquid level, making sure that the thermometer bulb does not touch the side of the tube. Center the test tube in the jacket tube. Stir the mixture rapidly using a 50-mm (2-in.) stroke, avoiding the introduc tion of air bubbles. Al.2.2 If the aniline-sample mixture is not miscible a room temperature, apply heat directly to the jacket tube sc 104 DU P0502 95770 D 611 |t the temperature rises at a rate of 1 to 3<'C (2 to 5F )/min ? removing or reducing the heat source until complete iscibility is obtained. Continue stirring and allow the fixture to cool at a-rate of 0.5 to ,1.0'C (1.0 to 1.8F)/min. |ntinue cooling to a temperature of 1 to 2C (2.0 to 3.5F) low the first appearance of turbidity, and record as the liline point the temperature at which the mixture suddenly icomes cloudy throughout (Note Al.l). This temperature, Id not the temperature of separation of small amounts of laterial, is the minimum equilibrium solution temperature. No t e Al.l--The true aniline point is characterized by a turbidity that is so cloudy as to obscure the thermometer bulb in reflected light. A 1.2.3 If the aniline-sample mixture is completely mis cible at room temperature, substitute a non-aqueous cooling bath for the heating source, allow to cool at the rate specified in A l:.2(2, and determine the aniline point as described. A 1.2.4 Repeat the observation of aniline point tempera ture by heating and cooling repeatedly until a report as directed in Section 11 can be made. A2. METHOD B DU P050295771 w Du 6o1111 DETAIL OF TUBE DETAIL OF PUMP BODY AND ROTOR FIG. A2.1 Details of Aniline Point Thin-Film Apparatus (Method B) Stirring Motor & Bakelite Cover "and Support Spring Clips Holding 'Aniline Point Tube in Place -Panel Lamp - -Pump-Stirrer -Leads to 0-8 Volts Bath FIG. A2.2 Assembly of Thin-Film Apparatus (Method B) adjustments and tests using a colorless sample-aniline mixture, and observing changes taking place in the body of the liquid and film. Make rough tests with dark oils to become familiar with the appearance of the film and light source as the mixture passes from the clear state above the aniline point, to the translucent state below. If the sample is such that there is difficulty in observing the exact point ofthe phase-change, make experiments with the sample, using various intensities of light and paying particular attention to the appearance of the light in the immediate vicinity of the lamp filament. A2.2.3 Repeat the observation of aniline point tempera ture by heating and cooling repeatedly until a report as directed in Section 11 can be made. 106 DUP050295772 # D 611 A3. METHOD C fi 5* tube; the tube contains sufficient light transformer oil to 'Aniline-Point Tube, of heat-resistant glass, of the ijfnd dimensions shown in Fig. A3.1, and fitted A\\y with a thin-walled glass thermometer tube, sealed Slower end. The latter tube accommodates a tight* prk stopper carrying the thermometer, the bulb of is on a cork ring or disk placed at the bottom of the cover the bulb of the thermometer. The inner tube is held in the top of the aniline-point tube by a tightly fitting stopper, and a clamp is provided to hold the stopper in position to prevent loss of vapor from the sample. No t e A3.1--Any other suitable arrangement, such as a screwed plastic gland carrying the thermometer, that will prevent the loss of vapor from the apparatus, may be used. In such cases it may be possible to omit the thermometer tube and immerse the thermometer bulb in the aniline-sample mixture. A3.1.2 Guard, of stout metal gauze and surrounding the aniline point tube. It should preferably be combined with the clamp for holding the thermometer tube in place. A3.2 Procedure A3.2.1 Clean and dry the apparatus. Pipet 5 mL of aniline (Note A3.2 Precaution see Note 3) and 5 mL of the dried sample (8.1), both cooled to a temperature at which the sample may be measured without loss of vapor. Close the tube by means of the stopper and fit the thermometer tube centrally so that the bottom is 5 mm from the bottom of the aniline point tube. Clamp the stopper in position and attach the guard. No t e A3.2: Precaution--Put on goggles of safety glass and plastic gloves impervious to aniline. A3.2.2 Follow the procedure described in A 1.2.2 and A1.2.3 but mix the sample and aniline by shaking the tube. If the rate of change of temperature is greater than 1C (2`>F)/min when the aniline point is being approached, place the tube in a jacket that has previously been wanned or cooled to an appropriate temperature. A3.2.3 Repeat the observation of aniline point by heating and cooling repeatedly until a report as directed in Section 11 can be made. A4. METHOD D .1 Apparatus AA.i.1 Bulb, 1.5 to 2.0-mlL capacity, blown from heatistant glass tubing, 5 mm in external diameter and 3 mm Internal diameter. A4.1.2 Guard, as for Method C. 4.2 Procedure A4.2.1 Dry the bulb thoroughly in an oven at 105 5C, low it to cool to room temperature, and charge it by means f the pipets with 0.5 mL of aniline (Warning--see Note 3) nd 0.5 mL of the dried sample (8.1). Cool the mixture thoroughly and rapidly draw out and seal the open end of the bulb at about 10 mm from the center of the bulb. No t e A4.1: Precaution--Put on goggles of safety glass and plastic gloves impervious to aniline. A4.2.2 Attach the bulb to the thermometer by rubber bands so that the bulb is adjacent to the thermometer bulb. Attach the mesh guard and follow the procedure described in Al.2.2 and Al.2.3 but mix the sample and aniline by shaking. A4.2.3 Repeat the observation of aniline point tempera ture by heating and cooling repeatedly until a report as directed in Section 11 can be made. 107 DUP050295773 # D 611 A5. METHOD E A5.1 Apparatus AS. 1.1 Automatic Aniline Point Apparatus, commercially available, using a modified thin film technique and direct heating of the sample-aniline mixture with electrical irinhersion heater. Detection of change of sample turbidity at the aniline point is by response of a photoelectric cell to collimated fight directed through the thin film ofsample. A5.2 Procedure A5.2.1 Determine the automatic aniline point in accord ance with instructions' provided with the apparatus. Correct the aniline point as follows: Corrected aniline point = (Xa - A)/B where: Xa ~ Asn&B = automatic aniline point; arid ' constants determined for each apparatus as described in A5.2.2. '" No t e A5.1--It has been established by cooperative tests that ob served aniline points determined by some automatic.apparatus are lower than the determinations by Methods A and B, The difference is greater, for automatic apparatus when relatively high sample-cooling rates are used, and increases as the aniline point increases! ; A5.2.2 Determine the aniline point by either Method A or Method B and also using the automatic apparatus for three or more samples with aniline points in each of the ranges 43 to 49C (110 toc120F), 60 to 66C(14Qto 150T), and 77 to 82C (170 to 180f r). Calculate the constants A and B by the least squares^ method by simultaneous solution of the fol lowing equations: .. WJ ^NA + B2{Xc) X(XJC) = AX(XC) + BX(X/) where: W sum of all aniline point data by automatic apparatus, 2W = sum of all aniline point data by either Method A or B, 2(AC2) sum of the squares of all aniline point data by either Method A or B, S() = sum of the products of aniline points deter mined by either Method A or B and by using the automatic apparatus for each sample, and N number of samples. No t e A5.2--Cooperative data were obtained from five laboratories for five samples with aniline points in the range from 34 to 87"C (93 to 188F). Constants A and B were calculated fpr the composite data as 0.79 and 0.991 respectively, ..Although a minimum number of nine samples is specified in this method, constants A and B in the preceding equation may be obtained with a slightly greater precision if data for a larger number of samples are used. A6. PRECAUTIONARY STATEMENT A6.1 n-Heptane Warning--Flammable. Harmful if inhaled. Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. ' Avoid prolonged breathing of vapor or spray mist. Avoid prolonged or repeated skin contact. The American Society for Testing and Materials takes no position respecting the validity of any patent rights assertedin connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and shbuld be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, whldh you may.attend. If you feel that yotir commenfs have not received a fetr hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 108 DUP050295774 jsignation: D 740 -- 89 Standard Specification for Methyl Ethyl Ketone1,2 This standard is issued under the fixed designation D 740; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or rea'pproval. specification covers two types of methyl ethyl at are used primarily as solvents in lacquers and coatings, but also in adhesives, printing inks, lube ling, and as chemical intermediates, specific hazard information and guidance, see the Material Safety Data Sheet for materials listed in ification. enced Documents STM Standards: Methods of Sampling and Testing Volatile Solvents Chemical Intermediate for Use in Paint and [ated Coatings and Material13 2 8 Test Method for Distillation Range of Volatile janic Liquids3 109 Test Method for Color ofClear Liquids (Platinumbait Scale)4 2196 Test Method for Odor of Volatile Solvents and (fluents3 353 Test Method for Nonvolatile Matter in Volatile iolvents for Use in Paint, Varnish, Lacquer, and Reited Products3 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer and Related Products3 2804 Test Method for Purity of Methyl Ethyl Ketone Using Gas Chromatography3 4052 Test Method for Density and Relative Density of liquids, by Digital Density Meter5 f:E 1 Specification for ASTM Thermometers6 j E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 1 This specification is under the jurisdiction ofASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcomjmittee DOI.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 740 - 43. Last previous edition D 740 - 87. 2 Also known as butanone and butanone-2. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 3 Annual Book ofASTMStandards, Vol 05.03. 6 Annual Book ofASTMStandards, Vols 05.03 and. 14.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. " Available from Standardization Documents Order Desk, Bldg 4 Section D, f 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Classification 3.1 Methyl ethyl ketone shall be of the following types, as specified: 3.1.1 Type I--regular, and 3.1.2 Type //---urethane grade. This type may be suited for use in urethane coatings, provided that the water content and alcohol content are acceptable. 4. Properties is 4.1 The physical and chemical properties of methyl ethyl ketone shall conform to the requirements specified in Table 1. 5. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 6.1.1 Acidity--Test Method D 1613. 6.1.2 Alcohol--Test Method D 2804. 6.1.3 Color--Test Method D 1209. 6.1.4 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 39C having a range from 48 to 102C and conforming to the requirements in Specifications E 1. 6.1.5 Nonvolatile Matter--Test Method D 1353. 6.1.6 Odor--Test Method D 1296. 6.1.7 Purity--Test Method D 2804. 6.1.8 Apparent Specific Gravity--Determine the apparent specific gravity by any method that is accurate to the third TABLE 1 Physical and Chemical Properties ot Methyl Ethyl Ketone Type l Type fl Commerical reference Acidity'4, weight %, max Alcohol, weight %, max Color, Pt-Co scale, max Distillation range, 760 mm Hg, C Initial boiling point, min Dry point, max . Nonvolatile matter, mg/100 mL, max Odor Purity, weight %, min Specific gravity, apparent 20/20C 25/2SC Water, weight %, max regular 0.005 io 78.5 81.0 5 nonresidual 99.5 0.805 to 0.807 0.801 to 0.803 0.2 urethane-grade 0.003 0.5 10 78.5 81.0 5 nonresidual 99.5 0.805 to 0.807 0.801 to 0.803 0.05 4 Free acid as acetic add. Equivalent to 0.047 mg potassium hydroxide (KOH) per gram of material. 9 Calculated as 2-butanol or sec-butyl alcohol. 109 DUP050295775 D 740 ' .1 decimal place, the temperature of both specimen and water being 20C or 25C. (See Specific Gravity section of Methods D 268, or Test Method D 4052.) 6.1.9 Water--Test Method D 1364. 7. Packaging and Package Marking 7.1 Package size shall be agreed upon between the pur chaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed Spec. PPP-C-2020. 8. Keywords 8.1 solvents; methyl ethyl ketone; regular grade; urethane grade The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must.be reviewed every five years and if not revised, either reapprbved dr withdrawn. Your comments are Invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at -a meeting of the responsible technical committee, which you may attend. If you fee! that your comments have not received si fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.110 1 110 DUP050295776 tiflL Designation: D 770 - 90 IP 'b'flj Standard Specification for Isopropyl Alcohol1,2 This standard is issued under the fixed designation D 770; 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. cope This specification covers isopropyl alcohol (99 % I). This standard does not purport ter address all of the jjfyproblems associated with its use. It is the responsibility > user ofthis standard to-establish appropriate safety and Hth practices and delermineihe applicability ofregulatory stations prior to use. For specific hazard statements, see jion 4. 63 For hazard information and guidance, see the sup|f's Material Safety Data Sheet. leferenced Documents 1 ASTM Standards: 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material13 2 1078 Test Method for Distillation Range of Volatile Organic Liquids3 ip1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)4 1296 Test Method for Odor of Volatile Solvents and Diluents3 I'D 1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 P1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1476 Test Method for Heptane Miscibility of Lacquer Solvents3 D 1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D1722'Test Method for Water Miscibility of WaterSoluble Solvents3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E I Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: 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 D0I.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 770 - 44. Last previous edition D 770 - 85. 2 This compound is also known under the name propanol-2 and isogropanol. * Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. ' 6 Annual Book ofASTM Standards, Vol 14.03. 1 Annual Book ofASTM Standards, Vols 06.03 and 1 S.05. PPP-C-2020 Chemicals, Liquid* Dry, and Paste: Packaging of8 3. Properties 3.1 Isopropyl alcohol shall conform to the following requirements: Apparent specific gravity, 20/20C 25/25'C Color, Pt-Co scale, max Distillation range, 760 mmHg Nonvolatile matter, max, mg/100 mL Odor Water, max, weight % Acidity, acetic acid, max, weight % Water miscibility 0.785 to 0.787 0.782 to 0.784 10 nonresidual 0.2 a 0.002c passes test A Distill entirely within a 1.5'C range which shall include 82.3"C. B This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20C. c Equivalent to 0.019 mg KOH per gram of sample. 4. Hazards 4.1 Isopropyl alcohol is a flammable liquid. Its vapors can form explosive mixtures with air. Repeated or prolonged contact may cause drying of the skin. 5. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 6.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20 or 25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Method D 4052. 6.1.2 Color--Test Method D 1209. 6.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 40C having a range from 72 to 126C and conforming to the requirements in Specification E 1. 6.1.4 Nonvolatile Matter--Test Method D 1353. 6.1.5 Odor--Test Method D 1296. -6.1.6 Water--Test Methods D 1364 and D 1476. 6.1.7 Acidity--Test Method D 1613. 6.1.8 Water Miscibility--Test Method D 1722. 8 Available from Standardization Documents Order Desk, Bldg 4 Section D. 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. Ill DUP050295777 7. Packaging and Package Marking 7.1 Package size shall be agreed upon between the pur chaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed Spec. PPP-C-2020. 8. Keywords 8.1 isopropyl alcohol The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited either forrevision of this standard of 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. 112 DUP050295778 r4, | ^Designation: D 801 - 57 (Reapproved 1987) Standard Test Methods for ft Sampling and festing Dipentene1 This standard is issued under the fixed designation D 801; the number immediately following the designation indicates the year of a i^'priginal 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. iilf: ' ' p*``. ' - se test methods cover procedures for sampling and satene and-'related terpene solvents, consisting f monocylic terpene hydrocarbons distilling above jjtfbr turpentine. i procedures appear in the following order I Removal of Separated Water Stand Mixed Aniline Point. Sections 3 4 5 6 7 8 9 10 11 12 13 14 15 16 E i Specification for ASTM Thermometers6 3. Sampling 3.1 Sample the material in accordance with the procedure described in Test Methods D 268. If a sample from close to the bottom of a tank shows a decided difference in color or appearance from samples taken at other depths, take an extra bottom sample and examine it separately from the com posite sample. In such case the composite sample shall not include any portion of such bottom sample. 4. Detection and Removal of Separated Water 4.1 Draw a portion ofthe dipentene by means of a glass or metal container with a removable stopper or top,7 or with a thief; from the lowest part ofthe container, or by opening the bottom valve of the level tank'car. If water is found to be present, draw it all out, record the quantity, and deduct it from the total volume of liquid delivered. ms-standard may involve hazardous materials, operf$d equipment. This standard does not purport to ||the safetyproblems associated with its use. It is. sibiiity of the user of this standard to establish tie safety and health practices and determine the iilityofregulatory limitations prior to me. . |irenced Documents |lS*fM Standards: fest Method for Flash Point by Tag Closed Tester2 iMethod for Distillation of Petroleum Products2 f Test Method for Saybolt Color of Petroleum Iticts (Saybolt Chromometer Method)3 ^ Methods of Sampling and Testing Turpentine4 ^ Methods of Sampling and Testing Volatile Sol ids and Chemical-Intermediates for Use in Paint and plated Coatings and Material4 70 Methods for Sampling Petroleum and Petroleum Productss l Test Methods Aniline Point and Mixed Aniline jf'oint of Petroleum Products and Hydrocarbon Sol vents? l Test Method for Water in Liquid Naval Stores4 these test methods are under the jurisdiction of ASTM Committee D-t on , Jliand Related Coatings and Materials and are the direct responsibility of imittee DO 1.34 on Hava] Stores. Btilt edition approved Sept. 30, 1957. Published November 1957. Originally |hed as D 801 - 44. Last previous edition D 801 - 48. fjMlinualBook ofASTM Standards, Vols 05.01 and 06.03. Annual Book ofASTM Standards, Vol 05.01. f * Iwtuat Book ofASTM Standards, Vo! 06.03. Sri5 Discontinued, see 1984 Annual Book ofASTM Standards, Vol 05.01. 5. Appearance 5.1 Examine a portion of the sample after agitation to determine whether its appearance, conforms to the specifica tions. 6. Color 6.1 Compare, in colorimeter tubes or in any other suitable apparatus (such as ordinary 4-oz oil-sample bottles having flat polished bottoms), the color of the sample with an equal depth of a fresh solution of potassium dichromate in distilled water containing 0.012 g of K2Cr207/L. No t e 1 --A 150-mm column ofthis solution has a color equal to that of a No. 1.5 Lovibond yellow glass. 6.2 As an alternative method, compare the color of the sample with that of the Saybolt standards as described in Test Method D 156. 6.3 If the color is equal or lighter than the potassium dichromate solution, or if the color is equal to Saybolt No. 16 or above, the dipentene is prime white. 7. Odor 7.1 Compare the odor of the sample with an agreed upon water-free reference sample kept in the dark in a completely filled well-stoppered bottle. In die absence ofsuch a reference sample, compare with samples of known purity similarly preserved. 6 Annual Book ofASTM Standards, Vol 14.03. 7 A detailed description of equipment suitable for such sampling is given in Methods D 270. 113 DUP050295779 D 801 TABLE 1 Temperature Corrections (C) for Barometric Pressure'4 Observed Barometric Pressure, mm Aneroid Barometer Mercurial Barometer Temperature of Barometer 20C 25C 30C 35C 780 -1.08 -0.94 -0.91 -0.87 -0.84 770 -0.54 -0.40 -0.37 -0.34 -0.30 760 0.00 +0.13 +0.17 +0.20 +0.23 750 +0.54 +0.67 +0.70 +0.74 +0.77 740 +1.08 +1.21 +1.24 +1.27 +1.31 730 +1.62 +1.75 +1.78 +1.81 +1.84 720 +2.16 +2.29 +2.32 +2.35 +2.38 710 +2.70 +2.82 +2.86 +2.89 +2.92 700 +3.24 +3.36 +3.39 +3.42 +3.45 A These corrections are calculated as follows: The observed barometric pressure is first corrected to what it would be at 0C, by means of the table in Circular F, Instrument Division, U. S. Weather Bureau. The corrected barometric pressure is then subtracted from 700 ran (or vice versa) and the difference multiplied by 0.054`C to give the temperature correction shown in the above table. The correction factor, C, of 0.054oC was calculated using the Sydney-Young equation: C 0.00012 (760 - P)|273 + T) where: P = observed pressure, corrected to 0C. mm, and T - mediam boiling temperature for dipentene, 180C. 8. Specific Gravity 8J Determine the specific gravity at 15.56/15.56C by any convenient method, reporting the value to the nearest 0.0005. Correct determinations made at any other tempera ture, using apparatus standardized at 15.56C, by adding to or subtracting from the observed reading 0.00082 for each degree Celsius that the temperature of the liquid is above or below 15.56C. 9. Refractive Index 9.1 Determine the refractive index with an accurate instrument at 20C, if possible. If tested at any other temperature, correct the reading obtained to 20C by adding or subtracting 0.00045 for each degree Celsius that the temperature at which the determination was made is, respec tively, above or below 20C. 10. Distillation 10.1 Apparatus--Use the distillation apparatus described in Method D 86, with the following exceptions: 10.1.1 Thermometer--Use an ASTM Partial Immersion Thermometer having a range from --5 to +300C and conforming to the requirements for Thermometer 2C as prescribed in Specification El or an ASTM Solvents Distil lation Thermometer haying a range from 95 to 255C and conforming to the requirements for Thermometer 42C as prescribed in Specification E 1. 10.1.2 Condenser--A Liebig glass condenser 560 mm in length with 400 mm in contact with the cooling water may be used in place of the bath-type condenser. 10.2 Procedure--With the receiving graduate, transfer exactly 100 mL of the sample directly, into the flask, allowing none to run into the side tube and allowing the graduate to drain thoroughly. If the sample contains dissolved or sus pended water it is advisable to add a few small pieces of pumice or broken glass to promote smooth distillation. Insert the thermometer so that the top of the mercury bulb (or the top of contraction chamber if the Solvents Distilla tion Thermometer is used) is level with the bottom of the side tube. Connect the side tube to the condenser, with the bottom of the flask resting securely in the opening in the asbestos board. Apply heat cautiously and regulate it so that the first drop of condensate falls from the condenser in not less than 5 nor more than 10 min. Record as the initial boiling point, the thermometer reading when the first drop falls from the end of the condenser. When the distillation begins, regulate the heat so that the distillate is collected at a ' rate of not, less than 4 nor more than 5 mL/min (approxi mately 2 drops/s). Observe and record the temperature when 5 mL have been collected in the receiving cylinder, and thereafter when the level of the distillate reaches each 10-mL division of the graduate, including a 95-mL reading. Discon tinue the distillation when the temperature reaches that specified for the minimum percentage requirement, or whenever the temperature rise stops and the thermometer reading starts to fall, and record the maximum temperature reached. Allow the condenser to drain and record the percentage distilled. Correct all observed temperatures to compensate for variations in barometric pressure, as de scribed in 10.3. 10.3 Barometric Correction--The distilling temperature of dipentene is affected by 0.054C for each millimetre variation of the atmospheric pressure. Therefore, the temper atures observed or specified shall be corrected to permit the distillation to be conducted as though the barometer reading, corrected to 0C, were exactly 760 mm. When about to begin the distillation, observe and record the barometric pressure and the temperature of the barometer. (No temperature correction on barometer reading is necessary for aneroidtype barometers.) From Table 1 determine the proper temperature correction corresponding to these atmospheric conditions, interpolating to the nearest 0.PC. If the baro metric pressure, corrected to 0C, is below 760 mm, the temperature correction must be added to the temperatures observed and subtracted from the minimum percentage requirement temperature; if above 760 mm, the correction must be subtracted from the temperatures observed and added to the minimum percentage requirement temperature. No t e 2: Example--Suppose the observed barometric pressure is 745 mra at 28"C, and the 5 % boiling point is observed to be 172.0C. From Table 1 by interpolating, the temperature correction is seen to be l.O'C. Therefore the corrected 5 % boiling point is 172.0 + 1.0 = 173.0'C. Furthermore the temperature observation point at the minimum percentage requirement (usually 188"C at 760 mm) must be altered to the same extent. Since the dipentene is distilling 1.0'C below what it would at normal pressure, distillation must be discontinued at 188.0 -- I. 0 = 187.0'C to determine the percentage distilling below 188C at 760 mm pressure. II. Polymerization 11.1 Determine the unpolymerized residue with 38 N sulfuric acid in accordance with the procedure described in Methods D 233. 12. Spot Test 12.1 Transfer five drops of the dipentene by means of a small pipet to the center of a clean white filter paper supported on a 70-mm crystallizing dish and allow the liquid to evaporate at room temperature, away from direct sunlight. After 30 min observe if there is any oily spot on the filter paper. 11. 114 DUP050295780 m # D 801 jer Corrosion ace a clean strip of mechanically polished pure |per, about lh in. in width and 3 in. in length (13 by t a glass test tube about % in. in diameter and 18 in. i (19 by 46 mm). Add a sufficient amount of the be tested to cover the strip completely and heat ^boiling (it is most-convenient to heat the tube by |bn in an oil bath'maintained at a temperature Ihigher than the initial boiling point of the dipentene). sample boiling,' without any actual distillation ace, for 30 min, and then examine the copper strip likening. Disregards slight tarnish, but any marked Bing shall be considered cause for rejection. Bsh Point 1 Determine the flash point by means of the Tag ^Tester as described in Test Method D 56. dissolved Water Distillation Method: 1.1 Apparatus. .1.1 Flask, a round-bottom, short-neck flask of 1000iapadty. fcl.t.2 Water Trap, a Dean and Stark water trap of |iL capacity. ,1.1.3 Condenser, a straiight-tube, water-cooled, glass, type condenser having a water jacket 400 mm in with an inner tube approximately 10 to 12 mm in Seter. .1.1.4 Heat Source, a gas burner or an electric heater ing suitable heat control. 5.1.1.5 Supportfor Flask, a piece ofwire gauze resting on g support. .1.2 Procedure--Weight 500 g of dipentene into the . Connect the flask, trap, and condenser with tightpg, metal foil-covered corks. Insert a snug-fitting buret ning brush into the top of the condenser in such a aner that the brush can be lowered at will down to where I condensation of the distillate take place. Apply heat and ulate it so that the condenser distillate falls from the end (the condenser at the rate of from 2 to 5 drops per second, ontinue the distillation for 45 min or longer until all water i been.distilled from the flask. Avoid prolonged heating; min should be sufficient (Note 2). Bring down any oplets of water adhering to the walls of the condenser by iding a few drops of dipentene at the top of the condenser Enough to wet the brush) and then moving the brush up and town at the lower end of the condenser. Allow the distillate |to cool and disconnect the flask and trap from the condenser. Bring down any droplets of water that adhere to the walls of the trap with the aid of a glass stirring rod. Record the jiivolume of water collected in the trap to the nearest 0.1 mL. ^Duplicate determinations should check within 0.1 mL of water collected, or 0.02 %. 15.1.3 Calculation--Calculate the dissolved water content : as follows: Dissolved water, % -- (mL of water/500) x 100 No t e 3--The presence of oxidized constituents will cause high apparent water content due to their decomposition by heat For old samples known to have been exposed to oxidation for a considerable length of time, as in stored partially filled containers, the alternate method referred to in 15.2 should be used. 15.2 Alternative Method--If a more rapid determination is desired, or if the condition of the sample and the results obtained by the distillation method (16.1) indicate oxidation, follow the procedure as described in Test Method D 890. 16. Aniline Point and Mixed Aniline Point No t e A--If desired, the aniline and mixed aniline points of dipentene may be determined as described in Test Method D61I instead of in accordance with the following Section 16. 16.1 Apparatus. 16.1.1 Test Tube--A test tube approximately 18 mL in capacity, 15 mm in diameter, and 125 mm in length, with a lip, and fitted with a two-hole cork stopper, one hole being for the thermometer and the other a 2-mm hole for the stirrer. 16.1.2 Stirrer--A stiff copper wire, approximately 1 mm in diameter, coiled at the lower end (3 to 5 coils). The coils shall be of such diameter that the stirrer can move freely up and down around the thermometer. The upper end of the wire stirrer shall extend several inches through the 2-mm hole in the cork stopper, with the end of the wire looped or bent to form a handle. 16.1.3 Thermometer--An ASTM Aniline Point Ther mometer having a range from -38 to +42C and conforming to the requirements for Thermometer 33C as prescribed in Specification E 1. 16.1.4 Bath--A 300-mL tail-form beaker or other con venient receptacle containing a suitable clear, nonaqueous medium, such as turpentine, kerosine, etc., for use as a cooling or heating bath. 16.2 Reagents: 16.2.1 Aniline--Dry cp aniline over KOH and redistill, discarding the first and last 10 % of the distillate. Preserve the purified aniline in small, amber-colored, glass-stoppered bottles. Suitable aniline should be practically colorless. 16.2.2 Normal Heptane--Normal heptane for use in the mixed aniline point test shall have a boiling point in the range from 98 to 98.5C. The n-heptane shall be dried before use by shaking for several minutes with anhydrous Na2S04 and filtering to obtain a clear, dry liquid. 16.3 Procedure for Aniline Point--Clean and dry the apparatus. Pipet into the test tube 5 mL of the sample, previously dried in accordance with the procedure for drying n-heptane (16.2). By means of a safety pipet (Note 4) or small buret fitted with a calcium chloride tube, add an equal quantity of aniline. Stopper the test tube with the cork containing the thermometer and the stirrer and mix the contents thoroughly with the wire stirrer. Clamp the test tube in a suitable position to permit raising and lowering of the beaker containing the prechilled cooling medium. (A tem perature of--15 to -20C may be required.) Immerse the test tube in the bath and stir the mixture rapidly, avoiding the inclusion of air bubbles. While stirring constantly, record the temperature at which the solution becomes cloudy or turbid throughout (Note 5). Allow the solution to warm up until cloud disappears and repeat the cooling process, again recording the temperature at which the solution becomes cloudy. The average of the temperatures at which the solution becomes cloudy throughout shall be reported as the 115 DUP050295781 D 801 aniline point. The readings should agree within 0.5C. No t e 5--Aniline is poisonous and should not be pipetted by direct applicationiof the mouth to the pipet, nor should any be allowed to remain on the hands, even in very small quantities, as aniline will be absorbed through the skin. ... No t e' 6--The true aniline point is characterized by a turbidity which increases sharply as the temperature is lowered. 16.4 Procedurefor Mixed Aniline Point--Pipet 2.5 mL of the sample, 2.5 mL of n-heptane, and 5 mL of aniline (Note 4) into the test tube. Proceed as described in 16.3, except that the solution may have to be warmed slightly above room temperature to produce a clear solution. To do this, immerse * the test tube in a warm bath and stir constantly until the l! solution is clear. Remove the test tube from the bath, and J allow the contents to cool while stirring constantly. Record the temperature at which the solution becomes cloudy! throughout Repeat the procedure and report the average- temperature as the mixed aniline point. The readings should agree within 0.5*0. > The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users dl this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. . This standard is subject to revision atany time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Yourcomments are Invitedeithertor 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, 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. Iff| ' - It i; 3 1 116 DUP050295782 esignation: D 802 - 82 (Reapproved 1987) Standard Methods of Sampling and Testing Pine Oil1 This standard is issued under the fixed designation D 802; 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 reapproyaL aese methods . cover procedures for sampling and pine oils, and/are applicable to both natural pine oils ' from pine stumps either by the steam and solvent s or by destructive distillation, and also to synthetic obtained by! the chemical hydration of terpene bons. this standard may involve hazardous materials, oper and equipment. This standard does .not purport to all ofthe safety problems associated with its use. It is ksponsibility of the user of this standard to establish riale safety and health practices and determine the lability ofregulatory limitations prior to use... ferenced Documents % ASTM Standards: 6 Method for Distillation of Petroleum Products2 5 Test Method for Water in-Petroleum Products and /Bituminous Materials by Distillation2 33 Methods of Sampling and Testing Turpentine3 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 .890 Test Method for Water in Liquid Naval Stores3 1 Specification for ASTM Thermometers4 npling .1 Sample the material in accordance with the procedure cribed in Methods D 268. Appearance 4.1 Examine a portion of the sample to determine its "tyand freedom from foreign matter and separated water. Color ; |5.1 Compare the color of the sample in any suitable or signated apparatus with the accepted or specified color tandard. 6, Specific Gravity 6.1 Determine the specific gravity at 15.56/15.56C by any convenient method, reporting the value to the nearest ' These methods are under the jurisdiction of ASTM. Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Stjbcommittee DO 1.34 on Naval Stores. Current edition approved March 26, 1982. Published June 1982. Originally published as D 802 - 44 T. Last previous edition D 802 - 57 (1981). 2 Annual Bode ofASTM Standards, Vols 05.01 and 06.03. 2 Annual Book ofASTM Standards, Vol 06.03t A Annual Book ofASTM Standards, Vols 14.03 and 05.03. 0.0005. (A pycnometer or specific gravity balance is recom mended. A hydrometer should not be used, on account of errors caused by surface tension oh the hydrometer stem.) Determinations made at any other temperature, using appa ratus standardized at 15.56C shall be corrected by adding to or subtracting from the observed reading 0.00080 for each degree Celsius that the temperature of the liquid is above or below 15.56C. - 7. Refractive Index 7.1 Determine the refractive index with an accurate instrumeiit at ; 20C, if possible. If tested at any other temperature, correct the reading obtained to 20C by adding or subtracting 0.00040 for each degree Celsius that the temperature at which the determination was made is, respec tively, above or below 20C. 8. Distillation ,8.1 Apparatus--Use the distillation apparatus, described in Method D 86, with the following exceptions; 8.1.t Thermcimeter--Msi? an ASTM Partial Immersion Thermometer having a,, range from --5 to +300C and conforming to the requirements for Thermometer 2C as prescribed in Specifications E 1, or an ASTM Solvents Distillation Thermometer having a range from 95 to 255C and conforming'to the requirements for Thermometer 42C as prescribed in Specifications E 1. 8.1.2 Condenser--A Liebig glass condenser 560 mm in length with 400 mm in contact with the cooling water may be used in place ofthe bath-type condenser. The temperature of the cooling-water should not Be below 20C. 8.2 Procedure--With the receiving graduate, transfer ex actly 100 mL'of the sample directly into the flask, allowing none to run into the side tube and allowing the graduate to drain thoroughly. If the sample contains dissolved or sus pended water it is advisable to add a few small pieces of pumice or broken glass to,promote smooth distillation. Insert.the thermometer so that the top.of the mercury bulb (or the top of the contraction chamber if the Solvents Distillation Thermometer is used) is level with the bottom of the side tube. Connect the side tube to the condenser, with the bottom of the flask resting securely in the opening in the asbestos board.. Apply heat cautiously at first. When distilla tion begins, regulate the heat so that the distillate is collected at the rate of not less than 4 nor more than 5 mL/min (approximately 2 drops per second). Observe and record the temperature when 5 ml has been collected in the receiving . cylinder, and thereafter when the level of the distillate reaches each 10-mL division on the graduate, including a 95-mL reading. Discontinue the distillation when the tem perature reaches that specified for the minimum percentage 117 DUP050295783 # D 802 requirement. Correct all observed temperatures to compen sate for variations of barometric pressure, as described in 8.3. Allow the condenser to drain and record the percentage distilled. Should the thermometer reading start to fall before the temperature specified for the minimum percentage requirement is reached, discontinue the distillation, record the maximum temperature reached, allow the condenser to drain, and record the percentage distilled. No t e 1--Because of the frequent presence of a small amount of dissolved water in pine oil, it is impractical to attempt to determine the initial boiling point. It is also not customary, to determine the end point in the distillation of pine oiL 8,3 Barometric Correction--The distilling temperature of pine oil is affected by 0.059C for each millimetre variation of the atmospheric pressure. Therefore, the distillation tem peratures observed or specified shall be corrected to permit the distillation to be conducted as though the barometer reading, corrected to 0C, were exactly 760 mm. When about to begin the distillation, observe and record the barometric pressure and the temperature of the barometer. (No temper ature correction on barometer reading is necessary for aneroid-type barometers.) From Table 1 determine the proper temperature correction corresponding to these atmo spheric conditions, interpolating to the nearest 0.1'C. If the barometric pressure, corrected to 0C, is below 760 mm, the temperature correction must be added to the temperatures observed and subtracted from the minimum percentage requirement temperature; if above 760 mm, the correction must be subtracted from the temperatures observed and added to the minimum percentage requirement temperature. No t e 2--Example--Suppose the observed barometric pressure is 747 mm at 28C, and the 5 % boiling point is observed to be 204.0G From Table 1, by interpolating, the temperature correction is seen to be l.0*C. Therefore the corrected 5% boiling point is 204.0.+ 1.0 = 205.0'C Furthermore the temperature observation point at the min imum percentage requirement (usually 225C at 760 mm) must be altered to the same extent. Since the pine oil is. distilling 1.0C below what it would at normal pressure, distillation must be discontinued at 225.0 -- 1.0 = 224.0X1 to determine the percentage distilling below 225`C at 760 inm pressure. TABLE 1 Temperature Corrections for Barometric Pressure4 Observed Baro metric Pressure, mnv 780 . 770 760 750 740 730 720 710 700 Aneroid Barometer -1.18 -0.59 0.00 +0.59 +1.18 +1.77 +2.36 +2.95 +3.54 Mercurial Barometer Temperature of Barometer 2QC -1.03 -0.44 +0.15 +0.73 +1.32 +1..9J +2.50 +3.09 +3.67 25C -0.99 -0.41 +0.18 +0.77 +1.36 +1.94 +2.53 +3.12 +3.71 30C 35"C -0.96 -0.37 +0.22 +0.81 +1.39 +1.98 +2.57 +3.15 +3.74 -0.92 -0.33 +0.25 +0.84 +1.43 +2.01 . +2.60 +3.19 +3.77 A These corrections are calculated as follows: The observed barometric pressure is first corrected to what it would be at QC, by means of the table in Circular F, Instrument Division. U. 8. Weather Bureau. The corrected barometric pressure is then subtracted from 760 mm (or vice versa) and the difference' multiplied by 0.059C. To give the temperature correction shown in the above table the correction factor, C, of 0.059"C was calculated using the Sydney-Young equation: C - 0.00012 (760 - P) (273 + T) where: p = observed pressure, corrected to 0C, in mm, and r * median boiling temperature for pine oil. 9. Polymerization :# 9.1 Determine the unpolymerized residue with 3g sulfuric add in accordance with the procedure described Methods D 233. 10. Moisture 10.1 Determine the moisture content in accordance with Method D 95, using a glass flask5 and using either petroleu naphtha, toluene, or xylene as the solvent. It is impor that the flask be scrupulously clean, for if it shows any whitf deposits (such as might be caused from attack by alt-aij.. during previous use), the percentage of water may erroneously high due to a slight decomposition of the terpen! alcohols in the pine oil. 10.2 Alternative Method--Determine the moisture con tent in accordance with Method D 890. 11. Total Terpene Alcohols6 11.1 Apparatus: 11.1.1 Flask--A round-bottom, short-neck, flask of 500i mL capatity. 11.1.2 Water Trap--A Dean and Stark (Barrett moisture trap, 20-mL capacity (Note 3). No t e 3--It is preferable to have all joints of the flask, moisture and condenser of the interchangeable ground-glass type, with starii 24/40 taper. 11.1.3 Condenser--A straight-tube, water-cooled, reflux type, having a water jacket 400 mm in length, inner tube approximately 10 to 12 mm in diameter. 11.1.4 Heat Source--A gas burner or an electric 1 having suitable heat control. 11.1.5 Support for Flask--Preferably a Transite or hard asbestos board with a 2`/2-in. (64-mm) opening in the center,5 resting on a ring support. A piece of wire gauze may alsobe used. 11.2 Reagents: 11.2.1 Kontak Clay (Silica Gel) or finely ground earth. f! 11.2.2 Syrupy Phosphoric Acid (cp 85 %). ^ 11.2.3 Dry Dipentene, Xylene, or Petroleum Hydrocarbon Solvent of similar boiling range, such as mineral spirits. No t e 4--If dipentene is used, it shall have been treated according>td this procedure, to remove traces of terpene alcohol that may be present! 11.3 Procedure--Weight 0.1 g of Kontak clay or Fuller'! earth and brush it into the 500-mL round-bottom flask adding a few glass beads. Tare the flask to the nearest 0.1 g on a triple beam side arm balance, and pipet 100 0.25 gof the sample into the flask, taking care to avoid dropping any on the neck or outside of the flask. (Should this occur, wipe dry with a cloth moistened with the dipentene or other solvent.) From a 1-mL graduated pipet add 0.3 mL of phosphoric acid to the flask. Apply a thin film of stopcock; lubricant to all ground-glass taper joints, and connect the apparatus. Raise the mercury into the graduated leg of the moisture trap, about 1 in. (25 mm) below the level ofthe side tube, and fasten the ring support of the reservoir to hold it 5 Borosilicate glass is satisfactory for this purpose. 6 This method of test consists of measuring the water evolved during lie rstfllvfi/' rippnmnnqifinn of the temfme alcohols 118 DUP050295784 # D 802 ert a snug-fitting buret-cleaning brush with long idle into the top ofthe condenser, allowing the brush near the top of the condenser but so that it can be at will down to where the condensation of the takes place. Apply heat gently at first until the gets under way. As the distillation proceeds, and d dipentene collect in the trap, gradually lower the "level in the graduated leg of the trap and increase of boiling. Bring down the droplets of water that the walls of the condenser by adding a few drops of cnt at the top of me condenser (enough to wet the d then moving the brush up and down at the lower he condenser. At 15/to 20-min intervals during the : the mercury reservoir slowly to return the supema;entene to the flask, retaining the water in the trap, lower the mercury level to collect additional ve. Discontinue the distillation at the end of 4 h, and Sown any droplets of water in the condenser with the Calculation--From the volume of water collected in p deduct the amount of moisture contained in the and calculate the percentage of total alcohols as Total alcohols, % -- r&L of H20 x 8.56 #= grams of terpene alcohol equivalent to 1 g of H2Q. A--Mercury reservoir is supported on ringstand. B--Connection for 12 in. straight-tube water condenser. C--Receiving trap with capacity of 13 mL, graduated in 0.1 mL. D--Connection for distilling flask. FIG. 1 Apparatus for Determining Alcohols in Pine Oil S--If desired, the moisture may be determined on the total sample (without addition ofa solvent as specified in Section 10), ,, the addition of the dehydrating agents, using a scrupulously clean 'and the trap shown in Fig. 1. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination 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 atany time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or 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. 119 DU P0502 95785 Designation: D 803 - 82 (Reapproved 1987) Standard Methods of Testing Tall Oil1 This standard is issued under the fixed designation D 803; 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 methods cover the test procedures to be applied to whole tall oils or refined tall oils. 1.2 The procedures appear in the following order Physical Tests Sections D 1240 Test Method for Rosin Acids inFatty Acids4 D 1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 '' D2196 Test Methods for Rheological Properties of Non- Newtonian Materials byRotational (Brookfield) > Viscometer6 7 E 70 Test Method for pH of Aqueous Solutions with the ^ j , * ` Viscosity: Brookfield Method (Preferred Method) Gardner-Holdt Method (Alternate Method) Pour Point Flash Point Color Moisture Ash Chemical Analysis 6 3 to 10 11 12 13 14 to17 18 to20 Sections Glass Electrode7; E 123 Specification for Apparatus for Determination of Water by Distillation8 .? 3. Sampling 1 No t e 1--Methods of sampling will be supplied later. Method D 270,1') Sampling Petroleum and Petroleum Products3 of the American Society, ;j| for Testing and Materials, and the Methods of Sampling Oils and Fats of the American Oil Chemists' Society are being Studied by the committee. Acid Number Potentiometric Method (Referee Method) Colorimetric Method (Alternate Method) Saponification Number Potentiometric Method (Referee Method) Colorimetric Method (Alternate Method) Rosin Acids: Potentiometric Method (Referee Method) Modified Wolff Method Qualitative Test for Rosin Unsaponifiable Matter (Sterols, Higher Alcohols, etc.) Fatty Acids 21 to 25 26 to 30 31 to 35 36 to 40 41 to45 46 to50 51 and 52 53 to 56 57 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. Some ofthese procedures will probably be proposed for sampling tall oiIlf.">V' .. | 4. Conditioning 4.1 Heat the entire sample in a closed container fitted with a capillary vent of its equivalent. Some kind of i agitation, even if done occasionally by hand, saves much ' p tithe. Heat by immersion in an open steam or boiling water ! ' bath to avoid overheating. Withdraw the specimens only '> when ail crystalline matter has dissolved and when the entire } sample becomes a homogeneous fluid after thorough stirring. \ 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.9 Other grades may be used, provided it is first ascertained that the reagent is of \ i , I 2. Referenced Documents sufficiently high purity to permit its use without lessening the accuracy of the determination. I 2.1 ASTM Standards: D93 Test Methods for Flash Point by Pensky-Martens 5.2 Unless otherwise indicated, references to water shall * be understood to mean distilled water. ^ Closed Tester1 D97 Test Methods for Pour Point of Petroleum Oils3 4 Annua! Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 6 Annua! Book ofASTM Standards, Vol 06.01. 1 These methods are under the jurisdiction of ASTM Committee D-I on Paint 7 Annual Book ofASTM Standards, Vol 15.05. 'Is and Related Coatings and Materials and are the direct responsibility of Subcom mittee IX) 1.34 on Naval Stores. 8 Annual Book ofASTM Standards, Vols 05.03 and 14.02. * "Reagent Chemicals, American Chemical Society Specifications,'' Am. Chem. Current edition approved March 26, 1982. Published June 1982. Originally* Soc,, Washington, D. C. For suggestions on the testing of reagents not listed by the published as D 803 -44 T. Last previous edition D 803 - 65 (1975). American Chemical Society, see "Reagent Chemicals and Standards" by Joseph 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. Rosin, D. Van Nostrand Co., Inc., New Yrirk, and the "United States 3 Annual Book ofASTM Standards, Vol 05.01. Pharmacopeia." f 120 DUP050295786 D 803 PHYSICAL TESTS gVISCOSITY BY THE SAYBOLT METHOD (Preferred Method) ermine the viscosity in accordance with Method D temperature of testing shall be 210F unless a jiperature is specified, but in no case may a ; offess thanT|180Fbe used. - . ' i IcOSITY BY THE GARDNER-HOLDT METHOD (Alternative Method) fatus fe" viscosity' 6f tall oils that contain no crystals at , be measured by means of Gardner-Holdt bubble :se tubes shall be of clear glass with a closed, flat, :om and shall have the following approximate ns and markings: uniform internal diameter throughout the length [be of 10.65 mm, internal length of 112 mm, ' An etched line around the ouiside ofthe tube 5 mm. open end, and isecond etched fine around the outside of the tube m the open end - fhe tubes shall provide results that are in agreement data shown in Table 1. sure "ill the tube with the sample, free of solid particles or tales, so that the apparent upper edge of the liquid is even with the lower etched' line on theTube. liring the fillesd,stoppered tube to equilibrium at 25 |f77 0.45F)[ r Invert the tube and allow to remain for twice the anticipated bubble time in order to bring the bubble to complete rest in the inverted tube. Quickly revert the tube to upright position, still at 25C, and, with the tube exactly vertical, carefully note the time, to 0.1 s, for the bubble to rise until the first sign of its deformation against the cork. Repeat this procedure and average the two results. 9. Report 9.1 Report the average ofthe two results as the viscosity in Gardner seconds to the nearest 0.1 s if the time is less than 10.0 s, and to the nearest second if the time is 10.0 s or more. This time, in seconds, may be translated to viscosity in stokes as follows: Vs = 0.73T- (0.5/T2) where: Vs- viscosity, St, and T = time, s. 9.2 Reasonable accuracy may be obtained by multiplying time in seconds by 0.73 on materials having a viscosity greater than 1.5 St. 9.3 Results may be reported by Gardner-Holdt letters, as defined in Table 1. 10. Precision 10.1 Duplicate results should be within 5 % by the same operator, and within 10 % by different operators, except at the limits of this method of measurement. POUR POINT 11. Procedure 11.1 Determine the pour point in accordance with Method D 97, reporting only the lower pour point. The upper pour point is not always reproducible because of the tendency of some tall oils to crystallize. FLASH POINT *A3 jBaHgmu - kB f sJIt rIN Gardner-Holdt Letter Definitions of Viscosity Reference ' Standards ' 1 Stokes Sec onds Letter Stokes Sec onds 0.00505 0.0624 0.144 0.220 0.321 0.50 0.65 0.85 1.00 1.25 1.40 1.65 2.00 2.25 2.50 2.75 3.00 3.20 3.40 3.70 4.00 ... . 1.2 1.3 1.5 1.6 1.9 2.1 2.3 2.8 3.1 3.4 3.8 4.1 4.4 4.7 5.1 - 5.5 Q R S r u V w X Y Z Z1 22 , zs Z4 ' Z5 Z6 Z7 28 Z9 Z10 4.35 4.70 ' 5.0 5.5 6.27 8,84 10.7 12.9 17.6 22.7 27:0 36.2' 46.3 63.4 98.5 148 388 -590 855 1066 : 6.0 6.4 6.8 7.6 8.6 12.1 14.7 17.7 24.0 31.0 37.0 50.0. 63.0 87.0 135.0 202.0 12. : Procedure 12.1 Determine the flash point in accordance with Method D 93. COLOR 13. Procedure 13.1 Determine the color in accordance with Method D 1544. MOISTURE 14.. Apparatus'(Fig. 1) 14.1 Flask--A 500-mL or a i-L short-neck, round- bottOm, glass flask, depending upon the weight of the sample used. 14.2 Oil Bath--An oil bath that does not smoke exces sively below 160C. No t e 2--An oil bath is specified because the radiant heat of electric heaters and most gas flames causes sufficient cracking to form appre ciable quantities of water especially where impurities such as black 121 DUP050295787 D 803 any moisture adhering to the walk of the condenser. The water in the receiver may be made to separate from the xylene by using a spiral copper wire. Move the wire up and down in the condenser occasionally, thus causing the water to settle to the bottom of the receiver. Reflux for at least 2 h and shut off the heat at the end of this period. Adjust the temperature of the distillate to 20C. Read the volume of water. 17. Calculation ^, f 17.1 Calculate the percentage of moisture as follows: Moisture, % -- (V/tV) X100 where: V = millilitres of water at 20C, and W = grams of sample. 17.2 Report the percentage of moisture to one significant digit following the decimal point A = 45 to 55 mm. B = 22 to 24 mm, Inside diameter. C = 9 to 11 mm, inside diameter. D = 235 to 240 mm. E = 146 to 156 mm. F and G are interchangeable joints, standard-taper 24/40. FIG. 1 Assembly of Apparatus for Moisture Test liquor, soaps, lignin, or other xylene insoluble matter is present. An electric heater may be used when more precise results are not required. 14.3 Condenser--A reflux condenser connected to the flask and discharging into a trap. 14.4 Trap--A trap of well-annealed glass constructed in accordance with Specification E 123 (see Fig. 11) and gradu ated to contain 5 mL at 20C shall be used.10 15. Reagent 15.1 Xylene, cp. 16. Procedure 16.1 For tall oik containing up to 1.0 % moisture use 500 2 g of the sample. For tall oil containing 1 % or more of moisture use 150 1 g of the sample. Weigh the tall oil into the flask and add either 200 mL of xylene for the 500-g sample or 100 mL of xylene for the 150-g sample. Attach the flask to the trap which is connected to the condenser. Prior to starting the determination, fill the receiver with xylene by pouring in through the reflux condenser. So that the re fluxing will be under better control, wrap the flask and tube leading to the receiver with asbestos cloth. Heat the oil bath with a gas burner or other source of heat and distill slowly. The rate at the start shall be approximately 100 drops per minute. When the greater part of the water has distilled, increase the distillation rate to 200 drops per minute until no more water is collected. Purge the reflux condenser dining the distillation with 5-mL portions of xylene to-wash down 10 Distilling Receivers, Bidwell and Sterling, Coming Glassworks Catalog No. 3642 and Kimble Glassware Catalog No. 22002 may be considered to fulfill the specification. ASH w 18. Apparatus 18.1 Platinum Dish--A platinum dish of 50 to 100-mL capacity. No t e 3--A porcelain or silica dish may be used in place of platinum, if the ash is not to be analyzed I 19. Procedure I& 19.1 Heat the platinum dish to redness and, after cooling in a desiccator, weigh to the nearest 0.0001 g. Place an approximately 20-g sample oftall oil in the dish and weigh to ti the nearest 0.1 g (Note 4). Heat the dish gently by means of a bunsen burner until the oil can be ignited at the surface (Note 5). Remove the burner and allow the oil to bum completely. Bum all free carbon on the sides ofthe dish and.;{ heat the residue with a strong flame, or in a muffle furnace, ! until all carbonaceous matter disappears. After cooling in a desiccator weigh the dkh to the nearest 0.0001 g. Repeat the j heating until a constant weight k obtained. | No t e 4--This size is suitable for ash contents in the range from 0.02 to 0.2 %; but in the case of lower or higher ash contents, a larger or smaller sample may be used. In such cases the result shall be specified or reported as follows: "Ash {... g sample)... percent." No t e 5--To avoid foaming and loss of sample in the case ofsamples containing moisture, it is advisable to add 1 to 2 mL ofabsolute alcohol before heating. 20. Calculation 20.1 Calculate the percentage of ash as follows: Ash, % = (R/W) x 100 where: R = grams of residue, and W - grams of sample, dry basis. 20.2 Report the percentage of ash to the third decimal place. 122 DUP050295788 # D 803 CHEMICAL ANALYSIS ItJMBER BY THE POTENTIOMETRIC METHOD (Referee Method) Ication ! method shall be used where the most reproduc- jj^are desired. By using the potentiometric inflection | the considerable error due to colorimetric end jliminated. N ratus '0Meteru--An indicating potentiometer having a tor not greater than 0.1 pH over a range from pH IIj , using an alkali-resistant glass electrode and a ' calomel half-cell. The pH meter shall conform to ements of Method E 70. tirrer--A variable-speed mechanical stirrer (with a glass propeller-type paddle. Weaker, tail-form, 300-mL capacity. turet--A buret of 50-mL, capacity with 0.1-mL ^ The so-called automatic buret is preferable as its rizes errors due to evaporation. The automatic iiould be guarded with soda-lime tubes against the ah of C02 from the air. buffer solution as described in Method E 70; then rinse the electrodes thoroughly with water and then with alcohol. 24.3 Adjust the beaker containing the solution of the sample so that the buret tip is close to the surface of the solution. Adjust the electrodes so that the lower half of each is immersed. Start the stirrer slowly; then adjust its speed for vigorous stirring without spattering. Record the initial pH if it is on the scale. Add suitable portions of alkali solution and, waiting after each addition until an unchanging potential has been established, record the pH and buret readings, Add 5-mL portions of alkali solution until the pH is about 8; then add 1-mL portions until the change in pH per portion added exceeds 0.3 pH unit; and then add 0.1-mL or smaller portions until the end point has been passed, as indicated by a significant decrease in pH change per unit volume of alkali solution added. After the pH change is less than 0.1 pH unit per 0.1 mL of alkali solution, the increments may be increased to 1.0 mL. End the titration at pH 12 or above. 24.4 Determine the inflection point (point of maximum change in pH per 0.1 mL of 0.5 N alkali solution) to the nearest 0.1 mL. This may be found by inspection of a plot of pH against millilitres of alkali solution added, or by plotting the change in pH per millilitre of alkali solution against the pH reading. The inflection point shaft be taken as the end point of the titration. Wfilcohol--MsthmcA (99.5 %), or ethyl alcohol (95 %) ^red by Formula No. 3A or No. 30 of the U. S. Bureau pal Revenue. i'-Alkali Solution, Standard Alcoholic (0.5 N)--Dis-. pather 33 g of KOH or 21 g of NaOH, preferably in ipjm, in alcohol conforming to 23.1 and dilute to 1 L ge alcohol.12 Standardize to 0.001 N with potassium hthalate in 100 mL of the alcohol to be used in the Pure plus sufficient wafer for a clear solution; 2.553 g of I0OOKCOOH will be neutralized by 25.00 mL of N KOH or NaOH solution. The standardized soluIhould be protected against evaporation and absorption |02 from the air. The solution should be standardized ently, either electromettically, or colorimetricaily using |bl blue (27.3) or phenolphthalein as the indicator. ^Procedure fp.4 Dissolve 3.95 to 4.05 g of the sample, weighed to the rest 0.001 g, in 100 mL Of alcohol in a 300-mL beaker, firl the beaker to dissolve the sample, warming slightly if essary. i.2 Turn the pH meter on and allow a few minutes for it :>me to equilibrium. Balance the meter, using a standard ft'' 25. Calculation and Report 25.1 Calculate the acid-number, expressed as milligrams of KOH per gram of sample, as follows: ' Acid number = (AN x 56.1)/B where: A -- millilitres of alkali solution required for titration of the sample, N -- normality of the alkali solution, and B -- grams of sample used (dry basis). 25.2 Report the acid number to one digit following the decimal point. ACID NUMBER BY THE COLORIMETRIC METHOD (Alternative Method) 26. Application 26.1 This method may be used where only approximate values are desired. The selection of the colorimetric end point varies with the analyst and with dark-colored samples is too indefinite for reliable results. 27. Apparatus .27.1 Buret--See 22,4. 27.2 Flask--A 250-mL wide-mouth Erlenmeyer flask. :11 pH meters that have been found'suitable for potentiometric titrations include | Beckman or Macbeth pH meter equipped with Beckman electrodes No;. 1170 a'1190E; Leeds & Northrup No. 7661-A1 assembly with Std. 1199-30 high Ijllkali-resistant glass electrode; Fischer titrimeter, Senior Model, with electrode No. ` 312-27; or equivalent pH meters. f ,,,(,,!2Some methods prescribe water instead of alcohol for the standard alkali Bmhition, but water is not recommended here because its presence tends to increase ethe fouling of the electrodes with deposits. 28. Reagents 28.1 Alcohol--See 23.1 28.2 Alkali, Standard Solution (0.5 N)--Dissolve either 33 g of KOH or 21 g of NaOH, either in water or in alcohol conforming to 28.1, and dilute to 1 L with the solvent selected. Standardize to 0.001 N. 123 DUP050295789 D 803 28.3 Thymol Blue Indicator Solution--Dissolve 0.1 g of thymol blue in 100 mL of methanol. 29. Procedure 29.1 Dissolve 3.95 to 4.05 g of the sample, weighed to the nearest 0.001 g, in 100 mL of alcohol in a 250-mL flask. Twirl the flask to dissolve the sample, warming slightly if necessary. Add 1 ml of thymol blue indicator solution and titrate with alkali solution. The end point'is a distinct blue., NpTE 6--For dark-colored tall pils the blue color will not be distinct. The ead point shall be taken as the firstpersistent distinct darkening of the solution. The end point can be seen more clearly if the titration is stopped'jiist short of the end point and a few drops ofthe, thymol blue solution allowed tb run down the side of the flask following each addition of 0.1 mL of alkali solution. < 30. Calculation and Report , , 30.1. Calculate the acid'number as described in' 25.1. Report the results to the nearest whole number. SAPONIFICATION NUMBER, BY THE POTENTIOMETRIC METHOD . ... (RefereeMethod) 31. Application ,, 31.1 This method shall be used where the most reproduc ible results are desired: By using the potentiometric inflection end point, the considerable error of a colorimetric end point is eliminated. 32. Apparatus 32.1 The apparatus shall consist of the items described in Section 22, and the following: : 32.2 Flask--A 250-mL wide-mouth Erlenmeyer flask of a chemically resistant glass13 with a standard-taper 34/45 neck. 32.3 Condenser--A water-cooled condenser with a joint fitting the flask described in 32.2. 33. Reagents 33.1 The reagents required are those dbsdjbed iri Section 23, using ethyl alcohol, and the following: 33.2 Acid, Standard (0.5 N)--Standardize a 0.5 N solu tion of H2S04 or HC1 to 0.001 N by , any accepted procedure. 34. Procedure 34.1 Transfer 2.95 to 3.05 g of the sample, weighed to the nearest 0.001 g, to the flask. Add 50.0 mL of the alkali solution and connect the flask to the condenser. Heat the flask in- a water bath and reflux for 30 min. Cool and transfer without delay to the 300-mL beaker, using a total of 100 mL of alcohol for at least five successive rinsings. 34.2 Prepare the pH meter as described in 24.2. 34.3 Titrate promptly with 0.5 N acid. Adjust the beaker containing the. solution of. the sample so that the acid buret tip is close to the surface of the solution. Adjust die 13 Coming or Kimble alkali-resistant glasses, or equivalent, are suitable for this purpose. Borosilicate flasks may be used, but they should either be new or be cleaned by rinsing with a hot solution of HF (2 or 3 percent). This removes from the flasks the adhering partially disintegrated silicates which would interfere with the determination. electrodes so that the lower half of each is immersed. Start the stirrer slowly; then adjust its speed for vigorous stirring without spattering. Record the initial pH if it is on the scale. Add suitable small portions of acid and, waiting after each addition until an unchanging potential has been established, record the pH and buret readings. Add 5-mL portions of the acid until the pH is about 12; add 1-mL portions until the change in pH per portion added exceeds 0.3 pH; and then add 0.1-mL qr smaller portions until the end point has been passed, as indicated by a significant decrease, in pH change per unit volume of add added. A%r the pH change is less than 0' 1 pH unit per 6.1 mL of acidi, the increments may be increased to 1.0 mL. End the titration at pH 8.0 or below. 34.4 Determine the inflection point (point of maximum change in pH per 0.1 mL of 0.5 N acid) to the nearest 0.1 mL: This may be found by inspection of a plot of pH against millilitres of acid added, or by plotting the change in pH pd millilitre of acid against the pH reading. The inflection point shall be taken as the end point of the titration.' 34.5 Blank--Make a blank determination, using 50.0 mt of the alkali solution and following the same procedure as for the sample. 35. Calculation and Report 35.1 Calculate the saponification number, expressed as milligrams of KQH per gram of sample, as follows: Saponification number .= [( -- A)N X 56.1J/C * where: B -- millilitres of acid required for titration of the blank,:: A = millilitres of-acid required for titration, of the sample, N,= normality of the acid, and C' -- grams of sample used (dry basis). 35.2 Report the saponiflcatipn number to one digit fol lowing the decimal point. SAPONIFICATION NUMBER BY THE COLORIMETRIC METHOD o (Alternative Method) 36. Application , 36.1 This method may be used where only approximat values are desired.-> The selection of the colorimetric en point varies with the analyst and is usually too indefinite fo reliable results. 37. Apparatus 37.1 The apparatus shall consist of the buret described i 22.4 and the flask and condenser described in Section 32. 38. Reagents 38.1 The reagents required are those described in Sectio 23, using ethyl alcohol, and 28.3. 39. Procedure 39.1 Transfer 2.95 to 3.05 g of the sample, weighed to tl nearest fr-OOfi g, to a 250-mL Erlenmeyer flask. Add 50.0 m of the alkali solution and connect the flask to the condense Heat the flask in a water bath and reflux for 30 min. Co and titrate promptly with ,0.5 N add, using 1 mL of tl thymol blue solution as the indicator. 124 DUP050295790 wfilnnk--Make a blank determination, using 50.5 mL wsblution and following the same procedure as for the Sjj*wt |eulation and Report pCalculale the saponification number as described in t the results to the nearest whole number. 3N ACIDS BY THE POTENTIOMETRIC METHOD (Referee Method) ope This method shall be used for tall oils containing not 15 % of rosin adds where the most reprodutible p5are desired. By using the potentiometric inflection [joints, the considerable error due to colorimetric end i is eliminated. For tail oils containing less rosin acids . D 1240 shall be used. ' The apparatus shall consist of the items described in as 22 and 32. Alternatively, an automatic titrator may IjReagents |li -Ethanol, conforming to 23.1. 3.2 Methanol (99.5 %). jfa Methyl Sulfuric Acid Solution--Slowly pour 100 g of l4(sp gr 1.82 to 1.84), While stirring constantly, into 400 Bhaethanol. Store in a glass-stoppered bottle. 1314 Potassium Hydroxide, Standard Alcoholic Solution Dissolve 33 g of KOH, preferably in pellet form, in Ithanol and dilute to 1 L. Standardize to 0.00 I N with assium add phthalate as described in 22.2; 2.553 g of |H4-COOKCOOH will be neutralized by 25.00 mL of j 00 N KOH solution. The standardized solution should i;protected against evaporation and the absorption of C02 . the air. Procedure !f44.1 Dissolve 4.95 to 5.05 g of the sample, weighed to the |earest 0.001 g, in 100 mL of methanol in a 250-mL flask. rl the flask to' dissolve the oil. Add 5 mL of methyl liilfuric acid solution and connect the flask to the condenser, leat the flask assembly and reflux for 30 min. Cool and sfer to a 300-mL beaker, using a total of 100 mL of fleohol (ethanol is preferable when an automatic titrator is pised) for at least five successive rinsings. | 44.2 Prepare the pH meter as described in 23.2. 44.3 Adjust the beaker containing the solution of the P Sample so that the buret is close to the surface ofthe solution, jfi. Adjust the electrodes so the lower half of each is immersed. Start the stirrer slowly; then adjust its speed for vigorous " stirring without spattering. Record the initial pH if it is on foe scale. Add suitable small portions of the KOH solution and, waiting after each addition until an unchanging poten tial has been established, record the pH and buret readings. Add 5-mL portions of KOH solution until a pH of 1.0 to 1.5 is reached; then add 1-mL portions until the change in pH per portion added exceeds 0.3 pH-unit; and then add 0.1 -mL or smaller portions until the first end point has been passed, as indicated by a significant decrease in pH change per unit volume added. Thereafter, add 1 to 2-mL portions until the pH change per portion added again exceeds 0.3 pH unit. Again add 0.1-mL or smaller portions until the second end point has been passed as indicated by significant decrease in pH change per unit volume of KOH solution added. After the pH change is less than 0.1 pH unit per 0.1 mL of KOH solution added, the increments may be increased to 1.0 mL. End the titration at pH 12 or above. 44.4 Determine the inflection points (points of maximum change in pH per 0.1 mL of 0.5 N KOH solution) to foe nearest 0.1 mL. They may be found by inspection of a plot of pH against millilitres of KOH solution added, or by plotting the change in pH per millilitre of KOH solution against the pH reading. The inflection points shall be taken as the end points of the titration. Alternatively, if an automatic titrator is used foe end points shall be taken at pH 4.0 and pH 10.5. 45. Calculation and Report 45.1 Calculate fop percentage of rosin acids as follows: Rosin acids, % = (AN/B) x 30.2 where: A = Millilitres of KOH solution required for titration between the first and second end points, N = normality of the KOH solution, and B -- grams of sample used (dry basis). 45.2 Report the rosin adds percent to one digit following the decimal point. ROSIN ACIDS BY THE MODIFIED WOLFF METHOD 46. Scope 46.1 This method may be used where only approximate values are desired. The selection of the colorimetric end point varies with the analyst and is too indefinite for reliable results. 47. Apparatus 47.1 The apparatus shall consist of the items described in Sections 22 and 32. 48. Reagents 48.1 The reagents required are described in Sections 28.3 and 43. 49. Procedure 49.1 Dissolve 4.95 to 5.05 g of the sample, weighed to the nearest 0.001 g, in 100 mL of methanol in a 250-mL flask. Twirl the flask to dissolve the sample. Add 5 mL of methyl sulfuric acid solution and connect the flask to the condenser. Heat the flask assembly in a water bath and reflux 30 min Cool and add 1 mL of thymol blue indicator solution. 49.2 Titrate with the KOH solution the first end point, about pH 4.0, when foe solution changes color from red to yellow. Record the reading or refill the buret. Continue the titration to the second end point, about pH 10.5, when the solution changes color from yellow to blue. Record to foe nearest 0.1 mL the millilitres of KOH solution required for titration between the two end points. 125 DUP050295791 D803 No t e 7--These end points approximate the inflection points under these nonaqueous conditions. 50. Calculation and Report 50.1 Calculate the percentage of rosin adds as described in 45.1. 50.2 Report the results to the nearest whole number. QUALITATIVE TEST FOR ROSIN 54.6 Potassium Hydroxide, Alcoholic Solution (132 KOH/L)--Dissolve 132 g of KOH pellets or sticks in 15Q | mL of water and dilute to 1 L with alcohol conforming to l 54.2. |j 54.7 Sodium Hydroxide Solution (10 g NaOH/litre)-J% Dissolve 10 g of NaOH in water and dilute to 1 L. ^ 54.8 Thymol Blue Indicator Solution--Dissolve 0.1 g off| thymol blue in 100 mL of alcohol. f 51. Reagents 51.1 Acetic Anhydride. . 51.2 Sulfuric Acid (sp gr 1.53)--Dilute 34.7 mL of H2S04 (sp gr 1.84) with 35.7 mL of water. 52. Procedure 52.1 In any case where the rosin acid, content is found to be less than 5 %, the actual presence of rosin should be checked qualitatively by the Liebermann-Storch test, as follows: Transfer about 2 mL of the sample to a test tube, add 5 mL of acetic anhydride, and dissolve by warming on a steam bath or by other gentle heating. Cool and pour about one half the solution into a small white porcelain evapo rating dish. Allow 1 drop of H2S04 (sp gr 1.53) to run down the side of the dish. If rosin adds are present a bright but fugitive violet coloration will appear where the liquids come into contact, changing rapidly to a brownish tinge. It is advisable to make a check test with a sample of fatty add to which a small quantity of rosin or rosin acid has been added. UNSAPONIFIABLE MATTER (STEROLS, HIGHER ALCOHOLS, ETC)14 53. Apparatus 53.1 Erlenmeyer or Other Flat-Bottom Flask, of 125-mL capacity, with standard-taper 24/40 joint. 53.2 Erlenmeyer Flask, 300-mL capacity, with wide mouth. 53.3 Separatory Funnels, of 300 to 500-mL capadty, with glass stoppers. 54. Reagents 54.1 Alkali, Standard Alcoholic Solution (0.1 N)--Dis solve 6.6 g of KOH or 4.2 g of NaOH, preferably in pellet form, in ethanol or alcohol conforming to 53.1, dilute to 1 L with the same alcohol, and standardize to 0.001 N. This solution should be restandardized at frequent intervals. 54.2 Ethyl Alcohol, Neutral--Neutral 95 % ethyl alcohol, or neutral denatured alcohol conforming to either Formula No. 30 or No. 3A of the U. S. Bureau of Internal Revenue. 54.3 Ethyl Ether. 54.4 Isopropyl Alcohol (91 to 99 %)--Making neutral to phenolphthalein by adding 0.1 N alkali solution dropwise. 54.5 Phenolphthalein Solution--Dissolve 1.0 g of phe nolphthalein in 100 mL of alcohol conforming to 54.2, and neutralize to a very faint pink color with 0.1 N alcoholic alkali solution. 14 Adapted from Method B of the Method D [065, Test for Utisaponifiable Matter in Rosin, which appeals in the Annual Book ofASTM Standards, Vol 06.03. 55. Procedure -fj 55.1 Weigh 5.00 0.01 g of the sample into the 125-nit Erlenmeyer or other flat-bottom flask, add 15 mL of the ' alcoholic KOH solution (132 g KOH/L), attach to the condenser, and reflux for 1.5 h, shaking occasionally. Re move the flask, add 50 mL of water, and transfer to a separatory funnel. Rinse the flask with 40 mL of ether, adding the rinsings to the separatory funnel. Shake the funnel and allow to stand until the ether layer separates., Draw off the aqueous soap solution (lower layer) into a t second funnel, allowing a few drops of the aqueous solution; to remain above the stopcock to, prevent loss of ether extract j by creepage through the ground-glass joint. ,1 55.2 To the soap solution in the second funnel, add 301 mL of ether and extract as before, drawing the soap layer!; into the original saponification flask. Add the ether in the second funnel to the first funnel. Then pour the soap!) solution from the flask into the second funnel, and again : extract with 30 mL of ether; Draw the soap layer into the flask again, and add the ether to the first ftmnel as before;! Now draw off and add to the solution in the flask all but a few drops of the soap solution which has collected below the combined ether layers in the first funnel. 55.3 Again pour the combined soap solutions into the second funnel and extract for the fourth time with 30 mL of ether. After separation of the layers, discard the soap solution and add the ether extract to the first funnel. Carefully draw off any remaining soap solution that may have collected above the stopcock. Add 2 mL of water, swirl the funnel gently, allow the water to settle, and then draw off and discard. Repeat this washing, once with 5 mL and twice with 30 mL of water. 55.4 Draw off the washed ether extracts into a dry, tared, wide-mouth Erlenmeyer flask, rinse the funnel with 15 mL of ether, add to the flask, and evaporate on a steam bath. If any droplets of water Collect in the flask, add a few millilitres ofethyl alcohol, and again evaporate on the steam bath until a clean, dry residue is obtained. Then place the flask in an oven at 100 to 105"C for 10 to 15 min, cool in a desiccator, and weigh. 55.5 Dissolve the contents in the flask in 50 mL of neutral isopropyl alcohol, add 1 mL of thymol blue or phe nolphthalein indicator solution, and titrate with the 0.1 N alcoholic alkali solution. When the solution is too colored to detect with-certainty the end point internally, titrate until a faint color change is noted. Then withdraw approximately 0.5 mL ofthe solution to the porcelain spot plate, and to the withdrawn portion add 1 drop of the indicator solution. Continue titrating with 0.1-mL portions ofalkali, and testing on the spot plate, until a definite color change that persists for at least 1 min is obtained. 126 DUP050295792 alculation and Report Calculate the percentage of unsaponifiable matter higher alcohols, etc.) as follows: saponifiable matter, % = [A -- (CN X 0302)/B] x 100 is of dried residue, as of sample used (dry basis), Millilitres of alkali solution used, and nrmality of the alkali solution. Report the results to the nearest 0.1 percent. FATTY ACIDS 57. Procedure 57.1 Calculate the fatty acids content of the tall oil as follows: Fatty acids, % = 100 -- (R + U) where: R = percentage of rosin acids, and U = percentage of unsaponifiable matter. 57.2 Report the results to one digit following the decimal point if the rosin acids number was determined by the potentiometric (referee) method. Report the results to the nearest whole number if the rosin acids number was deter mined by the modified Wolff method. The American Society lor Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are 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 ript revised, eitherreapproved or withdrawn. Yourcomments 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 19103,127 127 DUP050295793 Designation: D 804 - 79 (Reapproved 1987) Standard Definitions of Terms Relating to Naval Stores and Related Products1 This standard is issued under the Fixed designation D 804; 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. abietic acid, commercial grade--a product consisting chiefly of rosin acids in substantially pure ,form, separated either from rosin or tall oil commercially for . specific purposes and in which abietic acid and its isomers are the principal components. american turpentine (spirits of)2--a light-colored, volatile essential oil obtained from resinous exudates or. resinous wood associated with living or dead coniferous trees; particularly of the genus, Pinus, or more commonly, pines. Four kinds pf tiirpentine are now recognized: (1) gum turpentine or gum spirits, obtained by distilling the crude exuded gum or oleoresin collected from living pine trees. Gum turpentine contains mostly alpha-pinene with lesser substantial quantity of beta-pinene and a small quantity of other terpene hydrocarbons. (2) steam-distilled wood turpentine, obtained from the oleoresin within the wood of pine stumps or cuttings, either by direct steaming of the mechanically disintegrated wood or after solvent extraction of the oleoresin from the wood. Steam-distilled wood turpentine consists essentially of alpha-pinene, a small quantity of camphene, dipentene, menthenes, and small amounts of other terpene hydrocar bons of similar boiling range. (5) sulfate wood turpentine, recovered during the con version of wood to pulp by the sulfate (kraft) process. Sulfate wood turpentine contains essentially a mixture of alpha- and beta-pinene in which the amount of alphapinene exceeds the beta. Sulfate wood turpentine contains a small amount of other terpene hydrocarbons whose composition varies with the nature of the wood but represents C10H16 hydrocarbons in the boiling range of dipentene. {4) destructively distilled wood turpentine, obtained by fractionation of certain oils recovered from the destructive distillation of pine wood. Destructively distilled wood turpentine is a complex mixture of a wide variety of aromatic hydrocarbons with only moderate quantities of terpenes being present. colophony--a term denoting medium and high grades of rosin. erode stripper oil (see also d-limonene)--a by-product of the manufacture of citrus juice, composed largely of dlimonene and containing up to 1.5 % of aldehydes. 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 D01.34 on Naval Stores. Current edition approved June 29, 1979. Published August 1979. Originally published as D 804 - 44 T. Last previous edition D 804 - 63 (1977). 2 These products are defined by the Naval Stores Act of 1923 (42 Stat. 1435; 7-USC-91-99) and regulations promulgated thereunder by the United States Department of Agriculture. dipentene--the optically inactive form of the monocyclic terpene hydrocarbon-limonene. Commercial dipentenes contain substantial portions of other monocyclic and bicyclic, as well as some oxygenated, terpenes having ! closely related boiling ranges. They are generally obtained i by fractional, distillation from crude oils recovered in the several commercial methods of utilizing pine wood, also i by isomerization during die chemical processing of terpenes. The four kinds of commercial dipentene are: (J) steam-distilled dipentene, fractionated from the crude oleoresinous extract during the processing of related! steam-distilled wood naval stores. (2) sulfate dipentene, from the crude condensate of the vapors generated in the digestion of wood in the sulfate paper pulp process. (5) destructively distilled dipentene, from the lighter! portions of the oil recovered during the destructive distil-i lation of pine wood. (4) chemically processed dipentene, recovered as a by-! product in connection with the chemical treatment and ! conversion of other terpenes. No t e--There is no legal requirement under the Naval Stores Act that the source, origin, or kind of dipentene be shown in the commercial < designation. Consequently, coined trade names are sometimes used in selling this product. ester gum--a resin made from rosin or rosin acids and-a polyhydric alcohol, such as glycerin or pentaerythritol. gloss oil--a solution of limed rosin or limed rosin acids in-a-, volatile solvent, used chiefly in surface coatings. (Whetr made from tall oil, the source is usually indicated.) gum thus--botanically, the oleoresin from trees of Boswellia species native to Arabia and Somaliland; also known as olibanum or frankincense. As applied to the naval stores industry, the term refers to the crystallized pine oleoresin or "scrape" collected from scarified "faces" of trees being worked for turpentine. d-limonene--a purified optically active terpene hydrocarbon recovered from by-products of the citrus industry. It is used as a chemical intermediate and as a monomer in terpene resins. monocyclic terpenes--a designation sometimes used in the trade to describe a heterogeneous mixture of monocyclic, bicyclic, and other related terpene hydrocarbons recovered or removed in the fractionation of certain terpenes or other essential oils, or as a by-product in the chemical conversion of generally sold under trade names. (The term "other monocyclic hydrocarbons," used in statistical re ports of the U.S. Department of Agriculture, covers this type of material.) naval stores--chemically reactive oils, resins, tars, and pitches derived from the oleoresin contained in, exuded 128 DUP050295794  D804 _jted from trees chiefly of the pine species us), or from the wood of such trees, i ter-certain heavier fractions of the volatile oil | by distilling pine-tar oil to convert it into pine ritine--the pharmaceutical name for spirits of . which conforms to the requirements of the .Formulary. -pne gum, the nonaqueous secretion of resin olved in a terpene hydrocarbon oil which is: pduced or exuded from the intercellular resin I.living tree, 1 Accumulated, together with oxidation products, in . wood of weathered limbs and stumps. " fcicyclic terpene hydrocarbon, the principal con'pf all turpentine, and existing therein in two ; forms, alpha- and beta-pinene. The latter is found aable quantity only in gum spirits and sulfate turpentine. Pinene not otherwise described usually Kppha-pinene. ^a colorless to amber colored volatile oil with eristic pinaceous odor, consisting principally of ic tertiary and secondary cyclic terpene alcohols, Invariable quantities of terpene hydrocarbons, ethers, phenols, and phenolic ethers, the amount and r of which depend on the source and method of Ifacture. The four commercial kinds of pine oil iare: , steam-distilled pine oil, obtained from the crude |resinous extract of pinewood during the processing of [ steam-distilled wood, naval stores. destructively distilled pine oil, obtained from the er distillate from the destructive distillation (carbon1) of pine wood. synthetic pine oil, obtained by' chemical hydration sin hydrocarbons to form the terpin alcohols, or by ydration of terpine hydrate. Ifi) sulfate pine oil--a high boiling fraction obtained in fe refining and fractional distillation of the condensed apors released during the digestion of wood by the sulfate ifbcess. (needle oil--an essential oil of typical fragrance obtained ly steam distillation, of the leaves (needles) of certain Jfbspecies of pine or other coniferous trees. tar, kiln burned--the heavy, oily liquid resulting from ontrolled carbonization (slow burning) of pine knots and itump-wood to charcoal in earth-covered piles or "kilns," rith introduction of insufficient air to permit complete ambustion; contains undecomposed resin acids along &with the decomposition products. This product is some! times called "country tar." Sine tar, retort--the tar produced by removal of volatile oils p from pine tar oil by steam distillation. Several grades are ^marketed; namely: Thin, Medium, Heavy, and Extra IP Heavy, so classified on the basis of viscosity, and de pending upon the quantity of volatile oils removed. Sine tar, Stockholm--kiln-burned pine tar produced in Bf5 Scandinavian countries from wood of the Northern Euro pean pine, Pinus sylvestris. J pine tar oil--the oil obtained by condensing the vapors from ' the retorts in which resinous pine wood is destructively distilled (carbonized). pine pitch--the dark-colored to black solidified material, somewhat pliant and tenacious, obtained by distilling off practically all the volatile oil from a retort pine tar; the genuine contains no added free rosin, pitch, Archangel3--originally a genuine pine pitch made from pine tar in the Archangel district of Russia; in this country a similar product is made from residues of pine origin blended with various oils to make a pitch for caulking boats. pitch, Brewer's3--a term used to designate a type of pitch made by blending certain oils, waxes or other ingredients with rosin for the coating of beer barrels, pitch, Burgundy3--originally the solidified resin obtained by heating and straining the air-dried solid oleoresin exuded by the Norway spruce (Picea excelsa) and European silver fir (Abies pectinata)', now denotes an artificial mixture made by heatirig rosin with certain fixed oils, the combi nation being used for adhesive plasters, pitch, Navy3--a pitch obtained by melting rosin with pine tar, with or without rosin distillation residues, polymerization residue (sulfonation residue)--as applied to certain liquid naval stores, denotes that relatively small portion of a sairiple of material that resists sulfonation and remains undissolved in the fuming sulfuric acid reagent, When the sample is tested according to the ASTM Methods D 233, Sampling and Testing Turpentine.4 rectified tar oil--the volatile oil that is rectified by steam distillation of pine tar, obtained by destructive distillation ofvarious species of Pinus. It is a thin liquid, having a dark reddish-brown color and a strong empyreumatie odor and taste. It is miscible in all proportions with ethyl alcohol and is used in certain pharmaceutical preparations. The specific gravity of rectified tar oil is not less than 0.960 nor more than 0.990 at 77 F. resenes--as applied to naval stores, those constituents of rosin that cannot be saponified with alcoholic alkali, but which contain carbon; hydrogen, and oxygen in the molecule. resinates, metallic--rosin in which part or all of the rosin adds have been chemically reacted with those metals that give soaps or salts which are water insoluble. Limed rosin, zinc-treated rosin, and the resinates oflead, cobalt, copper, and manganese, are of the greatest industrial importance, rosin--a spedfic kind of natural resin obtained as a vitreous water-insoluble material from pine oleoresin by removal of the volatile oils, or from tall oil by the removal of the fatty add components thereof. It consists primarily of tricyclic monocarboxylic acids having the general empirical for mula C20H30O2, with small quantities of compounds saponifiable with boiling alcoholic potassium or sodium hydroxide, and some unsaponifiable matter. The three general classifications or kinds of rosin in commerce are: (1) gum rosin, obtained from the oleoresin collected from living trees. (2) wood rosin, obtained from the oleoresin contained in dead wood such as stumps and knots. 3 These terms have been in use in the naval stores industry for many years. They cover a wide variety of compounded products in which the one constituent common to all is a large proportion of rosin. 4 Annual Book ofASTM Standards, Vol 06.03. 129 DUP0502 95795 # D 804 (3) tall oil rosin, obtained.from tall oil. rosin, limed--see resinates, metallic, rosin, limed or zinc-treated--rosin that has been chemically reacted with a calcium or zinc compound, or both, to form a product containing a metallic salt of the rosin acids, along with unreacted rosin. The amount of calcium or zinc contained in finished products of this category may vary over a wide range. rosin, modified--rosin that has been treated with heat or catalysts, or both with or without added chemical sub stances, so- as to cause substantial change in the structure of the rosin acids, as isomerization, hydrogenation, dehydrogenation, or polymerization, without substantial effect on the carboxyl group. The following are types of modified rosin: (]) disproporiionated (dehydrogenated) rosin--rosin that has been subjected to chemical or physical treatment, or both, so as to cause substantial simultaneous hydroge nation and dehydrogenation of the rosin acids to form their hydrogenated and dehydrogenated counterparts. (2) heat-treated rosin--rosin in which a reduction of acid number and a positive shift in. optical rotation has been brought about by controlled heat treatment only, in order to improve its suitability for specific uses. (3) hydrogenated rosin--rosin that has been treated with hydrogen under conditions that cause a partial or complete saturation of the resin acids present, best indi cated by a drop in the refractive index. Commercial hydrogenated rosin is usually only partially saturated. (4) polymerized rosin--rosin that, has been treated by chemical or physical means, or both, in a manner so as to cause a union of a part of the rosin acids to form dimers to such an extent that the average molecular weight of such rosin will be measurably greater than that of the original rosin. rosin, reclaimed--rosin that has been recovered or reclaimed by any means from waste or deteriorated material, pro vided that the concentration of rosin acids is not below that normal for rosin, and any residual or contaminating component from the waste material itself or from any article used in the recovery process is not in sufficient quantity to cause the physical or chemical properties of the reclaimed product to differ materially from those of rosin, rosin acids--principally monocarboxylic acids with the em pirical formula Cl9H29-COOH.. They are classified into two groups; the abietic type and the pimaric type. Both types and their derivatives are found in wood, gum, and tall oil rosins. rosin oil--the relatively viscous, oily portion of the conden sate obtained when rosin is subjected to dry destructive distillation;, also used to describe specially compounded oils having a rosin oil base. rosin spirits--the relatively light, volatile portion of the condensate obtained in the first stages when rosin is subjected to dry destructive distillation, rosin standards--the combinations of assembled colored glasses having the colors designated as representative ofthe established U.S. grades used in classifying rosin. The recognized official standards are those developed and issued by the U.S. Department of Agriculture, or similar standards made of Lovibond glass, when certified by the same Government agency. The official grades established by or under authority of the Federal Naval Stores Act, for which standards are provided, are as follows in order of increasing color XC, XB, XA, X, WW, (VG, N, M, K, l, }jt G, F, E, D, and FF (the latter grade is used only for wood rosin). No t e--Rosin darker in color than the standard for Grade D or FF is graded B. The designation Opaque with the grade letters OP is used to describe rosin that, because of a turbid, cloudy, or nontransparent condition due to occluded moisture, ex cessive crystallization, or presence of foreign matter other than dirt, cannot be accurately graded by comparison with any of the above described rosin grade standards, rosin type (sample)--a sample of rosin, or a mold of thermosetting plastic material, used as an unofficial stan dard in grading rosin. Such sample shall be so selected,' sized, and surface-finished that it will have the form of an. approximate %-in. cube with at least two opposite face?, having smooth parallel surfaces, and shall have a color!' when viewed through these faces which matches withiffl rather narrow tolerances the color of the corresponding official Government standard made of glass, skimmings (tall oil)--the curd, not acidified or otherwise* processed, skimmed from the black liquor of the alkaline paper pulp industry, from which tall oil is obtained, tall oil--a generic name for a number of products obtained from the manufacture of wood pulp by the alkali (sulfate) process or more popularly known as the kraft process. To provide some distinction between the various products, designations are often applied in accordance with the process or composition, some of which are crude tall oil, acid refined tall oil, distilled tall oil, tall oil fatty acids, and tall oil rosin. No t e--The following designations for tall oil shall be considered obsolete: Crude resinous liquid Swedish pine oil Finn oil Swedish resin Liquid resin Swedish rosin Liquid rosin Swedish rosin oil Resin oil Sylvie oil Sulfate pitch Talloel Sulfate resin Tallol Sulfate rosin tall oil, crude--a dark brown mixture of fatty acids, rosin, and neutral materials liberated by the acidification of soap, skimmings. The fatty acids are a mixture of oleic acid and linoleic acid with lesser amounts of saturated and other unsaturated fatty acids. The rosin is composed of resin acids similar to those found in gum and wood rosin. The neutral materials are composed mostly of polycyclic hy drocarbons, sterols, and other high-molecular weight; alcohols. tall oil, acid refined--the product obtained by treating crude; tall oil in solvent solution with sulfuric acid under controlled conditions to remove dark color bodies and odoriferous materials. Removal of the solvent yields a product with lighter color and higher viscosity than crude tall oil with approximately the same fatty acids-to-rosin ratio. 130 DUP050295796 D 804 distilled--the class of products obtained by distilling *e tall oil in fractionating equipment under reduced ure under such conditions that the ratio of rosin acids tty acids is varied over a wide range. The products that Orally contain less than 90 percent of fatty acids, are wn as distilled tall oils. The fatty acids are a mixture of and linoleic acids with lesser amounts of saturated i,other unsaturated fatty acids. The remainder consists sin and neutral materials. Tfatty acids--the class of products generally containing ercent or more fatty apds obtained by fractionation of Je tall oil. The fatty aicids are a mixture of oleic and eic acids with lesser 'amounts of saturated and other * iirated fatty adds, the remainder consists of rosin . neutral materials. rosin (see also rosin)--separated from the tall oil fs, fatty acids, and tall oil pitch by fractional distilla- of tall oil. Such rosin shall have the characteristic 1, appearance, and other physical and chemical propes normal for other kinds of rosin. The fatty acid tent shall not exceed. 5 percent. 1heads (light ends)--the low-boiling fractions obtained the fractional distillation of prude tall oil under reduced ;ure. The composition of these products varies over a range but includes palmitic, oleic, linoleic, and 1C acids with lesser amounts of other saturated and 'saturated adds. The neutral materials content is nor"y high. il pitch--the tmdistilled residue from the distillation of ;de tall oil. It is generally recognized that tall oil pitches tain some high-boiling esters and neutral materials *th lesser amounts of rosin and fatty adds. oil soap--the product formed by the saponification or utralization of tall oil with organic or inorganic bases, lies--a class of unsaturated organic compounds having fe empirical formula C10HI6 occurring in most essential s and oleoresinous plants. Structurally the important enes and their derivatives .are dassified as monocyclic `pentene), bicyclic (pinene), and acyclic (myrcene). ene alcohol--an alcohol directly related to or derived im a terpene hydrocarbon; the following are common xamples: terpineol (tertiary cyclic), bomeol (secondary cyclic), geraniol (primary, acyclic), linalool (tertiary, acyclic). terpene resins--the products formed by polymerization of /-pinene, a-pinene, limonene and other terpene hydrocar bons; These resins have a variety of physical properties related to reaction conditions and raw materials, turpentine, oil of.--see oil of turpentine, turpentine, spirits of--the volatile oil consisting primarily of a number of terpene hydrocarbons of the general formula C10H16. Four kinds of turpentine are now recognized: (1) gum turpentine or gum spirits, obtained by dis tilling the crude exuded gum or oleoresin collected from living pine trees. (2) steam-distilled wood turpentine, obtained from the oleoresin within the wood of pine stumps or cuttings, either by direct steaming of the mechanically disintegrated wood or after solvent extraction of the oleoresin from the wood. (2) sulfate wood turpentine, recovered during the con version of wood to paper pulp by the sulfate process. Refined turpentine is the name for a commercially avail able grade that is produced by removing primarily sulfur compounds from sulfate wood turpentine. (4) destructively distilled wood turpentine, obtained by fractionation of certain oils recovered by condensing the vapors formed during the destructive distillation of pine wood. turpentines, various: Canada turpentine--Same as Canada balsam, the oleoresin obtained from trees of the Canadian silver fir (Abies balsamea). sulfite turpentine--this term is not in good usage, because the volatile oil recovered in the conversion of wood to pulp by the sulfite process consists chiefly of cymene (C10Hi4) rather than pinene and other terpenes. Venice turpentine--same as larch turpentine, the oleoresin of the European larch tree, Larix europea or Larix decidua. The term is also now used widely to describe the dear yellow liquid portion of pine oleoresin, or a synthetic product of similar composition made by dissolving rosin in a terpene solvent, turpentine substitute--this term is not recommended, be cause its use to describe a paint thinner of mineral oil origin is illegal under the U.S. Federal Naval Stores Act. 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 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 live years and knot revised, either reapproved or withdrawn. Your comments are Invited either for revision oi this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 131 DUP050295797 w i' Designation: D 856 - 48 (Reapproved 1987) Standard Test Methods for Sampling and Testing Pine Tars and Pine-Tar Oils1 This standard is issued undei- the fixed designation D 856; the number immediately following the designation indicates the year of original adoption pr, 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. The committee responsible for this standard has voted its withdrawal. In the absence ofsubstantial reasons that it should be continued, the Society will approve withdrawal from publication in March 1993. 1. Scope diameter of the container* so as to permit it to extend to the 1.1 These test methods Cover procedures for sampling and testing pine tars, both kiln and retort, and pine-tar oils, together with compounded tar products of naval stores origin. 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. bottom of the barrel or drum (thermal type of container) probe the tar at top and bottom, without too much agitation, to ascertain whether there is any appreciable quantity of water present. Remove as much of the water as possibly. Then insert the thief or probe rod to the bottom and stir the . tar up as much as possible. Rapidly raise then lower the rod eight or ten times, taking care to avoid pulling it out of the drum. In this way a layer of the tar and any accompanying water is brought onto the surface of the rod. Finally, quickly withdraw the rod and allow the adhering tar to flow into & bucket or other container in which a composite sample may 2. Referenced Documents 2.1 ASTM Standards: D 20 Test Method for Distillation of Road Tars12 D70 .Test Method for Specific Gravity of Semi-Solid Bituminous Materials3 D 88 Test Method for Saybolt Viscosity4 5 . D140 Practice for Sampling Bituminous Materials2 D270 Method of Sampling Petroleum and Petroleum Products? be collected. Repeat the procedure, taking two portions from each drum sampled. 3.3 Number ofDrums Sampled--In order to ascertain the ; average condition of a lot, at least 20 %, and if possible all of i the drums, shall be opened and examined. Take samples for further tests from at least 10 % of the drums, selecting those* drums which appear to be most representative of the general condition of the lot as indicated by the visual examination made as described in 3.2. D368 Test Method for Specific Gravity of Creosote and Oil-Type Preservatives6 E 1 Specification for ASTM Thermometers7 4. Preparation of Sample 4.1 Thoroughly stir and .agitate , the entire sample, prefer ably pouring it out into a large beaker .and stirring after first 3. Sampling 3.1 General Sampling Procedure--The material shall be sampled in accordance Math the applicable portions of Methods D 140 and D 270. 3.2 Kiln Pine Tar in Barrels or Drums--This type of tar may contain more than the small permissible quantity of stirring in the container. This is necessary to ensure complete mixing of any separated water or light oil and to obtain complete uniformity of sample. Strain through cheesecloth to remove any particles. All subsequent tests shall be made on portions taken after further thorough stirring of the sample. water usually present under good producing practice. The Vt water may be separated at the top, but it is not unusual to lli find it settled out at the bottom of the container, due to a high concentration of dissolved tar adds. (In good practice PHYSICAL TESTS CONDITION AND APPEARANCE most of this water should be removed at the point of production or preparation for shipment.) By means of a "thief' or a rod at least 1 ft (0.3 m) longer than the length or 5. Procedure 5.1 Flow a thin layer of the pine tar or pine-tar oil on a clear glass surface (as in a nartly filled glass container). Examine the film for suspen droplets of water and other 1 These test methods are under the jurisdiction of ASTM Committee D-l on foreign matter. Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO1.34 on Naval Stares. ' | Current edition approved Sept. 30,1949. Published November 1949. Originally COLOR published as D 856 - 45 T. Last previous edition D 856 - 46. 1 Annua/ Book ofASTM Standards, Vol 04.03. l: 3 Annual Book ofASTM Standards, Vols 04.03 and 04.08. 4 Annual Book ofASTM Standards, Vol 04.04. 5 Discontinued, see 1983 Annual Book ofASTM Standards, Vol 05.01. 6 Annual Book ofASTM Standards, Vol 04.09. 7 Annual Book ofASTM Standards, Vols 14.03 and 05.03. 6. Procedure 6.1 Rub out one drop of the pine tar or pine-tar oil between two sheets ofwhite writing paper. Observe the color of the resultant spot, along with that of the film of tar examined in accordance with Section 5. 132 i DUP050295798 1:--Clean tar has a bright golden or reddish brown color when in accordance with Section 6. SPECIFIC GRAVITY edure cific gravity of pine tar and pine-tar oil shall be as the ratio of the weight of a given volume of the at 25"C (ITT) to that ofan equal volume ofwater at ; (60*F) and shall be reported to the third decimal Specific gravity, 25/15.56`C. (77/60T).... The specific gravity may be determined at any conve oom temperature with a 25-mL Hubbard pycnometer ing bottle, as described in Method D 70, being sure Ithe weight of water contained by the pycnometer at iperature of the test. Since the specific gravity of pine pine-tar oil at room temperature changes by ~C change in temperature, add or subtract 0.0005 for degree that the temperature is, respectively, above or 25C. Finally convert such corrected value to the .56C basis by multiplying by the factor 0.998. As an alternative procedure, the specific gravity may ermined (somewhat less accurately) with a suitable pmeter, such as that described in Test Method D368. If 1 mperature of the tar is above or below 25C, correct the by means1 of the same value for change in specific that is 0,0005C. e 2--For very heavy viscous tars.it may be advantageous to the sample to 40 to, 45C, in which case the correction factor for ' `ng the observed reading of the hydrometer to 25"C will be '`a .. - VISCOSITY ypesofTest 1 For determining the viscosity of pine tars, the Stormer isimeter is recommended. The Saybolt Furol viscosimmay also be used to give close approximation of the Jute viscosity of pine tar, under the conditions set forth ..ow. Viscosity of pine tar shall be calculated and reported behtipbises. / Temperature of Tests ,% l Viscosity determinations shall be made either at 30C at 50C. For pine-tar oils, and for pine tars classified as Lin," the test shall be made at 30C, provided that when Stormer viscosity exceeds 180 s, or when the Saybolt "cl viscosity exceeds 360 s, the temperature of test shall be I For pine tars classified as "medium" or "heavy," the st shall be made at 50C. Stormer Method 10. Apparatus 10.1 The apparatus shall consist of a standard type ;5tormer viscosimeter (Fig. 1) equipped with the following: 10.1.1 Rotor, plated cylindrical (preferably gold-plated), 10.1.2 Test Cup (preferably gold-plated), with two side vanes, central baffle, and thermometer holder, 10.1.3 Weight--Weight box and sufficient shot for a total weight of 150 g, and FIG. 1 Stormer Viscosimeter with Cylindrical Rotor 10.1.4 Thermometer--An ASTM Stormer Viscosity Ther mometer having a range from 20 to 70C and conforming to the requirements for Thermometer 49"C as prescribed in Specification El. 11. Calibrationof Apparatus 11.1 Determine the values of factors K and a (see Section 13) for each instrument by making a series of preliminary runs with a suitable oil of which the absolute viscosities are known at several temperatures, following the procedure described in Section 12. Viscosity standard S-600 is suitable for this purpose.8 Having determined the average value of t for each temperature at which the absolute viscosity ofthe oil is known, substitute these values in the equation given in Section 13. Set the resulting equations down in pairs corresponding to each combination of temperatures, and solve the value of K for each such combination or pair of equations. From these data determine the average value ofK for the instrument. By substituting this value for K in the several pairs of equations, determine the two values for a for each pair of equations and then calculate the average value for the pair. From these averages calculate the mean value for a. No t e 3--For an instrument in good condition, a will usually be less than 1 s; therefore, if the correct value for a has not recently been determined, use 1.0 s as an assumed value for this factor. 11.2 After prolonged use of a viscosimeter on tar samples, the values of K and a should be checked by running another series of tests on a fresh portion of the standard oil. The - standard oil should be kept in a Ml or nearly full bottle, well stoppered and stored in a cool, dark place. 12. Procedure 12.1 Place the instrument on a horizontal shelf or table in 8Available from Cannon Instrument Co., P.O. Box 16, State College, PA 16801. 133 DUP050295799 # D 856 such a position that the weight may drop without obstruction through a sufficient distance (about 40 in.) to revolve the cylinder about 125 revolutions, as indicated by the pointer on the counter. Attach the rotating cylinder shaft to the instrument by pushing the shaft upward as far as it will go into the chuck, and secure it with the set screw. Fill the test cup with the sample until the latter is about 14 in. (6.3 mm) above the top of the vanes. Place the test cup in the water bath with the thermometer weil away from the upright support rod of the instrument, that is, to the left ofthe center when facing the counting dial. Raise the water bath with test cup until the contents of the latter covers the top ofthe rotor cylinder to such a depth that there is a stratum of liquid of equal thickness both above and below the rotating cylinder. Secure it in this position by tightening the set screw which engages one of the vertical supports. The. collar on the latter may be set to determine this position and assure its repetition in subsequent tests. 12.2 Place the thermometer in its position in the ther mometer well. Adjust the temperature ofthe sample as may be required by heating or cooling the bath. While the sample is being brought to the desired temperature, raise die operating weight so that it nearly touches the frame above it. Release the brake by a quarter turn ofthe milled head screw, thus revolving the cylinder and providing agitation of the sample. When sufficient time (longer time required for'more viscous samples) has been allowed for the temperature ofthe entire assembly of bath, cup, rotor, and sample to become uniform at the desired temperature, raise the weight to its starting position. With stopwatch in hand, release the brake and observe the motion of the pointer. After eight to ten revolutions have been made, time the next 100 revolutions. The temperature should be carefully controlled during this period. The average of several determinations shall be taken as the Stprmer viscosity in seconds per 100 revolutions for the instrument. 13. Calculation and Report 13.1 Convert the recorded or observed viscosity of the sample in seconds per 100 revolutions to absolute viscosity and report the value in centipoises calculated as follows: Absolute viscosity, cP = Km{t -- a) where: K = a constant or factor for the. apparatus, m = mass of the operating weight, g, t = time per 100 revolutions, s, and a = a time factor, to correct for mechanical friction in the apparatus. Saybolt Method 14. Procedure 14.1 Determine Saybolt viscosity in seconds with a Saybolt Furol viscosimeter in accordance with-Test Method D 88. Determine the density (not specific gravity) of the tar at the temperature oftest (a Hubbard specific gravity bottle is recommended). Convert the observed viscosity in seconds to absolute viscosity in centipoises as follows (Note 4): Absolute viscosity, cP = 2.13 tfd where; t = Saybolt Furol viscosity, s, / = a correction factor for the instrument. If a standard oil is used for calibration, having its viscosity stated in seconds for a standard instrument, this factor is equal to the ratio ofstandard seconds to observed seconds for the instrument used. If the viscosity is stated in centipoises, this value, with the observed time and the density of the oil shall be substituted in the above formula in order to calculate /for the instrument. The value of/should be calculated for both 30C and 50C. d = density of the sample at temperature of test. No t e 4--While the true Heischel formula for petroleum oils at 50C is C = [2.13/ -- (160//)] xdxf, experiments with pine tars indicate that results within the limit ofexperimental error, close enough for practical, purposes, and in good agreement with results obtained with the Stormef viscosimeter, may be expected by the use ofthe simpler formula given its Section 14. No t e 5--The Cannon Instrument Company's viscosity stands!#? S-600 is suitable for this purpose.8 ^ No t e 6--The value of/must be determined at both 30C and 50' DISTILLATION 15. Procedure 15.1 Determine the distillation range of pine tar pine-tar oils in accordance with Test Method D20. 15.2 Observe the total volume distilled at 170C, at 200*1 and the cumulative volume at each 25C interval thereaft When the maximum temperature to be read or stated in a* specification is indicated by the thermometer, or as soon as|p drop in temperature occurs before the maximum specified'* temperature is reached, discontinue the heating, allow the condenser to drain, and record the total quantity distilled to ;s that temperature. Record the maximum temperature % reached during the test if it is below the maximum tempera-*1 tore specified in the test. MOISTURE 'S 16. Apparatus 16.1 Flask, 500-mL short-neck, round-bottom with ii changeable ground-glass joint, standard 24/40 taper. 16.2 Trap to collect and measure condensed water return the condensed solvent to the flask. The trap shall a capacity of 10 mL and be graduated in 0.1-mL divisii The connections between trap and condenser and flask be interchangeable ground-glass joints, standard 24/40 16.3 Condenser, having a water jacket 400 mm in lei and interchangeable ground-glass joint for attachment to die trap, standard 24/40 taper. 17. Solvent 17.1 Xylene, or a petroleum solvent having a boiling ran such that not more than 5 % distills at 110*0 and not le$| than 90 % distills up to 150C. 18. Procedure 18.1 Weigh 200 g of the sample into a tared flask. Add} 100 mL of the solvent and attach the trap and condenser.*^ Heat the flask and reflux slowly at a rate of about 100 drops jf per minute. When most of the water has been trapped^ 134 DUP050295800 jfafl rate of reflux to 200 drops per minute and Ijliis rate until no more water is collected. During *|ig, wash down droplets ofwater which may collect "enser with 5-mL portions of solvent. Water in the d condenser may be made to separate by moving pper wire up and down. Reflux at least 1 h, shut off end of this period, and read the volume of water, the percentage of moisture, expressing the results 'ts. ASH atus Crucible or Dish, porcelain, silica, or quartz, having a of 50 to 60 mL. fi- edure v ^eat the crucible or dish, transfer to a desiccator, ' en cool, weigh to the nearest 0.0001 g. Place lately 20 g of the sample in the crucible or dish and the nearest 0.1 g. Heat gently with a gas flame and e sample, allowing it to bum completely. Bum offall On from the sides of the crucible or dish and finally | residue with a strong flame or in a muffle furnace (at 00C) until all carbonaceous matter disappears (Note r cooling in a desiccator, weigh the crucible or dish to st 0.0001 g. Repeat the heating until constant is obtained. Calculate the percentage of ash, ex- , the results in two digits. the latter undergoes the same color change in the transition from acid to alkaline solution, the 6 B indicator is,the one recommended for use in this test. 22. Calculation 22.1 Calculate the acid number, expressed in milligrams of KOH per gram, as follows: Acid number = (A x N x 56A)/W where: A = NaOH solution, mL, N = normality of the NaOH solution and W = sample, dry basis, g. VOLATILE ACIDS 23. Procedure 23.1 Transfer 10-g of the sample to a 500-mL, long-neck, round-bottom flask and add 125 mL of xylene and 10 mL of water. Connect the flask to a Liebig condenser and attach an adapter leading within about 1 in. (25.4 mm) of the bottom of a 250-mL widemouth Erlenmeyer flask containing 50 mL of distilled water. Distill slowly until about 75 to 80 mL of xylene has been collected. 23.2 Add 5 or 6 drops of phenolphthalein indicator and titrate with 0.1 N NaOH, shaking thoroughly after each addition. Calculate the percentage of volatile acids in terms of acetic acid. COPPER e 7--On account of the light fluffy nature ofthe ash from many extreme care must be taken to prevent particles of ash from blown out of the dish by drafts of air. It is advisable to cover the '"th a watch glass when it is removed from the flame or finance, hg the glass to remain until the dish is weighed. CHEMICAL ANALYSIS ACID NUMBER ^Procedure .1 In a small porcelain crucible or glass weighing Idle, accurately weigh 0.2 to 0.3 g of the sample. Place ; mL of alcohol (Formula 30 or other laboratory grade) in 50-mL widemouth Erlenmeyer flask, and add about 15 to ing of Alkali Blue 6 B (dry powder) (Note 8) from the end small spatula. The alcohol should take on a distinct blue br. Add 0.1 N NaOH solution dropwise until the color changes from blue to red. Introduce the crucible and pie and bring into solution by wanning on a hot plate. A ! e-green color will again develop. If the blue is masked by color of the tar, add additional indicator. Titrate with the ,aOH solution until no blue remains in the color of the lution when the flask is held at an angle against a white ckground. No t e 8--Alkali Blue 6 B for use as an indicator in this test is the dye ntified in the Color Index as No. 703, being the sodium salt of `phenylpararosanitine monosulfonic acid. A dye often sold as Alkali lue is Alkali Blue 4 B (Color Index No. 704), a mixture of the above jwith the sodium salt of diphenylrosaniline monosulfonic acid. Although 24. Procedure 24.1 Ash 50 g of the sample in a porcelain crucible or evaporating dish. Dissolve the ash in 15 mL of HN03 (1+3) and boil 5 min. Cool, add 25 mL of water, and filter off any insoluble matter. Add a slight excess of NH4OH (sp gr 0.90) and boil several minutes. Filter off the precipitate and wash with a few mL of warm water saving the filtrate. 24.2 Dissolve the precipitate in a few millilitres of HN03 (1+9). Bring to boiling, reprecipitate with NH4OH, and boil again. Filter and wash the precipitate, combining the fil trates. 24.3 Acidify the combined filtrates with H2S04 (1+5), add 5 mL of saturated bromine water, and boil off the excess bromine. Cool and add a slight excess of NH4OH. Boil to expel the excess NH4OH, acidify with 3 to 4 mL of acetic acid, boil for 1 min and cool to room temperature. 24.4 Add 10 mL of KI solution (300 g/L) and immedi ately titrate the liberated iodine with 0.02 N Na2S203, solution using starch indicator. 25. Calculation 25.1 Calculate the percentage of copper as follows: Copper, % = [(AN x 0.0636)/IP] x 100 where: + = Na2S203 solution required for titration, mL, N = normality of the Na2S203 solution, and W = sample used, g. 135 DUP050295801 D 856 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 Otis standard are expressly advised that determination of the validity of anysuch 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 if not revised, either reapproved orwithdrawn. Tourcomments are inviteid either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend. If you feel that your comments tmvenol received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ,t ,4 136 DUP050295802 Designation: D 889 - 58 (Reapproved 1987) Standard Test Method for Volatile Oil in Rosin1 This standard is issued under the fixed designation D 889; 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. pe This test method covers the determination of the oil content of rosin or similar material. The oil may of naturally occurring teipene oil, such as heavy as of turpentine, resulting from incomplete distillation processing of the rosin, or of foreign nonterpene oil g from incomplete removal of mineral or coal-tar' used to extract the rosin from wood or still wastes^ This standard may involve hazardous materials, oper > and equipment. This standard does not purport- to 'ss all ofthe safety problems associated with its use. It is sponsibility of the user of this standard to establish ipriate safety and health practices and determine the liability ofregulatory limitations prior to use. eferenced Document il ASTM Standard: 233 Methods of Sampling and Testing Turpentine2 pparatus .1 Flask, 500-mL round-bottom having a thermometer 11 and a 24/40 standard-taper ground joint for connection th the trap. .2 Trap (Fig. 1), designed so as to overcome the tendency droplets of oil to remain below the surface of the water, p to the greater viscosity of the volatile oils recovered from in, and thus be returned to the flask (Note 1 j. The trap II be fitted with 24/40 standard-taper ground joints to vide tight connections with the flask and condenser, in der to avoid vapor loss. No t e 1--This trap is a modification of the original Clevenger trap 1 to recover oils lighter than water. In that trap the Oil and water ndensate drop directly into the graduated part of the trap. Due to the 'scous character, density, and surface tension ofthe oils recovered from :sin, cylindrical columns of oil were formed below the surface of the rater in the graduated section of the trap, which were not penetrated by : water condensed immediately thereafter. This resulted in alternate columns of oil and water in the graduated section. These were returned to the distilling flask in the same order as they occurred, through the side arm of the trap. As this condition continued indefinitely, it was impossible to completely remove all the oil from the rosin. By raising the opening of the side arm of the trap to the position shown, to bring the Surface of the liquid into the wide part of the trap above the narrow graduated section, the oil is collected in a thinner film that can be 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 1.34 on Naval Stores. Current edition approved Sept. 22, 1958. Published November 1958. Originally published as D 889 - 46. Last previous edition D 889 - 50. 2 Annual Book ofASTM Standards. Vol 06.03. penetrated readily by the droplets of water falling from the end of the condenser, and only the water is thus collected in the narrow graduated section. At the end of the test, the oil is slowly brought down into the graduated section and its volume read. The system or apparatus loss amounts to not more than 0.1 mL of oil. 3.3 Condenser, straight-tube, 300-mm, water-jacketed reflux type, with a 24/40 standard-taper ground joint for connection with the trap. 3.4 Heat Source--An oil bath containing high-tempera ture-resistant oil, or an electric heater of the mantle type in which the heating elements are encased in a glass cloth mantle of such shape as to partially or completely surround the flask being heated. 4. Procedure 4.1 Place 50 g ofthe crushed sample in the flask, add 125 mL of a glycerin-water solution (4+1), insert an ebullition tube, and connect the flask with the trap. Fill the trap (Fig. 1) with water through the top opening until the water level is even with the bottom of the seal of the small return tube to the side arm. Place some mercury in the thermometer well, insert the thermometer, and connect the condenser. 4.2 Regulate the applied heat until the liquid in the flask is brought to a boil and distillation continues at a constant temperature, which will be about 125C at the start. At this stage, open the stopcock slightly and withdraw the water from the trap into a small graduated cylinder at the rate of 1 drop to 5 drops off the lower end of the condenser. Control the reflux rate so that no uncondensed vapors escape from the top 6f the condenser. The withdrawal of water from the system should be at the rate ofabout 1 mL/min. Increase the heat from time to time to maintain uniform continuous operation with slowly rising temperature. Discontinue the distillation when the temperature reaches 180C. 4.3 Remove the source of heat and allow the distillation to subside (Note 2). Draw offwater until all the oil is brought into the graduated section of the trap and note the volume. The density of the oil is usually very close to 1.00. No t e 2--The contents of the flask should be poured out while still warm, before the rosin has become viscous or solid, to facilitate cleaning and avoid strain on the glass when the rosin becomes cold. 5. Report 5.1 Properly made rosin yields not more than 0.5 mL of residual volatile oil per 50 g of sample. If the recovered oil is within such limit, report the rosin as free of excess volatile oil. If more than 0.5 mL of oil is recovered, report the total volume obtained. No t e 3--The volatile oil recovered from gum rosin consists prima rily of high-boiling terpene components of the crude gum, most of which under proper distillation will have been recovered as turpentine by the time the rosin is drawn from the still. Faulty distillation or premature 137 DUP050295803 D 889 withdrawal may yield a roan giving a higher than normal recovery ofoil, with a refractive index below 1.483. The polymerization residue should have a refractive index not lower than t.500. In the case ofwood rosins, generally obtained by extraction from stumpwood with a petroleum or naphtha solvent, any recovered oil would probably consist of unrecovered solvent. The refractive index of both the recovered oil and the polymerization residue therefrom would be well under the above figures for gum rosin. 6. Additional Examination of Oil 6.1 Drain off the water, transfer the oil to a small gla^ container, stopper, and allow to settle until clear. Note the odor and taste and determine the refractive index. For further information on the nature of the oil, volume permit ting, make a polymerization test according to the procedure given in Methods D 233. BOTTOM OF SEAL OF SMALL RETURN TUBE TO BE AT OR " SLIGHTLY ABOVE STARTOF TAPER OF THE LARGE TUBE. FIG. 1 Trap The American Society for Testing and Materials takes no position respecting trie 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 technicalcommittee and must be reviewed every five years and ifnotrevised, either reapproved or withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, 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. 138 DUP050295804 signation: D 890 - 58 (Reapproved 1987) Standard Test Method for Water in Liquid Naval Stores*1 This standard is issued under the fixed designation D 890; 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. test method covers the quantitative determinaolved or occluded water present in any proportion plored, liquid naval stores, such as turpentine, idipentene, or pine oil. It is based on the reaction water and a complex reagent2 consisting of iodine, "oxide, pyridine, and methanol, whereby the iodine is to a colorless compound. The appearance of a ' t iodine color in the reaction mixture indicates the te removal of free water by reaction with the reagent. T--The Karl Fischer reagent prescribed in`this test method is . in two solutions, in which form it is metre stable and. less :by atmospheric moisture. However, the single solution reagent f in Test Methods D 1364 and Method D 1123 may be used if it `readily available. The solvents and proportions specified in this od should be employed if the single solution reagent is used. This standard may involve hazardous materials, oper and equipment. This standard does not purport to 2s all ofthe safety problems associated with its use. It is esponsibility of the user of this standard to establish yiaxe safety and health practices and determine the friability ofregulatory limitations prior to use. ferenced Documents 1 ASTM Standards: ,1123 Test Method for Water in Engine Coolant ConcenJ trate by the Karl Fischer Reagent Method3 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)4 . Reagents jX 1 lodine-Pyridine-Sulfur Dioxide Reagent: ,s3.1.1 Solution 1--Transfer 450 mL of anhydrous pyridine d 450 mL of anhydrous methanol to a 1-L Erlenmeyer ak. Stopper and weigh. Cool in an ice bath to about 4C, nd add 90 g of S02 at a fairly rapid rate. The temperature J&hould be kept low; if necessary, periodically interrupt the t: 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 D01.34 on Naval Stores. Current edition approved Sept. 22, 1958. Published November 1958. Originally published as D 890 - 1946. Last previous edition D 890 - 51. 2 This procedure has been adapted from the method of Kari Fischer published in Zeilschrift fur Angewcmdle Chemie, Vol 48, 1935, p. 395; Chemical Abstracts, Vol 29, 1935, p. 6532; as modified by Smith, Bryant, and Mitchell, Journal, Am. Chemical Soc., Vol. 61, 1939, p. 2407; and further modified by Axel Johansson, Svensk Papperstidning, Vol 50, No. 1 IB, 1947, p. 124; see also Publication 19 of the Swedish Wood Research Institute, Wood Chemistry and Paper Technique (Stockholm) (1947). 3 Annual Book ofASTM Standards, Vol 15.05. 4 Annual Book ofASTM Standards, Vol 06.03. addition of SOz and allow the solution to cool. If liquefied S02 is not available, pass dry S02 (dried by passing through H2S04 (sp gr 1.84)) into the mixture from a tank or generator until the weight (Note 2) ofthe solution in the flask has been increased by the prescribed amount. The required quantity of S02 may be generated by treating 160 g of NaHS03 or 190 g of Na2S03 (10 % more than the theoretical amount) with H2S04 (sp gr 1.84) in a simple generator fitted with a dropping funnel. Gentle heating will help to bring about continued reaction after each addition of the acid seems to have spent itself. Store the solution in a brown glass bottle having a tightly fitting ground-glass stopper. No t e 2--The term "weight" is temporarily used in this standard because Of established trade usage. The word is used to mean both "force" and "mass," and care must be taken to determine which is meant in each case (SI unit for force = newton and for mass = kilogram)." 3.1.2 Solution 2--Transfer 60 g of chemically pure iodine to a 250-mL Erlenmeyer flask. Add 125 mL of anhydrous methanol, stir, allow to settle, and decant into a 1-L volumetric flask. Repeat this operation with successive portions of methanol until all the iodine is dissolved and transferred. Finally add sufficient methanol to make a total of 1 L. Mix the solution and preserve in a brown glass bottle with tightly fitting ground-glass stopper. Transfer portions of Solutions 1 and 2 as needed to 50-mL burets equipped with drying tubes. 3.2 Methanol, Anhydrous--Anhydrous methanol con forming to the specifications of the American Chemical Society shall be used. The moisture content shall not exceed 0.1 %. 3.3 Methanol-Water, Standard Solution--From a weigh ing pipet, weigh 1.5 to 2.0 g of water into a 1-L volumetric flask and fill to the mark with anhydrous methanol. Mix thoroughly and keep the flask tightly stoppered. 3.4 Pyridine, Anhydrous--Allow 1 L of reagent-grade pyridine to stand for several days over 100 g of BaO (or 150 g of CaO) in a tightly stoppered flask, with occasional shaking. Filter off the dry agent and redistill, rejecting the first 30 mL. Preserve in a dark-colored bottle with tightly fitting glass stopper. 4. Standardization of Iodine Reagent 4.1 Draw off from the buret into a titration flask, 15 mL of Solution 1. Immediately add from the other buret a quantity of Solution 2 until the lemon-yellow color changes to a red-brown color. (Mechanical agitation during titration is preferred.) Add to this solution 10 mL of the standard ethanol-water solution from a pipet and again titrate with Solution 2 until the red-brown color just appears. Record the millilitres of Solution 2 required to titrate the standard 139 DUP050295805 methanol-water solution that was added. Duplicate determi nations should check within 0.2 mL. No t e 3--Alternative Titration--The end point may be determined electrometrically by means of the apparatus and procedure described in 3.1 of Method D 1364. 4.2 In the same way, titrate 10-mL portions of the anhydrous methanol used in preparing the standard metha nol-water solution. Duplicate titrations should agree within 0.1 mL. 4.3 Calculate the water equivalent of the iodine reagent, in grams of water per millilitre Of reagent, as follows: A=WJ(.T-B) where: ' 1 A =' water equivalent of the iodine reagent, g/mL, Wa - grams of weighed water present in 10 mL of the standard methanol-water solution, c T = millilitres of iodine reagenf (Solution 2) required for titration of 10 mL of the standard methanol-water > solution, and ; . .. B ' = millilitres of iodine recent (Solution 2) required for titration of 10 mL1 Of absolute methanol. ' '` . 4.4 Haying determined the water equivalent of the iodine solution, calculate the total water content, in grams, of 10 mL ofthe standard methanol-water solution (3.4) as follows: W, = Tx A *' where: Wt = total water, in grams, in each 10 mL of the methanol- water solution, and rand A = same values as in 4.3. This yalue can be used in standardizing the iodine reagent (before each day's use) rherely by titrating lp-mL portions of the standard methanol-water solution. 5. Procedure for Hydrocarbon Oils 5.1 Withdraw 25 mL of Solution 1 into a titration flask and add ,80 mL of a one-to-one mixture of benzene and methanol. Titrate with Solution 2 until the lemon-yellow*! color changes to a red-brown, or alternatively to an electrometric end point. Stopper and weigh the flask. Add 50 mL (or an amount that will contain 50 mg or less ofwater) of the saimpie to be tested into* the flask, stopper, and reweigh. Titrate with Solution 2 until the red-brown color just appears. Record the millilitres of Solution 2 required to titrate the water in the sample. Duplicate determinations should check within 0.2 mL. 5.2 Calculation--Calculate the percentage of water as follows: Water, % = (Tx A x 100)/G . where: T = millilitres of iodine reagent (Solution 2) required for titration of the sample, A = water equivalent of the iodine reagent, and G = grams of sample used. 5.3 Duplicate tests should check within 0.002 % of water.1! 6. Procedure for Pine Oil < 6.1 Withdraw 15 mL of Solution 1 info a titration flask arid add 20 mL ofmethanol. Titrate with Solution 2 until the! leinon-yellow color changes to a red-brown, or alternatively, to an electrometric end point. Stopper the flask and weigh. Add 10 mL (dr an amount that will contain 50 mg or less of water) of the pine oil to the flask, stopper, and reweigh,' Titrate with Solution 2 until the red-brown color just appears. Record the millilitres of Solution 2 required to titrate the water , in the sample. Duplicate determinations should check within 0.2 mL. 6.2 Calculation--Calculate the percentage of water as directed in Section 5.2. 6.3 Duplicate tests should check within 0.005 % of water. The American Society for Testing and Materials takes ho 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 bythe responsible technical committee and must be reviewed every five years and ifnot rey/sed, eitherreapproved or withdrawn. Youroommente are invited eitherforrevision ofthis standardor 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 attend1.- If \rou 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, 140 DUP050295806 gnation: D 960 - 79 {Reapproved 1988) Standard Specification for Raw Castor Oil1 This,standard is issued under the fixed designation D 960; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. i specification covers castor oil suitable for use in : protective coatings, including iacquers. This is Own ib the trade as No. 1 castor oil. ced Documents TM Standards: [Guide for Testing Drying Oils2 Test Method for Sampling Liquid Oils and Fatty sCommonly Used in Paints, Varnishes, and ReMaterials2 Test Method for Color of Transparent Liquids -dner Color Scale)3 i Test Method for Viscosity of Transparent Liquids l^ubble Time Method3 39 Test Method for Acid Value of Organic Coating ierials4 7 Test Method for Hydroxyl Value ofFatty Oils and *&S2 9'Test Method for Iodine Value of Drying Oils and tty Acids2 969 Test Method for Loss on Heating of Drying Oils2 "62 Test Method for Saponification Value of Drying ils, Fatty Adds, and Polymerized Fatty Acids2 965 Test Method for Unsaponifiable Matter in Drying .ils, Fatty Acids, and Polymerized Fatty Acids2 090 Test Method for Clarity and Cleanness of Paint and Ink Liquidss is specification is under the jurisdiction ofASTM Committee D-l on Paint "ted Coatings and Materials and is the direct responsibility of Subcoms DO).32 on Drying Oils, urrent edition approved Oct. 29, 1979. Published January 1980. Originally ished as D 960 - 63 T. Last previous edition D 960 - 73. . Annual Book ofASTM Standards, Vol 06.03. f Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. * Annual Book ofASTM Standards, Vol 06.01. is Annual Book ofASTM Standards, Vols 06.02 and 06.03. 3. Properties 3.1 Castor oil shall conform to the requirements given in Table 1. 4. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance with the ASTM test methods listed in Table 1. 5. Sampling 5.1 Sampling shall be conducted in accordance with Test Method D 1466. 6. Significance and Use 6.L The significance of the test methods enumerated under Section 2 of this specification is discussed in Guide D555. TABLE 1 Properties of Castor Oil Property Requirement ASTM Test . Method Add value, max Clarity Color (Gardner), max Hydroxyl value Loss on heating, max, % Refractive index, 25C Saponification value Solubility in alcohol'4 Specific gravity. 25/25C Unsaponifiable. max. % Viscosity. St iodine value 2.0 clear 2 160 to 168 0.3 1.4764 to 1.4778 176 to 184 complete 0.957 to 0.961 0.7 6.3 to 8.9 83 to 88 D1639 D 2090 D1544 D1957 D1960 01962 D1963 D1965 D1545 D 1959 A Castor oil shall be completely soluble without turbidity at 20c in two volumes of specifically denatured alcohol (95 36) conforming to Formula 3A of U. S. Bureau of Alcohol, Tobacco, and Firearms. 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 forrevision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 141 DUP050295807 Designation: D 961 - 86 (Reapproved 1990) Standard Specification for Dehydrated Castor Oil1 This standard is issued under the fixed designation D 961; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapprovai. 1. Scope 1.1 This specification covers a drying oil made from castor oil that has been treated to remove the elements of water. Two types of dehydrated castor oil are covered: unbodied and Z-3 bodied. No t e--Other types of bodiedl dehydrated castor oil are commercially available but are not covered by this specification. 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)2 D 555 Guide for Testing Drying Oils3 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products'4 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 142 D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method5 D 1639 Test Method for Acid Value of Organic Coating Materials4 D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature4 D1955 Test Method for Gel Time of Drying Oils3 , 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 D 01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 961 -48T. Last previous edition D961 -80. 2 Annual Book ofASTM Standards, VoJ 05.01. 3 Annual Book ofASTM Standards, V6106;03. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. D1959 Test Method for Iodine Value of Drying Oils and* Fatty Acids3 D1962 Test Method for Saponification Value of Drying, Oils, Fatty Acids, and Polymerized Fatty Acids3 D1963 Test Method for Specific Gravity of Drying Oils, : Varnishes, Resins, and Related Materials at 25/25C 3 t D2090 Test Method for Clarity and Cleanness of Paint, and Ink Liquids6 E 1 Specification for ASTM Thermometers7 3. Properties 3.1 Dehydrated castor oil shall conform to the require ments prescribed in Table 1. ' 4. Test Methods 4.1 The properties enumerated in this specification shall be deteririined in accordance with the appropriate methods given in Table 1 with the following exceptions: 4.1.1 Gel Time--Determine the gel time in accordance with Test Method D 1955 but with the following changes; 4.1.1.1 Use an ASTM Partial Immersion Thermometer having a range from 20 to 760F and conforming to the requirements for Thermometer 3F as prescribed in Specifi cation El. 4.1.1.2 Heat the bath to 600 1F (315 0.5C) , insert the tubes containing the oil in the bath, maintain the bath at 600 1F for the duration of the test, and 4.1.1.3 Raise the glass rods a fraction of an inch at 1-min intervals after 125 min in the case ofthe unbodied oil or after 25 min in the case of the bodied oil. 4.1.2 Iodine Value--Use the procedure described in Method D 1959, to determine the iodine value, except that the specimen weights shall be 0.11 to 0.13 g of oil. 4.2 The significance of and comments on the referenced methods are discussed in Guide D 555. * Annual Book ofASTM Standards, Vols 06.02 and 06.03. ''Annual Book ofASTM Standards, Vol 14.Q3. Viscosity at 25C Specific gravity. 25/25C Add value, max Saponification value Iodine value (Wijs) Color No. (Gardner), max Gel time at 600F (315C), min Set-to-touch time, h Refractive index at 25C Clarity TABLE 1 Requirements for Dehydrated Castor Oil UnbocSed Bodied Ftol 0.926 to 0.937 6 188 to 195 125 to 145 6 145, approximately 2.5, approximately 1.4805 to 1.4825 clear and transparent at 25C Z2 to Z4 0.944 to 0.966 6 188 to 195 100 min 7S3, approximately 1.4, approximately 1.4860 to 1.4890 clear and transparent at 25C ASTM Method D 1545, D 445 D 1963, D 1475 D 1639 D1962 D 1959 D 1544 D 1955 D 1640 D 2090 142 DUP050295808 # D 961 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 entirety their own responsibility. This standard is subject to revision atarty time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Yourcomments are invited either for revision 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, 1918 Race Sf., Philadelphia, PA 19103.143 143 DUP050295809 Designation: D 1007 - 90 Standard Specification for sec-Butyi Alcohol1,2 This standard is issued under the fixed designation D 1007; 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 specification covers .sec-butyl alcohol for use in PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 paint, varnish, lacquer, and related products. 1.2 This standard does not purport to address all of the 3, Properties 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 Section 4. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: 3.1 scc-Butyl alcohol shall conform to the following requirements: Apparent specific gravity: 20/20*C 25/25-C Color, Pt-Co scale, max Distillation range, 760 mmHg, C as: Initial boiling point, min Dry point, max Nonvolatile matter, max, mg/100 mL Odor Water, max, weight % Acidity, as acetic acid, max, weight % 0.807 to 0.809 0.804 to 0.806 10 98.0 101.0 5 nonresidual 0.5A 0.002* D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 A This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20"C. * Equivalent to 0.019 mg of KOH per gram of sample. D1078 Test Method for Distillation Range of Volatile Organic Liquids3 4. Hazards D1209 Test Method for Color of Clear Liquids (Platinum- 4.1 scc-Butyl alcohol is a flammable liquid. Its vapors can Cobalt Scale)3 form explosive mixtures with air. Repeated or prolonged D1296 Test Method for Odor of Volatile Solvents and contact may cause drying of the skin. Diluents3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re 5. Sampling '1 J f! lated Products3 D1364 Test Method for Water in Volatile Solvents 5.1 The material shall be sampled in accordance with Practice E 300. (Fischer Reagent Titration Method)3 D 1476 Test Method for Heptane Miscibility of Lacquer 6. Test Methods Solvents3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 6.1.1 Apparent Specific Gravity--Determine the apparent specific gravity at 20 or 25C by a convenient method that is accurate to the third decimal place. See Methods D 268 or Test Method D 4052. E 300 Practice for Sampling Industrial Chemicals6 6.1.2 Color--Test Method D 1209. 2.2 U.S. Federal Specification: 6.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 40C, having a range from 72 to 126C and conforming to the 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 DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1007 - 49 T. Last previous edition D 1007 - 85. 2 This compound is also known under the names 2-butanol and secondary butanol. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 05.03. 5 Annual Book ofASTM Standards, Vol 14.03. 6 Annual Book ofASTM Standards, Vols 06.03 and 15.05. in Specification E 1. 6.1.4 Nonvolatile Matter--Test Method D 1353. 6.1.5 Odor--Test Method D 1296. 6.1.6 Water--Test Methods D 1364 and D 1476. 6.1.7 Acidity--Test Method D 1613. 7Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 144 DUP050295810 D 1007 llkaging and Package Marking i Package size shall be agreed upon between the pur- |r and the supplier. Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 8. Keywords 8.1 rec-butyl alcohol The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Hem ihentioned Inthls 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 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 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 ASfM Committee on Standards, 191S Race St., Philadelphia, PA 19103. 145 DUP050295811 (Jj jM Designation: D 1063 - 51 (Reapproved 1987) Standard Test Method for Ash in Rosin1 This standard is issued under the fixed designation D 1063;the number immediately following the designation indicates the year of original adoption o j t , 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. The committee responsible forthis standard has voted its withdrawal. In the absence of substantial reasons that it should be continued, the Society will approve withdrawal from publication in March 1993. 1. Scope 1.1 This method covers the determination of the nonvol atile matter remaining after a sample of rosin is completely burned and ignited.1 2. Procedure 2.1 Ignite a platinum or other heat-resistant dish (por celain, quartz, silica) having a capacity of 50 to 100 ml, cool in a desiccator, and weigh to the nearest 0.0001 g. 2.2 Weigh 20.0 g, to the nearest 0.1 g, of rosin into the dish. Place it on a ring-stand close under a flue pipe in a hood and heat gently with a bunsen burner until the rosin can be ignited at the surface. (Rosin bums with an extremely 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D0I.34 on Naval Stores. Current edition approved Sept. 30, 1951. Originally issued 1949. Replaces D 1063 - 49 T. smoky flame and the smoke must be carried off through the flue.) Remove the burner and sallow the rosin to bum completely, reheating from timeUo- time to bring about a continuous combustion. When the'flame finally dies out, remove the dish from under the flue and bum offas much of the carbon residue with the burner as can be so removed. Stir the contents of the dish once or twice with a fine platinum or nichrome wire to break up any sintered carbon residue. 2.3 Place the dish in a muffle furnace, preferably electrv*| cally heated, at a temperature of about 250C, and raise the y temperature slowly to 500C. Maintain the temperature at i 500 to 550C until all carbonaceous matter has been ^ consumed. Remove the dish from the furnace to a desio cator, covering at once with a wanned watch glass to prevent^ air currents from carrying off any of the light, fluffy ash, ^ Allow to cool to room temperature and weigh to the nearest 0.0001 g. , 2.4 Calculate the percentage of ash to the nearest 0.01 9<. i TheAmerican Society for Testing and Materials takes no position respecting the validity ofany pstentrights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnotrevised, eitherreapproved or withdrawn. Your comments are invited either forrevision ofthis standardor toradditionalstandards f.I 1 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. 146 J DUP050295812 'Designation: D 1064 - 58 (Reapproved 1981) te' i stanc|ar(| Test Methods for Iron in Rosin1 This standard is issued under the fixed designation D 1064; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision, A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These methods have been approvedfor use byagencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. ' |ese test methods cover colorimetric procedures for ination of iron in rosin. Both spectrophotometric Hi) methods are covered. ents urity ofReagents--Reagent grade chemicals shall be pIM tests. Unless otherwise indicated, it is intended f reagents shall conform to the specifications of the ee on Analytical Reagents of the American Chemliety, where such specifications are available.2 Other iay.be used, provided it is first ascertained that the of sufficiently high purity to permit its use without the accuracy of the determination, references to water in these methods shall be Stood to mean distilled water. SPECTROPHOTOMETRIC METHOD iiciple of Method gjjiJFerrous iron, in a dilute hydrochloric acid solution, i a red-colored complex with 1,10-phenanthroline. The fjisity of the color is measured at approximately 503 nm leans of a photoelectric photometer. fr|pparatus Photometer--Any photoelectric spectrophotometer or photometer that will measure accurately the transmiti of the solutions in the range from 500 to 520 nm. Dishes, high-silica glass,3 silica, or porcelain, 50 and *mL capacity. |o t e 1--Platinum or platinum-rhodium dishes are not recom as they sometimes cause a color interference with the nthroline reagent 5.3 Watch Glasses, to cover the dishes described in 4.2. 4.4 Pipets--One 100-mL, two 10-mL, three 5-mL, and 12-mL pipets. These test methods are under the jurisdiction of ASTM Committee D-! on aint and Related Coatings and Materials and are the direct responsibility of Ubcommittee D01.34 on Naval Stores. Current edition approved Sept. 22, 1958. Published November 1958. Originally jjblished as D 1064 - 49. Last previous edition D 1064 - 51. 2 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemal Soc., Washington, DC. For suggestions on the testing of reagents not listed by he American Chemical Society, see "Reagent Chemicals and Standards," by oseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States 'harmacopeia." 1 Vycor has been found satisfactory tor this purpose. 4.5 Measuring Pipet, Mohr-type, 10-mL. 4.6 Volumetric Flasks, 1-L and 50-mL capacities. 4.7 Absorption Cells, having a capacity of at least 25 mL. Smaller cells may be used when the color is developed in a flask or beaker. 5. Reagents 5.1 Hydrochloric Acid (1+19)--Dilute 1 volume of HC1 (sp gr 1.19) with 19 volumes of water. 5.2 Hydroquinone Solution--Dissolve 2.5 g of hydroquinone, reagent or photographic grade, in 100 mL of HC1 (1+200). Keep in a refrigerator at about 10C when not in use. 5.3 Hydroxylamine Hydrochloride Solution--Dissolve 10 g of hydroxylamine hydrochloride in 190 mL of water. This reagent is stable at room temperature. 5.4 Iron Solution, Standard (1 mL = 0.1 mg Fe)--Dissolve 0.1000 g of pure iron wife (99,85 % iron) in 10 mL of H2S04 (1+9) and 3 mL of HN03 (sp gr 1.42), Dilute with water to 1 L in a volumetric flask. 5.5 Iron Solution, Standard (1 mL = 0.01 mg Fe)--Pipet 100 mL of standard iron solution (1 mL = 0.1 mg Fe) into a 1-L volumetric flask and dilute to the mark with HC1 (1+19). 5.6 1,10-Phenanthroline Solution--Dissolve 0.5 g of 1,10phenanthroline in 500 mL of water. 5.7 Sodium Acetate Solution--Dissolve 100 g of NaC2H302 3H20 in 400 mL of water. 6. Preparation of Calibration Curve 6.1 Pipet 0.5, 1.0, 2.0, 3.0, 4.0, and 5.0-mL aliquots of standard iron solution (1 mL = 0.01 mg Fe) into absorption cells and dilute to 10 mL with HC1 (1+19) measured with a Mohr-type pipet. Add 10 mL of HC1 (1+19) to an additional absorption cell and carry through as a reagent blank. 6.2 Develop color in the solutions as described in 7.4. 6.3 Measure the transmittance of the solution at approxi mately 503 nm with the spectrophotometer adjusted to read 100 % transmittance for the reagent blank. . 6.4 Using semilogarithmic paper, plot the percentage transmittance of the solutions against milligrams of iron present. 7. Procedure 7.1 Weigh 5.00 g of the sample into a high-silica glass, silica, or porcelain dish. If the iron content is less than 5 ppm, use a weight of sample such that the solution on which the spectrophotometer reading is made will contain from 0.05 to 0.050 mg of iron. 147 DUP050295813 # D 1064 7.2 Place the dish in an electrically heated muffle furnace and raise the temperature slowly until the sample is com pletely charred. Then raise the temperature to 500C and maintain at 500 to 550C until the sample is greyish white. This usually required 4 to 6 h, but no harm will be done if the sample is allowed to remain in the muffle overnight. Remove the dish from the muffle furnace, cool to room temperature, and add 5 mL of HC1 (1+1) in such a manner that any ash on the sides of the dish is washed to the bottom. Cover the dish with a watch glass and heat just to boiling. 7.3 Transfer the sample to a 50-mL volumetric flask, using water to wash the last trace from the dish and watch glass Dilute to the mark with water and mix thoroughly. 7.4 Pipet 10 mL of the solution into an absorption cell (Note 1). When the iron content is too high to be read from the calibration curve, take a smaller aliquot and dilute to 10 ml. with water. Add 2 mL of hydroxylamine hydrochloride or hydroquinone solution, 5 mL of 1,10-phenanthroline solution, and 5 mL of sodium acetate solution, using volumetric pipets. Mix thoroughly after each addition. No t e 1--When 25-mL absorption cells are not available for the spectrophotometer, develop color as described in 7.4, but in a flask, beaker, or large test tube, and'transfer an aliquot of the solution to a suitable absorption cell. 7.5 Blank--Run a blank along with the sample to be sure none of the reagents have become contaminated (Note 2) and for a reference solution against which the transmittance of the sample is measured. Measure the transmittance of the blank with the spectrophotometer adjusted to read 100% transmittance at a wave length between 500 and 550. nm when the absorption cell contains water. No t e 2--When the reagents contain more than 0.002 or 0.003 mg-of iron, prepare new reagents and look for.the source of contamination. 7.6 Measure the transmittance of the sample solution at approximately 503 nm with the spectrophotometer adjusted to read 100 % for the blank. Read the iron content of the sample solution in milligrams from the calibration curve. 7.7 Calculation^-Calculate the iron content ofthe sample in parts per million as follows: Iron, ppm = (A/B) x 1000 where: A ?= milligrams of iron found, and B = grams of sample represented in the aliquot used. 7.8 Check Determination--Make a single determination daily using 1 to 5 mL of standard iron solution (1 mL = 0.01 mg Fe) and proceeding as directed in 6.1 and 6.2. If the determined and known values do not agree within the limits of experimental error (1 % transmittance) repeat the test. If the second results do not agree, prepare a new standard solution. If determined and known values do not check after preparing a new standard, investigate for errors in techique and reagents, and if none can be found, prepare a new calibration curve. This should not be necessary, and all other factors should be thoroughly investigated before doing this. VISUAL METHOD 8. Principle of Method .8.1 Ferrous iron, in a dilute hydrochloric acid solution, ! forms a red-colored complex with 1,10-phenanthroline. TheU intensity of the color is compared visually in matched! Nessler tubes against reference color standards containing!! known amounts of iron, in which color has been developed in the same manner.. | 9. Apparatus - :S 9.1 Nessler Tubes--For visual comparison of colors, matched 50-mL Nessler tubes shall be used. ; 10. Reagents J 10.1 See Section 5i. . `flf 11. Preparation of Reference Color Standards ,3 11.1 Pipeti 0.5, 1.0, .1.5, 2.0, 2.5, and 3.0-mL aliquots oft standard iron solution (1 mL;= 0.01 mg Fe) into 50-ttffl matched Nessler tubes. Dilute to 10 mL with HC1 (1+19)1 measured with a Mohr-type pipet. Add 10 mL ofHQ (1+19)1 to an additional 50-mL Nessler tube and carry through as al reagent blank. , iff 11.2 Develop the iron color as directed in 12.2. A set slj standards may be kept for 2 to 3 weeks if the Nessler tubes| are stoppered. During this period the standards shall tjef| checked daily, or whenever tests are made, by preparing i single fresh standard and comparing it with the one of t same concentration in the series. Use a different concent: tion of iron each time the standards are checked. When 1 do not check, a new series of standards shall be prepared. 12. Procedure 12.1 Proceed as directed in 7.1 through 7.3. 12.2 Pipet 10 mL of the solution into a 50-mL Ne tube. When the iron content is too high for accurate vis comparison, reduce the size of the aliquot. Add 2 mL * hydroxylamine hydrochloride or hydroquinone solutic mL of 1,10-phenanthroline solution, and 5 mL of sodiu acetate solution, using volumetric pipets. Mix thoroug after each addition. Dilute to 50 mL with water and thoroughly. 12.3 Compare the resultant color with standards prepared, as directed in Section 11. Estimate the iron content to tbs nearest milligram and calculate the iron present as describ in 7.7. The American Society for Testing amt Materials takes no position respecting the validity Many 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 live years and ifnot revised, eitherreapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 148 y*9r<nt DUP050295814 designation: D 1065 - 62 Standard Test Methods for Unsaponifiable Matter in Rosin1 . This standard is issued under thei fixed designation D 1065; 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 in editorial change since the last revision or reapproval pese methods are intended fpr determining the : of material in rosin, other than insoluble dirt or visible foreign matter, that does not yield a liable soap when the rosin is saponified with potasroxide. Two methods are covered, as follows: iethod A--Continuous Extraction, and ^'Method B--Extraction by Means of a Separatory He both methods may be expected to give fairly ant results. Method A, using the continuous exobe, shall be used as the referee method in case of a aent in the results obtained by different analysts. |ty of Reagents leagent grade chemicals shall be used in all tests, j otherwise indicated, it is intended that all reagents |onform to the specifications of the Committee on Seal Reagents of the American Chemical Society, liich specifications are available.2 Other grades may be pvided it is first ascertained that the reagent is of litly high purity to permit its use without lessening the ' of the determination. Unless otherwise indicated, references to water shall iderstood to mean distilled water. I Separation of Sample The sample taken for analysis shall consist of small : of rosin chipped from a freshly exposed part of a lump aps, and thereafter crushed to facilitate weighing and pion. The sample shall be so prepared the same day on the test is begun, in order to avoid changes in ties due. to surface oxidation, that is very pronounced pound rosin having a large surface area exposed to the 250-mL capacity, withstandard-taper 24/40 joint. 4.2 Erlenmeyer Flask, 300-mL capacity, with wide mouth. 4.3 Extractor Tube--A special extractor tube (Fig. 1) 420 mm in length, with a side tube 220 mm above the bottom. The bottom qf the side tube and tfie top of the extractor tube shall be fitted with standard-taper 24/40 joints. The extractor tube should have a permanent mark at the 50-mL level! 4.4 Conductor Tube, 350 mm in length (Fig. 1), for conducting condensed solvent to the bottom of the extractor tube. The top shall be flared to funnel shape .and the bottom perforated with'three 1-mm holes. 4.5 Reflux Condenser, water-cooled, 400 mm in length, and fitted with a standard-taper 24/40 joint. 4.6 Separatory Funnel, 300 to 500-mL capacity, with glass stopper, 4.7 Spot Plate, white porcelain. 5., Reagents 5.1 Alkali, StandardAlcoholic Solution (0.1 N)--Dissolve 6.6 g of KOH or 4.2 g of NaOH, preferably in pellet form, in methanol (99.5 %\ or ethyl, alcohol (95 %) denatured by. METHOD A--CONTINUOUS EXTRACTION 1 (Referee Method) ,, Apparatus (Figs. 1 and 2) A. 1 Erlenmeyer or Other Flat-Bottom Flasks, of 125 and* * 1 These methods are under the jurisdiction of ASTM Committee D-l on Paint Related Coatings and Materials and are the direct responsibility of Subcomiee D01.34 on Naval Stores. Current edition approved March 26, 1982. Published June 1982 Originally iblished as D 1065 - 49 T. Last previous edition i> 1065 - 56 (198 i). * "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. ic., Washington, D. C. For suggestions on the testing of reagents not listed by the merican Chemical Society, see "Reagent Chemicals and Standards," by Joseph osin, D. Van Nostrand Co., Inc., New York, N. Y,, and the "United States harmacopeia." 149 FIG. 1 Extractor and Conductor Tubes DUP05029S815 D 1065 Formula No. 3A or No. 30 of the U.S. Bureau of Internal Revenue. 5.2 Ethyl Ether 5.3 Isopropyl Alcohol (91 to 99%)--Make neutral to phenolphthalein by adding 0.1 N alkali solution dropwise. 5.4 Phenolphthalein Solution--Dissolve 1.0 g of phenol- phthalein in 100 mL of alcohol conforming to 5.1, and neutralize to a very faint pink color with 0.1 N alcoholic alkali solution. 5.5 Potassium Hydroxide, Alcoholic Solution (132 g of KOH/L)--Dissolve 132 g of KOH pellets or sticks in 150 ml. of water and dilute to 1 L with alcohol conforming to 5.1. 5.6 Sodium Hydroxide solution (10 g/L)--Dissolve 10 g of NaOH in water and dilute to 1 L. 5.7 Thymol Blue Indicator Solution--Dissolve 0.1 g of thymol blue in 100 mL of methanol. 6: Procedure 6.1 Weigh 5.00 0.01 g of the sample into the 125-mL Erlenmeyer or other flat-bottom flask, add 15 mL of the alcoholic KOH solution (132 g KOH/L), attach to the condenser, and reflux for 1.5 h, shaking occasionally. Re move the flask and boil 1 min longer, swirling the flask gently, to evaporate about 3 to 5 mL of the alcohol. Then add 10 mL of water and transfer the solution, while hot, to the extractor tube. Wash the flask twice with 10-mL portions of hot water and add to the extractor tube. Adjust the volume in the tube to 50 mL. Add 100 mL of ethyl ether to the 250-mL Erlenmeyer flask and assemble the extraction apparatus (Fig. 2). Heat the flask and adjust the boiling rate to give a reflux rate of condensed solvent of 3 drops per second. Extract for 1 h. 6.2 Transfer the ether solution to a separatory funnel containing a few drops of water. Rinse the flask with two 15-mL portions of fresh ether and add the rinsings to the solution in the separatory funnel. Extract with 50 mL of NaOH solution (10 g/L). Draw off the aqueous layer into a second separatory funnel, add 50 mL of ether, and shake thoroughly. Allow the ether and water phases to separate, and discard the aqueous layer. Transfer the ether to the first separatory funnel and wash the combined ether solutions three times with 50-mL portions of water. 6.3 Transfer the washed ether solution quantitatively to a weighed 300-mL, wide-mouth Erlenmeyer flask and evapo rate on a steam bath. If any droplets of water collect in the flask, add a few milliliters of ethyl alcohol, and again evaporate on the steam bath until a clean, dry residue is obtained. Then place the flask in an oven at 100 to 105C for 10 to 15 min, cool in a desiccator, and weigh. 6.4 Dissolve the residue in the flask in 50 mL of neutral isopropyl alcohol, add 1 mL phenolphthalein indicator, and titrate with the 0.1 N alcoholic alkali solution. When the solution is too colored to detect the end point internally, titrate until a faint color change is noted. Then withdraw approximately 0.5 mL of the solution to the porcelain spot plate, and to the withdrawn portion add 1 drop of phenol phthalein solution. Continue titrating with 0.1-mL portions of alkali, and testing on the spot plate, until a definite pink color that persists for at least 1 min is obtained. 7. Calculation and Report 7.1 Calculate the percentage of unsaponifiable matter in the rosin as follows* and report the results to the nearest 0.1 %: Unsapotfifiable matter, % = [(A ~ {CN x 0.302))/B] x 100 where: A = grams of dried residue, B = grams of sample used (dry basis), C = millilitres of alkali solution used, and N = normality of the alkali solution. METHOD B--EXTRACTION BY MEANS OF A SEPARATORY FUNNEL 8. Apparatus 8.1 Erlenmeyer or Other Flat-Bottom Flask, of 125-mL capacity, with standard-taper 24/40 joint. 8.2 Erlenmeyer Flask, 300-mL capacity, with wide mouth. 8.3 Separatory Funnels, of 300 to 500-mL capacity, with, glass stoppers. 9. Reagents 9.1 See Section 5. 10. Procedure 10.1 Weigh 5.00 0.01 g of the sample into the 125-mL Erlenmeyer or other flat-bottom flask, add 15 mL of the alcoholic KOH solution (132 g KOH/L), attach to the condenser, and reflux for 1.5 h, shaking occasionally. Re- Scap FIG. 2 Complete Extraction Apparatus 150 DUP050295816 # D 1065 Plflask, add 50 mL of water, and transfer to a I ,,funnel. Rinse the flask with 40 mL of ether, ! rinsings to the separatory funnel. Shake the rand allow to stand until the ether layer separates. <Sf the aqueous soap solution (lower layer) into a Innnel, allowing a few drops of the aqueous solution un above the stopcock to prevent loss of ether extract page through the ground-glass joint. 'g the soap solution in the second funnel, add 30 er apd extract as before, drawing the soap layer Iginal saponification flask. Add the ether in the nnel to the first funnel. Then pour the soap from the flask into the second funnel, and again th 30 mL of ether. Draw the soap layer into the n, and add the ether to the first funnel as before, W oi ff and add to the solution in the flask all but a bf the soap solution which has collected below the ether layers in the first funnel, gain pour the combined soap solutions into the iinel and extract for the fourth time with 30 mL of qr separation ofthe layers, discard the soap solution the ether extract to the fust funnel. Carefully draw remaining soap solution that may have collected le stopcock. Add 2 mL of water, swirl the funnel allow the water to settle, and then draw off and discard. Repeat this washing, once with 5 mL and twice with 30 mL of water. 10.4 Draw off the washed ether extracts into a dry, tared, wide-mouth Erlenmeyer flask, rinse the funnel with 15 mL of ether, add to the flask, and evaporate on a steam bath. If any droplets of water collect in the flask, add a few millilitres of ethyl alcohol, and again evaporate on the steam bath until a clean, dry residue is obtained. Then place the flask in an oven at 100 to 105C for 10 to 15 min, cool in a desiccator, and weigh. 10.5 Dissolve the contents in the flask in 50 mL ofneutral isopropyl alcohol, add 1 mL of thymol blue or phenolphthalein indicator, and titrate with the 0.1 A alcoholic alkali solution. When the solution is too colored to detect with certainty the end point internally, titrate until a faint color change is noted. Then withdraw approximately 0.5 mL of the solution to the porcelain spot plate, and to the withdrawn portion add 1 drop of the indicator solution. Continue titrating with 0.1-mL portions of alkali, and testing on the spot plate, until a definite color change that persists for at least 1 min is obtained. 11. Calculation and Report 11.1 Calculate the percentage of unsaponifiable matter in the rosin, and report the results to the nearest 0.1 %, as directed in Section 7. The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard is suB/ect to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.151 . 151 DUP050295817 (|jjjj$ Designation: D 1078 - 86 Designation: 195/81 Standard Test Method for Distillation Range of Volatile Organic Liquids1 This standard is issued under the fixed designation 01078; the number immediately following the designaiion indicates the' year of ' original adoption or. in the case of revision, the year; of last revision. A number in parentheses'indicates the year oflast reapproval A superscript epsilon (t) indicates an editorial change since thelast revision or reapproval. This test methodwas adoptedas ajoint ASTM-1Pstandard in 1986. . ; ' This test method has been approvedfor use by agencies ofthe Department ofDefense to replaceMethod 4301,1 ofFederal Test Method Standard No. I41a amtfor listing in the DoD Index efSpecifications and Standards. 1. Scope 1.1 This test method covers the determination of the distillation range of liquids boiling between 30 and 350C, that are chemically stable during the distillation process. 1.2 This test method is applicable to organic liquids such as hydrocarbons, oxygenated compounds, chemical interme diates, and blends thereof. 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 Section 7, 2. Referenced Documents 2.1 ASTM Standards: D 86 Method for Distillation of Petroleum Products2 E l Specification for ASTM Thermometers3 E 133 Specification for Distillation Equipment4 E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals5 E 299 Test Method for Trace Amounts of Peroxides in Organic Solvents6 3. Terminology 3.1 Definitions: 3.1.1 initial boiling point--the temperature indicated by the distillation thermometer at the instant the first drop of condensate leaves the condenser tube. 3.1.2 dry point--the temperature indicated at the instant the last drop of liquid evaporates from the lowest point in the ' 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 25, 1986. Published June-1986. Originally published as D 1078 - 49 T. Last previous edition D 1078 - 83. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 14.03. 4 Annual Book ofASTM Standards, Vol 14.02. 5 Annual Book ofASTM Standards, Vol 15.05. 6 Annual Book ofASTM Standards, Vols 06.03 and 15.05. distillation flask, disregarding any liquid on the side of the flask. 3.1.3 decomposition point--the thermometer reading that coincides/with the first indications of thermal decomposition of tlie liquid in the flask. . 3.2 Descriptions of Terms Specific to This Standard: * 3:2'. 1 final boiling point--the maximum thermometer1' | reading obtained during the test. This usually occurs after the1 evaporation of all liquid from the bottom of the flask. The term "maximum temperature" is a frequently used syn onym. 3.2.2 end point 5 minutes--the thermometer reading obtained 5 min after the, 95 % distillation point if no dry or- final boiling point occurs. f 4. Summary of Test Method - 4.1 A 100-mL "specimen is distilled, under conditions i equivalent to a simple batch differential distillation. The ; temperature of the mercury in the thermometer is equili brated with that of the refluxing liquid before the distillate is ; taken over. Boiling temperatures observed on a partial- ! immersion thermometer are corrected to standard at- j mospheric pressure to give true boiling temperatures. I 5. Significance and Use J 5.1 This test method provides a method of measurement I of distillation range of volatile organic liquids. The relative volatility of organic liquids can be used with other tests for identification and measurement of quality. Therefore, this . test method provides a test procedure for assessing compli- : ance with a specification. 5.2 This test method also provides an empirical value of residue, solvent recovery capacity, and loss (or non-recovery) on heating. Organic liquids are used as solvents in many chemical processes. As the relative volatility, residual matter and recovery capability affect the efficiency of these pro cesses, this test method is useful in manufacturing control. 6. Apparatus 6.1 Distillation Apparatus--See Condenser and Cooling Bath section. Figs. 1 and 2, and Metal Shield or Enclosure for Flask section of Specification E 133. 6.2 Distillation Flasks, 200-mL of borosilicate glass com plying with the specifications given in Distillation Flask section, Fig. 3, and Flask C of Specification E 133. 152 DUP050295818 # D 1078 ijviidi superheating in a new flask may be prevented by .amount of carbon in the bottom of the flask. This shed by heating ancj decomposing a pinch of tartaric "bf the flask. The flask is then prepared for use by ater, rinsing with acetorie, and drying. ejyfHeat--^. adjustable gas burner or electric structed tftaf sufficient heat can be obtained to Suet at the uniform rate specified in Section 8. ange (less than 2C) liquids, an electric heater only if it has been proven to give results to those obtained when using gas heat. (See ' factors that cause superheating, and Appendix ission on the use of electric heaters;) \r--A 100-mL cylinder graduated in 1-mL fltid having an overall height of250 to 260 mm. 'lometers--Vaxtidi immersion thermometers as ble 1, conforming to Specification E 1. Both bore Bifid either ice or steam standardization correcbtnmended. ration---Certain solvents and chemical intermedi'cularly, hut not only ethers and unsaturated ma^' form peroxides during storage. These ay present a violent explosion hazard when (he distilled' "especially as the dry point is ap When peroxide formation is likely because of | type or length of storage, the material should be " for peroxides (See Test Method E 299.) and if they hazardous concentrations, appropriate precautions taken such as destroying the peroxide before On, shielding, or destroying the sample and not file test. lost organic solvents and chemical intermediates will 1ft-'the operation of the distillation apparatus, use a batch pan and shielding to contain spilled liquid in of accidental breakage of the distillation flask, ovide adequate ventilation to maintain solvent centrations below the lowef explosive limit in the tte vicinity of the distillation apparatus, and below shold limit value in the general work area. eparation of Apparatus Clean and dry the condenser tube by swabbing with a lof soft lint-free cloth attached to a wire or cord or by 6ther suitable means. Use the thermometer listed in the material specificaTor the product under study. If iio thermometer is Ified, select one frdm Table 1 with the smallest graduas that will 'cover the entire distillation range of the rial. Center the thermometer int6 the neck of the flask ough a tight-fitting cork stopper so that the upper end of if contraction chamber (or bulb if Thermometer 2C or IP nometer 62C is used) is level with the lower side of the ar tube at itsjunction with the neck of the flask: (See Fig, 'Method D 86.) 2--It is far more important that the greatest volume-of be immersed in the refluxing zone than that the immersion : on the thermometer be placed at any specific point. 1;8,3 Insert the vapor tube of the distillation, flask into the 'ndenser, making a tight connection with a well-rolled cork. TABLE 1 Thermometers} ASTM Thermometer Number 2C" ' 3C* 37C 38C 39C 40C ktc 42C* .1020 103C 104C 105C 106C 107C IP 62CA 73CA 77C 78C 79C . 80C `81C 82C* 83C 84C 85C 86C 87C 88C. Range,- C -5 to +300 -5 to +400 -2 to +52 24 to 78 48 to 102 72 to 126 98 to 152 95 to 255 .123 to 177 148 to 202 173 to 227 198 to 252 223 to 277 . 248 to 302 . Sub division, "C .1.0 8 0.2 0.2 0.2 0.2 0.2 0.5 0.2 0.2 0.2 0.2 02 02 A These thermometers-have more temperature lag than the other thermome ters listed herein and are not satisfactory for use with narrow-boiling range liquids. 8 1 to S01-C; 1.5C above 301C. Adjust the position of the asbestos boards or heater shield so that the neck bf the flask is vertical and the vapor tube extends into the condenser tube a distance of 25 to'50 mm. Hive the bottom of the flask resting firmly in the llA or l`/2-in. (32 or 38-mm) opening of the upper asbestos cement board. No t e 3--For low-boiling materials, cool the apparatus to room temperature before starting the test. 8.4 Fill the condenser bath with water of the appropriate temperature shown in Table 2. No t e 4--When distilling pure compounds-always ensure that the condenser bath-'temperature is above the crystallizing point of the compound. 8.5 Adjust the temperature of the appropriate portion of the sample to the applicable temperature shown in Table 2. 9. Procedure 9.1 Using the graduated receiver measure 100 0.5 mL of the temperature-adjusted sample. Remove the flask from' file apparatus and transfer the fresh specimen directly to the ' flask, allowing the graduate to drain for 15 to 20 si No t e 5--For. viscous liquids,, a longer drainage period may. be necessary to complete the transfer of the specimen to the flask, but the drainage time should not exceed 5 min. Do not allow any of the specimen to enter the vapor tube. 9.2 Connect the flask to the condenser and insert the thermometer as described in 8,2. Place the receiver, without drying, at the outlet of the condenser tube in such a. position that the condenser tube extends into the graduate at least 25 mm but does not extend below the 100-mL mark. If the initial boiling point qf the material is below 70"C, immerse the cylinder in a transparent bath and maintain at a Initial Boiing Point, c Below 50 50 to 70 70 to 150 Above 150 . TABLE 2, Temperatures Condenser, C 0 to3 OtolO 25 to 30 35 to 50 : Sample, C , 0 to 3 10 to 20 20 to 30 20 to 30 153 DU PO50295819 # D 1078 temperature of 10 to 20C throughout the distillation. Place a flat cover on the top of the graduate to prevent condensed moisture from entering the graduate. 9.3 A certain amount of judgment is necessary in choosing the best operating conditions to get acceptable accuracy and precision for materials having different dis tilling temperatures. As a general guide, it is recommended that: 9.3.1 For materials having an initial boiling point below 150C, the following conditions be established: 9.3.1.1 Heat Shield--Hole size, l'A-in. (32-mm) diam eter. 9.3.1.2 Heating Rate---Time from application of heat to first drop of distillate, 5 to 10 min, and time of rise of vapor column in neck of flask to side arm, 2lh to 31/2 min. 9.3.2 For materials having an initial boiling point above 150C, the following conditions should be established: 9.3.2.1 Heat Shield--Hale size, V/i-in. (38-mm) diam eter. 9.3.2.2 Heating Rate--Time from application of heat to first drop of distillate, 10 to 15 min, and time of rise of vapor column in neck of flask to side arm, sufficiently rapid to permit collection of the first drop of distillate within 15 min of the start of heating. 9.4 Adjust the heat input so that the distillation proceeds at a rate of 4 to 5 mL/min (approximately 2 drops per second), and move the receiving cylinder so that the tip of the condenser tube touches one side of the cylinder after the first drop falls (initial boiling point). Record the readings of the distillation thermometer after collecting 5,10,20, 30,40, 50, 60, 70, 80, 90, and, 95 mL of distillate. 9.5 Without changing the heater setting, continue distilla tion beyond the 95 % point until the dry point is observed. Record the temperature at this point as the dry point (Section 3). If a dry point is not obtained (that is, if active decomposition should occur before the dry point is reached, as evidenced by a rapid evolution of vapor or heavy fumes; or if there is liquid remaining on the bottom of the flask when the maximum temperature is observed on the distilla tion thermometer), record this fact. 9.6 When a dry point cannot be obtained, report as the end point the maximum temperature observed on the distillation thermometer or final boiling point (Section 3). When active decomposition is encountered, the rapid evolu tion of vapor and heavy fumes is usually followed by a gradual decrease in the distillation temperature. Record the temperature and report as the decomposition point (Section 3). If the expected drop in temperature does not occur, record the maximum temperature observed on the distilla tion thermometer 5 min after the 95 % point has been reached, and report as "end point, 5 min." This notation shows that a true end point could not be reached within the given time limit. In any event, the end point should not exceed 5 min after the 95 % point. 9.7 Read and record the barometric pressure. 9.8 After the condenser tube has drained, read the total volume of distillate and record it as recovery. The total yield of distillate from a material having a distillation range of I0C or less should be not less than 97 % for nonviscous liquids. For viscous liquids and materials having a wider distillation range than 10C, a yield of 95 volume % is satisfactory. If yields are not obtained within these limit! repeat the test. ^ t 9.9 If any residue is present, cool to room temperatur and pour into a small cylinder graduated in 0.1-mL subdi sions. Measure the volume and record it as residue. Recor the difference between 100 and the sum of the residue pi recovery as distillation loss. 10. Factors Causing Superheating 10.1 In general, any condition whereby the temperah surrounding the vapor exceeds the temperature of the vapf in equilibrium with the liquid will cause superheat! Specific factors conducive to superheating are as follows, t should be avoided: 10.2 Flame in Contact with the Flask--The applied i flame should be prevented from contacting more than i specified portion of the flask by the following procedures:, 10.2.1 Maintain the correct overall dimensions and sp ified hole diameter of the asbestos cement board. The 1 must be perfectly circular, with no irregularities. 10.2.2 Use a board that is free of cracks and checks. 10.2.3 Set the flask snugly in the hole in the up insulating board. 10.3 Application of Heat--Attention should be givefr burner placement, position, and character of flame, follows: 10.3.1 Apply the source of heat directly beneath the f|r Any variation would result in heating a larger portion/ surrounding air to a higher temperature than that of flask. s 10.3.2 The flame should not have a larger cross sectio than is necessary, and should be nonluminous. 10.3.3 Place the burner at a level such that the combustion area of a nonluminous flame is approxiti % in. (20 mm) below the board. 10.4 Extraneous Heat Source--An extraneous sour heat such as sunlight falling directly on the flask can < superheating. 10.5 Condition of Equipment--Observe caution in ploying the apparatus for immediate reuse. For low-boilffil materials, cool the heating unit to room temperature be starting the test. 10.6 Use of Electric Heaters--Electric heaters general1." cause superheating. These should be used only after-f have been proven to give results comparable to obtained when using gas heat. The superheating efffil obtained from electric heaters may be minimized, but ri completely eliminated, by selecting a heater that, by design, concentrates the heating elements to a minicw|; area, and contains a minimum amount of ceramic mate, in its overall construction. The fulfillment of these requil| ments will reduce, but not completely eliminate, the an of extraneous heat radiating around the perimeter oft asbestos-cement board on which the distillation placed.7 (See Appendix XI for a more complete discussio' the problems encountered in the use of electric heaters.) 7 The Lo-Cap heater, available from the Precision Scientific Co., Chicago,general, fulfills the requirements for electric heaters. 154 DUP050295820 # D 1078 foils mpmeter Bore Correction--Apply the correc; variations in the bore of the thermometer as jpaiibration. ^tometer Bulb Shrinkage Correction--Apply jtion for shrinkage of the mercury bulb of the ' :fcr as determined by any change in its ice or steam tjj t|pplicable. Other means can be employed, such e of a platinum-resistance thermometer or a "Bureau of Standards thermometer. "rorheter Correction--After applying the correc*rmometer error, correct each reading for devia ^barometric pressure from normal by adding She correction calculated as follows: arvalues of K in degrees Celsius per millimetre of TABLE 3 Change of Boiling Point with Pressure Compound Acetone ' n-Amyl alcohol n-Amyl acetate Aromatic solvent naphtha Value of K, C per mm Hgat Baling Point 0.039 0.041 0.048 0.049 K, C per mbar at Boiling Point 0.029 0.031 0.036 0.037 Bolling Point at 760 mm Hg, C 56.1 138.0 149.5 Benzene Isobutyl acetate n-Butyl acetate sec-Butyl acetate Isobutyl alcohol n-Butyl alcohol sec-Butyl alcohol 0.043 0.045 0.045 0.045 0.036 0.037 0.035 0.032 0.035 0.035 0.034 0.027 0.028 0.026 80.1 117.3 126.1 112.4 107.9 117.7 99.5 j- Correction = (760 - P) `change ofboiling point with pressure, in degrees % per millimetre, as given in Table 3 (Note 6), "I'' metric pressure in millimetres of mercury at ard temperature. ``br values of K in degrees Celsius per millibar Correction = (1013 - P) Diacetone alcohol Diethylene glycol Dipropylene glycol Ethyl acetate Ethyl alcohol Ethylene glycol 2-Butoxyethanol 2-Ethoxyethanol 2-Ethoxyethyl acetate Hexylene glycol n-Hexy] acetate 0.050 0.050 0.051 0.041 0.033 0.045 0.047 0.044 0.046 0.045 0.050 0.037 0.037 0.038 0.030 0.025 0.033 0.035 0.033 0.035 0.033 0.037 245.0 232.8 77.2 78.3 197.6 171.2 135.1 156.3 197.1 171.6 ` of change of boiling point with pressure, in degrees sius per millibar, as given in Table 3 (Note 6), and metric pressure in millibars at standard tempera- and pressure. For other pure compounds not listed.in Table 3, the value be obtained from the literature. For narrow-boiling hydroaterials, the value of may be assumed as 0.00012 times the iling point on the absolute temperature scale. < the overall distillation range of the sample does not "C, combined thermometer (bore irregularities and ge) and barometric corrections may be made on > of the difference between the observed 50 % boiling d the true boiling point at 760 mm as given in Table Isophorane Methyl alcohol Methyl ethyl ketone Methyl isoamyl acetate Methyl Isoamyl ketone Methyl isobutyl carbinoi Methyl isobutyl ketone Perchloroethylene Isopropyl alcohol Isopropyl acetate Propylene glycol Pyridine Toluene Trichloroethylene Vinyl acetate 0.057 0.033 0.043 0.048 0.048 0.041 0.046 0.048 0.033 0.041 0.043 0.046 0.046 0.043 0.040 0.043 0.025 0.032 0.036 0.036 0.030 0.035 0.036 0.025 0.030 0.032 0.035 0.035 0.032 0.030 215.3 64.5 79.6 146.2 144.9 131.8 116.2 121.2 82.3 88.5 187.6 115.4 110.6 87.1 72.7 port Xylene (mixed isomers) 0.049 0.037 fcReport the results in a manner conforming with the cations ofthe material tested. If no definite manner of that have a wide boiling range at elevated temperatures. The is specified, report the corrected temperatures at values shown for the different solvents may be used as rerved volume, and report the volume percentages of examples of the precision obtainable with this test method at e, recovery, and distillation loss. the 95 % confidence level. For a better estimate of precision for a particular case, a cooperative study should be made on ecision.8 the compound or product of interest. 1: The precision of this test method is based on three 13.1.1 Repeatability--Two results, each the mean of two iboratory studies involving ten laboratories and several runs, obtained by the same operator should be considered ts. It was established that, in general, the precision suspect ifthey differ by more than the values shown in Table " ves with increasing purity and decreasing boiling point 4 for a material with' similar boiling range and 50 % point. material being tested, while it is poorest for mixtures* 51 13.1.2 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 pporting data are available from ASTM Headquarters. Request RR; 51. values shown in Table 4 for a material with a similar boiling range and 50 % point. 155 DUP050295821 # D 1078 TABLE 4 Summary of Precision14 Initial Bolling Point, C Mean Value Checking Limits Repeatability Reproducibility Acetone 55.87 0.09 0.10 0.09 0.42 Acetate Ester of Diethylene' Glycol Mono ethyl Ether 215.33 0.31 0.77 0.87 153 StknL Point. "C Glycol Mixture . 190.70 i 0.42s 0.76 0.51 1.92 Xylene-Pseudocumene 141.03 052 0:50 0.34 2.36 Mean Value Checking Limits Repeatability Reproducibility l' 66.03 0.07 0.07 0.15 0.32 218.24 0.24 0.21 0.58 1.16 Dry Point, C 192.83 0.35 0.40 0.34 1.57' 146.18 4; 0.37 056 0.81 1.75 Mean Value Checking Limits Repeatability Reproducibility 56.36 0.11 0.27 0.24 0.51 220.03 0.29 0.46 0.57 1.35 Distillation Range, C 202.51 + 0.74 0.57 0.77 3.36 168.75 Q.57 0.80 : . 1.20 2.70 Mean Dp--Average Ibp Checking Limits Repeatability Reproducibility 0.49 4.7 " 0.29 . 0.90 0.26 1.04 0.66 2.04 11.8 0.95 0.93 . 3.88 A AB values are at the 95 % confidence level and were calculated in accordance with Practice E180. 27.8 0.95 : 1.25 3.59 Mineral Spiri^M 163.68 l)XlSl 1.13 2.13 2.19 ,'j H rfH ~l|j 175.02 0 26 - j 0.93 ' 71 0.48 f 1.20 ./. l -- 200.35 1 1.22 0.80 3.50 | 36.7 1:67 2.28 4.13 J :* 1 ;.| APPENDIX v . . (Nonmandatory Information) ,. '!i XI. DISCUSSION ON THE USE OF ELECTRIC HEATERS WHEN APPLYING TEST METHOD D 1078/IP 195 TO THE DETERMINATION OF THE DISTILLATION RANGE OF NARROW RANGE (<2Q PURE COMPOUNDS Xl.l Test Method D 1078/IP 195, in the hands of a competent operator using properly designed equipment, has been found over the years to be a valuable tool in detecting the presence of low-boiling and high-boiling impurities in relatively pure compounds. XI.2 In recent years many laboratories, for reasons of safety and convenience, have eliminated the availability of natural or artifxcal gas, with the resulting trend toward the exclusive use of electric heaters in place of gas burners. The use of electricity instead of gas as the source of heat, coupled with the application of this test method to materials of extremely high purity and narrow distillation ranges (2C or less), has resulted in the distortion of the dry point. This distortion effect can be .illustrated by comparing the distilla tion range results using gas and electric heat on a sample of TABLE X1.1 Determination 1: Initial boiling point Dry point Determination 2: Initial boiling point Dry point Mean range Comparison of Gas Versus Electric Heat Gas Heat Electric Heater5 Range Range 64.5 64.8. 64.5 64.9 0.3 0.4 0.35 645 66.0 64.5 66.4 1.5 1.9 1.7 high-purity methanol (Table XI. I): The purity of the riicth- anol employed was established by gas chromatography and other instrumental procedures. XI.3 The higher dry point obtained with the ele<f heater is due to the large amount of extraneous heat radiating around the distillation flask which in turn is due to the relatively large area of the distillation board exposed to' the heating elements of the electric heater. For example, the heating elements of the electric heater5 cover an area of 2V4 . by 3 in. (63.5 by 76 mm) whereas the flame of a properly adjusted gas burner can be concentrated to an area no larger than the 1 '/4-in. (32-mm) hole of the supporting asbestos j cement (or ceramic) board. This means that when the 5 heating elements of the electric heater are brought up to j sufficient temperature to effect the proper distillation rate of i the methanol, a relatively large area of the board also is i exposed to the heat ofthese elements so that as the end of the ; distillation is approached, a considerable amount of heat is j being radiated from the board to the air surrounding the ! distillation JIask. This hot air surrounding the flask is sufficient to cause a distortion of the dry point as- the last drop of liquid is vaporized from the bottom of the flask. Conversely, the ability to concentrate the gas flame to only the 1 >/4-in, exposed area of the flask minimizes the extent of, the extraneous heat radiating from the board, which, in trim, eliminates the distortion of the dry point from this cause, i 156 II nm D U PO502 95822 D1078 ^conclusion was substantiated by results from the g experiment: The board with the l'A-in. hole was ! by a lxh by IVi-m. (190.7 by 190.7-mm) stainless late in which a 1 'A-in. hole had been cut. Four turns of ;(6.4-mm) copper tubing with sufficient inlet and outlet ere silver-soldered to the underside ofthe plate so that could be circulated through the tubing during the of the distillation. With this "water-cooled board" "tuted for the standard board, only the heat from the leal elements immediately under the l'A-in. outlet reach the distillation flask. The heat emanating from uter perimeter ofthe heater was dissipated by the water Sting through the tubing on the underside ofdie board, denced by the ability to hold one's finger on top of the /-cooled board" during the course of the distillation. the same high-purity methanol employed in the ous experiment, distillation ranges were determined s heat, electric heat, and electric heat with the r-cooled board" substituted for the standard board, results are given in Table XI.L. . 1.4 The results from the above experiment demonstrate fleet the extraneous radiant heat from the electric heater !bn the dry point, and also suggest a means whereby this could be greatly reduced. .5 Despite the fact that the use of a "water-cooled " in conjunction with an electric heater eliminated the leous radiant heat surrounding the distillation flask, it 'dent from the results in Table XI.2 that the dry point 'ned when using the electric heater and "water-cooled d" was still significantly higher than the dry point 'ned when using gas heat. The assumption was made this "residual" interference to the dry point was caused .infrared radiation from the glowing electric heating ents. This assumption has been supported by the owing experimental evidence: The bottom of a standard -mL distillation flask was coated with a 1 */2-in. (38-mm) eter circle of black ceramic marking ink. The black ink ` in turn fired into the glass by heating the bottom of the to a dull-red heat with a gas-oxygen glass blowtorch, e presence of this black coating on the bottom of the flask would absorb any infrared radiation emanating from the electrical heating elements, thus preventing it from affecting the bulb of the thermometer at the end of the distillation. Distillation ranges were then determined on the same methanol as used in the previous experiments following Test Method D 1078/IP 195, except that in one case a standard 200-mL flask was used with an electric heater plus the "water-cooled board," and in the other case, the specially prepared "black bottom" 200-mL flask was employed. Both of these special conditions were compared to the standard procedure using gas heat. The results of this experiment, given in Table XI.3, show that the use of the "black-bottom flask" in conjunction with the electric heater and "wa ter-cooled .board" causes a significant lowering of the dry point which confirms the theory that infrared radiation emanating from the electric heating elements causes a slight distortion of the dry point. XI .6 The above discussion and experimental evidence are presented to show how and why the use of electric heater causes a distortion of the dry point when carrying out the procedure as specified in Test Method D 1078/IP 195. Al though this distortion is of a minor nature, and therefore of little importance when applying this test method to com pounds or mixtures which have distillation ranges of 5C or . more, the effect becomes significant when the method is applied to narrow range (2C or less) pure compounds. It is the further objective of this discussion to suggest to those laboratories equipped with only electricity, a technique whereby the distillation range results obtained with electric heaters may be made equivalent to those obtained with gas heat. . XI.7 The sponsoring subcommittee of this test method has not had the opportunity to apply this technique to a sufficiently large number ofcompounds over a wide range of boiling temperatures to warrant including it as a part of Test Method D 1078/IP 195; and is, therefore, presenting it for information purposes only. Comments are solicited from those attempting to employ the suggestions contained in this report as well as other ideas that might be employed to equate the use of electric heat with gas heat. 157 DUP050295S23 Determination 1: Initial boiling point Dry point Determination 2: Mai boiling point Dry point Mean range Determination t: initial boiling point. Dry point Determination 2: Initial boiling point Dry point Mean range TABLE X1.2 Comparison of Electric Heat Plus Water-Cooled Board to Gas Heat Gas Heat Electric Heat6 Range Range Electric Heat6 plus Water-Cooled Board Range ' 64.5 0.3 64.B 64.6 0.3 64.9 0.3 64.5 66.1 ' 64.5 65.9 1.6 1.4 1.5 TABLE X1.3 Effect of Infrared Radiation on Dry Point Gas Heat Electric Heater6 with Water-Cooled Board and Standard Flask. Range Range 64.5 0.3 64.8 64.5 0.4 64.9 0.35 64.5 65.1 64.6 65.2 0.6 0.6 0.6 64.5 65.0 0.5 64.5 65.1 ' $ "* . tl, ' I, 0.6 0.55 Electric Heater5 with Water-Cooled: - Board and B|ack-Bottom Flash. : 64.6 64.8 Range , ii 0.2 64.6 64.9 0.2 0.25 ' The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in conneotion 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 reapprovedor withdrawn. Your comments are invited either forrevision 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. .I-! 'I158 158 b. DUP050295824 Designation: D 1131 - 53 (Reapproved 1981)f1 w Standard Methods of Testing fl' Rosin Oils*1 r'liP This standard is issued under the fixed designation D 1131; 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 if superscript epsilon (<) indicates an editorial change since the last revision or reapproval. f m t- ' et No t e--Section 2 was added editorially and subsequent sections renumbered in May 1985. H|KMft, pe X1 These methods are intended for use in determining [Ira rosin oil conforms with the specifications and pirients usually applied to ensure its suitability for a liar use. In general, hot all of the tests will be required Seifmine the fitness ojf an oil for a specific use. The term "'"oil" includes the'oils obtained by dry destructive jpibn of rosin* with or without subsequent redistil- ffljland also certain compounded oils prepared from a "fpibase. It has no relationship to the product formerly Ijsrai as liquid rosin, for which the term "tall oil" has been pted. perenced Documents IHSTAf Standards: 3 Test Method for Sayboll: Viscosity2 _j Test Method for Flash and Fire Points By Cleveland spen Cup3 Test Methods for Flash Point by Pensky-Martens losed Tester3,4 95 Test Method for Water in Petroleum Products and Bituminous Materials By Distillation3,4 805 Methods of Testing Tall Oil5 856 Test Methods for Sampling and Testing Pine Tars Rnd Pine-Tar Oils4 *T063 Test Method for Ash in Rosin4 *1500 Test Method for ASTM Color of Petroleum ` Products (ASTM Color Scale)3 Appearance |.l Exariiine a sample of the oil in a clear glass tube by nsmitted light, to ascertain whether any separated water, litals, or insoluble foreign matter are present. (Color ikl Determine the color of the oil by reference to the ITM Color Numbers, in accordance with Test Method U500. jpThese methods are under the jurisdiction of ASTM Committee D-l on Paint 1 Related Coatings and Materials and are the direct responsibility of Subcom- : DO 1.34 on Naval Stores, jl Current edition approved Sept. 15,1953. Published November 1953. Originally |tblished as D 1131 - 50 T. Last previous edition D 1131 - 50 T. P*Annual Book ofASTM Standards, Vol 04.04. T*Annual Book cfASTM Standards, Vol 05.01. * Annual Book ofASTM Standards, Vol 06.03. S'* Discontinued; see 1976 Annual Book ofASTM Standards, Part 22. 4.2 Compare the color of the oil with any suitable or specified reference standard, using a vessel similar to that in which the reference standard is contained. When nonliquid standards are used, the container shall be specified in terms ofthe distance between two opposite faces through which the oil is viewed, and such distance shall be shown on the report. 4.3 For oils of such dark color that accurate and satisfac tory color comparisons cannot be made, a portion of the oil shall be diluted with an equal quantity of redistilled toluene, and the color shall be determined on such diluted oil. In such case the report shall carry the notation "50 % toluene dilution." 5. Specific Gravity 5.1 Determine the specific gravity of the oil at 25C (77F) by means of any convenient apparatus that has been calibrated at 15.56C (60F). Report the specific gravity to the third decimal as: Specific gravity, 25/15.56C (77/60F) Such observed specific gravity may be converted to the 25/25C (77/77F) basis by multiplying the observed reading by the factor 1.002. No t e 1--If a Hubbard pycnometer or weighing bottle is used, the weight of water contained by the pycnometer at 25C shall be deter mined, in which case the ratio of oil to water will be the specific gravity at 25/25C. To convert this to the 25/!5.56C (77/60F) basis, multiply by the factor 0.998. 6. Viscosity 6.1 Determine the viscosity of the oil at 25C (77F) by comparing the rale of movement of an air bubble through the oil in a closed tube with the movement of similar size bubbles in any suitable liquid reference standards. The identity of such standards shall be shown in the report. 6.2 Determine the viscosity of the oil by means of a standard viscosimeter by one of the following procedures. 6.2.1 At 100, 130, or 210F, using a Saybolt Universal Viscosimeter, in accordance with Test Method D 88. Report the viscosity in seconds. 6.2.2 At 30 or 50'C, using a Stormer Viscosimeter, in accordance with Sections 9 to 11 of Methods D 856. Report the viscosity in s/100 r, or convert the observed reading to centipoises by means of the formula given in Section 12 of Methods D 856. 7. Flash Point 7.1 Determine the flash point of the oil either in accor dance with Test Method D 92 or in accordance with Test 159 DUP050295825 # D 11?1 Jjj 4 Method D 93. Report the method used. 8. Acid Number 8.1 Weigh 4.95 to 5.05 g, to the nearest 0.01 g, of the sample into a 300-mL Erlenmeyer flask. Add 100 mL of a solvent containing equal parts of acetone and either 95 % ethyl alcohol (Formula No. 3A or No. 30 denatured) or methyl alcohol. Place on a steam bath and dissolve the oil in the solvent, connecting in air-tube condenser to the neck of the flask and heating for not more than 15 min, if necessary. Cool, add 1 mL of phenolphthalein indicator solution, and titrate with either aqueous or alcoholic 0.2 N standard alkali solution. Calculate the acid number, in milligrams of KOH per gram of sample, as follows: Acid number = (V x N x 56.1 )/5 where: iV = normality of the standard alkali solution. V -- millilitres of alkali solution. 9. Free Rosin Acids 9.1 Calculate the percentage of free rosin acids in the oil, oh the basis of a molecular weight of 302 for such adds, as follows: Rosin acids, % = (KxJVx 0.302 x 100)/5 = acid number'X 0.539 No t e 2--If the sample is a compounded oil containing tall oil or other fatty acid components, it will be necessary todetermine the rosin acid .number by an esterification process such as the modified Wolfe procedure given in the Methods D 805 after which the percentage of rosin acids present is determined by multiplying the rosin acid number by the factor 0.539.10 10. Volatile Matter 10.1 Weigh 5.0 g of the oil into a tared flat-bottom straight-side metal dish having a diameter of approximately 3 in. (76 mm). Place in an oven at 105 2C for 2 h. Retnojjf to a desiccator, cool, and weigh. The loss in weight shaHjf %Mreported as volatile loss on heating, to the nearest 0.1 No t e 3--Wide deviations in the percentage of volatile matter!! rosin oil may result when different types ofovens are used for this tesla a purchaser ofrosin oil establishes a limit for volatile matter, the type! oven used, whether convection or forced draft, should be clMjfS indicated. ' * 11. Moisture 11.1 Determine the moisture in rosin oil on a 200-ej l S sample in accordance with Sections 15 to 17 of Method D 856 or as described in the Test Method D 95, using either xylene or petroleum naphtha as the solvent. 12. Ash \ 12.1 Determine the ash in rosin oil. inAk, accordance Test Method D 1063. 1 13. Mineral Oil , i|r 13.1 -Transfer 10 mL of the rosin oil to a 300-tffl round-bottom Florence flask, and cool by immersion oftfl body of the flask in an ice bath. Introduce dropwise into sample from a dropping pipet, 40 mL of fuming nitric aeit| (90 % HNO3), starting at a rate of 1 drop/2 s and shakinglh! flask after each drop falls into the sample. When the reactioif. becomes less violent, the interval between drops may be ^ shortened. When all the acid has been added, shake the ^ contents of the flask vigorously for a few seconds, keeping it cool until the reaction is complete. ^ 13.2 Transfer the sample to a 50-mL graduated cyliink 1 and allow to stand. Unreacted mineral oil will rise to Ihe^ surface of the mixture. The refractive index ofthe mineral-oil t should be less than 1.500. 13.3 Read the volume of mineral oil and calculate 1he percentage to the nearest 0.2 %. The American,Society for. Testing and Materials takes no position respecting the validity otany patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity df 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 orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments wm 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. 160 DUPO 502 95826 esignation: D 1133 - 90 Standard Test Method for Kauri-Butanol Value of Hydrocarbon Solvents1 This standard is issued under the fixed designation D 1133; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A Superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 5191 ofFederal TestMethod Standard No. 141a. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. as test method covers the determination of the Solvent power of hydrocarbon solvents used in paint Her formulations. This test methof is suitable for use vents having an initial boiling poilit over 40"C and a T under 300C when determined in accordance with dures ip Note 1. 1--Method D 86 is used to determine the initial boiling point .point for tnineral spirits and similar petroleum solvents. Test D 1078 is used for pure compounds and narrow boiling range This standard does not purport to address the safety s associated with its use. It is the responsibility ofthe if this standard to establish appropriate safety and ipractices and determine the applicability ofregulatory ions prior to use. For specific hazard information and guidance, consult pplier's Material Safety Data Sheet, ferenced Documents ASTM Standards: ` Method for Distillation of Petroleum Products2 04 Specification for n-Butyl Alcohol (Butanol)2 611 Test Methods for Aniline Point and Mixed Aniline oint of Petroleum Products and Hydrocarbon Solvents2 _41 Specification for Nitration Grade Toluene2 1078 Test Method for Distillation Range of Volatile liOrganic liquids3 p efinition 4 kauri-butanol value--of a solvent, the volume in 'litres at 25C of the solvent, corrected to a defined dard, required to produce a defined degree of turbidity en added to 20 g of a standard solution of kauri resin in rmal butyl alcohol. The kauri resin solution is standardagainst toluene* which has an assigned value of 105, and mixture of 75 % /2-heptane and 25 % toluene on a volume is, which has an assigned value of 40. 4. Significance and Use 4.1 The kauri-butanol value is used as a measure of solvent power of hydrocarbon solvents. High kauri-butanol values indicate relatively strong solvency. 5. Apparatus 5.1 Water Bath, a clear-glass vessel, maintained at 25 1C. Alternatively, a room maintained at 25 1C may be used. 5.2 Volumetric Flash 200-mL capacity. 5.3 Erlenmeyer Flash 250-mL capacity. 5.4 Buret, 50-mL capacity. ' 5.5 Print Specimen--A sheet of white paper having on it ' black 10 on 12 point print, No. 31 Bruce old style type. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise specified. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi nation. 6.2 Kauri-Butanol Solution5--Place in a 3-L flask 400 g of clean, pale, bold kauri resin of Grade XXXX, XXX, or XX ground to pea-size or smaller. Add, while agitating vigor ously, 2000 g of n-butyl alcohol, (conforming to Specifica tion D 304). Shake on a mechanical shaker until the resin goes into solution, warming to about 55C, if necessary to aid solution. If a mechanical shaker is not available, fit the flask with a reflux condenser and heat on a steam bath until all of the kauri resin is dissolved. Permit the solution to stand 48 h and then clarify by filtering through a Buchner funnel with suction, using double filter paper and changing as frequently as necessary. 6.3 Standard Toluene conforming to Specification D 841 for-use as a high-solvency standard. 6.4 Heptane-Toluene Blend consisting of 25 0.1 % 1 This tea method is under die jurisdiction of ASTM Committee D-l on Paint d Related Coatings and Materials and is the direct responsibility of Subcomttee DOl.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally blished as D 1133 - 50 T. Laa previous edition D 1133 - 86. 1 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 06.03. * "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." 5 Prepared kauri-butanol solutions are available from the Chemical Service Laboratories, 5543 Dyer St., Dallas, TX 75206. 161 DUP050295827 # D 1133 toluene and 75 + 0.1 % n-heptane on a volume basis, for use as a low-solvency standard. The heptane shall conform to the requirements for knock test grade n-heptane prescribed in Table 1 of Test Methods D 611. Nora 2--The blend of 25 0.1 % toluene and 75 0.1 % heptane can be prepared in any way that will give the desired accuracy. The following technique is adequate: Bring the toluene and heptane and a calibrated 200-mL volumetric flask to the same temperature, preferably in a constant-temperature room or thermostat. Run 50 mL of toluene into the 200-mL volumetric flask, using a buret or pipet calibrated to deliver 50 mL of toluene at the chosen temperature (preferably 25C). Rll the volumetric flask to slightly below the calibration line with n-heptane, insert the ground-glass stopper of the volumetric flask, and mix carefully by repeatedly inverting the flask. Allow to stand for a few minutes; then bring to the 200-mL calibration mark with heptane and again carefully mix. 7. Standardization 7.1 Weigh out 20 0.10 g of kauri-butanol solution in a 250-mL Erlenmeyer flask and place in the water bath at 25C. Titrate with the standard toluene into the flask, with constant swirling, while maintaining the mixture in the flask at 25 1C. Gradually reduce the successive amounts of toluene added as the end point is approached. The end point is reached when the sharp outlines of 10-point print placed directly beneath the water bath and observed through the liquid are obscured or blurred, but not to the point where the print becomes illegible. Check the temperature in the flask immediately after the end point has been reached, and if over 26C or under 24C, repeat the titration. 7.2 The volume of toluene used, in millilitres, represents the actual titer for the particular kauri-butanol solution at hand. This value should lie reasonably close to 105 mL, but not oyer 110 nor under 100 mL. If these limits are exceeded, adjust the concentration of the kauri-butanol solution to bring the total volume of toluene within them. Designate the final value using toluene as A. 7.3 Weigh out 20 0.10 g of the kauri-butanol solution (adjusted as described in 7.2) in a 250-mL Erlenmeyer flask and place in the water bath. Titrate with the heptane-toluene blend in the same manner as described in 7.1. Designate the volume, in millilitres, ofthe blend used in this titration as B. No t e 3--Ifthe composition of the blend is known to differ from 25 .1.0% toluene, but is within the range from 22 to 28 % toluene, the constant in the blend factor equation will differ from 40.0 by 0,60 units for each 1 % toluene. For example, at 28 % toluene, the constant is 41.8 instead of 40.0. No t e 4--Freshly prepared kauri-butanol solution may change in standardization from day to day. It is, therefore, desirable to permit the solution to age before initial standardization and, in any case,- the standardization should be rechecked on successive days until the toluene factor and blend factor remain constant 8. Procedure 8.1 Weigh 20 + 0.10 g of the adjusted kauri-butanol solution into a 250-mL Erlenmeyer flask. Place the flask is the water bath at 25 1C. Fill the 50-mL buret with the solvent being tested and titrate the solvent into the Erlenmeyer flask with constant swirling while maintaining the mixture in the flask at 25C. Gradually reduce the successive amounts of solvent added as the end point is approached. The end point is reached when the sharp outlines of 10-point print (see 5.5) placed directly beneath the water bath and observed through the liquid are obscured or blurred, but not to the point where the print becomes illegible. Check the temperature in the flask immediately after the end point has been reached and if over 26C or under 24C, repeat the titration. Designate the volume of solvent, in millilitres, to produce turbidity as C. 9. Calculation ( 9.1 Calculate the kauri-butanol value, vF, as follows: V = [65<C - B)/(A - B)] + 40 where: A = toluene required to titrate 20 g of kauri-butano: solution (7.2), mL, B - heptane-toluene blend required to titrate 20 g o: kauri-butanol solution (7.3), mL, and C = solvent under test required to titrate 20 g of kauri butanol solution (Section 8), mL. 9.2 If the buret is maintained at a temperature other thai 25 1 C, correct the volume of solvent used, S, in millilitres to standard temperature as follows: C(25 - r) x 0.0009 where: C = solvent used in the titration, mL, and T = temperature of the solvent in the buret, C. 10. Precision and Bias 10.1 The following criteria should be used forjudging th acceptability of the results in the range from 30 to 90 at th 95 % confidence level. 10.1.1 Repeatability--Two results, each the mean of di plicates, obtained by the same operator on different daj should be considered suspect if they differ by more than 0.0 K -- 0.1, where K = mean kauri-butanol value. 10.1.2 Reproducibility--Two results, each the mean ( duplicates, obtained by two laboratories should not t considered suspect unless they differ by more than 0.03 K 1.0 where K = mean kauri-butanol value. 10.2 Bias--Test bias can result if the kauri-butanol soli tion is not carefully standardized and adjusted (see 7.2 an 7.3). 11. Keywords 1 l.l kauri-butanol value; hydrocarbon solvents The American Society for Testing and Materials takes noposition respecting trie validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination oi the validity of any such patera rights, and the risk oi infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor 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 carefut consideration at a meeting of the responsible technical committee, which you may attend, ti 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. 162 DUP050295828 Designation: D 1152 - 89 & Standard Specification for Methanol (Methyl Alcohol)*1 This standard is issued under the fixed designation D 1152; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A numbfer in parentheses indicates the year of last reapproval. A 'i superscript epsilon (<) indicates an editorial change since the last-revision or reapproval. cijpe 1Jfhis specification covers methanol (99.85 % grade). fThis standard may involve hazardous materials, oper and equipment. This standard does not purport to jail ofthe safety problems associated with its use. It is %ponsibility of the user of this standard to establish riate safety and health practices andi determine the ability of regulatory limitations prior to use. For c hazard statements, see Section 5. For specific hazard information and guidance, see tire `er's Material Safety Date Sheet for materials listed in specification. pferenced Documents V2.1 ASTM Standards: 1296 Test Method for Odor of Volatile Solvents and (Diluents2 1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re flated Products2 -. 300 Practice for Sampling Industrial Chemicals3 346 Methods for Analysis of Methanol4 -2 U.S. Fed. Specification: P-C-2020 Federal Specification Packaging of Chemi cals, Liquid, Dry, and Paste5 Properties 3.1 Methanol (99.85 % grade) shall conform to the fol ding requirements: ** This specification is under the jurisdiction of ASTM Committee D-l on Paint 1 Related Coatings and Materials and is the direct responsibility of Subcom- `ttee D01.35;on Solvents, Plasticizers and Chemical-Intermediates. Current edition approved March 31, 1989. Published May 1?89. Originally ublished as D 1152 - 31. Last previous edition D 1152 - 84". 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vots 06.03 and 15.05. " Annual Book ofASTM Standards, Vd 15.05. 5 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. Apparent specific gravity: 20/20"C 25/25'C Color, Pt-CO. max Distillation range, C, max Nonvolatile matter, mg/100 mL, max Odor Water, weight %, max Acidity (free add as acetic acid), weight %, max Acetone, weight %, max Hydrocarbons Sulfuric acid wash test (carbonizable impurities) Color, Pt-Co, max Permanganate time, min. 0.7920 to 0.7930 0.7883 to 0.7893 10 1.0 (to include 64.6 6.1) 5 nonresidual 0.10 0.003, equivalent to 0.028 mg KOH per gram of material 0.003 to pass test 50 50 4. Sampling 4.1 Sample the material in accordance with Practice E 300. 5. Hazards 5. i Methanol is toxic both as a liquid and as a vapor, and is dangerous if not properly handled. Avoid any skin contact. 5.2 Methanol is flammable and its vapor is explosive in air. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with Methods E 346 and the following methods: 6.1.1 Nonvolatile Matter--Test Method D 1353. 6.1.2 Odor--Test Method D 1296;. 7. Packaging and Package Marking 7.1 Package size shall be agreed upon between the pur chaser and the supplier. 1.2 Packaging shall conform to applicable earner rules and regulations or when specified shall conform to U.S. Fed. Spec. PPP-C-2020. TheAmerican Society for Testing and Materials takes no.posltion 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 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/eot to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn.. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments 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. 163 DUP050295829 Designation: D 1153 - 90 Standard Specification for Methyl isobutyl Ketone1,2 This standard is issued under the fixed designation D 1153; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has beat adopted by the Department ofDefense. 1. Scope 1.1 This specification covers methyl isobutyl ketone (99.0 % grade). 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint Related Coatings and Material13 * D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale)3 D1296 Test Method for Odor of Volatile Solvents and Diluents3 . D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1476 Test Method for Heptane Miscibility of Lacquer Solvents3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D 3329 Test Method for Purity of Methyl Isobutyi Ketone by Gas Chromatography3 /s D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 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 01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct 26,1990. Published December 1990. Originallypublished as D 1153 - 51 T. Last previous edition D 1153 - 87. 1 This compound is also known under the name of 2-methyl pentanooe-4. 3 Annual Book ofASTM Standards, Vol 06.03. * Annual Book ofASTM Standards, Vol 05.03. 5 Annual Book ofASTM Standards, Vote 05.03 and 14.03. 6 Annual Book ofASTM Standards. Vols 06.03 and 15.05, 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 191U-5094. 3. Properties 3.1 Methyl isobutyl ketone (99,0 % grade) shall conform to the following requirements: Methyl isobutyl ketone wt %, min Apparent specific gravity: 20/20'C 25/25'C Color, Pt-Co units, max Distillation, C Initial boiling point, min.. Dry point, max Nonvolatile matter, mg/100 mL, max Odor Water, wt %, max-4 Acidity (free acid as acetic arid), wt %, max Methyl isobutyi carbine!, wt %, max 99.0 0.800.to 0.803 0.796 to 0.799 15 114.0 117.0 5 nonresidual 0.1 0.01 0.3 4 This quantitative water'limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20"C. 4. Sampling 4.1 The material shall be sampled in accordance with Practice E300. 5. Test Methods 5.1 The properties enumerated in this application shall be determined in accordance with the following ASTM test Methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the. third decimal place, the temperature of both specimen and water being 20 or 25C. See Test Methods D 268 or D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer having a range from 98 to 152"C and conforming to the requirements for Thermometer 41C as prescribed in Specification E 1. 5.1.4 Nonvolatile Matter--Test Method D 1353, 5.1.5 Odor--iTest Method D 1296. 5.1.6 Water--Test Method D 1364 or D 1476. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Alcohol and Purity--Method D 3329. 6. Packaging and Package Marking 6.1 Package site shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 ketones; methyl isobutyi ketone (MIBK); solvents 164 DUP050295830 # D 1153 The American Society tor Testing and Materials takes no position respecting the validity ofarry 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. Yourcomments are Invited either for revision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of 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 19103.165 .i 165 DUP050295831 Designation: D 1193 - 91 Standard No. 7816 Standard Specification for Reagent Water1 This standard is issued under the fixed designation D 1193; the number immediately following the designation indicates tfie year of original adoption or', in the case of revisioif, 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 ike specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This specification covers requirements for water suit able for use in methods of chemical analysis and physical testing. Four grades are specified: Type! Type II Typeffl Type IV Electrical conductivity, 0.056 1.0 0.25 5.0 max, pS/cm at 298 K <2SC) Electrical resistivity, min, 18.0 1.0 4.0 0.2 MS-cm at 298 K (25"C) pH at 298 K. (25"C) A A A 5.0 to 8.0 Total organic carbon 100 50 200 o limit (TOC), max, pg/L Sodium, max, pg/L l 5 10 50 Chlorides, max, pg/L 1 5 10 50 Total silica, max, pg/L 3 3 500 no limit Microbiological contamination---When bacterial levels need to be controlled, reagent grade types should be further classified as follows: Type A Type B Type C Maximum heterotropic 10/1000 mL 10/100 mL 100/10 mL bacteria count Endotoxin, EUfl <0.03 0.25 not appli- cable * The measurement of pH in Type I, II, and 111 reagent waters has been eliminated from this specification because these grades of water do not contain constituents in sufficient quantity to significantly alter the pH. 3 EU Endotoxin Units. 1.2 The method of preparation of the various grades of reagent water determines the limits of impurities and shall be as follows: 1.2.1 Type I grade of reagent water shall be prepared by distillation or other equal process, followed by polishing with a mixed bed of ion exchange materials and a 0.2-p.m membrane filter. Feedwater to the final polishing step must have a maximum conductivity of 20 pS/cm at 298K (25C). 1.2.2 Type II grade of reagent water shah be prepared by distillation using a still designed tq produce a distillate having a conductivity ofless than 1.0 pS/cm at 298 K (25C). Ion exchange, distillation, or reverse osmosis and organic adsorption may be required prior to distillation if the purity cannot be attained by single distillation. No t e--Because distillation is a process commonly relied upon to produce high purity water, the levels specified for Type II reagent water were selected to represent the minimum quality of water that a distillation process should produce. 1.2.3 Type III grade of reagent water shall be prepared by distillation, ion exchange, reverse osmosis, or a combination thereof, followed by polishing with a 0.45-pm membrane filter. 1.2.4 Type IV grade of reagent water may be prepared by distillation, ion exchange, reverse osmosis, electrodialysis, or a combination thereof. 1.3 The choice of one of the various grades may be designated by the method or by theinvestigator. 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 appropriate safety and health practices and determine the applicabttity of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1125 Test Methods for Electrical Conductivity and Resistivity of Water2 D 1129 Terminology Relating to Water2 D1293 Test Methods for pH of Water2 D 1428 Test Methods for Sodium and Potassium in Water and Water-Formed Deposits by Flame Photometry3 D4453 Practice for Handling of Ultra-Pure Water Samples2 D45I7 Test Method for Low-Level Total Silica in High- Purity Water by Flameless Atomic Absorption Spectros copy4 D4779 Test Method for Total, Organic, and Inorganic Carbon in High Purity Water by Ultraviolet (UV) or Persulfate Oxidation, or Both, and Infrared Detection4 F 1094 Test Methods for Microbiological Monitoring of Water Used for Processing Electron and Microelectronic Devices by Direct Pressure Tap Sampling Valve and by the Presterilized Plastic Bag Method5 3. Terminology 3.1 Definitions--For definitions used in this specification refer to Terminology D 1129. 4. Significance and Use 4.1 Different analytical methods and industrial processes require water of different purities. Also, different types of contaminants affect these methods and processes differently. This specification is intended to provide the user with a s|j ! ijj fl r jjfi M | \ | \: I f \ t j j j ? d 1 This specification is under the jurisdiction of ASTM Committee D-19 on Water and is the responsibility of Subcommittee D19.02 on General Specifica tions, Technical Resources, and Statistical Methods. Current edition approved Sept. 15,1991. Published November 1991. Originally issued as D 1193-51 T. Last previous edition D1193-77 (1983)1. 2 Annual Book ofASTM Standards, Vol 11.01. 3 Discontinued 1990--See 1989 Annual Book ofASTM Standards, Vo! 11.01. 4 Annua! Book ofASTM Standards. Vol 11.02. 5 Annual Book ofASTM Standards, Vol 10.04. 166 DUP050295832 D 1193 |fdifferent grades of water having different purities as in Section 1. It is intended to satisfy the require- for normal laboratory prd^dures, but does not idly apply to the large-scale production of pure water jtecific applications. Different grades of water may be ""by other ASTM specifications or guides, or by the -ents of other standards organizations. and Application The method of preparing Type I reagent water may nic contaminants to the water by contact with the hange materials. It should be noted also that the may or may not remove non-ionized dissolved gases. 1 The dissolved or particulate organic contamination : normally range from 30 to 50 pg/L. The concentraf rionionized dissolved gases may exceed 5 mg/L. The quality of the effluent water depends upon the ge, and method of regeneration of the ion exchange Is. Likewise, the flow rate through the ion exchange bed will change the conductivity of the effluent water. structions of the manufacturer of the resins or the cartridge bed should be followed. The use of the membrane filter in the preparation of I and Type III water may add a small amount of :c components to the water first produced. 1 Some membrane filters contain as much as 8 % of soluble components resulting from the manufacprocess. .2 If the contamination of the water by the organic onent is of significance to the test, Type II water should ed or the membrane should be rinsed by discarding the 10 mL of water produced per square centimetre of filter and until a test for the organic components shows them ave been reduced to less than the specified level. Type II grade of reagent water should be sterile and gen-free as produced and generally may be used whenr freedom from organic or biological contaminants is able. However, the method of storage and handling of e water may itself result in contamination. 5.4.1 Type II water should be pyrogen-free, but must be sted in conformance with the requirements of the current ition of U.S.P. if proof is needed. 5.4.2 The description of Type II reagent water is intended characterize the product of distillation. 5.4.3 Distilled water is often specified when freedom from otes and silica is required, or when surface-active organics are proven to be a problem, and when alternative processes jjave been found to be inadequate. 5.5 Types I, II, and HI reagent water should be protected from atmospheric contamination and from solution of container and tubing materials. 5.5.1 Extreme care must be exercised in handling samples when making an analysis. Sample containers and tubing should be made of TFE-fluorocarbon, titanium, tantalum. block tin, quartz, 18-8 stainless steel, polyethylene, or other material proven to be sufficiently resistant to chemical attack so as not to cause contamination in the intended use. Practice D 4453 should be consulted. 5.6 Because atmospheric gases and impurities rapidly recontaminate exposed water, in-line electrodes should be employed for determining the electrical conductivity of reagent water Types I, II, and III. The measurement of pH in Type I, II, and III reagent waters has been eliminated from this specification because the values would be a function of the instrumentation. 5.7 Since freedom from biological contaminants may be important in the test procedure using any of the reagent waters specified, a classification of bacterial levels is included and should be specified ifit is of significance to the test being performed. 5.7.1 To obtain sterile water, any of the types of reagent water listed in this section may be produced, bottled, and heated to 394 K (121 C) for 20 min. This procedure is most easily carried out by autoclaving at 103 kPa (15 psi) for 20 min. 5.8 Thefollowing requirement is beyond the requirements ofthe general specifications: The use of reagent grade water should recognize that analytes may exist in water that meets the criteria listed in Section 1, but these analytes may interfere with the use of the water. If levels of other analytes are important, it is the user's responsibility to specify their limits. 6. Requirements 6.1 Reagent water shall conform to the requirements specified in Section 1. 6.2 Additional requirements concerning specific contami nants or methods of preparation may be included in this specification by mutual agreement between the parties con cerned. 7. Test Methods 7.1 Electrical Conductivity and Resistivity--Refer to Test Methods D 1125. 7.2 pH--Refer to Test Methods D 1293. 7.3 Silica--Refer to Test Method D 4517. 7.4 Sodium--Refer to Test Methods D 1428. 7.5 Chlorides.6 7.6 TOC--Refer to Test Method D 4779. 7.7 Endotoxins--Refer to LAL Test Method.7 7.8 Microbiological Contamination--Refer to Test Methods F1094. 8. Keywords 8.1 laboratory analysis; reagent; water 6 A new test method, for trace anions and cations in high purity water by ion-chromatography procedure, is under development by Subcommittee D19.ll. 7 Published in U.S. Pharmacopeia by The U.S. Pharmacopeia Convention, Inc. 167 DU P0502 95833 D 1193 The American Society for Testing and Materials takes no position respectingthe validity of any patent rights asserted in canhection with any item mentioned in this standard, Users of. this standard are expressly advised that determination of the validity of any'puch 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 ftve years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should peaadressed.to, ASTM Headquarters. Your comments wilt 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, 1916 Race St., Philadelphia, PA 19103. v, I I I ij 168 DUP050295834 Designation: D 1209 - 84 (Reapproved 1988)e1 Standard Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)1 * This standard is issued under the fixed .designation D1209; 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 reappravaL A superscript epsilon (<) indicatesan editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4243.1 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications andStandardsfor the specificyear ofissue which has been adopted by the Department ,qfDefense. " No t e--Paragraph 1.3 and Footnotes 6, 7, and 10 were added editorially and subsequent footnotes renumbered in March 1988. iiThis test method describes a procedure for the visual ement of the color of essentially light colored liquids 1). It is applicable only to materials in which the producing bodies present have light absorption characnearly identical with those of the platinum-cobalt standards used. E 1--A procedure for estimating color of darker liquids, de fer soluble nitrocellulose base solutions, is given in Methods v This standard may involve hazardous materials, oper* and equipment. This standard does not purport to ssall ofthe safety problems associated with its use. It is esponsibility of the user of this standard to establish ppriate safety and health practices and determine the icability of regulatory Imitations pripr to use. For 5c hazard statements see Section 6. 3 For hazard information and guidance, see the sup-. *s Material Safety Data Sheet. fefenceif Documents .1 ASTM Standards: 156 Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method)* 365 Test Methods for Soluble Nitrocellulose Base Solutions3 1193 Specification for Reagent Water4 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals5 E-202 Method for Analysis of Ethylene Glycols and J i . Propylene Glycols5 sE 34.6 Method for Analysis of Methanol6 * 8 1This test method is under the jurisdiction of ASTM Committee D-l on Paint id Related Coatings and Materials and is the direct responsibility of SubcomHtee 001.35 bn Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27, 1984. Published August 1984. . Originally Wished as D 1209 - 52. Last previous edition D 1209 - 79. \Anmtal Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Bode ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Bode ofASTMStandards, Vol 15.05. 6 Annual Book ofASTM Standards, Vol 15.05. 3. Significance and Use 3.1 The property of color of a solvent varies in impor tance with the application for which it is intended, the amount of color that can be tolerated being dependent on the color characteristics of the material in which it is used. The paint, varnish, and lacquer solvents, or diluents com mercially available on today's market normally have little or no color. The presence or absence ofcolor in such material is an indication of the degree of refinement to which the solvent has been subjected or of the cleanliness of the shipping or storage container in which it is handled, or both. 3.2 For a number of years the term "water-white" was . considered sufficient as a measurement of solvent color. Several expressions for defining "water-white" gradually appeared and it became evident that a more precise color standard was needed. This was accomplished in 1952 with the adoption of Test Method D 1209 using the platinumcobalt scale. This test method is similar to the description givSn in Standard Methods for the Examination of Water and Waste Water7 and is referred to by many as "APHA Color." Die preparation of these platinum-cobalt color standards was originally described by A. Hazen in the American Chemical Journal in which he assigned the number 5 (parts per ten thousand) to his platinum-cobalt stock solution. Subsequently, in their first edition (1905) of Standard Methods for the Examination of Water, the American Public Health Association, using exactly the same concentration of reagents, assigned the color designation 500 (parts per million) which is the same ratio. The pails per million nomenclature is not used since color is not referred directly to a weight relationship. It is therefore recommended that the incorrect term "Hazen Color" should not be used. Also, because it refers primarily to water, the term "APHA Color" is undesirable. The recommended nomenclature for referring to the color of organic'liquids is "Platinum-Cobalt Color, Test Method D 1209." 3.3 The petroleum industry uses the Saybolt colorimeter Test Method D 156 for measuring and defining the color of hydrocarbon solvents; however, this system of color mea surement is not commonly employed outside of the petro- 1 Standard Methods for the Examination of Water and Waste Water, M. Franson, Ed., American Public Health Assoc., 14th ed., 1975, p. 65. 8 Hazen, A, "New Color Standard for Natural Waters," American Chemical Journal, Vol XIV, 1892, p. 300-310. 169 DUP050295835 D 1209 TABLE 1 Absorbance Tolerance Limits For No. 500 PlatinumCobalt Stock Solution Wavelength, nm Absorbance 430 0.110 to 0.120 455 0.130 to 0.145 ` 450 0.105 to 0.120 510 0.055 to 0.065 leum industry. It has been reported by various sources that a Saybolt color of +25 is equivalent to 25 in the platinumcobalt system or to colors produced by masses of potassium dichromate ranging between 4.8 and 5.6 mg dissolved in 1 L of distilled water. Because of the differences in the spectral characteristics of the several color systems being compared and the subjective manner in which the measurements are made, exact equivalencies are difficult to obtain. 4. Apparatus 4.1 Spectrophotqnietef,''equipped for.liquid samples and for measurements in the visible regioft.9 ! No t e 2-7-The spectrophotometer used must be clean and in first- class operating condition. The. instrument should be calibrated in accordance with the instructions given in the Standards for Checking the Calibration of Spectrophotometers (200 to 1000 ran).910 4-2 Spectrophotometer Cells, matched haying a 10-mm light path. < . 4.3 Color Comparison Tubes--Matched. 100-mL, tail- form Nessler tubes, provided with ground-on, optically clear, glass caps. Tubes should be selected so that the height of the 100-mL graduation mark is 275 to ,295 min above the bottom of the tube. 4.4 Color Comparator--A color comparator constructed to permit visual comparison of light , transmitted through tail-form, 100-mL Nessler tubes in the direction of their longitudinal axes. The comparator should be constructed so that white light is passed through or reflected offa,white glass plate and directed with equal intensity through the tubes, and should be shielded so that no light enters the tubes from the side.11 5, Reagents ' 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are ,available!12 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water 9 The Beckman Model B and its equivalents have been found satisfactory for this purpose. 10 See National Bureau of Standards Letter Circular LC-1017. 11 A unit available from Scientific Glass and Instruments, Inc., P.O. Box 6, Houston, TX 77001, has been found suitable for this purpose. 12 "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." TABLE 2 Platinum-Cobalt Color Standards Color Standard Number 5' 10 15 20 25 30 35 40 50 60 Stock Solution, mL 1 2 3 4, -. 5 . 7 8 10 12 Color Standard Number 70 V 100 150 200 : 250 < x 300- v 350 400 ' 450 500 Stock Solution, mL 14 20 30 40 50 60 70 80 90 100-* A This is platinum-cobalt color No. 10 in Methods D 365. conforming to Type IV of Specification D 1193. 5.3 Cobalt Chloride (CoCI2-6H20). 5.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro- chloric acid (HC1). . 5.5 Potassium Chloroplatinate (K2PtCl6). 6. Hazards 6.1 Concentrated hydrochloric acid is a corrosive chem ical. 7. Platinum-Cobalt Reference Standards 7.1 Platinum-Cobalt Stock Solution--Dissolve 1.245 g of potassium chloroplatinate (K2PtCl6) and LOO g of cobalt chloride (CoCl2 6H20) in water. Carefully add 100 mL of hydrochloric acid (HC1, sp gr 1.19) arid dilute to 1 L with water. The absorbance of the 500 platinum-cobalt stock solution in a cell having a 10-mm light path, with reagent water in a matched cell as the reference solution,13 must; fall within the limits-given in Table 1. 7.2 Platinum-Cobalt Standards--From the stock solu tion, prepare color standards in accordance with Table 2 by diluting the required volumes "to 100 mL with water in the Nessler tubes. Cap the tubes and seal the caps with shellac or a waterproof cement. When properly sealed and stored, these standaids are stable for at least 1 year and do not degrade markedly for 2 years.14 7-2.1 For a more precise measurement of light colors below 15 platinum-cobalt, prepare color standards from the stock solution in accordance with Table 3 by diluting the required volumes to 100 mL with water in the Nessler tubes. Use a semi-microburet for measuring the required amount of stock solution. 8. Procedure 8.1 Introduce 100 mL of. specimen into a Nessler tube, passing the specimen through a filter if it has any visible turbidity. Cap the tube, place in the comparator, and compare with the standards. 9. Report 9.1 Report as the color the number of the standard that 13 See the manufacturer's instruction manual for complete details for operating the spectrophotometer. 14 Scharf, W. W., Ferber, K. H., and White, R. G,, "Stability of PlatinumCobalt Color Standards." Materials Research and Standards, Vot 6, No. 6, June 1966, pp. 302-304. 170 DUP0502 95836 D 1209 |jjj; ptatimim-Cohalt Color Standards for Very Light Colors H stock Ip Solution, Hgr mL Color Standard. Number j Stock Solution, mL f". 0.20 |i 0.40 fr 0.60 Ji 0.80 || 1.00 1.20 s 1.40 y 1.60 9 10 11 12 13 . 14 1 ---- 1.80 2.00 2.20 2.40 2.60 ' 2.80 3.00 **nearly matches the specimen. In the event that the es midway between two standards, report the darker K .: S; If, owing to differences in hue between the specimen jie* standards, a definite match cannot be obtained, range over which an apparent match is obtained, seport the material as "off-hue." iecisionIS [Color Standards: These precision statements are. based upon an IJpratory study in which five platinum-cobait standlaying values of 25, 75,, 170, 385, and, 475 were red in accordance with the instructions given in Section this test , method and were given coded labels. These ions were tested by ope analyst in each of ten different atories making a single observation on one day and (repeating the observation on a second day. The analysts : requested to estimate the color to the nearest one unit ^solutions below 40 platinum-cobalt, to the nearest five for solutions between 40 and 100 platinum-cobalt and lie nearest ten units for solutions above 100 platinum- cobalt. In this interlaboratory study, the within-laboratory coefficient of variation was found to be 1.8 % with 60 degrees of freedom, and the between-laboratories coefficient of variation was found to be 5.3 % with 54 degrees of freedom. Based oh these results, the following criteria, calculated in accordance with Practice E 180, should be used for judging the acceptability of results at the 95 % confidence level when the results are obtained under optimum condi tions where ithe hue of the sample matches exactly the hue of the standards. Poorer precision will be obtained in varying degrees as the hue of the sample departs from that of the standards. 10.1.1.1 Repeatability--Two results, obtained by the same analyst on different days, should be considered suspect if they differ by more than 5.1 %. 10.1.1.2 Reproducibility--Two results, obtained by ana lysts in different laboratories, should be considered suspect if they differ by more than 15 %. 10.2 Specimen:16 10.2.1 In ah interlaboratory study of this'test method in which the standards described in Table 3 were used, the within-laboratory standard deviation was found to be one platinum-cobalt unit at 56 degrees of freedom and the between-laboratory standard deviation was found to be 2 platinum-cobalt units at 25 degrees of freedom. Based on these standard deviations, the following criteria should be used for judging, at the 95 % confidence level, the accept ability of results obtained on light , colored samples. 10.2.1.1 Repeatability--Two results, each the mean of duplicates, obtained by the same operator on different days should be considered suspect if they differ by more than two platinum-cobalt units. 10.2.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than seven platinum-cobalt units. i'3,Supporting data are available from ASTM Headquarters. Request RR; J111024. 16 These precision statements are based on interlaboratory studies conducted by Committee E-15 on industrial Chemicals on samples of ethylene glycol and methanol as reported in Method E 202, Method E 346, and research report RR: E15-28. The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this Standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and the risk o/ 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, eitherreapprgved or withdrawn. Your comments are invitedeithertorrevision ofthis standard orfor additional standards 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 oh Standards, 1916 Race St., Philadelphia, PA 19103. 171 DUP050295837 Designation: D 1240 - 82 Standard Test Method for Rosin Acids in Fatty Acids1 This standard is issued under the fixed designation D 1240; 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 method covers the determination of rosin adds in fatty adds when the rosin adds content does not exceed 15%. 2. Summary of Method 2.1 The rosin acids are determined by titration, after esterification ofthe fatty adds with methanol in the presence of sulfuric acid as a catalyst. Followed by separation of the acids. The method requires use of an experimentally deter mined cprrectioh factor, dependent upon the amount of rosin acids present.2 3. Apparatus 3.1 Flask, 250-mL flat-bottom, of chemically resistant glass with a standard-taper 24/40 neck. 3.2 Condenser, water-cooled; with a joint fitting the flask described in 3.1. 3.3 Separatory Funnel, 500-mL,' pear-shaped, fitted with a glass stopper. 3.4 Buret, 50-mL capacity, with 0.1-mL divisions. 4. Purity of Reagents and Water 4.1 Unless otherwise indicated, it is intended that all reagents shall conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Society,3 where such specifications are available. 4.2 References to water shall be understood to mean distilled water. 5. Reagents 5.1 Alcohol--Neutral methanol, neutral isopropanol (91 to 99 %), neutral 95 % ethanol, or neutral denatured alcohol conforming to formula No. 30 or No. 3A of the U. S. Bureau of Internal Revenue. 1 This method is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.34 on Naval Stores. Current edition approved March 26, (982. Published June 1982. Originally published as D 1240 - 52 T. Last previous edition D1240 - 54 (1981). 2 For information on the development ofthis method and the establishment of the correction factor, see Herrlinger, R. and Compeau, O. M., "The Determination of Rosin in Fatty Acids," Journal ofthe American Oil Chemists' Society. JAOCA, August 1952, pp. 342-344. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. Soc-, Washington, D. C 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, N. Y., and the "United States Pharmacopeia," . 5.2 Ethyl Ether. * 5.3 Methanol (99.5 %). 5.4 Methyl Orange Indicator Solution--Dissolve 0.1 g of methyl ottmge in 100 mL of water. 5.5 Phenolphthalein Indicator Solution--Dissolve 1 g of phenolphthalein in 100 mL of methanol. 5.6 Potassium Hydroxide Standard Alcoholic Solution (0.2 N or 0'.5 N)--Dissolve 13.3 g of KOH (preferably in pellet form) for a 0.2 A solution or 33.3 g for a 0.5 Ab solution (see 6.3) in methanol (99.5 %) and dilute to 1 L with methanol. Standardize to 0.001 N. The standardized solu tion should be protected against evaporation and the absorp tion of C02 from the air, and should be restandardized frequently. 5.7 Sodium Sulfate Solution (100 g Na2S04/litre)-- Dissolve 100 g of anhydrous Na2S04 in water and dilute to 1 L. The resulting solution should have a pH of 7.2 0.4 (Note 1). No t e 1--A suitable pH adjustment may be made by adding dilute (5 %} NaOH solution to a faint pirik-red phenol phthalein color,; then ' adding dilute H2SQ4 (5 %) solution until the color ^discharged. 5.8 * Sulfuric Acid (sp gr 1.84)c 6. Procedure 6.1 Dissolve 40 0.1 g<of the sample in 100 mL of methanol in a 250-mL flat-bottom flask. Twirl, the flask,to dissolve the oil and add a clean boiling chip. Add slowly 5 mL of H2S04, while swirling the flask vigorously. Connect the flask to the condenser, apply heat, and reflux the contents for 10 min. Cool the flask to room temperature with cold water. 6.2 Add 250 mL of the Na2S04 solution to a 500-mL separatory funnel. Pour the contents of the flask into the funnel and complete the quantitative transfer of the flask contents with 100 mL of ether. Thoroughly shake the mixture in the funnel. Allow to settle, draw offthe salt layer, and discard. Wash the contents of the funnel twice again with 250-mL portions of Na2S04 solution. The last washing should not react pink to methyl orange indicator. 6.3 After removing the last wash, drain the contents of the separatory funnel into a 500-mL Erlenmeyer flask. Rinse the funnel with 20 mL of ether and add the rinsings to the flask. Add 20 mL of ethyl alcohol and 1 mL of the phenol phthalein indicator solution. Titrate to the appearance of a pink-red color using 0.2 N alcoholic KOH solution if the rosin acids content is less than 5 % or 0.5 N if more than 5%. 172 DUP050295838 1< ! don culate the percentage of rosin acids as follows: >0sin acids, % = (1.031 xANx 30.2)/S-0.74 D 1240 where: A = millilitres of KOH solution used for titration of the sample, N = normality of KOH solution, S -- grains of sample used, and 0.74 = correction factor2 for a rosin acids content not over 15 %. The American Society for Testing amt Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users 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 subfcpt to revision at any time by the responsible technical committee and must be reviewedevery five years and ifnot revised, eitherredffprpved or withdrawn. Your comments are Invited either forrevision of thisstandard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, 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. .' 173 DUP050295839 Designation: D 1257 - 90 Standard Specification for High-Gravity. Glycerin1,2 This standard is issued under the fixed designation D 1257; the number immediately following the designation 'Indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers high-gravity glycerin (98.7 weight %, minimum) for use in the manufacture of alkyd and other synthetic resins. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standard: D1258 Test Method for High-Gravity Glycerin13 2 2.2 U.S. Federal Standard: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of4 174 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1257 - 79. Last previous edition D 1257 - 84. 2 Also known as 1,2,3-propanetriol and glycerol. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Phikidelphia, PA 19111-5094, Attn; NPODS. 3. Properties 3.1 The glycerin shall conform to the following require ments: Apparent specific gravity, min: 15.6/15.6"C (60/60F) ' 25/25C Color, Pt-Co scale, max Sulfate ash, max, weight % Acid value, max, mg KOH per g of material ;J.2620 1.2587 < 20 0.1 0.3 4. Test Methods and Sampling 4.1 The material shall be sampled and the properties enumerated in this specification determined in accordance with Test Method D 1258. 5. Packaging and Package Marking 5.1 Package size to be agreed upon between the purchaser and supplier. 5.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 6. Keywords 6.1 high-gravity glycerins The American Society for Testing andMaterials takes no position respecting tire validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either tor revision 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 tee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 174 DUP0502 95840 Designation: D 1258 - 90 Standard Test Method for High-Gravity Glycerin1,2 This standard is issued under the fixed designation D 1258; 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. pe This test method covers the procedures for the samand testing of glycerin (1,2,3-propanetriol) for use in anufacture of alkyd resins and other synthetic resins. This standard does not purport to address the safety 'ems associated with its use. It is the responsibility ofthe. of this standard to establish appropriate safety and 'fh practices and determine the applicability ofregulatory dions prior to use. _ For ha2ard information and guidance, see the supsi Material Safety Data Stieet. .eferenced Documents 1 ASTM Standards: 891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals13 2 ,1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)4 >1613 Test Method for Acidity in Volatile Solvents and ,, Chemical Intermediates Used in Paint, Varnish, Lac quer and Related Products4 ID4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 300 Practice for Sampling Industrial Chemicals6 175 Significance and Use f; .'3,1 This test method provides a measurement of purity of gh-gravity glycerin. The results of these measurements can e used for specification acceptance. 1 This test method is under the jurisdiction of ASTM Committee D-I on Paint land Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.35 on Solvents,.Plasticizers, and Chemical intermediates. . Current edition approved May 25, 1990. Published July 1990. Originally published as b 1258 - 53. Last previous edition D 1258-86. 2 Also known as 1,2,3-pfopanetriol and glycerol." 3. Annual Book ofASTM Standards, Vol 15.05. 4 Annual Book ofASTM Standards; Vol 06,03. 5 Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 4. Sampling 4.1 Sample the material in accordance with Practice E 300. 5. Procedure 5.1 Apparent Specific Gravity--Determine the apparent specific gravity by a pycnometer method that is accurate to 0.0002, such as in Test Methods D 891 or D 4052. 5.2. Color--Determine the color in accordance with Test Method D 1209. 5.3 Sulfate Ash--Weigh to the nearest 0.001 g, 50 g of glycerin sample, into ap open, shallow dish of porcelain, platinum, or other suitable material. Heat the dish carefully until the contents can be ignited with a flame and allow it to burn without further application of heat in a place free of drafts. When burning ceases, allow the dish to cool to room temperature and then moisten the residue with 0.5 mL of concentrated sulfuric acid. Cautiously heat the dish until fumes are no longer evolved and the carbon is completely consumed. Ignite, cool in a desiccator, and weigh to 1 mg. Repeat until weight is constant within 1 mg. Calculate the percent of sulfate ash, A, as follows: A = (R/S) x 100 where: R = sulfate ash, g, and S = specimen used, g. No t e--The sulfate ash procedure is equivalent to the "Residue on Ignition" determination for glycerin in the Pharmacopeia of the United States, nineteenth revision. 514 Acid Value--Determine the percent acid in accord ance with Test Method D 1613. 6. Precision and Bias 6.1 The precision and bias of the test procedures pre sented in this test method have not been determined. 7. Keywords ' . 7.1 high-gravity glycerin , The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not 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, li you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1976 Race St, Philadelphia, PA 19103. 175 DUP0502 95841 Designation: D 1296 - 84 (Reapproved 1988)e1 Standard Test Method for Odor of Volatile Solvents and Diluents1 This standard is issued under the fixed designation D 1296; 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 standard has been approvedfor use by the Department ofDefense to replace Method 4401 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. 41 No t e--Sections 1 and 4 were changed editorially in March 1988. 1. Scope ' i 1.1 This test method covers a comparative procedure for having odor characteristics satisfactory to purchaser and manufacturer, are required. ; observing the characteristic aiid residual odors of volatile organic solvents and diluents to determine their odor accept 4. Hazards /,, 1 ability in a solvent system. . 4.1 Many solvents and diluents, such as some; akmiaji<| 1.2 It is not intended that this test method be employed to and aliphatic hydrocarbons, are hazardous or toxic. Tale i determine subtle odor differences between materials or to special precautions while determining the odor of these determine odor intensity. products. The tests should be made only as frequently as is 1.3 It is recommended that this test method not be necessary for control and the evaluations should be based on employed to determine the residual odor of a liquid if its short sniffs, inhaling'as little vapor as possible. time for evaporation to dryness at room temperature exceeds 4.2 Provide adequate ventilation to maintain solvent or 30 min or as agreed upon. diluent concentration below the personnel exposure limit 1.4 This standard may involve hazardous materials, oper value established for the general work area. ations, and equipment. This standard does not purport to 4.3 Other hazards may also be present. These may be, but address all ofthe safety problems associated with its use. It is are not limited to, flammable, combustible, corrosive, or 1 the responsibility Of the user of this standard to establish explosive (monomers) hazards. appropriate safety and health practices and deterhiine the applicability of regulatory limitations prior to use. For 5. Procedures specific hazard statements, see Section 4. 1.5 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 5.1 Characteristic Odor--Dip 25 by 75-mm strips of rapid qualititive paper, free of foreign odor, to a depth of 50 mm into the material and the reference standard, each contained 2. Significance and Use 2.1 The comparative odor characteristics can be used, combined with other tests, for product identification and assessing compliance with a specification. 2.2 The residual odor characteristics can be used to judge the presence of nonvolatile materials that may be associated with manufacture or contamination, during distribution. Since volatile solvents and diluents are used in a wide variety of chemical processes and residual materials may affect the efficiency of such processes, this test method provides a in a beaker or other suitable container. Make an immediate comparison between the odor of the two materials on the filter papers. 5.2 Residual Odor--Dip 25 by 75-mm strips of a rapid qualitative paper, free of foreign odor, to a depth of 50 mm into the material under test and the reference sample, each contained in a beaker or other suitable container. Permit the papers to dry in air at room temperature and examine them at suitable intervals for differences in odor (see 1.3). The evaporation step may be omitted if only the "characteristic" odor of the material is to be determined. 'ii comparative test for manufacturing control and assessing compliance with a specification. 6. Report 6.1 Characteristic Odor--Report the odor as "character istic" if, upon immediate examination, the odor of the wet 3. Reference Standards filter paper containing the sample is similar to the odor ofthe 3.1 Samples of the particular products being tested, filter paper containing the standard. However, report the Odor as "noncharacteristic, unsatisfactory" if the odor of the sample, compared with the standard, is unsuitable for its 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 D01.35 on Solvents, Plasticizers, and ChemicaJ Intermediates. Current edition approved Nov. 14, 1984. Published January 1985. Originally published as D 1296 - 53. Last previous edition D 1296 - 79. intended solvent use. 6.2 Residual Odor--Report the odor as "nonresidual" if no odor is detectable on the sample paper after both the standard and sample papers appear dry. It is assumed that the standard, which is acceptable to both consumer and 176 DUP0502 95842 D 1296 ":if an odor persists on the sample paper after none & 'on and Bias standard specified in the procedure, no^ statement is mt the precision of assessing either characteristic or )dor. zs--No statement is made about the bias of either the characteristic or residual odor. Some analysts have little olfactory sensitivity to some materials, while other analysts have extreme sensitivity to either the main or (if any) minor component. In either case, the accuracy of odor measure ments should be considered suspect. In case of differing results between purchaser and supplier, it may be helpful to employ an odor panel consisting of no more than three persons. Consideration should be given to the qualifications of the panelists, such as the following: familiarity with odor determinations, length of time exposed to either the main or suspected minor component, and the environment in which the test is to be conducted. 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 ofinfringement of such rights, are entirety their own responsibility. This standard Is subject to revision et any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either teepproved or withdrawn. Yourcomments are Invltedeither forrevision of this,standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a far hearing you should make your vleiws known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103,177 I 177 DUP050295843 Designation: D 1310 - 86 (Reapproved 1990)61 Standard Test Method for Flash Point and Fire Point of Liquids by Tag Open-Cup Apparatus1 This standard is issued under the fixed designation D 1310; 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 epsilcm (r) indicates an editorial change since the last revision or reapproval. 6'No t e--Keywords were added editorially in September 1990. 1. Scope ^ 1.1 This test method covers the determination by Tag Open-Cup Apparatus of the flash point and fire point of liquids having flash points between 0 and 325F (--18 arid 165C) and fire points up to 325F. 1.2 This test method, when applied to paints and resin solutions that tend to skin over or that are very viscous, gives less reproducible results than when applied to solvents. No t e 1--In order to conserve time and sample, the fire point of a materia] may be determined by the Tag Open-Cup Method by con tinuing the heating of the specimen to its fire point. Fire points may also be determined by Test Method D92, which should be used for fire points beyond the scope of this test method. 1.3 This standard should be used to measure and describe the properties of materials, products, or assemblies in re sponse to heat and flame under controlled laboratory condi tions and should not be used to describe or appraise the fire hazard orfire risk ofmaterials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a fire risk assessment which takes into account all ofthefactors pertinent to an assessment ofthefire hazard ofa particular end use. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. D1016 Test Method for Purity of Hydrocarbons from : Freezing Points4 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1364 Test Method for Wafer in Volatile Solvents , (Fischer Reagent Titration Method)3 D2268 Method for Analysis of High-Purity n-Heptane f and /jooctane by Capillary Gas Chromatography5 * D2699 Test Method for Knock Characteristics of Motor I Fuels by the Research Method6 D2700 Test Method for Knock Characteristics of Motor and Aviation Fuels by the Motor Method6 E 1 Specification for ASTM Thermometers7 E 29 Practice for Using Significant Digits in Test Data to i Determine Conformance With Specification8 3. Terminology 3.1 Definition: 3.1.1 flash point--the lowest temperature, corrected to a pressure of 760 mm Hg (101.3 kPa, 1013 mbar), at which application of an ignition source causes the vapor of the specimen to ignite under specified conditions of test. 3.2 Description of Term Specific This Standard: 3.2.1 fire point--the lowest temperature at which a spec imen sustains burning for a minimum of 5 s by the procedure described. 2, Referenced Documents 2.1 ASTM Standards: D 92 Test Method for Flash and Fire Points by Cleveland Open Cup2 D850 Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D 1015 Test Method for Freezing Points of High-Purity Hydrocarbons4 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.22 on Health and Safety. Current edition approved April 25, 1986. Published June 1986. Originally published as D 1310 - 52 T. Last previous edition D 1310 - 85. 2 Annual Book ofASTM Standards, Vols 05.01 and 10.03. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards. Vols 05.01 and 06.03. 4. Summary of Method 4.1 The specimen is placed in the cup of a Tag Open-Cup Apparatus and heated at a slow, but constant rate. A small test flame is passed at a uniform rate across the cup at specified intervals until a flash occurs. To determine the fire point, the test is continued until the application of the test flame causes the specimen to ignite and burn for at least 5 s. 5. Significance and Use 5.1 Flash point and fire point of a liquid are physical properties that may be used to define their flammability 5 Annua! Book ofASTM Standards. Vol 05.02. 6 Annual Book ofASTM Standards, Vol 05.04. 7 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 8 Annual Book ofASTM Standards. Vols 02.03, 03.01,03.03, 03.05 and 14.02. 178 DUP050295844 point may be used to classify materials in ||dlations. . ip-'--' ` ftter--Tag Open-Cup Apparatus (Fig. 1), as Hpil in Annex Al. ^Cdescribed in detail in Annex Al. 6.3 Thermometers, conforming to Specification E 1, as listed in Table 1. 6.4 Flasks, 500-mL, two, with rubber stoppers. 7. Materials 7.1 Water-Glycol Solution (1 + 1), for flash points from 0 to 200F (--18 to 93C). In. 2'Vis 33/ie 6% mm 71.4 81 174.5 FIG. 1 Tag Open-Cup Apparatus 179 DUP050295845 D 1310 TABLE 1 Thermometers metal' shims as required , from between the taper, and the > FtashPoint/ Fire Point: 0tO;60'F -i8tol5<,C 60 to 200F 15 to 93C 200 to 3259F 93 to 165C ASTM Thermometer, Number . J Thermometer Flange Thermometer Subdivisions .33F-75 33C-75 ' 9F-75 9C-75 35F-79 35C-79 --36;5 to +1Q7.5F -38 to +42SC 20to`230F -5 to 110C 194to338F 90 to 170C ' . 0.5"F 0.2"P 1F `: 0.59C 0.5F 0.29C ` vertical supporting member of the swivel holder. 8.4 With the glass cup in place in the bath, adjust the j Jthermometer holder so that the thermometer is supported * firmly in a vertical position halfway between the center and1 ftedge of the cup and on a line passing through the center of the cup and the pivot of the taper. Place the thermometer so' 1 that the bottom ofthe bulb is14 in. (6.4 mm) from the inner bottom of the cup. 8.5 Set the draft shield around the tester so that the sides form right angles with each other and the tester is well 7.2 Solid Carbon Dioxide-Acetone or other Coolant. toward the back of the shield. 1 7.3 Silicone Fluid, inert, high boiling, having a flash point exceeding the test temperatures by at least 110F (60C) for flash and fire points from 200 to 325F (93 to 165Q. 7.4 n-Heptane9 for determination of flash points from 0 to 60F (-18 to 16C). See Annex A2 for specifications. 9. Procedure 9.1 Flash Points from 0 to 60F (--18 to 16C): * :i| No t e ; 3--Caution--Meticulous attention to all details relating to the <- taper, size of taper flame, rate of temperature increase, and rate of ' 7.5 p-Xylene,9 for determination of flash points from 60 passing the taper over the sample is necessary for good results. `< to 200F (16 to 93C). See Annex A2 for specifications. 7.6 Isopropanol (isopropyl alcohol),10 for determination of flash points from 60 to 200'F (16 to 93C). See Annex A2 for specifications. 7.7 Diethylene Glycol,11 for determination of flash points from 200 to 325F (93 to 165C). See Annex A2 for specifications. 9.1.1; Equip two 500-mL flasks with rubber stoppers ; through which are inserted ASTM 33F (33C) thermometers. ' Cool a quantity of 1 + 1 water-glycol solution in one stoppered 500-mL flask to approximately --20F (--30C) by immersing the flask in a solid carbon dioxide-acetone bath or other coolant. Use extreme care not to ' Contaminate the " water-glycol solution with either acetone or carbon dioxide. 8. Assembly and Preparation of Apparatus 9.1.2 Pour the cooled water-glycol solution into the tester ,i bath to a predetermined level Vs in. (3.2 mm) below the top 8.1 Place the tester in a level position on a solid table free when the cup is in place. An overflow is desirable for of vibration, in a location free of perceptible draft, and in a controlling the liquid level in the bath. dim light Maintain a room temperature of 75 5F (24 9.1.3 At tiie same time the water-glycol coolant is being 3C) throughout the test. Other room temperatures may be chilled, cool a portion ofJhe sample to approximately--10F | specified on agreement betweenbuyer afid seller. : (-'25C) "in the second stoppered 500-mL flask. If solid No t e 2--For materials with vapors or products of pyrolysis that are objectionable, it is permissible to place the apparatus with shield in a fume hood with the ventilation turned off. The; ventilation can then be turned on at completion of the test or wheri and if fumes become carbon dioxide and acetone or other volatile solvents are used as a coolapt, extreme care must be exercised to avoid contamination of the sample. Cool the glass cup and place it in the bath. Position the appropriate thermometer (Table 1) objectionable. as described in 8.4 and fill the cup with cooled sample to a 8.2 Adjust the horizontal and vertical positions of the taper so that the jet passes on the circumference of a circle * depth approximately Vs in. (3.2 mm) ... determined by the leveling device. below the edge as having a radius of at least 6 in. (150 mm); Thejet shdlld pass .... No t e 4--Remove all bubbles from the surface of the liquid before across the center of the cup at right angles to a diameter starting a determination. passing through the thermometer and in a plane Vs in. (3.2 9.1.4 Light the ignition flame and adjust it to form a mm) above the upper edge of the cup as measured from the , flame .of spherical shape matching in size the 5/3z-in. (4.0- center of the orifice. mm) sphere on the apparatus or the Vri-in. hole in the 8.3 Using the leveling device as a gage, adjust the height of leveling device.; ' the taper so that the center of the orifice is exactly Vs in. (3.2 9.1.5 Make the final adjustment of the specimen level in mm) above the top edge of the glass cup when it is in place. the cup when the temperature is 20F (10C) below the It is imperative that this adjustment be made as accurately as, anticipated flash point Two trial determinations may be possible. Raising or lowering the taper can be achieved by necessary to select the proper temperature at which to bending it slightly or preferably by adding and removing thin9 10a1d1just the liquid level. A hypodermic syringe or medicine dropper provides a convenient means of adding or removing 9 Satisfactory K-heptane and ywtylene can be obtained from Special Products Division, Chemical Department, Phillips Petroleum Company, Drawer O, Border, TX 79607. sample from the cup, 9.1.6 Allow the temperature of the specimen to increase spontaneously without applying any heat until the rate of 10 Satisfactory isopropanol may be obtained from Exxon Chemical, Americiis P. O. Box 3272, Houston, TX 77001, Shell Chemical Co., One ShelLPIaza, Houston, TX 77002, or Union Carbide Co., P. O. Box 8361, South Charleston, WV 25303. temperature rise decreases to 2*F (lC)/min. At this point, apply heat to maintain an increase in temperature at a rate of 2 0.5"F (1 0.25C)/min. 11 Satisfactory diethylene glycol may be obtained from Union Carbide Co., S. Charleston, WV. No t e 5--With viscous materials, this rate of heating cannot always be maintained;;' 180 DUP0502 95846 # DT310 Determine the approximate flash point by passing Aflame across the specimen at intervals of 2F (1C). first pass qf the taper flame immediately-after the stment of the specimen level, as in 9.1.5. The time to pass the ignition flame across the surface of the id be 1 s. Each pass must be in one direction only, jtper should be kept in the "off' position at. one.or -Tend of the swing except when the flame is applied imen. In case the material tends to. "creep" oyer i of the cup, carefully wipe the edge with absorbant remove frost and liquid just prior to passage pf the er the cup. ti--When determining the flash point or fire point; or both, of .liquids and those liquids that tend to form a surface film, the procedure is suggested: About 15 s before the taper is passed (Surface, insert the end of a stirring rod to a depth ofabout Mi in. l) in approximately a vertical position. Move the rod from side of the cup for three or four complete passes following lately the path of the taper, remove, and make the test. 1--Discontinue heating and checking flash point if the specils before flashing. Record that the material has no flash point boiling. ,8 Continue with procedure in 9.4. Flash Pointsfrom 60 to 200F(16 to 93C) (See Notes , and 6): ' Fill the bath with cold water or water-glycol solution redetermined level lh in. (3:2 mm) below the top when p is in place. The bath liquid should be at least '30F below the anticipated flash point. .2 If necessary, cool a portion of the sample to at least (10"C) below the anticipated flash point. Exercise uate care to avoid coritaiiiination of the sample ; with ~t liquid or vapors. Fill the glass cup with the cooled pie to a depth approximately Vs in. (3.2 mm) below the * as determined by the leveling device with the proper ometer (see Table 1) positioned as described in 8.4. .2.3 For final adjustment of the specimen level, see 9.1.5. ,2.4 Light the ignition flame and adjust it as described in .4. ' r: . ' ; .2.5 Apply heat to the liquid bath and adjust so that the perature of the specimen increases at a rate of 2 0.5F ft ' 0:25C)/min; ^.6 Determine the approximate flash point by passing e taper flame across the specimen at intervals of 2F (tC) described in 9.1.7. 9.2.7 Continue with procedure in 9,4. 9.3 Procedure for Flash Points from 200 to 325F (93 to 65C) (See Notes 3, 4, 5, and 6): 9.3.1 Fill the bath with a high-boiling inert silicone fluid i a predetermined level Vs in. (3.2 mm) below the top when (cup is in place. .3.2 With the appropriate thermometer (see Table 1) roperly positioned (8.4), fill the glass cup with sample at room temperature to a depth slightly more than Vs in. (3.2 mm) below the edge as determined by the leveling device. 9.3.3 For final adjustment ofthe specimen level, see 9.1.5. 9.3.4 Light the ignition flame and adjust it as described in 9.1.4. 9.3.5 Apply full heat to the liquid bath and when the temperature of the specimen reaches approximately 190F (90C), adjust the heat input so that the temperature of the specimen increases at a rate of 2 0.5F (1 0.25C)/min. No t e 8;-~The heaters on some testers do not have sufficient capacity to maintainthe proper rate of heating when the temperature approaches 250F. (120C) or above. The heat input to the liquid bath may be increased if necessary by using a variable transformer to increase the voltage to the heater or by wrapping the bath with electrical heatingtape. The. application of suitable insulation to the outside of the bath to prevent heat loss is also permissible. The important factor is to maintain the rate , of temperature increase of the specimen at 2 0.5F (1 0.25"C)/min. 9.3.6 Determine the approximate flash point by passing the taper flame across the specimen at intervals of 2F (1C) t as described in 9.1.7, 9.4 Determine and record not less than three test values, as follows: 9.4.1 After the initial test to determine the approximate flash point of the materials, repeat the procedure by cooling a fresh portion of the sample, the glass cup, the bath solution, and the thermometer to more than 2Q"F" (10C) below the approximate flash point. When the temperature of the" specimen is exactly 20F below the approximate flash point, adjust the denter ofthe liquid level to `A in. (3.2 mm) below the upper edge of the cup as determined With the leveling device placed across the diameter of the cup. 9.4.2 Resume heating, or allow the temperature to rise spontaneously in the case of materials flashing below 60F (16C). Following the instructions given in 9.1.7, pass the taper flame, across the specimen at two intervals of 5F (3C) and then at intervals of 2F (1C) until the flash point is . reached. 9.5 Fire Point .(Sustained Burningk 9.5.1 Except for the initial test, after determining the flash . point, continue heating the apparatus so that the tempera ture of the specimen increases at the rate of 2 0.5F (1 0.25C)/min. At intervals of 2F (1C), pass the taper across the surface ofthe specimen as described in 9.1.7 and in Note 7 and determine the temperature at which burning is sustained for 5 s after ignitioh (fire point). Time the duration of burning from the time the taper (ignition source) has completed its passage across the surface of the liquid. 9.5.2 Determine and record the results obtained from the continuation of three or. more flash point tests (9.4). . 10. Standardization and Calibration No t e 9--The calibration procedure provided in this test method eliminates the effect of barometric pressure if calibration and tests are run at the same pressures. 10.1 Flash Pointsfrom 0 to 60F (-18 to, 16"C) (see Notes 9 and 10): 10.1.1 Make at least five determinations of the flash ppint (9.1) of standard n-heptane that meets the specifications set forth in Aiinex A2, and calculate the mean. If the mean differs from 23T (-5C) by more than 3F (1,5C), adjust the height of the taper and repeat the standardization. No t e 10--The height ofthe taper arm is very important. Raising the taper 0.01 in. (0.25 mm) increases the flash point about 2"F (1C). Therefore, if it is suspected that the taper arm has been jarred or bent, the apparatus should be recalibrated. Each unit ofapparatus should have its calibration checked about once a week, if in constant use, or on each occasion of use, when used only occasionally. 10.1.2 Calculate the correction as follows: F = 23"F minus mean observed flash point of -heptane in F "C = --5C minus mean observed flash point of n-heptane in "C 181 DUP0502 95847 m D 1310 Round the correction to 1*F (0.5C) in accordance with Recommended Practice E29. Apply this correction to all flash-point determinations between 0 and 60F (--18 to 16C). 10.2 Flash Points from 60 to 200F (16 to 93C) (see Notes 9 and 10): 10.2.1 Make three determinations of the flash point (9.2) of standard p-xylene and the standard isopropyl alcohol that meet specifications set forth in Annex A2. Calculate the mean for each compound. If the difference between the values for these two compounds is less than 15"F (8.5C) or more than 27F (16C), repeat the determinations or obtain fresh standards. 10.2.2 Calculate the correction factor as follows: xF = 92T minus mean flash point ofp-xylene in "F x'C - 33"C minus mean flash point of p-xylene in C yT = 7IT minus mean flash point of isopropanol in "F y'C = 22<IC minus mean flash point of isopropanol in C correction factor = (x + y}/2 Round the correction to the nearest l'F (0.5"C) in accordance with Practice E 29. Apply this correction to all flash point determinations between 60 and 200F (16 and 93C). 10.3 Flash Points from 200 to 325F (93 to 165C) (see Notes 9 and 10): 10.3.1 Make at least five determinations of the flash point (9.3) of standard diethylene glycol that meets the specifica tions set forth in Annex A2. Calculate the mean and, if it differs from 295F (146`C) by more than 10F (5.5C), adjust the height of the taper and repeat the standardization. 10.3.2 Calculate the correction factor as follows: T= 295"F minus mean observed flash point of diethylene glycol in F "C = 146'C minus mean observed flash point of diethylene glycol in C Round the correction to T1F (0.5C) in accordance with Practice E 29. Apply this correction to afl flash-point deter minations between 200 and 325F (93 and 165C). 10.4 Correct the fire-point results with the applicable flash-point factor determined in .10.1, 10.2, or 10.3.11 11. Report 11.1 Report the mean of not less than three corrected recorded tests, other than the initial test, to the nearest 1F (0.5C), Three multiple runs are acceptable for averaging if the difference between the extreme values does not exceed 7F (4"C) (95 % confidence level). 12. Precision12 12.1 The following criteria should be used for judgingthc' acceptability of results between 0 and 200F (-18 and 93Qy '* at the 95 % confidence level). 12.1.1 Repeatability--Two results, each the mean ofthiee determinations, obtained by the same operator should be considered suspect if they differ by more thart 4F (2C). 12.1.2 Reproducibility--Two results, each the mean of three determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 7F (4C). 12.2 The following criteria should be used for judging flash points between 200 and 325F (93 and 165"C) at the 95 % confidence level. 12.2.1 Repeatability--Two results, each the mean of thiee determinations, obtained by the same operator should be considered suspect if they differ by more than 9F (5C). 12.2.2 Reproducibility--Two results, each the mean of three determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 12F (7C). 12.3 On the basis of an .interlaboratory test of the method using viscous, heavily-pigmented materials that tended to form a surface film, the within-Iaboratory standard deviation was found to be 3F (2C) and the between-faboratories standard deviation was found to be 7F (4C). Based on these ., standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 12.3.1 Repeatability--Two results, each the mean ofthree determinations, obtained by the same operator on different , days should be considered suspect if they differ by more than 9F (5C). 12.3.2 Reproducibility--Two results, each the mean of three determinations, obtained by operators in different.. laboratories should be considered suspect if they differ by more than 24F (13C). 12.4 The precision of fire points will be determined. See Test Method D 92 for precision using the Cleveland Open Cup. 12.5 Bias--No estimate of bias of flash point, and fire point tests can be determined as no absolute values are available. The tests,are equipment and method dependent. 13. Keywords 13.1 fire point; flash point; liquids: paints; resin solutions; Tag tester u Supporting data are available from ASTM Headquarters. Request RR:D0I - 1002. j i 182 DUP0502 95848 ANNEXES (Mandatory Information) Al. APPARATUS ;1 Tag Open-Cup Apparatus, shown in Fig. 1. It ; of the following parts, 'which must conform to the (ions shown, and have the additional characteristics as V32 0.8 1i6 30.1 5.5 1% 34.9 %2 7.0 1% 38.1 5*6 7.5 m 47.6 % 9.5 2 50.8 % 15.9 2V32. 51.6 2V32 16.6 2Vte 55.5 m 63.5 FIG. A1.1 Glass Test Cup Al.1.1 Copper Bath, preferably equipped with a constantlevel overflow so placed as to maintain the bath liquid level % in. (3.2 mm) below the rim of the glass cup. Al.1.2 Thermometer Holder, supplied with the tester as shown in Fig. 1 to support the thermometer firmly in a vertical position. No t e Al .1--The spring clamp holding the thermometer part may be replaced by a set-screw facing out away from the bath as shown in Fig. 1. This may make it easier and safer to extinguish the fire after the fire point has been reached. Al.1.3 Class Test Cup (Fig. Al.l), of molded clear glass, annealed, heat-resistant, and free from surface defects. A 1.1.4 Leveling Device, or gage, for proper adjustment of the liquid in the cup (Fig. A 1.2) made ofpolished aluminum or stainless steel l/s in. (3.2 mm) thick, with two projections for adjusting the liquid level in the glass cup to 0.125 in. 0.003 in. (3.18 0.08 mm) below the top edge or rim of the cup. This leveling device may also be used to adjust the size of the test flame and for gaging the height of the taper above the edge of the cup. Al.l.5 "Micro" or Small Gas Burner, of suitable dimen sions for heating the bath. A screw clamp may be used to help regulate the gas. A small electric heater controlled by a variable power transformer may be used. A 1.1.6 Ignition Taper, a small, straight blow-pipe type gas burner with the tip approximately `/re in. (1.5 mm) in diameter and the orifice Vn in. (0.8 mm) in diameter. The ignition taper should be maintained in a fixed horizontal plane above the test cup by means of a swivel device so that the test flame passes on the circumference of a circle having a radius of at least 6 in. (150 mm). Al.l.7 Draft Shield, consisting of two rectangular sheets of noncombustible material, 24 by 28 in. (610 by 710 mm), fastened together along the 28-in (710-mm) side, preferably by hinges. A triangular sheet, 24 by 24 by 34 in. (610 by 610 by 860 mm), is fastened by hinges to one of the lateral sheets (to form a top when shield is open). The interior of the draft shield shall be painted a flat black. A draft-free fume hood may be used. 183 DUP050295849 " # D 1310 ------------------------------------------ 5in.------------------------------------------- - i 5/32in.centered l/8in. from bottom end lin. 1 in. from end. 1/32in.centered 0.125t0.OO3in.from .'bottom and 2 1/2 in.from v \/ L ------- ^2in.------------ --(in.------- *------------- 2in,------------- I I 0.125+ 0:003in. Metric Equivalents In. mm V32 V. 0.125 0.003 %2 : 1 2 m 5 0.S 3.2 3.18 + 0.08 4.0 25.4 50.8 63.5 127 FIG. A1.2 Leveling device for Adjusting Liquid Level in Test Cup, Height of Taper above Cup, and Sizegtrf Test Flame A2. SPECIFICATIONS FOR n-HEPTANE, ^XYLENE, ISOPROPANOL, AND DIETHYLENE GLYCOL A2.1 Specifications for n-Heptane9 (ASTM Knock Test Reference Fuel)--n-Hqptane shall conform to the following requirement: A2.1.1 Purity--99.75 % when determined by Method D 2268. No t e A2.1--This is the same grade of'n-heptane specified in Test Methods D 2699 and D 2700. A2.2 Specifications for p-Xylene (Flash Point Check Gradef--^Xylene shall conform to the following require ments: A2.2.1 Specific Gravity--15.56/15.56'C--0.863 0,003 max. A2.2.2 Boiling Range--2C max from start to dry point, when tested in accordance with Method D 850 or Test Method D1078. The range shall include the boiling point of pure p-xylene, which is 281.03T (138.35Q. ^ A2.2.3 Freezing point 11.23C, min calculated in accord ance with Test Method D 1016, from the experimentally determined freezing point, measured by Test Method D 1015. A2.3 Specifications for Isopropanol (Isopropyl Alcohol) 91% (Volume):10 Isopropanol shall conform to the fol lowing requirements: A2.3.1 Specific Gravity--0.8180 0.0005 at 20/20"C as determined by means of a calibrated pycnometer. A2.3.2 Distillation Range--Shall "entirely distill within a 1.0C range that shall include the temperature 80.4C as determined by Test Method D 1078. A2.4 Specifications for Diethylene Glycol11--Diethylene glycol shall conform to the following requirements: A2.4.1 Specific Gravity--1.1185 0.0015 at 20/20C as determined by means of a calibrated pycnometer. A2.4.2 Distillation Range--Shall entirely distill within a 5.0 range which shall include the temperature 245.8C as determined by Test Method D 1078. A2.4.3 Water--Not more than 0.2 % as determined by Test Method D 1364. The American Society for Testing end Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapprovedor withdrawn, vour comments are invitedeither forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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. 184 DUP050295850 Designation: D1353 - 90 Standard Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, anci Related Products1 This standard is issued under the fixed designation D 1333; 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 i indicates an editorial change since the last revision or reapproval. This lest method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4045 ofFederal Test Method Standard No. 141A andfor listing in theDoD Index ofSpecifications andStandards. je This test method covers the determination pf the latile matter in volatile solvents for use in paint, h, lacquer, and related products. ; This standard does not purport to address all of the i,problems associated with its use. It is the responsibility ` user ofthis standard to establish appropriate safety and practices and determine the applicability ofregulatory lions prior to use. For specific hazard statements, see n 5. > 4 For hazard information and guidance, see the sup 's Material Safety Data Sheet feferenced Documents 1 ASTM Standards: .180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial ^Chemicals2 299 Test Method for Trace Amounts of Peroxide in Organic Solvents3 Significance and Use .1 This test method describes the analytical measure:t of residual matter in solvents that are intended to be 0 % volatile at 105 5C. Volatile solvents are used in the ufacture of paint, varnish, lacquer, and other related bducts, and the presence of any residue may effect the duct quality or efficiency ofthe process. This test method seful in manufacturing control and assessing compliance i specifications. Apparatus 4.1 Oven, thermostatically controlled at 105 5C. 4.2 Dish, evaporating, platinum, 125-mL. 4.3 Cylinder, graduated, 100-mL. 4.4 Analytical Balance, precision to 0.1 mg. Hazards 5.1 Warning--Certain solvents and chemical intermedi- 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 D 01.35 on Solvents, Plasticizers, and Chemical Intermediates. Currentedition approved Sept. 12, 1990. Published November 1990. Originally published as D 1333 - 34 T. Last previous edition D 13S3 - 86. 2 Annual Book ofASTMStandards, Vol 15.05. 2 Annual Book ofASTM Standards, Vols 06.03 and 15.05. . ates, particularly, but not only ethers and unsaturated compounds,inay forin peroxides diirihg storage. These per oxides may present a violent explosion hazard when the chemicals are evaporated. When peroxide formation is likely because of chemical type or length of storage, analyze the material for peroxides (see Test Method E 299). If they exist in hazardous concentrations, take appropriate precautions such as destroying the peroxides before evaporation, shield ing, or disposal of the sample and not running the test. .6 Procedure 6.1 Dry a 125-mL platinum evaporating dish in an oven at 105 5C and cool in a desiccator. Repeat until the weight is within 0.1 mg of the previous weighing. 6.2 With the graduated cylinder, measure 100 mL of sample at room temperature into the conditioned platinum evaporating dish; place on a steam bath and . evaporate the specimen to dryness. Dry the outside of the dish with a clean, lint-free cloth and heat in an oven at 105 5C for approximately 1 h. Cool in a desiccator and weigh the evap orating dish and contents to 0.1 mg. 6.3 Return the dish and contents to the oven for 15 to 30 min, cool, and reweigh. Repeat, if necessary, until the weight is constant to within 0.1 mg of the previous weighing. 7. Report 7.1 Report as nonvolatile matter the residue obtained from the specimen as milligrams of nonvolatile residue/100 mL. 8. Precision and Bias4 8.1 Precision--The precision statements are based upon an interlaboratory study in which one operator in each of eight different laboratories analyzed one sample of methyl ethyl ketone in duplicate on two different days. This sample was prepared by adding 0.006 % of a nonvolatile resin to commercial methyl ethyl ketone. The results were analyzed in accordance with Practice E 180. The within-laboratory standard deviation was found to be 0.26 mg/100 mL, and the between-laboratories standard deviation 0.71 mg/100 mL. Based upon these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 8.1.1 Repeatability--Two results, each the mean of dupli- 4 Supporting data are available from ASTM Headquarters. Request RR: D01 - 1044. 185 DUP050295851 # D 1353 cates, obtained by the same operator on different days should be considered suspect ifthey differ by more than 0.9 mg/100 8.1.2 Reproducibility--Two results, each, the mean of duplicates, obtained by operators iir different laboratories should be considered suspect if they differ by more than 2 4 mg/100 mL. 8.2 Bias--Bias has not-,been determined for this tea method. 9. Keywords 9.1 'nonvolatile matter; volatile solvents The American Society for Testing and Materials takesno 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 01 me validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed, every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or lor,.additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee; which you may attend. If you fee/that your comments have not received a fair hearing you should make your views known to the tSTM Committee on Standards, 19t6.PaceSt., Philadelphia, PA 19103. -r vt y 186 DUP050295852 Designation: 01358 - 86 (Reapproved 1990) Standiard Test Method for Spectrophotometric Diene Value of Dehydrated Castor Oil and This standard is. issued under the fixed designation D 1358; 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 (<) indicates an 'editorial change since the last revision or reapproval. test method covers the determination of the ^photometric diene value as a measure of the content |gated dienoic adds in dehydrated castor oil and its ves. Due to the high linoleic add content in dehyleastor oil and its derivatives, the'absolute conjugated add content cannot be determined by this test This standard does ,not purport to address all of the problems associated with its use. It is the responsibility fever uses this standard to consult and establish Mate safety 'and health practices and determine the |ability of regulatory limitations prior to use. Specific . statements are given in Section 6. inscription of Term Specific to This Standard | ppectrophotometric diem value--under the conditions pest method, the percent of conjugated dienoic acids. Significance and Use In the process of dehydrating pastor oil, a double bond armed in the ricinoleic add to make either conjugated. leic or normal linoleic fatty acid segments in the oil. This [ method attempts to measure the amount of conjugated aturation by means of the absorbance at a specific |yelength which is in. the ultraviolet' radge'. Since some |prption is due to linoleic acid, a, correction factor is jtuded in the calculation. This test method is only appli3le to dehydrated castor oil products. Apparatus .1 Spectrophotometer--Ultraviolet photoelectric spectroliotometer,2 covering a spectral range from 200 to 350 nm, 14th a wavelength scale readable to 0.1 nm, and equipped dth an absorption cell compartment3 for holding 10.00-mm ells. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint |nd Related Coatings and Materials and is the direct responsibility of Subcom- nittee D01.32 on Drying Oils. Current edition approved March 27. 1986. Published May 1986. Originally published as D 1358 - 55 T. Last previous edition D 1358 - 58 (t984)tl. 2 The Beckman Model DU photoelectric quartz spectrophotometer, Catalog No. 2500 DU, Beckman Laboratories, S. Pasadena, CA, has been found satis factory for this purpose. 'The cell compartment assembly, as Catalog No. 2510, and the ultraviolet accessory set, as Catalog No. 2501, that includes the No. 2230 hydrogen discharge lamp, the No. 2511 adapter. No. 23-10-10-89 cells, and No. 2504 cover, both available from Beckman Laboratories, S. Pasadena, CA, have been found satis factory for this purpose. 4.2 Absorption Cells, quartz, matched pains of lengths 10.00 0.05 mm. The cells in a pair, when filled with water or riooctane, shali match within 0.01 absorbancy unit (Note 1). The cells may be the 10.00-mm nondemountable type made of quartz, or the demountable type consisting of a chemically resistant glass4 5cell body of outside diameter of about 22 mm with centered-ground glass stopper, threaded metal caps, polished crystalline quartz windows, and cork gaskets. No t e 1--If the cells do' not match within 0.01 absorbancy unit, they may be filled with water or irooctane and calibrated against each other at the specified wavelength. The necessary correction in absorbancy units is then applied where necessary. Highest precision is obtained by the method of reversing cells. The absorbancy of the solution is read against the solvent blank. The cells are then cleaned and the solvent blank put in the cell previouslyused for the solution and the solution iri the cell previously used for the blank and the absorbancy measured. The two absorbancies are then averaged to obtain. A,, the observed absorbancy. The cells should be rinsed with solvent, water, concentrated nitric acid, water, and solvent; in that sequence, before each reading. .4.3 Filter Tube, 32 by 13A in. (810 by 45 mm). 4.4 Cork Stopper covered with aluminum foil to fit loosely in the top of the filter tube. 4.5 Dropping Bottle, stoppered, for weighing the samples. 4.6 Volumetric Flasks, glass-stoppered, having capacities of 100 m'L, 50 mL, and 25 mL. 4.7 Volumetric Pipets, precision grade, assorted sizes, for making dilutions when required. " 5. Reagents and Materials 5.1 Silica Gel, 28 to 200-mesh.s 5.2 Glass Wool. 5.3 Isooctane (2,2,4 Trimethylpentane)--Pure or spectro scopic grades of riooctane are satisfactory. Check the absorbancy of a 10-mm layer of the /sooctane against distilled water at 233 nm. The absorbancy compared with distilled water set at zero absorbancy shall not be more than 0.070 at 233 nm. If the /sooctane does not meet these requirements, purify it as follows: Place about 3% in. (90 mm) ofglass wool above the lower end ofthe filter tube. Add about 20 in. (500 mm) of silica gel and about 2 in. (50 mm) of glass wool. Fasten the tube vertically to a ring stand and place a funnel and 2-L amber bottle under the tube. Pour the /sooctane slowly into the tube, filling about three-fourths full, and allow the /sooctane to filter through the silica gel. Renew the silica gel in the tube as often as necessary to yield 4 Borosilicate glass has been found satisfactory for this purpose. 5 Silica gel available from Davison Chemical Co., Baltimore, MD, as Code [-08, or the equivalent, has been found satisfactory for this purpose. 187 DUP050295853 # D 1358 isooctane conforming to the transmission limit given above. A constant flow can be maintained by feeding the wooctane from a 500-mL glass-stoppered separatory funnel, the tip of which is below the surface of the isooctane in the filter tube. The 2-L amber bottle used Ibr storing the purified isooctane should be rinsed with a little of the first eluate from the column, and the rinse should be discarded. An aluminumlined screw cap should be used to close the bottle for storage. 6. Hazards 6.1 /sooctane is an extremely flammable solvent with a flash point of JOT (-10C). Keep away from heht and open flame. Can' react vigorously with reducing materials; See supplier's Material5 Safety Data Sheet for further-informa tion. 7. Calibration <of Spectrophotometer. : 7.1 Operational, instructions for .spectrophotometers vary with different models. Consult the manufacturer's literature for, establishing optimum conditions for the specific instru ment used.' !. . ' . ' . V. 8. Procedure 8.1 Weigh by difference into a 100-mL volumetric flask, to 0.1 mg, 90 to 130 mg of the sample. Add about 75 mL of purified /sooctane. " ;! ' 8.2 Rotate the flask arid warm the contents, if necessary, to dissolve, the specimen completely. Cool td rooim tejripera- ture, and allow to stand atfeast 15 min to attain temperature equilibrium. Dilute to volume with purified solvent and mix thoroughly. - '' 8.3 Make necessary dilutions, in no greater than ten-fold steps, to give a final concentration of about 0.01 g of the sample per litre. Measure the absorbancy of the solution at 233 nm (Note 2). Use a matched cell containing purified solvent, Only for the blank cell. Take several readings and calculate the mean. The observed absorbancy readings should lie between 0.35 and 0.55; otherwise change rhe weight or the dilution to give the required reading. NpTE 2--For highest precision, when making dilutions, allow suffi cient tune for t,he solutions to reach room, temperature. 9. Calculation and Report 9.1 Calculate the percent of conjugated dienoic acids, C2, as follows: ' - = 8.4[(^ySe)Cl ' where: a0, = 0.07 for esters, ,5 , = 0.03 for acid, As = observed absorbancy at 233 nm, b - cell length, mm, and v c = sample per litre of the final dilution used for the absorption measurement, g. 9.2 Report the percent of conjugated dienoic acids to thre? significant figures. !' 10. Precision ' -- ' 10.1 Repeatability--Two results obtained by the same operator on the same apparatus should riot differ from the mean by moire than 0.39., . 10.2 Reproducibility--Two results obtained by operators in different laboratories should not differ from the mean by more than 1.26. 10.3 Bias--Bias has not been determined. The'American Society for Testing and'Materlala takes no position respecting the validity ol any patent rights asserted in connection wlttreny item mentioned In this standard. Users of this standard are expressly advised that determination ef the validity of any such patent rights, and the risk of infringement ofsuch tigpts, are entirely their own responsibility, This standard is subjgcttorevlslgpatany time by the responsible technical committee and must be reviewed svety five years and ifnotrevised, eitherreapprovad drWithdrawn. Yourcomments are invitedeither for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend.: If you, feel that yew comments have not received/a fair hearingyou should make your views known to the ASTM Committee on Standards, 1916 Recast., Philadelphia, PA 19103. V; v; 3 m i ________________ ______ i ...... DUP050295854 Designation; D 1363 - 38 Standard Test Method for Permanganate Time of Acetone and Methanol1 This standard is issued under the fixed designation D 1363; 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 `fol. superscript epsilon (e) indicates an editorial change since the last revision pr reapproval. This standard has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index ofSpecifications arid Standardsfor the sj>ecific year of issue which has been adopted by the Department ofDefense. pe IJhis test method covers the detection in acetone and ol of the presence of impurities that reduce potas- irmanganate. . l!- Thisstandard may involve-hazardous materials, oper and equipment. This standard does nob purport to ..s aliofthe safety problems associated with its use. It is Jsponsibility of the user of this standard to establish fixate safety and health practices and determine the ability of regulatory lifnitations prior to use. ' For specific hazard information and guidance,1 consult tpplier's Material Safety Data Sheet. ferenced Documents C ASTM Standards: 329 Specification for Acetone2 * ;j j52 Specification for Methanol, (Methyl Alcohol)2 1193 Specification for Reagen.t Water* 1209 Test Method for Color 6f Clear Liquids (PlatinumCobalt Scale)4 180 Practice for Determining the Precision of ASTM Methods for. Analysis and Testing of Industrial Chem icals5 Summary of Test Method 3.1 Substances reacting with potassium permanganate in 'tral solutions reduce it to manganese dioxide which "ors the solution yellow. In the permanganate test the time, quired for the eolor ofthe test solution to change to that of : standard solution is measured. The color of the test lution changes from pink-orange to yellow-orange. t Significance and Use 4.1 The permanganate time can be used to judge the presence of oxidizable materials that may be associated with manufacture or contamination during distribution and to assess compliance with a specification. 4.2 Many chemical processes that use acetone or meth anol, or both, involve catalyst, metals, or ligand complexes 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved June 24, 1988. Published November 1988. Originally published as D 1363 - 55 T. Last previous edition D 1363 - 84. 2 Annual Book ofASTM Standards, Vol 06.03. ' Annual Book ofASTM Standards, VoLs 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 15.05. that are sensitive to oxidation. Since oxidizable contami nants may affect the efficiency of these processes, this test method provides a comparative test for manufacturing ^control and assessing compliance with a specification. 5. Apparatus 5.1 Color Comparison Tubes--Matched 50-mL, tall form Nessler tubes, provided with ground on, optically clear, glass caps, 512 Constant-Temperature Bath, capable of maintaining a temperature of 15.0 0,5'C or of 25.6 0,5C. It is important that the constant-temperature bath be protected from direct light. If a glass constant-temperature bath is employed, it should be wrapped or coated with an opaque material. 5.3 Pipet, capable of delivering 2.0 mL of solution. 5.4 Interval Timer and Clock, capable of measuring a time interval of 120 min or more. An alarm arrangement may be desirable. 6. 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.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 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 6.3 Potassium Permanganate Solution (0.200 g/L)--Dis solve 0.200 g of potassium permanganate (KMn04) and dilute to 1 L with freshly boiled water. Clean glassware is essential to the stability of this solution. The solution should be stored in brown bottles and be prepared every week needed. 6.4 Cobaltous Chloride-Platinum Cobalt Standard Solu tion--Weigh on analytical balance 175 mg of cobaltous chloride (CoCl2'6H20) and add 21.4 mL of 500 Pt-Co standard (Note 1). Transfer to a 50-mL volumetric flask, dilute to the mark, and mix thoroughly. This standard 6 "Reagent Chemicals, American Chemical Society Specifications,1' 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." 189 DUP050295855 D 1363 solution represents the color of the end point to which the than X minutes." Ifthe residual pink color of the specimen is sample solution fades in the KMn04 test. The solution is equal to that of the standard, report the permanganate time stable and should be kept in a 50-mL glass-stoppered Nessler as "X minutes." If the residual pink color of the specimen isi1 tube exactly the same as those in which the test is run. less than the standard, report as "less than X minutes," where; No t e 1--The preparation of the 500 Pt-Co standard is covered in "JF minutes" is the minimum time specified for the material I Test Method D 1209. being tested (see 7.1). 8.1.2 An estimate, of the actual permanganate time ma\ 7. Procedure be made by closely observing the sampleyjpd reporting to the 7.1 Employ the following time and temperature condi nearest minute the time when the c^lbr of the specimen tions during the test: Temperature Permanganate matches that of the standard. Duplicate determinations that agree within 3.0 % are suitable for averaging (see Section 9). of Test, "C Time,min Acetone 25 D 329 9. Precision and Bias7 190 Methanol t5 -'01152 9.1 Precision--These precision statements are based on No t e 2--Clean test Cylinders and permanganate storage and han dling equipment with concentrated hydrochloric acid (HO, sp gr 1.19) to remove residual manganese dioxide (Mn02) which catalyzes reduc tion of KMn04. Remove the acid with not less than ten rinsings with reagent water. 7.2 Pill a 50-mL Nessler tube beyond the mark with the sample under test and place in the constant-temperature bath. Maintain the water level in the bath approximately 25 mm (1 in.) below the top ofthe .tube. When the specimen has reached the specified temperature, bring the level to the 50-mL mark. With a pipet, add 2 mL of the KMn04 solution. Stopper the tube, invert once to mix the contents, return to the bath and note the time. At the end of the minimum time specified for the material being tested, remove the tube and compare it to the color standard by viewing downward through the tube against a white back ground froth which diffused white light is reflected. an interlaboratory study in which three samples of methanol having average permanganate times of 60, 73,. and 95 min were each analyzed by Fourteen different laboratories in duplicate on two different days. In this interlaboratory study, the within-laboratory coefficient of variation was found to be 2.35 % with 40 df and the between-laboratories coefficient of variation 8.20 % with 12 df. Based upon these coefficients' 1calculated in accordance with Practice E 180, the following criteria should be used forjudging the acceptability of results* at the 95 % confidence level: 9.2 Repeatability--Two results, each the mean of dupli cates, obtained by the same operator on different days should be considered suspect if they differ by more than ,6.7 %. 9.3 Reproducibility--Two results, each the mean of dupli cates, obtained by operators in different laboratories should be considered suspect if they differ by more than 25.2 %. 9.4 Bias--Bias has not been determined"for this test 8. Report method. 8.1 Report the following information: 8.1.1 If the residual pink color of the specimen is greater than the standard, report the permanganate time as "greater 7 Supporting data are available from ASTM Headquarters. Request RR:DOl1033. 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 cf 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 everyfive years and if not revised, eitherreapproved or withdrawn. Yourcomments are Invited eitherforrevision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Tour 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 16103. 190 DUP0502 95856 Designation: D 1364 - 90 Standard Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)1 This standard is issued under the fixed designation D 1364; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This lest method has been,approvedfor use by agencies ofthe Department ofDefense to replace Method 4082.1 ofFederal Test Method Standard Np. 141A ahfytr listing in the DoD Index ofSpecifications and Standards. This test method covers the determination of water in oportion in volatile solvents and chemical intermedised in paint, varnish, lacquer, and related products. This test method is not applicable in the presence of Iptans, peroxides, or appreciable quantities of aldei or amines. [ This standard does not purport to address all of the Iproblems associated with its use. It is the responsibility fuser ofthis standard to establish appropriate safety and i practices and determine the applicability ofregulatory Rations prior to use. For hazard information and guidance, see the sup|s Material Safety Data sheet. eferenced Document WASTM''Standard: 500 Test Method for A.STM Color of Petroleum |1:;Prbducts (ASTM Color Scale)2 |0escriptions of Terms Specific to This Standard 1.1 instrumental end point--that point in the titration Jen two small platinum electrodes, upon which a potential gpO to 50 mV has been impressed, are depolarized by the lition of 0.05 mL of Fischer reagent (6 mg of H20 per L), causing a change of current flow of 10 to 20 jiA that sists for at least 30 s. {PDfare 1--This end point is sometimes incorrectly called the "dead pip" which is the reverse of the above. | 3.2 color end point--During the titration, the solution : turns yellow, then later deepens towards the end of the ation; the end poiitt is indicated by the change from pillow to orange-red which is quite sharp and easily repeated. She orange-red color must persist for at least 30 s in order to idicate an end point. No t e 2--View the color by transmitted daylight or by transmitted ftp*'from an artificial daylight lamp, such as the one which complies fwith the specifications given in Test Method D 1500. ' [ 4. Summary of Test Method 4.1 This test method is based essentially upon the reduc 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings aad Materials and is the direct responsibility of Subcom1 mittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 26, 1990. Published December 1990. Originally ; published as D 1364-55 T. Last previous edition D 1364 - 87I, 2 Annual Book ofASTM Standards, Vol 05.01. tion of iodine by sulfur dioxide in the presence of water. This reaction can be used quantitatively only when pyridine and an alcohol are present to react with the sulfur trioxide and hydriodic acid produced according to the following reac tions: H20 +12 + S02 + 3C5H5N -* 2C5H5N HI + C5H5N-S03 CsH5N-S03 + ROH -> C5H5N-HS04R 4.2 To determine water, Fischer reagent (a solution of iodine, pyridine, and sulfur dioxide, in the molar ratio of 1+10+3) dissolved in anhydrous 2-methoxyethanol is added to a solution of the sample in anhydrous pyridine-ethylene glycol (1+4) until all water present has been consumed. This is evidenced by the persistence of the orange-red end-point color; or alternatively by an indication on a galvanometer or similar current-indicating device which records the depolar ization of a pair of noble-metal electrodes. The reagent is standardized by titration of water. 5. Significance and Use 5.1 Volatile solvents are used in a variety of chemical processes which may be affected by water. Therefore, this test method provides a test procedure for assessing compliance with a specification. 6. Apparatus 6.1 Titration Vessel--For color end point titrations, use a 100 or 250-mL volumetric flask which need not be cali brated; a 250-mL flask fitted with interchangeable electrodes (Fig. I)3 may also be used for the instrumental end point and is particularly suitable for titrations at ice temperatures. For permanently mounted assemblies, the vessel should have a capacity about equal to that of a 300-mL tail-form beaker; and be provided with a light-fitting closure to protect the sample and reagent from atmospheric moisture, a stirrer, and a means of adding sample and reagents and removing spent reaction mixture. It is desirable to have a means for cooling the titration vessel to ice temperature. 6.2 Instrument Electrodes--Platinum with a surface equivalent to two No. 26 wires 5 mm long. The wires should be 3 to 8 mm apart and so inserted in the vessel that 25 mL of liquid will cover them. 6.3 Instrument Depolarization Indicator, having an in ternal resistance of less than 5000 SI and consisting of a means of impressing and showing a voltage of 20 to 50 mV across the electrodes and capable of indicating a current flow 3 Such flasks are made by Rankin Glass Blowing Co., 3920 Franklin Canyon Road, Martinez, CA. 191 DUP050295857  D 1364 No t e--All dimensions in millimetres. FIG. 1 .Titration Flask Assembly- of 10 to 20 pA by means of a galvanometer or radiotuning eye circuit.4 6.4 Buret Assembly for Fischer reagent, consisting of a 25 or 50-mL buret connected by means of glass , (not robber) connectors to a source of reagent; several types of automatic dispensing burets5 may be used. Since the reagent loses strength when exposed to moist air, all Vents must be protected against atmospheric moisture by adequate drying tubes containing indicating calcium sulfate drying-agent All stopcocks and joints should be lubricated with a lubricant not particularly reactive6 with the reagent. 6.5 Weighing Bottle, of the Lunge or Grethen Type, or equivalent 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.7 8Other 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. * A type similar to the Precision Scientific Co. "Aquatrator," or Fisher Scientific Co. "Fisher Titrimeter," is suitable for the measurement of the instrument end point. 5 A type simitar to Catalog No. J-821 of Scientific Glass Apparatus Co., Bloomfield, NJ, or Catalog No. 750 of Eck and Krebs, New York, NY, has bein specifically designed for this purpose and presents the minimum contact ofreagent with stopcock lubricant. 6 Suitable lubricants are Apiezon, N (James G. Biddle and Co., Philadelphia, PA); High Vacuum'Silicone Grease (Dow Coming Co.,: Midland; MI); Sisco 300 (Swedish Iron and Steel Co., New York, NY), 7 "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." 7.1.1 Fischer Reagent (equivalent to 6 mg of H20 per mLf--For each liter of solution, dissolve 133 1 g of I2 in 425 2 mU of anhydrous (less than 0.1 % HzO) pyridine in | a dry glass-stoppered bottle. Add 425 2 mL of anhydrous (less than 0.1 % H20) 2-methoxyethanol. Cool to below 4C in an ice bath and add gaseons* S02, dried by bubbling through concentrated H2S04 (sp gr 1.84); determine the amount of S02 added by measuring the change in weight of the S02 cylinder (102 1 g) or the increase in volume (70 + 1 mL) of the reagent mixture. Alternatively, add 70 mL of freshly drawn liquid S02 in small increments. 7.1.2 Solvent Mixture--Mix 1 volume of anhydrous (less than 0.1 % H20) pyridine with 4 volumes of anhydrous (less than 0.1 % H20) ethylene glycol. No t e 3--Pyridine, ethylene glycol, arid 2-methoxyetlianoI, each, containing less than 0.1 % water, are available and should- be used. No t e 4--If adequately dry reagents cannot", be .procured, they can each be dried by distillation through a multiple-plate column, discarding the first 5 % of material distilling overhead and using the 95 % remaining. Drying may also be accomplished by the addition of 1 volume oftoluene or cyclohexane to 19 volumes of thepyridine-glycol, or of the pyridine ethylene glycol monomethyl ether mixture, followed by distillation; the first 5 % distilled is discarded and the residual 95 % iteii used. 8. Standardization of Reagent 8.1 Standardize the Fischer reagent each day used by either the color or instrument end point (Section 3) method using the same procedure as used for titrating the sample. 8.1.1 Add to each flask 25 mL of ethylene glycol-pyridine 1 mixture, and titrate this as described in Section 10. Add to the solvent thus titrated, in place of the sample, 0.15 to 0.18 g of water from a weighing pipet, weighed to the nearest 0.1 mg. Complete titration with Fischer reagent as. described in Section 10. 8.1.2 Calculate the equivalency factor, W, of the reagent in terms of water content per millilitre by means of the following equation: ` . ' W-AjV ; where: W = equivalency factor, mg of water per mL, A = weight of water used in the standardization, mg, and V = volume of Fischer reagent required, mL. 9. Sampling 9.1 Lacquer Solvents--It is essential to avoid changes in the. water content of the material during sampling opera tions. Errors from this source are particularly significant in the analysis of materials having low water content. When analyzing materials that absorb water readily (for example, absolute alcohols), limit as much as possible contact with air in transferring the specimen into the titration vessel. Avoid intermediate sample containers, if possible. 10. Procedure 10.1 Introduce 10 to 25 mL of the anhydrous solvent mixture (pyridine-glycol, 1+4) into the titration vessel, 8Karl Fischer Reagent is available from various laboratory suppliers. Pyridinefree adaptations are available and may be used ifprecision can be established. One such mixture is HYDRANAL, a trademark of Riedel-de Haen AG, distributed by Fisher Scientific/Allied, 711 Forbes Ave, Pittsburgh, PA 15219. 192 DU P0502 95858 D 1364 Bure, if an instrument end point apparatus is used, tfjielectrodes are covered by this amount of solvent. If He | end point is to be determined, make up a sefcond well. * Adjust the stirrer, if any, ,to prpyide adequate mixing .Sit splashing. Titrate the mixture to the instrumental |jpint (see 3.1), or the coltir en^ppint (see'3.2), with leagent If the color end point is to be observed, ffijie flask to the orange-red end point and the second jh the first. Set aside the first flask as a comparison aro for titrating the specimen. Ifo the titration mixture thus prepared, add an |of specimen as indicated in Table 1. Exercise care specimen is transferred so that water is not Ffrom the air, particularly under conditions of high y. Again, titrate the mixture with Fischer reagent to ae instrumental or color end point previously em|[Record the amount of reagent used to titrate the i the specimen. :5{ Ketones--In titrating ketones when greatest precision is ~ cool the reaction mixture in ice water during the addition of agent. Organic Acids--Cool the reaction mixture in ice water prior to |tion of Fischer reagent 6--When using the volumetric flask type titration vessel in Jimates, place a piece ofthin sheet rubber over the mouth ofthe provide a small hole for introducing the buret tip. In less humid i it is sufficient to lower the tip of the buret deeply into the long Ithe titration flask. fg 7--In titrating with the volumetric flask type titration vessel, jiwetting the stopper and upper end of the flask with either the gffijjor the sample solvent. Each time the titration is interrupted, gpe buret tip to the neck of the flask to remove droplets which, if uoved, would absorb moisture from the atmosphere. When the Is removed from under the buret tip, wipe the tip with a clean dry Bn a downward motion. alculation |1 Calculate the water content of the specimen as vs: Water, %, by weight -- (Vx fV)/(lO x S) volume of Fischer reagent required for titrating by the specimen, mL, `equivalency factor for Fischer reagent, water per |f millilitre of reagent, mg, and = specimen weight used, g. TABLE 1 Recommended Specimen Sizes Water ' Content, X 'Specimen Size: Manner Specimen Taken 2.5 to 10 0.5 to 2.5 Below p.5 weight containing 0.15 to 0.18 g of HsO . 10 mL 25 mL ., weighing pipet calibrated volumetric pipet sanpe as for 0.5 to 2.5 13. Precision and Bias9 13.1 On the basis ofan interlaboratory study in which one operator made duplicate determinations in each of eight different laboratories, on two days, on samples of acetone containing 0.118 and 0.406 % water and of methyl ethyl ketone containing 0.050 and 0.176 % water, the following criteria should be used for judging at the 95 % confidence level the acceptability of results on samples containing less than 0.5 % water: 13.1.1 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 0.015 % absolute. 13.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operator in different laboratories should be considered suspect if they differ by more than 0.027 % absolute. 13.2 In another interlaboratory study, one operator in each of seven different laboratories, on two different days, made duplicate determinations on five randomly coded samples of hexyl acetate containing 0.015, 0.034, 0.052, 0.071, and 0.098 % water. One ofthe seven laboratories used three different equipment or procedural variations, or both, thereby making this, in effect, a nine interlaboratory study. The statistically designed study covered a variety of equip ment, analytical methods, and reagents using the Karl Fischer chemistry. 13.2.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same analyst should be considered suspect ifthey differ by more than 0.030 Vx % absolute. 13.2.2 Reproducibility--Two results, each of the mean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 0.060 Vx % absolute. 13.3 Bias has not been determined for this test method. Refer to Notes 5, 6, and 7 for factors that might influence test bias. Report 12.1 For water concentrations below 0.5 %, report all ilts to 0.001 %. Two determinations which agree within 7o, absolute, are acceptable for averaging (95 % confi- hce level). 14. Keywords 14.1 Karl Fisher method; solvents; water content s Supporting data is available from ASTM Headquarters. Request RR: D01 - 1049. 193 DU P050295859 # D 1364 The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised (hat 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 ti not revised, eitherreapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7916 Race St., Philadelphia, PA 19103. 1 'I I 194 DUP050295860 |> Designation: D 1392 87 Standard Specification for Safflower Oil*1 This standard is issued under the fixed designation D 1392; the number immediately following the designation indicates the year of original adoption or, in tire case of revision, the year of last revision. A number in parentheses indicates the year oflast reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapproval. JPe pThis specification covers a safflower oil suitable for g protective coatings. lerenced Documents -ASTM Standards: 55 Guide for Testing Drying Oils2 i Test Method for Sampling liquid Oils and Fatty fikcids Commonly Used in Paints, Varnishes, and Re nted Materials2 1475 Test Method for Density of Paint, Varnish, Lac|guer, and Related Products3 11541 Test Method for Total Iodine Value of Drying Oils Hand Their Derivatives2 i 1544 Test Method for Color of Transparent Liquids P (Gardner Color Scale)4 >1639 Test Method for Acid Value of Organic Coating ^Materials3 >J.952 Test Method for Quantitative Determination of Break in Drying Oils2 sfiVJD1959 Test Method for Iodine Value of Drying Oils and 1 Fatty Acids2 1960 Test Method for Loss on Heating of Drying Oils2 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Adds2 This specification is under the jurisdiction of ASTM Committee D-l on Paint Related Coatings and Materials and is the direct responsibility' of Subcomttee D01.32 on Drying Oils. Current edition approved Oct. 30, 1987. Published December 1987. Originally blished as D 1392 - 56. Last previous edition D 1392 - 70 {I981)ei. . A Annual Book ofASTM Standards, Vol 06.03. i ^ Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 2 D1967 Test Method for Measuring Color After Heating of Drying Oils2 3. Properties 3.1 Safflower Oil shall be the oil obtained solely from safflower seed, shall be free of dirt or other contamination, and shall conform to the requirements in Table !. 4. Test Methods 4.1 Sampling--Sampling shall be conducted in accord ance with Test Method D 1466. 4.2 The properties enumerated in this specification shall be determined in accordance with the applicable ASTM test methods listed in Table 1. The significance ofthe methods of testing enumerated under properties in this specification is discussed in Methods D 555. 1 TABLE 1 Physical Properties Property Requirement ASTM Method Specific gravity, 25/25C Refractive index. 25C iodine value Acid value, max Saponification value Loss on heating at 105 to 110C, max, % Break, max, % Clarity Color (Gardner), max Color after heating, max 0.922 to 0.927 1.4740 to 1.4750 140 to 150 3.0 189 to 195 0.3 0.003 dear and transpar ent at 65C 12 5 D 1963, D 1475 D 1541,0 1959 D1639 D1962 D 1960 01952 D 1466 D 1544 D 1967 The American Society for Testing end Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years end ifnot revised, eitherreapproved or withdrawn. Your comments are Invitedeither torrevision 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. 195 DUP050295861 Designation: D 1399 - 90 Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate1 This standard is issued under the fixed designation D 1399; 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 amount of unsaponifiable impurities in tricresyl phosphate. 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 Section 7. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water12 5 3. Summary of Test Method 3.1 The specimen is refluxed in the presence of an aqueous solution of sodium hydroxide which converts the phosphate ester to water-soluble salts. The saponified mate rial is extracted with, petroleum iether which dissolves any unsaponifiable or water-insoluble material. The combined extracts are evaporated in a tared evaporating dish, and the residual nonvolatile material is determined. 4. Significance and Use 4.1 This test method determines the amount of unsaponifiable impurities in tricresyl phosphate remaining after manufacture or that may, be introduced during han dling and storage. 4.2 Water-insoluble materials, which do not evaporate on a steam bath or in a drying oven operated at 75 5C for 1 h, will be included as unsaponifiable material. 5. Apparatus 5.1 Reflux Apparatus, consisting of a 250-mL Erlenmeyer flask equipped with a 24/40 standard-taper joint attached to an Allihn-type reflux condenser similarly equipped with a 24/40 standard-taper joint. 5.2 Separatory Funnel, having a capacity of 250 mL. 5.3 Evaporating Dish, porcelain or glass, having a ca pacity of 120 mL. 5.4 Steam Bath. 5.5 Drying Oven, thermostatically controlled, at a tempera- ture of 75 5C. 6. Reagents 6.1 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.3 >: Otherwise, the best available grade shall be used. | 6.2 Purity of Water--References to water shall be under- f stood to, mean reagent water conforming to Type IV of J Specification D 1193. | 6.3 Petroleum Ether, having a boiling range from 30 to !: 65C. 6.4. Sodium Hydroxide (NaOH) Pellets. S 7. Hazards 7.1 Tricresyl phosphate is hazardous through inhalation or skiii absorption. Care should be taken in handling the material. 7.2 Ortho-isomer of tricresyl phosphate is considered toxic. Trace amounts may be present in tricresyl phosphate specimens. S. Procedure 8.1 Place approximately 30 mL of water in the 250-mL Erlenmeyer flask and to this carefully add approximately 10 g of NaOH pellets. Carefully swirl the flask to dissolve the NaOH, and cool the solution to room temperature. 8.2 By means of a weighing pipet, transfer a 10-g spec imen, weighed to 1 mg, to the flask. Add several boilingstones, connect the flask to the reflux condenser, and reflux for 1 h. (Warning--See 7.1 and 7.2.) 8.3 At the end of the refluxing period remove the flask from the heat and wash the condenser down with 50 mL of water. 8.4 Cool the flask to room temperature and transfer its content to the 250-mL separatory funnel. Extract the sapon ified material three times with 25-mL portions of petroleum ether. Exercise particular care in separating the two phases so that none of the. aqueous phase is. occluded in the ether phase. 8.5 Combine the ether extract and place in the 120-mL evaporating dish, weighed to 1 mg. Place on the steam bath and carefully evaporate to dryness. Dry the bottom of the 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1399 - 56 T. Last previous edition D 1399 - 85. 2 Annual Hook ofASTM Standards, Vols 06.03 and 11.01. 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." 196 DUP050295862 fating dish with a clean lint-free doth and place in the j oven set at 75 5C for 1 h. Cool in a desiccator and i the evaporating dish and its contents to 1 mg. Ilcvlation 10. Precision and Bias 10.1 Precision--Results should not differ from the mean by more than the following amounts: Repeatability (One operator and apparatus) Reproducibility (Different operators and apparatus) Calculate in weight percent the unsaponifiable coriU, of the specimen as follows: U = (R/S) x 100 Unsaponifiable content, weight % absolute 0.05 0.1 10.2 Bias- -Bias has not been determined for this test method. "plesidue weight from evaporation, g, and 11. Keywords specimen weight, g. 11.1 tricresyl phosphate; unsaponifiable content Ir The Atnerican 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 ara expressly advised that determination of the validity of any such patentrights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject fo revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM. Committee on Standards, 1916 Race St., Philadelphia, PA 19103. sir;- 197 DUP050295863 Designation: D 1462 - 87 Standard Specification for Refined Soybean Oil1 This standard is issued under the fixed designation D 1462; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers refined soybean oil suitable for use in the paint and varnish industry. 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)2 ' D 555 Guide for Testing Drying Oils3 D 1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)5 198 D 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method5 D 1639 Test Method for Acid Value of Organic Coating Materials4 D1952 Test Method for Quantitative Determination of Break in Drying Oils3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Adds3 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 1.32 on Drying Oils. Current edition approved Oct. 30, 1987. Published December 1987. Originally published as D 1462 - 57. Last previous edition D 1462 - 70 (i981)ei. 2 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Bock ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. D 1960 Test Method for Loss on Heating of Drying Oils3 i D 1962 Test Method for Saponification Value of Drying f Oils, Fatty Acids, and Polymerized Fatty Acids3 ? D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 3 , ? D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 - D1967 Test Method for Measuring Color After Heating of ? Drying Oils3 sj . < - ;ij 3. Properties 3.1 Refined soybean oil shall conform to the requirements in Table 1. 4. Test Methods { -fll f 4.1 Sampling--Sampling shall be conducted in accor dance with Test Method D 1466. 4.2 The properties enumerated in this specification shall be determined in accordance with the applicable ASTM test methods listed in Table 1. The significance of the test methods enumerated under properties in this specification is discussed in Methods D 555. ' '* . 1 TABLE 1 Physical Properties Property Requirements ASTM Method Specific gravity, 25/25"C Acid value, max Saponification value Unsaponifiable matter, max, % Iodine value (Wijs), min Loss on heating at 105 to 11 CPC, max, % Clarity Color (Gardner), max Color (after heating), max Break, max, % Viscosity, approximate stokes 0.917 to 0.924 0.3 189 to 195 1.5 126 0.3 clear and trans parent at 65C 6 4 0.02 0.32 to 0.50 D1963,D 1475 D 1639 D 1962 D 1965 D1959 D 1960 D 1466 D 1544 D 1967 D 1952 D 1545, D 445 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 ofinfringement ofsuch rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM. Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 198 DUP050295864 Jesignation: D 1466 - 86 (Reapproved 1990) Standard T&bt Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Related Materials1 This standard is issued under the fixed designation JD 1466; 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. fatais test method covers procedures for obtaining Optative samples of oils, fatty acids, and polymerized gilds that are commonly used in paints, varnishes, and ^.materials, and that are in a liquid state when Ijsd. iplis standard does not purport to address all of the fproblems associated with its use. It is the responsibility pqver uses this standard to consult and establish yriate safety and health practices and determine the Ability ofregulatory limitations prior to use. nunary of Test Method 1 Samples of drying oils, fatty acids, and polymerized \ acids are subjected to various test methods for deter- ig physical and chemical characteristics. It is necessary tain a sample or a composite of several samples in such ter and from such locations in the container, that the le or composite will be truly representative of the luct. The precautions required to assure such a represen sample are numerous, depending on the type of luct, the container, the cleanliness of the sample coniter,, and the sampling procedure that is to be used. Significance and Use 3.1 Because precipitated saturated acids or oils containing |{gh proportion of saturated acids, foots, or other insoluble litter may not be homogeneous, the sampling procedure |ust be designed so that the sample obtained is representave of the overall composition of the material. Different Impling procedures are presented such that a representative ample may be obtained from material stored in different pes of containers. Ip. Apparatus 4.1 Oil Thief: 4.1.1 Liquid Oils and Fatty Acids--A glass tube, % to lh in. (9.5 to 12.7 mm) in internal diameter and approximately 140 in. (1 m) in length. One end shall be constricted by a short taper to approximately V* in. (6 mm), and the other end shall be constricted sufficiently so that it can be lised as a finger valve. This thief is used for sampling casks, drams, etc. 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 D01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 1466 ~ 57. Last previous edition D 1466 - 67 (I984)CI. 4.1.2 Polymerized Fatty Acids--A glass tube, 3A to 1 in, (20 to 25 mm) in internal diameter, and approximately 40 in. in length. One end shall be constricted so it can be used as a finger valve. This thief shall be used for sampling casks, drums, etc. 4.2 Zone Sampler, 12-in. (305-mm) oil thief,2 consisting of a graduated glass tube with either aluminum or cadmiumplated brass fittings. 4.3 Compositing Pail, noncorrosive compositing pail, made of stainless steel, aluminum, enamelware, polyeth ylene, or comparable material. 4.4 Graduated Cylinders: 4.5 Sample Containers, clear glass or brown glass bottles, or cans (for other than fatty acids and polymerized fatty acids). The clear glass bottles are advantageous because they may be examined visually for cleanliness, sediment, etc. The brown glass bottles afford some protection from light. Only cans that do not have any solder flux on the interior are permissible for storing oils. Cans shall not be used for fatty acids or polymerized fatty acids. 4.5.1 The closure for the glass bottles may be good quality corks, with or without tin or aluminum foil. Screw caps may be used for both , bottles and cans. 4.5.2 All sample containers shall be clean and free of water, lint, dirt, washing compounds, solvents, flux or acids, rust, oil, etc. 5. Samples 5.1 The size of the sample should be kept to a minimum. In most instances, 1 qt (0.9 L) of material should suffice. However, in many tests, a minimum of 3 gal (11 L) is required--1 gal (3.8 L) for the purchaser, 1 gal for the seller, and 1 gal in reserve for a possible arbitration umpire test. If refining or bleaching tests are required, the minimum quantity is approximately 1 gal. 5.2 The oil shall be completely liquid for proper sampling. The temperature during melting should not exceed the melting point by more than 15C. If the oil is completely liquid, it should have a minimum temperature of 10C. Polymerized fatty acids should be heated to a temperature only sufficiently warm to facilitate flow. 5.. 3 Oil drums shall be placed in a warm place for several hours or longer prior to sampling, so that their contents will completely liquefy. 2 Samples manufactured by the W. H. Curtin Co.. Houston, TX, has been found suitable for this purpose. 199 DUP050295865 -S # D 1466 5.4 Tank cars, if equipped with heater coils in proper condition, may be slowly heated to 15C above the melting point of the oil, keeping in mind that prolonged heating might discolor the product, particularly fatty acids and polymerized fatty acids. 5.5 Labels shall be so affixed to the containers that the adhesion is of a permanent nature and the labeling does not smear. 5.6 The labels shall identify the sample as to material, date received, date sampled, shipper, car number, container size, number of containers, temperature and volume in containers, receiving slip number, and batch number. 5.7 On agreement between the purchaser and the seller,; samples shall be stored in a cupboard orstoreroom out of the direct rays of the sun and for no longer than 6 months. 6. Procedure 6.1 Sampling Drums or Casks--Mix the contents of the drum or cask by rolling it through a few complete revolu tions; up-end the drum or cask, introduce the oil thief through the bung opening, and slowly lower it to the bottom. Close the end opening of the thief with a finger and remove quickly. Place the contents of the thief in a container and repeat the sampling until sufficient material has been ob tained. When sampling of each drum or cask is not feasible, sample a minimum of 10 % of the containers to form the composite sample. 6 2 Sampling Tank Cars When No Solids Are Present-- With the zone sampler (see 4.2), sample the top, middle, and bottom portions of the tank car in that order. If no water or solids are noted, make a composite by blending one part of the top, two parts of the middle, and one part of the bottom sample. ' 6.3 Sampling Tank Cars When Suspended Solids Are Present--With the zone sampler (see 4.2), sample the top, middle, and bottom portions of ttys tank car in that order. If the bottom zone sample shows 'the; presence of water or suspended' solids, note the depth bi the foots layer to the nearest xh in. (12.5 mm). Transfer the entire contents of the 12-in. (305-mm) zone sampler to a clean, dry container marked "bottom sample," and report the depth of foots in the sampler. Also report the capacity of the car in gallons. i Composite the footy oil with the upper oil in the laboratory I or under the direct supervision of the laboratory as follows: f 6.3.1 Blend one part of the top sample with two parts of the middle sample. 6.3.2 Using the depth ofsuspended solids and the capacity of the car reported, determine from Table 1 the number of parts of well-mixed bottom sample to be blended with the one part top and two parts middle sample blended in accordance with 6.3.1. 6.3.3 Measure in a graduated cylinder the correct amount ofwell-mixed bottom sample determined from Table 1. Pour ! it into the one part top and two parts middle sample blended in accordance with 6.3.1. Rinse the remaining suspended1 * solids adhering to the walls of the graduated cylinder with ' some of the composite just prepared, and then return the j rinsings to the composite sample. ,t 6.3.4 Stir vigorously until the foots have been uniformly ' distributed; then subdivide into several identical portions (usually three, of about % gal (3 L) each) in appropriate containers and mark clearly so as to define the contents, or . as may be designated by trading rules or regulations gov erning the transaction represented. 7. Precision and Bias 7.1 Precision and bias are not applicable to this test method. Depth of Stratified Matter in Oil Thief, in. (mm) t (25) 2(50) 3(75) 4(100) 5(125) 6 (150) 7 (180) 8 (200) 0 (230) 10 (250) 11 (280) 12 (300) TABLE 1 Parts of Bottom Sample to Be Blended with Top and Middle Sample (see 6.3) 4000-gal (15 100-L) Car, approximately 60-in. (1-5-m) dia 6000-gal (22 700-L) Car, approximately 72-in (1.8-m) dia 8000-gal (30 000-L) Cat, approximately 78-in. (2-fn) dia 10 000-gal (37 800-L) Car, approximately 87-in. (2.2-m) dia 0.35 0.34 0.36 0.38 0.40 0.43. ' 0.45 0.47 0.49 0.51 0.53 0.55 0.24 0.24 0.26 0.27 0.29 . 0.31 0.32 0.34 0.36 0.37 0.38 0.40 0.23 0.22 .0.24 0.26 0.27 0.28 0.30 0.31 0.32 0.34 0.35 0.36 ' . 0.20 0.19 0.20 0.21 0.22 0.24 0.25 0.26 0.27 0.28 0.29 0.30 12 000-gal (45 400-L) Car, approximately 92-in, (2.3-rti) dia 0.19 0.18 ' 0.19 0.20 0.21 , 0.22 0.23 0.24 0.25 0.26 0.27 0.28 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 200 DUP050295866 Designation: D1467 - 89 Standard Guide for Testing Fatty Acids Used in Protective Coatings1 fi''-' ... This standard is issued lihSer the fixed designation D 1467; the number immediately following the designation indicates the year of original, adoption or, inthe 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. ope |j,l This guide covers the selection and application of dures for testing.fatty adds such as cottonseed, linseed, |n, dehydrated castor, tall oil, etc. used in protective jgs. I The test methods included are listed as follows: i Test Method pValue prance W ... ,i . Section ASTM Test Method 4 13 9 13 . D 1980 D 1544 D 1951 D 2090 , Ipiier htirium - CoBalt Change After Hearing Hy Acid Composition oxyl Value isin Acids jpling bonification Value pi- ' : gppniliable Matter pration: Slene Value Jjfjlodine Value ' ... 14 J4 6 12 10 II 3 7 15 .8 5 5 D 1544 D 1209 D 1981 D 1983 D 1957 D 1240 D 1466 D 1962 PT982 D 1965.. D 1358 D 1959 .3 This standard may involve hazardous materials, opertfms, arid equipment. This standard does not purport to dress all ofthe safety problems associated with its use. It is Ie responsibility of the user of this standard to establish ppropriate safety and health practices arid determine the pplicability of regulatory limitations prior to use. \. Referenced Documents 2.1ASTM Standards: D 1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale)2 D1240 Test Method for Rosin Adds in Fatty Acids3 D1358 Test Methods for Spectrophotometric Diene Value of Dehydrated Castor Oil and Its Derivatives3 D1466 Test Method for Sampling Liquid Oils and Fatty ' Acids Commonly Used in Paints, Varnishes, and Re lated Materials3 D1541 Test Method for Total Iodine Value of Drying Oils and Their Derivatives3 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)2 1 These methods urc under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcom mittee DOf .32 on Drying Oils. Current edition approved March 31, 1989. Published May 1989. Originally published as D 1467-57 T. Last previous edition D 1467 - 72 (1981)". 2 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 06.03. D 1951 Test Method for Ash in Drying Oils and Fatty Acids3 D 1957 Test Method for Hydroxyl Value of Fatty Oils and Acids3 ' . D 1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 D 1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds and Polymerized Fatty Acids3 D1980 Test Method for Acid Value of Fatty Acids and Polymerized Fatty Acids3 D1981 Test Method for Measuring Color After Heating of Fatty Acids3 D 1982 Test Method for Titer of Fatty Adds3 D 1983 Test Method for Fatty Add Composition by Gas-Liqdid Chromatography of Methyl Esters2 D 2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids41 D 3457 ' Test Method for Preparation of Methyl Esters' from' Fatty Acids for Determination of Fatty Add Composition by Gas-Liquid Chromatography3 2.2 American Oil Chemists' Society (AOCS) Methods? Tj-la Polyunsaturated Adds Cc-13b Color, Wesson Method (Lovibond) Td-2a Photometric Index 3. Sampling 3.1 Sample the material in accordance with Method D 1466. 3.2 Fatty acids are frequently solid at room temperature and shall be completely liquified and blended prior to testing. Temperatures during liquefying of the fatty adds should not exceed 10 to 15C above die melting point of the sample. 3.3 Samples should be stored preferably in the dark, in full glass containers. Partially filled containers should be filled with inert gas or carbon dioxide to prevent oxidation. 4. Add Value 4.1 Acid value is a measure of the quantity of free fatty acids and is defined as the number of milligrams of potas sium hydroxide required to neutralize the fatty acids in 1 g of sample. Acid value determination is useful in establishing the identity and purity of a fatty acid. 4.2 Determine the acid value in accordance, with Test Method D 1980 which is the referee method. Other solvents A Annual Book ofASTM Standardly Vols 06.02 and 06.03. 5 Available from American Oil Chemists Society, 508 S. 6th St., Champlain, IL 61820. 201 DUP050295867 # D 1467 should be checked out carefully before using for control 8. Unsaponifiable Matter purposes. 5. Unsaturation 5.1 Iodine value is a convenient test for expressing the degree of unsaturation of a fatty acid. Iodine value is the weight percent of iodine absorbed. 5.2 Determine the iodine value in accordance with Test Method D 1959 which gives fairly good accuracy and preci sion (Note 1) when applied to normal fatty acids. When Test Method D 1959 is applied to fatty acids containing conju gated double bonds such as dehydrated castor or tung an empirical figure is obtained giving only a relative measure of the total unsaturation. Refer to Test Method D 1541 for a more accurate procedure for the determination of the total unsaturation of tung oil adds. When Test Method D 1959 is used for dehydrated castor acids, a spedmen weight of 0.11 to 0.13 g of fatty acids must be used to get comparative results between laboratories. 8.1 The term unsaponifiable matter; includes all of those substances that are not saponified by alkali and that are soluble in the ordinary fat solvents. Included are the higher aliphatic alcohols, sterols, and hydrocarbons. 8.2 Determine unsaponifiable matter in accordance with Test Method D 1965. Normal fatty acids contain small amounts of unsaponifiable matter, usually under 2 %. When excessive amounts of unsaponifiable matter are found, low quality is indicated. 9. Ash 9.1 The ash in fatty acids is deterfnined by igniting the acids under specified conditions and determining the amounts of noncombustible material. Carry out this proce dure in accordance with Test Method D 1951. The ash content of normal fatty acids should be very small. 10. Hydroxyl Value No t e 1--The analyst is cautioned to follow the test method exactly as written since small deviations in sample size, reagents, and time of reaction will definitely affect the accuracy and precision of die test method. 5.3 When Test Methods D 1358 is applied to dehydrated castor adds an empirical value is also obtained due.to the high linofeic acid content. In this method the conjugated 10.1 Hydroxyl value is defined as the number of milli grams of potassium hydroxide equivalent to the hydroxyl (OH) content of 1 g of sample. Hydroxystearic acid is the only common fatty acid to which this test is applicable. 10.2 Determine the hydroxyl value in accordance with Test Method D 1957. diene content is derived from spectrophotometric measure ments. Determine the amount of conjugated diene content of fatty adds in accordance with Test Methods D 1358, noting the empirical nature of the result for dehydrated castor acids. .. 5.4 The iodine value of'tall oil fatty adds containing appredable amounts of rosin acids is not a reliable measure of the fatty add unsaturation because of the unsaturation of the rosin acids. 11. Rosin Acids 11.1 Fatty acids derived from tall oils will normally contain varying amounts ofrosin acids. When the amount of the rosin acids does not exceed 15 %, determine their content in accordance with Test Method D 1240. 11.2 In Test Method D 1240 the rosin acids are deter mined by titration after esterification of the fatty acids with methanol in the presence of sulfuric acid as a catalyst, followed by separation ofthe acids. The test method requires 6. Color Change After Heating 6.1 The color stability of fatty adds when subjected to use of an expeiirhentally determined correction factor, dependent upon the amount of rosin acids present, elevated temperatures is of importance to many commercial users of fatty acids.. The conditions under which the color stability is determined such as temperature, time of heating, time of upheat, exposure to air, etc, all affect the final results. 6.2 Measure the color of fatty acids after heating by Test 12. Fatty Acid Composition 12.1 Fatty acid composition can be determined in accord ance with Test Method. D 1983 after esterification of the fatty acids in accordance with Test Method D 3457. Method D 1981, which is applicable to all normal fatty acids. No t e 2--The types and amounts of polyunsaturated acids in a I It has been shown to have good precision within and between sample of fatty acids may also be determined by use of an ultraviolet laboratories and should be used as the referee test method. spectrophotometer. By using this test method the percent of conjugated diene, triene, tetraene, and pentaene acids, and of linoleic, linolenic, 7. Saponification Value arachidonic, and pentaenoic acids can be calculated. This test method is time-consuming and the techniques required do not lend themselves to 7.1 Saponification value is a measure of the alkali-reactive groups in fatty acids and is expressed as the number of milligrams of potassium hydroxide that will react with 1 g of good accuracy or precision. The ultraviolet spectrophotometric method is not included in the ASTM methods, and reference should be made to AOCS Method Tj-la. sample. The saponification value on a good grade of vege table fatty acids is normally only I or 2 points above the acid 13. Appearance value as determined in accordance with Test Method ' 13.1 Observations for appearance of fatty acids should be D 1980. The difference between the saponification value and made on the liquefied sample. Transfer the sample to a the acid value is frequently referred to as the ester value. viscosity tube as described in Test Method D 1544 and check Saponification value can be used to calculate the average for haze, dirt, skins, or other materials that might indicate molecular weight of the fatty acid. contamination of the material. 7.2 Determine the saponification value in accordance 13.2 Determine the clarity in accordance with Test with Test Method D 1962. Method D 2090. 202 DU P 0502 95868 lor The color reference standards described in Test D 1544 provide a rapid and sufficiently accurate for determining color on most fatty acids (Note 3). the hue of the fatty acids sample does not exactly that of the reference sample it is suggested that the :ty of color be matched rather than attempting to hue. Where extremely light colored fatty adds are en tered, use Test Method D 1209. e 3--No accurate correlation between Test Methods D 1209 and 1 has been possible. 14.3 Lovibond glasses (AOCS Official Method Cc-13b) and spectrophotometric measurements (AOCS Method Id2a) are occasionally used to measure fatty acid colors. No t e 4--No correlation has been established between these methods and Test Method D 1544 when used for fatty acids. 15. Titer 15.1 Titer is the solidification point of fatty acids under specified conditions. Determine titer in accordance with Test Method D 1982. The titer value can be correlated with the degree of unsaturation of a fatty acid and is useful in determining the identity and purity of a fatty acid. 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 ofthis standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rtghfs, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and mustbe reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additionalstandards and should be addressed toASTM 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 Pace St., Philadelphia, PA 19103. ' 203 DUP050295869 Designation: D 1468 - 84 (Reapproved 1988)1 Standard Test Method for Volatile Matter in Tricresyl Phosphate1 This standard is issued under the fixed designation D 1468; 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 (t) indicates an editorial change since the last revision or reapproval. r This test'method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standards for the specific year of issue which has been adopted by the Department ofDefense. `i No t e--Sections 1 and 4 were changed editorially in March 1988. 1. Scope 1.1 This test method covers a procedure for determining the volatile matter in tricresyl phosphate. 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 4. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Apparatus 2.1 Oven, thermostatically controlled at 105 5C. 2.2 Petri Disk, 100-mm diameter, or equivalent. 3. Significance and Use 3.1 This test method provides a measurement of volatile matter in tricresyl phosphate. The results of this measure ment can be used for specification acceptance and deter- 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27, 1984. Published August 1984. Originally published as D 1468 - 57 T. Last previous edition D1468 - 79. mining performance in plasticizer use. 4. Hazards t 4.1. Tricresyl phosphate is hazardous and special precautions.should be taken when handling it. Avoid eye and skin . contact and inhalation of vapors. 5. Procedure 5.1 Place a flat aluminum, glass, or porcelain dish in an oven at 105 5C for 1 h. Cool in a desiccator and weigh to 10 mg. Spread evenly over the bottom of the dish approxi mately 25 g of the sample. Weigh the dish and the specimen to 10 mg and place in an oven at 105 5C for 3 h. Cool the dish and specimen in a desiccator, and reweigh to 10 mg. .6 Calculation 6.1 Calculate the volatile matter in tricresyl phosphate as follows: Volatile matter, % = [(5 - R)/S] x 100 where: S = weight of specimen used, g, and R = weight of specimen after heating, g. 7. Precision and Bias 7.1 Results should not differ from the mean by more than the following amounts: Within laboratory Between laboratories Volatile matter, weight % 0.05 0.1 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Asm mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnet revised, either reapprovedor withdrawn. Yourcomments are Invited ether for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 204 DUP050295870 "signation: D 1476 - 88 Standard Test Method for Heptane Miscibility of Lacquer Solvents1 This standard is issued under the fixed designation D 1476; 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 (s) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4083 of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. , _,V _iis test method covers determination of the raiscilacquer solvents with heptane. It ihay also be used to Qualitatively the presence of moisture in esters and l_For the quantitative determination of water content, see thod D 1364, his standard may involve hazardous materials, oper. and equipment. This standard does not purport, to % all ofthe safety problems associated with its use. It is sponsibility of the user of this standard to establish ipriate safety and health practices and determine Ihe ^ability ofregulatory limitations prior to use. :For hazard information and guidance, see the sup-1 Material Safety Data Sheet. eferenced Documents i ASTM Standards: ' 611 Test Methods for Aniline Point and Mixed Aniline ;Point of Petroleum Products and Hydrocarbon Sol vents2 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 * This test method is under the jurisdiction of ASTM Committee D-l on Paint Related Coatings and Materials and is the responsibility of Subcommittee ;\35 on Solvents, Plasticizers, and Chemical Intermediates. (Current edition approved March 14, 1988. Published May 1988. Originally fished as D 1476 - 57 T. Last previous edition D 1476 - 84. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03, 2 Annual Book ofASTM Standards. Vo! 06.03. 3. Significance and Use 3.1 Water in a solvent may interfere with many uses of the solvent. This test method provides a measure of the miscibility of lacquer solvents with a nonpolar mediumheptane. It also provides a qualitative indication of the presence or absence of moisture in these solvents (often esters and ketones). The results of these measurements may be used for specification acceptance. 4. Reagents 4.1 Heptane, containing not less than 99 % n-heptane. No t e 2--Detailed requirements for 99 % n-heptane are specified in Table 1 of Test Method D 611. 5. Procedure 5.1 Both the specimen and the heptane shall be at a temperature of 20 1C. Transfer 5 mL of the specimen to a 100-mL glass-stoppered (graduated) cylinder and add 5-mL increments of heptane until the total specified volume has been added, shaking well after each addition. A clear solution indicates miscibility and a turbid solution indicates immiscibility or the presence of water in the specimen, or both. 6. Report 6.1 If the solution remains clear after the addition of the specified amount of heptane, report the specimen as passing this test. 7. Precision and Bias 7.1 Because of the pass-fail nature of this test procedure, no precision or bias statement is presented. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are 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 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. 205 DUP050295871 Designation: D 1537 - 60 (Reapproved 1988)f1 t Standard Specification for Distilled Soybean Fatty Acids1 This standard is issued under the fixed designation D 1537; 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. el No t e--Paragraph 1.1.1 was editorially changed in October 1988. 1. Scope 1.1 This specification covers distilled acids derived from the distillation of soybean oil. Three types are covered, as follows: 1.1.1 Type I--Usually produced from degumtned soy bean oil and referred to as water white soybean fatty adds. 1.1.2 Types 11 and III--Usually produced from recovered soybean oil. 2. Referenced Documents 2.1 ASTM Standards: D1467 Guide for Testing Fatty Adds Used in Protective Coatings2 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 D01.32 on Drying Oils. Current edition approved Sept. 19, 1960. Originally issued 1958. Replaces D 1537- 58 T. 2 Annual Book ofASTM Standards, Vol 06.03. D 1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 D1962 Test Method for Saponification Value of Drying. Oils, Fatty Acids, and Polymerized Fatty Acids2 D 1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Acids2 D1980 Test Method for Acid Value of Fatty Adds and Polymerized Fatty Acids2 D 1982 Test Method for Titer of Fatty Acids2 ^ 3. Properties 3.1 Distilled soybean fatty acids shall conform to the requirements in Table 1. 4. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance with Methods D 1467. 3 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. Acid value Saponification value Onsaponifiable matter, max, % Iodine value, min Color, Gardner, max Titer, 'C TABLE 1 Requirements for Distilled Soybean Fatty Acids ASTM Test Methods Type 1 Type II D1980 D1962 D1965 D 1959 D 1544 1982 197 to 204 197 to 204 1.0 133 2 21 to 24 195 to 205 197 to 207 2.0 125 4. 23 to 29 Type III 195 to 205 197 to 207 2.0 120 6 23 to 29 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Rem 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 mustbe reviewed every five years and ifnotrevised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 206 DUP050295872 Designation: D 1538 - 60 (Reapproved 1988)e1 Standard Specification for Distilled Linseed Fatty Acids1 This standard is issued under the fixed designation D1538; 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. i No t e--Paragraph 1.1.1 was editorially changed in October 1988. -Pe ' ; This specification covers distilled acids derived from distillation of linseed oil. Two types are covered as ' s: i`1.1 Type I--Usually produced from degummed linseed and referred to as water white linseed fatty acids. .1.2 Type II--Usually produced from recovered linseed tnd referred to as regular distilled linseed fatty acids. referenced Documents U ASTM Standards: . 1467 Guide for Testing Fatty Acids Used in Protective Coatings2 D1544 Test Method for Color of Transparent Liquids 1 (Gardner Color Scale)3 iv: This specification is under thejurisdiction ofASTM Committee D-1 on Paint Related Coatings and Materials and is the direct responsibility of Subcomlee D01.32 on Drying Oils. Current edition approved Sept/ 19, 1960. Originally issued 1958. Replaces 1538-58 T. 2 Annual Book ofASTM Standards, Vol 06.03. % Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids2 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Acids2 D 1980 Test Method for Acid Value of Fatty Acids and Polymerized Fatty Acids2 D1982 Test Method for Titer of Fatty A.cids2 3. Properties 3.1 Distilled linseed fatty acids shall conform to the following requirements: Arid value Saponification value Unsaponifiable matter, max, % Iodine value, min Color, Gardner, max Titer, "C ASTM Test Methods D 1980 D 1962 D 1965 D 1959 D 1544 D 1982 Type I 197 to 204 197 to 204 1.0 179 3 17 to 20 Type II 195 to 202 195 to 202 2.0 155 7 19 to 25 4. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance with Methods D 1467. 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 era 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 for revision of this 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 lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 207 DUP050295873 Designation: D 1539 - 60 (Reapproved 1988) Standard Specification for Dehydrated Castor Acids1 This standard is issued under the fixed designation D 1539; 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 acids produced from dehy drated castor oil. Two types are covered as follows: 1.1.1 Type /--Distilled dehydrated castor adds. 1.1.2 Type //--Undistilled dehydrated castor acids. 2. Referenced Documents 2.1ASTM Standards: D1358 Test Method for Spectrophotometric Diene Value of Dehydrated Castor Oil and Its Derivatives2 D 1467 Guide for Testing Fatty Adds Used in Protective Coatings2 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 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 DO 1.32 on Drying Oils. Current edition approved Sept 19, 1960. Originally issued 1958. Replaces D1539-58 T. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. TABLE 1 Requirements for Dehydrated 'Castor Acids ASTM Test Method' Type 1 Type II Acid value Saponification value Iodine value Color, Gardner Spectrophotometric diene value D198'b D1962, D 1959 D 1544 D 1358 195 to 200 195 to 200 150 to 156 1 max 28 to 35 187 to 195 193 to 199 138 to 143 - 5 to 8 25 to 32 D1959 Test Method for Iodine Value of Drying Oils and' Fatty Acids2 D1962 Test Method for Saponification Value of Drying: Oils, Fatty Acids, and Polymerized Fatty Acids2 D1980 Test Method for Acid Value of Fatty Acids and. Polymerized Fatty Acids2 * 3. Properties 3.1 Dehydrated castor adds shall conform to the fol lowing requirements given in Table 1. 4. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance with Methods D 1467, except that the spectrophotometric diene value shall be determined in accordance with Test Method D 1358. 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 ofthe validity of any such patent rights, and the risk of Infringementof such rights,we entirely their own responsibility. : This standard is subject to revision at any time by the responsible technical committee and must be reviewed every the years and if not revised, eitherreapproved or withdrawn. Yourcomments are Invited either forrevision at 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. 208 DUP050295874 .signation: D 1541 - 86 (Reapproved 1990) Standard Test Method for Total Iodine Value of Drying Oils and Their Derivatives1 This standard is issited under the fixed designation D 1541; the number immediately following the designation indicates the year of original adoption of, 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. `s test method2 covers the determination of total Aue. , is test method is applicable to oils, fatty acids, and ils. While this test method is applicable to all oils : adds and bodied oils, .it is particularly useful for ing oils or derivatives that have conjugated ation. '-is standard does not purport to address all of the roblems associated with its use. It is the responsibility o` ever uses this standard to consult and establish note safety and health practices and determine the Ability of regulatory limitations prior to use. Specific statements are given in Sections 6 and 7. renced Documents t .ASTM Standards: 193 Specification for Reagent Water3 ,959 Test Method for Iodine Value of Drying Oils and Fatty Adds4 5 sfinitioB j^l total iodine value--a measure of the total "turation present in fats and oils (Note 1), expressed as number of centigrams of iodine equivalent to the Saturation present in 1 g of sample (weight percent of bed iodin,e). 'o t e I--When the total iodine value is determined on oils having jugated systems, the result is a measure of the total unsaturation. !s is in contrast to the iodine value method described in Test Method .1959 which determines only part of the total unsaturation of -jugated systems. Significance dad Use 4.1 This test method measures the total amount of unsaturation including conjugated unsaturation by addition of bromine in a catalyzed bromine solution to the double bonds. The amount of bromine absorbed is determined by back titration of the excess bromine, and then compared to a 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 1541 -58 T. Last previous edition D 1541 -60(1984). 2 This procedure is essentially identical with that of Planck, R. W., Pack, F. C,, and Goldblatt, L. A., as published in the Jotirnal, Am. Oil Chemists' Soc., Vol 30, 1953, p. 417, using the Rosenmund-Kuhnhenn reagent. Previously Benhain, G. H., and Klee, L. /., published data on the use of this reagent for determining unsaturation in the Journal, Am. Oil Chemists' Soc., Vol 27, 1950, pp. 127-130. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.03. blank determination. This test method is preferred over Test Method D 1959 for products containing conjugated unsaturation. 5, Apparatus 5.1 Iodine Flasks, glass-stoppered, of250-mL capacity. , No t e 2--The test may be run either in a photographic-type dark room Under red safelight illumination3 or in a darkened laboratory in which the light intensity is adjusted to 0.5 footcandle (5.4 lx) or less. The darkroom with red safelights permits the use of clear flasks. If the test shall be run ina darkened laboratory, low-actinic (amber) flasks, or clear flasks protected from light by covering as described below, must be used: Alternative modes of using clear flasks in a darkened laboratory are described as follows. The type of covering is left to the discretion of theanalyst: (1) Place the clear iodine flask in a suitable metal can so that the neck of the flask is level with the can rim. Over the top of the can, place apiece of heavy cardboard, with a hole precut in the center to just fit over the neck of the flask; die top of the flask should just protrude out of the hole in the cardboard cover. Then run the analysis as usual in a darkened laboratory. ' (2) Wrap heavy aluminum foil around the iodine flasks so as to cover all but the top rim. The foil can be then removed at the latter stage of titration. Run the analysis in a darkened laboratory. , (3) Place the flask in an opaque bag that has a drawstring neck. The rim of the iodine flask should just protrude from the bag to allow addition of reagent 5.2 Graduates, 5, 25, and 50-mL capacity. 5.3 Volumetric Pipets, 10, 20, and 50-mL capacity. No t e 3--The bulb of the 50-mL pipet should be covered with aluminum foil. 5.4 Buret, 50-mL capacity graduated in 0.1-mL divisions. 5.5 Weighing Device for Sample--A small, wide-mouth vial, fitted with a cork stopper and medicine dropper, may be used to weigh the sample by difference. Alternatively, the sample may be weighed directly into a 1-mL microbeaker, and carefully dropped into the iodine flask. 5.6 Photoelectric Light Meter--Any suitable meter for measuring room illumination in footcandles. If a darkroom and red safelight illumination are to be used, a meter is not required. ! 5.7 Erlenmeyer Flasks, three, 250-mL. 5.8 Volumetric Flasks, four, 1-L, glass-stoppered. 5.9 Bottle, Amber, one, 4-L, glass-stoppered. 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- 5 Wratten No. 1 safelights have been found satisfactory for this purpose. 209 DUP0502 95875  D 1541 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 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type I of Specification D 1193. 6.3 Carbon Tetrachloride (CC14)--(Warning--See 7.1) 6.4 Mercuric Acetate Solution--Dissolve 25 g of mercuric acetate (Hg(C2H302)2) (Warning--See 7.2) in glacial acetic acid (CH3COOH) and dilute to 1 L with glacial acetic acid. (Wanting--See 7.3) 6.5 Potassium Iodide Solution (150 g/L)--Dissolve 150 g of potassium iodide (KI) in water and dilute to 1 L. 6.6 Rosenmund-Kuhnhenn Reagent--Place 40 mL of gla cial acetie acid (CH3COQH) in each of three 250-mL Erlenmeyer flasks. To the first, add slowly 28.4 0.2 g of pyridine, (Warning--See 7.4) with cooling in an ice bath. To the second flask, add slowly 35.5 0.2 g of concentrated sulfuric acid (H2S04, sp gr 1.84) with cooling as above. When cool, add the contents of the second flask to the contents of the fust flask, with further cooling. To the third flask, add the contents ofa 1-oz (28.4-g) bottle (or ampule) of bromine. Add the bromine solution to the mixture of the first two solutions. Transfer to a 1-L volumetric flask with the aid of glacial acetic acid, and make up to 1 L with glacial acetic acid. Mix thoroughly and transfer to a 4-L, amber, glass-stoppered bottle. Add an additional 2.5 L of glacial acetic acid, making a total of 3.5 L of reagent. In this way, the weighing or measuring of bromine is eliminated. The reagent is approximately 0.1 N with respect to bromine. Fresh reagent should be prepared if the bromine concentra tion drops below 0.99 N. The normality of the reagent can be checked by running a reagent blank titration as described in 8.4, but eliminating the 1-h standing time. No t e 4--The stock bottle containing the Rosenmund-Kuhnhenn reagent should be kept stoppered when it is not in use to minimize loss of bromine. 6.7 Sodium Thiosulfate, Standard Solution (0.1 N) (Warning-See 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7)--Dissolve 24.8 g of sodium thiosulfate (Na2S203 5H20) in water and dilute to 1 L. Add 0.5 g of sodium carbonate (Na2C03) and a few drops of chloroform, as a preservative. Standardize against potassium iodate (KI03) primary standard as follows: Weigh, to the nearest 0.1 mg, into a 250-mL Erlenmeyer flask about 0.12 to 0.17 g of the KI03 and dissolve in 50 mL ofwater. Add 2 g of KI, and as soon as this is dissolved, 1 mL ofconcentrated hydrochloric acid (HC1, sp gr 1.19) diluted to 10 mL. Titrate the liberated iodine immediately with the Na2S203 solution, using starch indicator near the end point. Calculate the normality of the Na2S203 solution as follows: Normality == W7(0.03567 x V) where: W = KI03 used, g, and 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." V = Na2S203 solution required for titration of the KJO mL. ' No t e 5--The Na^C^ may be standardized against potassium dichrqmate (K3Cr207), if desired, as described in Test Method D 1959 6.8 Starch Indicator Solution--Make a paste with 10 g of 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 as a; preservative. Iflong storage is reqture$,,'keep the solution ina< refrigerator at 40 to 50F (4 to l0C). Prepare fresh indicator : when the end point of the titration, from blue to colorless fails to be sharp. 7. Hazards 7.1 Carbon Tetrachloride is a very hazardous liquid. It is absorbed by. the skin. Its vapor is hazardous through inhala tion. It is an irritant to skin and eyes; avoid breathing5 (TLV-10 ppm). It causes liver and kidney damage and has; cumulative effects. Use with adequate ventilation (in a hood) and wear rubber gloves. See supplier's Material Safety Data Sheet. 7.2 Mercuric Acetate--Mercuric acetate and other organic:, mercury compounds are poisonous by oral ingestion and can. be absorbed by the skin. Overheating results in decompose= tion. Mercuric acetate and its solutions should not be flushed down a drain but disposed of as hazardous wastes. See supplier's Material Safety Data Sheet. 7.3 Acetic Acid, Glacial, is corrosive and may cause burns to the skin and eyes. See supplier's Material Safety Data Sheet 7.4 Pyridine is a flammable liquid and hazardous by : inhalation. It is an eye, skin and respiratory irritant (TLV-5 ppm). May cause liver and kidney damage. Use with adequate ventilation; perform all operations in a hood. See supplier's Material Safety Data Sheet. 7.5 Sulfuric Acid is corrosive' to skin, eyes, and mucous1' membranes in form of liquid, mist or fumes. It causes severe' i bum. Take care to prevent the contact of the acid with eyes, skin, or on clothing. In making dilute solutions, always add I the acid to water with care. See supplier's Material Safety Data Sheet. 7.6 Bromine is a powerful oxidizer and may cause fire on contact with organic matter. Liquid and vapor may cause severe burns. The gas is toxic (TLV-0.1 ppm) and, as such, is a serious respiratory irritant. Use with adequate ventilation (in a hood); avoid contact with skin and eyes. Handle bromine with rubber gloves. See supplier's Material Safety Data Sheet. 7.7 Chloroform is a hazardous liquid that can be absorbed through the skin. Its vapor is hazardous through inhalation. It is a narcotic. Use only with adequate ventilation (in a hood). It is also extremely flammable. See supplier's Material Safety Data Sheet. 8. Procedure 8.1 To a 250-mL glass-stoppered iodine flask (Note 2), add 5 mL of CC14. In this dissolve the specimen, weighed to 0.1 mg, using the weight of specimen prescribed in Table 1. No t e 6--The specimen weight is so chosen as to result in a 200 to 250 % excess of reagent of the amount absorbed. After running the analysis, use the following calculation to determine whether the proper 210 DUP050295876 D 1541 1 Iodine Value in Relation to Weight of Specimen iodine file Weight of Specimen, g 200 % Excess 250 56 Excess ftOO `25 ISO .'175 0 25 50 75 300 0.212 0.169 0.141 0,121 0.106 0,094 0.085 0.073 0.071 0.182 0.145 0.121 0.104 0.091 0.081 0.073 0.066 0.061 V size has been used: E, % = [K,/(B - V )] X 100 ||xcess reagent, ,,bia,S203 solution required for titration of the specimen, mL, ,.ana |.Na2S203 solution required for titration of the blank, mLv >reagent excess falls outside these limits, the analysis must be fctl using the proper specimen size. sMake sure that the specimen is completely dissolved, len in a darkened room oflight intensity preferably less 0.5 footcandle (5.4 lx), as measured with a light meter, a darkroom under red safelight illumination, pipet into sk 10.0 mL of the Hg(C2H302)2 solution. Swirl the two or three times, add 50:0 mL of the Rosenmundnhenn recent, and note the time. Stopper the flask, add I amount of KI solution to the well of the flask to seal `irl until the contents are well mixed (2 or 3 s), and place flask in a dark place at a temperature of 23 to 27C. ,3 Exactly 1 h after the addition of the Rosenmundnhenn reagent to the specimen, bring the flask out into darkened laboratory (or darkroom under red safelight), 20.0 mL of KI solution by pipet, swirl two or three $, add 20 mL ofwater, swirl again, stopper the flask, and i.it to stand for 1 min. Them, using normal illumination, e the stopper and neck of the flask with about 10 mL of .ter. |8.4 Titrate the released iodine with Na2S203 solution by adding rapidly from the 50-mL buret, with continuous agitation, about 25 to 30 mL (all but 5 to 10 mL) of the required Na2S203 solution. Then, if low-actinic flasks are being used, transfer the contents.to a colorless flask, rinsing three times with a total of about 30 mL of water, and complete the titration in the usual manner using starch indicator when near the end point. If clear flasks are used, there is no need to transfer. Simply add 30 mL of water and complete the titration as described, using starch indicator solution when near the end point. 8.5 With each group of samples, conduct at least two blank determinations following the same procedure as de scribed in 8.1 through 8.4, except that no sample is added. In the titration, run into the flask about 40 to 45 mL of Na2S203 solution before completing the titration as de scribed. 9. Calculation and Report 9.1 Calculate the total iodine value, T, as follows: r=[(j5- V)xNx 12.691/5 where: B = Na2S203 solution required for titration of the blank, mL, V = Na2S203 solution required for titration of the spec imen, mL, N = normality of the Na2S203 solution, and S - specimen used, g. 9.2 Report the total iodine value to the first decimal place. 10. Precision and Bias 10.1 Repeatability--Two results obtained by the same operator should be considered suspect, at the 95 % confi dence level, if they differ by more than 3.6 in iodine level (3.6 % absolute). 10.2 Reproducibility--Two results, each the mean of two determinations, obtained by operators in different laborato ries should be considered suspect, at the 95 % confidence level, if they differ by more than 6.1 in iodine value (6.1 % absolute). 10.3 Bias--Bias has not been determined. 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 Ibis 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 if not revised, either reapproved or withdrawn. Your comments are invited either tor revision ofthis standard ortor additional standards and should be addressed to ASTM Headquarters. Your comments Witt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you tee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 211 DUP050295877 Designation: D 1544 - 80 (Reapproved 1989)61 Standard Test Method for Color of Transparent Liquids (Gardner Color Scale)1 This standard is issued under the fixed designation 1*1544;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 (s) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4248 ofFederal Test Method StandardNo. 141. Consult the DoD.Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. " No t e--Editorial changes were made ftirougbout in April 1989. 1. Scope 1.1 This test method covers the measurement of the color of transparent liquids by means, of comparison, with arbi trarily numbered glass standards. It applies to drying oils, varnishes, fatty acids, polymerized fatty acids, and resin solutions. Its application to other materials has not been tested;' 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport 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:. D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method12 E 308 Method for Computing the Colors of Objects by Using the CIE System3 3. Apparatus 3.1 Glass Standards, 18, numbered separately, and having the color characteristics given in Table 1. A suitable proce dure for their calibration is contained in Appendix Al. The color shall be produced by the glass components only. 3.2 Glass Tubes, clear, 10.65 mm in inside diameter and about 114 mm in outside length. (Viscosity tubes, as described in Test Method D 1545, are satisfactory.) 3.3 Suitable apparatus for comparing sample and standard. The apparatus may be of any design, but should have the following characteristics: 3.3.1 Illumination--CIE Illuminant C. 3.3.2 Surrounding Field--The field should not differ significantly in brightness from the samples and standards and should be essentially achromatic. 3.3.3 Field of View--The specimen and one or more TABLE 1 Color Specifications of Reference Standards Gardner Color Standard Number Chromalicaty Coordinates'1 X v ' Luminous Transmittance Transmittance Tolerance, Y,% . } 1 0.3177 0.3303 2 0.3233 0.3352 '3 > 0.3329 .0.3452 4 0.3437 0.3644 5 ,0.3558, 0.3840 6` 0.3767 0:4061 7` 0.4044 0.4352 8 . . 0.4207 , 0.4498 . 9 0.4343 . 0.4640 10. 0.4503. 0.4760 11 ' 0.4842 0.4818 12 0.5077 0.4638. .. , 13 0.5392 . 0.4458 14 0.5646 0.4270 15 0.5857 ` 0.4089 16 0.6047 0.3921 17 0.6290, 0.3701 .18 0.8477 0.3521 80 79 76 75 74 71 67 64- 61 57 45 36 30 22 ' 16 11 6 4 7 is 7 6 It 5, 4 r 'M 4 4 ff .4 4 4 4- s5 6. 14 6 2 1 1 1 f| A A duplicate, standard shal have chromaticlty coordinates that differ from the reference standard by no more than one third of the difference in x or y between adjacent reference standards. In any one set, no two standards shall be closer together than two thirds of the difference In x or y between corresponding reference standards. - -> standards should subtend a visual angle of about 2 deg and be in the field of view simultaneously. 3.3.4 Separation of Standard and Specimen--There .. should be a perceptible separation between specimen and ' standard, but this should be as small as is mechanically possible. 4.Procedure 4.1 Fill a glass tube with the material under test. If the material is perceptibly cloudy, first filter it. 4.2 Compare with glass standards, determining which standard most closely matches the specimen in brightness and saturation. Ignore hue differences. 1 This method is under the jurisdiction ofCommittee D-l on Paint and Related Coatings and is the direct responsibility of Subcommittee DO 1.26 on Optical Properties. Current edition approved March 10, 1980. Published May 1980. Originally published as D 1544 - 58 T. Last previous edition D 1544 - 68 (1974). 2 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 3 Annual Book ofASTM Standards, Vot 14.02. 5. Report * 5.1 Report the color as the number of the standard most closely matching the specimen. If more precise measure ments are needed, report as either matching a standard or lighter or darker. Thus, between colors 5 and 6, the steps will be 5, 5+, 6--, and 6. 212 D UP 050295878 # D 1544 sion and Bias On the basis of a study in which one observer at each laboratories; made duplicate determinations on four :s, the "between?5 and "within" standard deviations 'bund to be 0.5 and 0.1 color number, respectively. ' on these standard deviations, the following criteria [ be used for judging the acceptability of results at the confidence level. f Repeatability--Two results obtained by a single operould be considered suspect ifthey differ by more than birds of a color number. ' Reproducibility--Two results, each of the mean of Jhte measurements, made by operators in different ~ries should be considered suspect if they differ by more than four thirds of a color number. No t e 1--If desired, liquid standards matching the colors given in Table 1, in glass tubes similar'to the sample tubes may be used. These may be filled with potassium chloroplatinate for the light colors and solutions of ferric chloride and cobalt chloride in hydrochloric acid for the darker colors. The specifications and approximate composition of these solutions are given in Test Method D 1544 ,- 5&T.4 2M1a3ny Glass Standards in current use do not conform to the values of Table t. No t e 2--The precision data were obtained using an instrument in which two standards are viewed simultaneously. There are other instruments available for color matching which would be expected to give similar results, but the statement above applies only to the instrument checked. 4 See 1961 Book o/ASTMStandards, Part 8. t*i-: APPENDIX (Nonmandatory Information) XI. CALIBRATION OF GLASS REFERENCE STANDARDS LI Select a dual beam spectrophotometer with a suffiy small light beam at the sample position so (hat all will pass through the standards to be calibrated. Alter- yely equip the spectrophotometer with a condensing lens jmplish this purpose. 1,2 Place the standards in turn in the sample position of spectrophotometer. If the comparator is provided with a *te 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. X1.3 Obtain spectral transmittance data for each glass reference standard by following Method E 308. XL4 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 Illuminant C (see Method E 308). : 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 standardis subject (6 revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Yeur comments are invited either for revision of this standard or for additionalstandards andshould 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. 213 DUP05 0295879 #' D t54 1 Recommended Numerical Standards for Comparator Viscosity Tubes4 Tube0 ,e| Number Stokes GardnerHoldt Letter Tube0 Number Stokes GardnerHoldt Letter 0.10- 0.13-A3 Q.16- 10-13-16-- 10 -W is- X ie- 0.22- 1- - 0.34,90- 0.50- ioo-- 0.68- 0.20-A2! 0.250.32- -At 0.400.50- -A 0.63- 0.80- 20-- 25-32- 40 50-)03- 80-- 20- -Z 25- Z1 32- -Z2 40- Z3 5063- Z4 80- [45-- - 0.92- 1.15- ;55-|- 145- 1.85- >.20-- 1.802.15- ,65- 2.65- <3.20- - 3.20- 4.00- 4.00- 1.00--D 1.25- E l-F 1.60' G 2.00- H I 2.50- J K -L 3.20- -M -N -O 4.00- 100125- 1604- -Z5 100 125- Z6 160- 200-- 200- 250-- 250- 320-- 320- -Z7 400- 400- 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. No t e 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. 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." No t e 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 STP 500, Section 3.2.9.3 6. Precision and Bias 6.1 On the basis of an interlaboratory study4 of this test method in which ten laboratories tested liquids ranging in viscosity from 4.5 to 440 St, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 6.1.1 Two results obtained by the same operator should be considered suspect if they differ by more than 4.9 % relative. 6.1.2 Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 9.0 % relative. 5.00- 5.004- 5.00- 500- - 500- 6.30-4 8.00 6.30-8.00- - 6.308.00- 630- 800- - Z8 630800- Z9 10.0-- 10.0- - 10.0- 1000- 1000 Z10 A Arranged to show relationship between stokes, bubble seconds, and :Gardner-Holdt tetters. Stokes are shown in logarithmic progression. 8 The bubble tine, in seconds, ol the numerical tubes under 4 s was determined by a technique employing a movie camera. For reference purposes only. Numbered tubes are no longer commercially available. 0 Above 2.65 the bubble seconds as measured by the kinematic method are approximately equivalent lor most products. Below 2.65 this relationship does not hold. . 1 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. 215 DUP050295880 # 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 pf this standard am expressly advised that determination of the validity of any such patent rights, and the flak of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any tine by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments am invitedeitherfor 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.. ; 216 DUP050295881 Designation: D 1585 - 82 Standard Test Methods for r..t,rr Fatty Acids Content of Tall Oil Rosin1 This standard is issued under the fixed designation D 1585; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. These methods cover the determination of residual eids in tall oil rosin, as defined in Definitions D 804. ferenced Documents | ASTM Standards: 5 Test Methods for Acid Number of Rosin? Definitions of Terms Relating to Naval Stores and elated Products2 193 Specification for Reagent Water3 i Test Method for pH of Aqueous Solutions with the lass Electrode4 i.> unary of Methods The fatty acids are calculated from the acid number ' e rosin acids content. The acid number is determined by either the potenetric or the indicator method described in Methods 5. The rosin acids content is determined using either the sed potentiometric Wolff method or the modified ~tor Wolff method, described in Sections 6 to 17-. > The same method for end point detection, either intiometric or indicator, should be used for both acid ber and rosin adds content determination* in order to d slight variations that might occur. :;5 Since the fatty acids remaining in tall oil rosin consist Meic add with varying amounts-of other, saturated and ^titrated adds, it has become customary to calculate and Jrt the fatty add content as oleic acid. " '' Purity of Reagents ' .1 Reagent grade chemicals shall be used in all tests, less otherwise indicated, it is intended that all reagents conform to the specifications of the'Committee on jalytical Reagents of the American Chemical Society, `"ere such spedfications are available.5 Other grades may be ed, provided it is first ascertained that the reagent is of 1 These methods are under the jurisdiction of ASTM Committee D-l on Paint i Related Coatings and Materials and are the direct responsibility of Subcom- ittee D01.34 on Naval Stores. Current edition approved March 26, 1982. Published June 1982. Originally Wished as D 1585 - 58 T. Last previous edition D 1585 - 63 (1981). * Animal Book ofASTM Standards, Vo! 06,03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. s "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. ;., Washington, D.C. For suggestions on the testing of reagents not listed by the ~erican. Chemical Society, see "Reagent Chemicals and Standards," by Joseph :=n, Di Van Nostiand Co., Inc., New York, N.Y., and the "United States armacopeia." sufficiently high purity to permit its use withoutlessening the accuracy of the determination. 4.2 Unfess otherwise indicated, references to water shall be understood to mean reagent water conforming to the Specification D 1193. 5. Preparation of Sample 5.1 Prepare the sample for analysis by chipping small pieces from a freshly exposed surface of a lump of lumps and crush to g coarse powder to facilitate weighing and solution. Prepare fresh qn the same day, prior to weighing, in order to avoid changes due to surface oxidation of crushed rosin on exposure to the air. ROSIN ACIDS CONTENT BY THE MODIFIED WOLFF-POTEN- TIOMETRIC METHOD . (Referee Method) 6. Scope 6.1 This method covers the determination of rosiri acids content of tall oil rosin where the most reproducible results are desired. By using the potentiometric inflection end points, the error due to colorimetric end points is avoided. 7. Summary-of Method 7.1 A sample is refluxed with methyl sulfuric add to esterify the fatty acids. The rosin acids and sulfuric acid are then titrated pptentiometrically, and the rosin acids content calculated from the difference between the two inflection points obtained. ' 8. Apparatus '' 8.1 pH Meter6--Ah indicating potentiometer having ai limit of eiror not greater than 0.1 pH over a range of pH 1 to pH 13, using an alkali-resistant glass electrode and a saturated calomel half-cell. The pH meter shall confoun to the requirements of Method E 70. Alternatively, an auto matic potentiometric titrator may be used. 8.2 Stirrer, mechanical, equipped with a glass propellertype paddle. 8.3 Buret, 50-mL capacity; with 0.1-mL divisions. The so-called automatic buret is preferable as its use minimizes errors due to evaporation. The automatic buret should be guarded with soda-lime tubes against the absorption of C02 from the air. 6 pH '-meters that have been found suitable for potentiometric titrations include the Beckman or Macbeth pH meter equipped with Beckman electrodes Nos. 1170 and 1190E; Leeds & Northrup No. 7661-A1 assembly with Std. 1199-30 high alkali-resistant glass electrode; Fischer titrimeter. Senior Model, with electrode No. 9-312-27; or equivalent pH meters. 217 DUP050295882 # D 1585 ';\4 8.4 Erlenmeyer Flask, 250-mL of a chemically-resistant glass with a standard-taper 24/40 joint. 8.5 Condenser, water-cooled, equipped with a joint fitting the flask described in 8.4. 9. Reagents 9.1 Alcoholic Alkali, Standard Solution (0.5 N)--Dissolve 33 g of potassium hydroxide (KOH), preferably in pellet form, in methanol (CH3OH) and dilute to 1 L with the alcohoL Standardize to 0.001 N with potassium acid phthalate (C6H4 COOKCOOH) in 100 mL of methanol plus sufficient water for a clear solution; 2.553 g of potassium acid phthalate will be neutralized by 25.00 mt of 0.5 N KOH solution. Protect the standardized solution against evaporation and absorption of carbon dioxide (C02) from the air. Restandardize the solution frequently, either electrometrically, or colorimetrically using phenolphthalein as the indicator. 9.2 Toluene. 9.3 Ethanol (95 %)--Denatured alcohol conforming to Formula No. 3A or No. 30 of the U.S. Bureau of Internal Revenue, neutralized by the addition of KOH. 9.4 Methanol (99.5 %). 9.5 Methyl Sulfuric Acid Solution--Slowly pour 100 g of concentrated sulfuric acid (H2S04, sp gr 1.82 to 1.84), while stirring constantly, into 400 g of methanol. Store in a glass-stoppered bottle. 10. Procedure 10.1 Dissolve 3.95 to 4.05 g of the sample, weighed to the nearest 0.001 g, in 25 mL of benzene in a 250-mL flask. Add 100 mL of methanol and 5 mL of methyl sulfuric add and connect the flask to the condenser. Heat the flask assembly and reflux for 2 min. Cool and transfer to a 400 mL beaker, using a total of 100. mL. of methanol (Note 1) in three successive rinsings. No t e I--Ethanoi is preferable when an automatic titrator is used. 10.2 Turn the pH meter on and allow a few minutes for it to come to equilibrium. Balance the meter using a standard buffer solution as described in Method E 70; then rinse the electrodes thoroughly with water and then with alcohol. 10.3 Adjust the beaker containing the solution of the sample so that the buret tip is close to the surface of the solution.. Adjust the electrodes so the lower half of each is immersed. Start the stirrer slowly;.then adjust its speed for vigorous stirring without spattering. Record the initial pH if it is on the scale. Add suitable small portions of the KOH solution, and, waiting after each addition until an un changing potential has been established, record the pH and buret readings. Add 5-mL portions of KOH solution until a pH of 1.0 to 1.5 is reached; then add 1-mL portions until the change in pH per portion added exceeds 0.3 pH unit. Continue to add the KOH solution in 0.1-mL . or smaller portions until the first end point has been passed, as indicated by a significant decrease in pH change per unit volume added. Thereafter, add 1 to 2-mL portions until the pH change per portion added again exceeds 0.3 pH unit. Again add 0.1-mL or smaller portions until the second end point has been passed as indicated by significant decrease in pH change per unit volume of KOH solution added. After Jthe pH change is less than 0.1 pH unit per 0.1 mL of KOH solution added, the increments may be increased to 1.0 mL End the titration at pH 12 or above. if 10.4 Determine the inflection points (points of maximum I change in pH per 0.1 mL of 0.5 N KOH solution) to the I nearest 0.1 mL. They may be found by inspection ofa plot of I pH against millilitres of KOH solution added, or by plotting | the change in pH per millilitre of KOH solution against the I pH reading. The inflection points shall be taken as the end <| points of the titration. Alternatively, if an automatic titrator 1 is used the end points shall be taken at pH 4.0 and pH 10.8. ' 11. Calculation and Report , 11.1 Calculate the percentage of rosin acids as follows: Rosin acids, % = (AN/B) x 30.24 where: A = millilitres of KOH solution required for titration between the first and second end points, N = normality of the KOH solution, B = grams Of sample used, and `i 30.24 = (mol wt of abietic acid X 100)/1000 i 11.2 Report the percentage of rosin acids to the first decimal place. |i ROSIN ACIDS CONTENT BY THE MODIFIED WOLFF-INDICATOR METHOD (Alternative Method). i 12. Scope 12.1 This method covers the determination of rosin acids content of tall oil rosin using an internal indicator for the f determination of the end point. It gives good results when j routinely applied by a skilled analyst. However, where most ; reproducible results by different analysts and laboratories are ; desired, the referee method (Sections 6 to 11) should be used. 13. Summary of Method 13.1 A sample is refluxed with methyl sulfuric acid to | esterify the fatty acids. The rosin acids and sulfuric acid are ' then titrated in the presence of thymol blue indicator. The rosin acids content is then calculated from the difference between the two color end points obtained. 14. Apparatus 14.1 The apparatus for the esterification and titration of the sample shall consist of the flask,, condenser, and buret described in Section 8. 15. Reagents 15.1 Alcoholic Alkali, Standard Solution--See 9.1. 15.2 Toluene. 15.3 Methanol--See Section 9.4. 15.4 Methyl Sulfuric Acid Solution--See 9.5. 15.5 Thymol Blue Indicator Solution (1 g/L)--Dissolve 0.1 g of thymol blue in 100 mL of methanol. 16. Procedure 16.1 Dissolve 3.95 to 4.05 g of the sample, weighed to the nearest 0.001 g, in 25 mL of benzene in a 250-mL flask. Add 100 mL of methanol and 5 mL of methyl sulfuric acid and 218 DUP050295883 flask to the condenser. Heat the flask assembly for 2 min. Cool and add 1 mL of thymol blue itrate with the KOH solution to the first end point, . 4.0, when the solution changes color front-red to ecord the reading or refill the buret. Continue the to the second end point, about pH 10.8, when the changes color from yellow to blue. Record to the i.l mL the millilitres of KOH solution required for between the two end points. -These end points approximate the inflection points under tieous Conditions employed. cutation and Report Calculate the percentage of rosin acids as described dull. Report the percentage of rosin acids to the first place. ACID NUMBER 18. Procedure 18.1 Determine the acid number by either the potentio- metric.ar the indicator modification described in Methods D465. FATTY ACIDS 19. Calculation and Report 19.1 Calculate the percentage of fatty acids from the acid number and the percentage of rosin acids as follows: Fatty acids as oleic acid, % = [A -- (R X 1.855)]/1.986 where: A - acid number of original sample, R = percentage of rosin acids, 1.855 =* (56.1 x 1000)/(302.4 x 100) = factor to convert the percentage of rosin acids to acid number, and 1.986 -- (56.1 x 1000)/{282.4 x 100) = factor to convert acid number to percentage of oleic acid. 19.2 Report the percentage of fatty acids to: one decimal place. The American Society f6r Testing arid Materials takes no position respecting trie validity ofany patent rights assertedin connection with any item mentioned lit this standard. Users of this standard are expressly advised that determination of the validity at any such patent rights, endthe risk of Infringement ofsuch 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, eitherreapproved or withdrawn. Your comments are Invited eitherlor revision ofthis standard or for additional standards and Should be addressed to ASTM Headquarters. Your comments wi!) 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 Standard-1916 Race St., Philadelphia, PA '19103. 219 DUP050295884 Designation: D 1612 -90 Standard Test Method for Acetone in Methanol (Methyl Alcohol)1 1. Scope This standard is issued under the fixed designation D 1612; 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. : ' . t , , - where such specifications are available. Other grades may be 1.1 This test method covers a procedure for detecting the presence of acetone in methanol (methyl alcohol) in amounts greater than 0.003 weight %.. 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. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 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. 'J 6.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type IV * of Specification D 1193. It is essential that the reagent water be free of ammonia. * '> 6.3 Acetone Standard--Pipet 6.0 mL of acetone^ into a; 1-L volumetric flask and dilute with water to the 1-L mark. ' Take 1.0 mL of the resulting solution and make up to LL,. with water in a volumetric flask. Five millilitres of this 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water12 ., solution contain Q.024 mg of acetone. Under conditions " outlined for this test method, the- standard made up for j comparison is equivalent to a methanol specimen containing 0.003 weight % of acetone. 1 3. Summary of Test Method 3.1 The specimen is reacted with Nessler's reagfent and the turbidity that is produced is compared to a standard con taining the equivalent of 0.003 weight % of acetone. 6.4 Nessler's Reagent: " . 6.4.1 Solution A--Dissolve 270 g of sodium hydroxide . (NaOH) pellets in water and dilute to 1 L. | 6.4.2 Solution B--Dissolve 36 g of potassium iodide (KI) > crystals and 13.6 g of mercuric chloride (HgCl2) powder in 4. Significance and Use 4.1 This test method can be used to detect residual amounts of carbonyl compounds in synthetic and natural methanol. The carbonyl compounds are quantified by com water and dilute to 500 mL. To prepare the Nessler's reagent, f mix three parts of Solution A with 5 parts of Solution B and ? allow to stand until clear before,using. ; 7. Procedure * parison to a known standard of acetone solution. 7.1 Carefully pipet 1 mL of the sample and 4 mL of water ; 4.2 Carbonyl compounds may be present as a result of contamination during storage, distribution, or manufacture. This test method may be used in assessing compliance with a into one of the matched test tubes and mix thoroughly. J Carefully pipet 5 mL of the acetone standard into a second matched test tube. Pipet 5 mL of the Nessler's reagent into : specification. each of the tubes containing the specimen and the acetone - 5. Apparatus standard. Quickly mix the contents of each tube and allow , both to stand for 5 min. At the end of the 5-min standing ; 5.1 Volumetric Pipets, 1, 4, and 5-mL capacity. period, compare the turbidity of the specimen to the 5.2 Test Tubes, matched for color, 1.5 by 15 cm. turbidity of the acetone standard. 6. 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, 8. Report 8.1 If the turbidity of the specimen is less than that of the acetone standard, report the acetone content is "less than 0.003 weight %." If the turbidity of the specimen is greater than that of the acetone standard, report the acetone content as "greater than 0.003 weight 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1612- 58 T. Last previous edition D 1612-36. 2 Annual Book cfASTM 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." 220 DUP050295885 D 1612 ecision and Bias 1 Precision--Because of the "pass-fail" nature of this lure, there is no precision statement. Bias--Any material or ;contpninant that will react fessler's reagent will affect the results. . 1 The results are reported "less than" or "greater than" as acetone. Since various ketones or other carbonyl com pounds may be present, the actual level of acetone may be different. 10. Keywords 10.1 methanol; acetone content 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 standardIs subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited eitherforrevision of this 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. 221 DUP050295886 Designation: D 1613 - 91 Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products1 This standard is issued under the fixed designation D 1613; 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 method has been approvedfor use by agencies of the Department of Defense to replace Method 5252 of Federal Test Method Standard No. MIA. . Consult theDoD Index ofSpecifications and Standardsfor the specific fear ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the determination of total acidity as acetic acid, in concentrations below 0.05 %, in organic compounds and hydrocarbon mixtures used in paint, varnish, and lacquer solvents and diluents. It is known to be applicable to such mixtures as low molecular weight saturated and unsaturated alcohols, ketones, ethers, esters, hydrocarbon diluents, naphtha, and other light distillate petroleum fractions. 1.2 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.3 For specific hazard information and guidance consult supplier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D 770 Specification for Isopropyl Alcohol2 D 1193 Specification for Reagent Water3 E 200 Practice for Preparation, Standardization, and Storage of Standard Solutions for Chemical Analysis4 3. Summary of Test Method 3.1 The specimen is mixed with either an equal volume of water or an equal volume of alcohol, and titrated with aqueous sodium hydroxide solution to the phenolphthalein end point. 4. Significance and Use 4.1 This test method is useful for determining low levels of acidity, below 0.05 %, in organic compounds and hydro carbon mixtures. The total acidity is calculated as acetic acid or milligrams of sodium hydroxide per gram of sample. 4.2 Acidity may be present as a result of contamination, decomposition during storage or distribution, or manufac 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May IS, 1991. Published July 1991. Originally published as D 1613 - 64 T. Last previous edition D 1613 - 85. 2 Annual Book ofASTM Standards, Vo! 06.03. Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. ture. This test method may be used in assessing compliance with a specification. 5. Apparatus 5.1 Buret, 10-mL, graduated in 0.05-mL subdivisions. 5.2 Erlenmeyer Flask, 250-mL capacity. 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.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 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 7. Reagents 7.1 Alcohols, refined, ethyl or isopropyl. No t e 1--Isopropyl alcohol (99 % grade) conforming to Specification D 770, or 190 proof ethyl alcohol conforming to formula No. 3A ofthe U.S. Bureau of Internal Revenue is suitable for use as the solvent. The use of methyl alcohol is not recommended. 7.2 Phenolphthalein Indicator Solution, (10 g/L)--Dis solve 1 g ofphenolphthalein in ethyl or isopropyl alcohol (see Note 1) and dilute to 100 mL with the alcohol. 7.3 Sodium Hydroxide, Standard Solution (0.05 N)-- Prepare and standardize a 0.05 AT sodium hydroxide (NaOH) solution (Note 2) in accordance with Sections 12 to 17 of Practice E 200. No t e 2--Alternatively, KOH solution may be used. 8. Procedure 8.1 Measure into a 250-mL Erlenmeyer flask 50 mL of water, if the sample is completely water-soluble, or 50 mL of alcohol, if the sample is not completely, water-soluble. ' 8.2 Add 0.5 mL of phenolphthalein indicator solution. 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." 222 DUP0502 95887 tie water or alcohol with 0.05 N NaOH solution to perceptible pink color. let 50 mL of the sample into the flask. Titrate with jyV NaOH solution to the same first perceptible pink ` [tally obtained. ations culate the acidity of the sample as follows: as acetic acid, weight % - (VN x 0A2)/D M: ;:dity as mg KOH per g of sample - (VNx 1.12)/D NaOH solution required for titration of the sample, , ^ mL, , I tiomality of the NaOH solution, and ;sp gr of die specimen at die test temperature. "port Report the percent of acetic acid to the nearest 'o. Duplicate runs that agree within 0.0005 %, abso- fe acceptable'for averaging (95 % confidence level). Islon and Bias Precision porting data are available from ASTM Headquarters. Request RR: I. 11.1.1 The following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 11.1.1.1 Repeatability--The normal range between two results, each the mean of duplicate determinations, obtained by the same analyst on different days, is estimated to be 0.0003 %, absolute. Two such values should be considered suspect if they differ by more than 0.0008 %, absolute. 11.1.1.2 Reproducibility--The normal range between two results, each the mean of duplicate determinations obtained by analysts in different laboratories, is estimated to be 0.0005 %, absolute. Two such values should be considered suspect if they differ by more than 0.0014 %, absolute. No t e 3--The above precision estimates are based on an inter laboratory study on two samples each of n-butyl acetate, n-butyl alcohol, and methyl ethyl ketone containing 0.0058, 0.0112, 0.0007, 0.0046, 0.0026, and 0.0067 % acetic acid, respectively. Each of four laboratories analyzed all six samples, with two analysts in each laboratory per forming duplicate deteniiinations using both 99 % isopropyl alcohol and formula 3A ethanol as solvents; and repeating on a second day, for a total of 384 determinations. 11.2 Bias: 11.2.1 Any material or contaminant that will react with NaOH under the test conditions will affect the results. 11.2.1.1 Various acidi or other acidic materials may be present. Common practice, including the method used here, calculates these as acetic acid. The actual weight percent of acidic materials may be different. 12. Keywords 12.1 solvents, acidity; total acidity as acetic acid TheAmerican Society tor Testing and Materials takes no position respecting the validity otany patent rights asserted in connection with any item mentioned In this standard. Users di this standard are expressly advised that determination ot the validity ot any such patent rights, and the risk of infringement of such rights, 'are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you 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. 223 DUP050295888 h |||M Designation: D 1614-91 Standard Test Method for Alkalinity in Acetone1 This standard is issued under the fixed designation D 1614; 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. This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which, has been adopted by the Department ofDefense 1. Scope 1.1 This test method covers the determination in acetone of alkalinity calculated as ammonia (NH3). 1.2 This standard does not purport to address the safety problems, if anyj. associated with its use. It is the responsi bility of whoever uses this standard to -considt and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 1.3 For specific hazard information and guidance; con sult the supplier's-Material Safety Data Sheet., 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 E 200 Practice for Preparationy Standardization, and Stor age of Standard Solutions for Chemical Analysis3 3. Summary of Test Method 3.1 The specimen is added to water previously neutralized to the methyl red end point. If alkalinity is detected, it is titrated with 0.05 N H2S04 and reported as weight percent of NHj. ' - .4 Significance and Use 4.1 This test method provides a measurement of alkalinity in acetone. The results of this measurement can be used for specification acceptance. 5. Apparatus 5.1 Buret, 10-mL, graduated in 0.05-mL subdivisions. 5.2 Erlenmeyer Flask, 250-mL capacity. 6. Reagents and Materials 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-! on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 15, 1991. Published July 1991. Originally published as D 1614-58. Last previous edition D 1614- 87. 2 Annua/ Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 15.05. 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 wilhoui 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 IV of Specification D 1193. 6.3 Methyl Red Indicator Solution (1 g/L).--Dissolve 0.2 g of methyl red in 100 mL of methanol, ethanol, un isopropanol. Prepare a fresh solution at least once a month ` as needed. 6.4 Sodium Hydroxide, Standard Solution (0.05 N)-- Prepare and standardize a 0.05 N sodium hydroxide (NaOH) solution (Note) in accordance with Sections 12 to 17 of Practice E 200. No t e--Alternatively, potassium hydroxide (KOH) solution maj be used. 6.5 Sulfuric Acid, Standard Solution (0.05 N)--Prepare and standardize a 0.05 TV sulfuric, acid (H2?Q4) solution. 7. Hazards 7.1 Acetone is a highly flammable liquid. 7.2 The reagents, sulfuric acid and sodium hydroxide are hazardous as they can cause severe bums of the skin or e; es 8. Procedure 8.1 To a 250-mL Erlenmeyer flask, add 50 mL of water and 3 drops of methyl red indicator solution. If the water is basic, neutralize to the first faint pink coloration with 0.05 N H2S04. If acidic, neutralize to the first yellow coloration with 0.05 N NaOH solution and then to the first faint pink coloration with 0.05 N H2S04 solution. Now add 50 mL of sample to the neutralized water. If there is no change in the color of the solution, the sample may be considered free of alkalinity. If, however, the solution turns yellow, titrate it with 0.05 N H2S04 to the first pink coloration. 9. Calculation 9.1 When it is necessary to titrate the solution with the 0.05 VH2S04 calculate the percent of alkalinity as ammonia (NH3) as follows: - NH3, % = (VN x 0.034)//? 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." 224 DUP0502 95889 D 1614 lgf method in which operators in eleven laboratories analyzed R2S04 required for titration of the specimen, mL, one sample of acetone with a mean alkalinity of 0.0009 %, Rormality of the H2S04, and the within-laboratory standard deviation ,was found to be Igtpecific gravity of the specimen at the test temperature. 0.00002 % absolute with nine degrees of freedom and the between-laboratories standard deviation 0.00007 % absolute with eight degrees of freedom. Based on these standard deviations; the following criteria should be used for judging |f If the solution does not turn yellow, report alkalinity the acceptability of results at the 95 % confidence level: 11.1.1.1 Repeatability--Two results, each the mean of I jjji If the solution is alkaline,, report the percent of duplicates, obtained by the same operator on different days jfinia to the nearest 0.0001 %. Duplicate runs that agree should be considered suspect if they differ by more than jp 0.00007 % absolute are acceptable for averaging 0.0001 % absolute. pconfidence level). ' r 11.1.1.2 Reproducibility--Two results, each the mean of m;' ' . (precision and Bias5 -i duplicates,,obtained by operators! in different laboratories should be considered suspect if they differ by more than b ^Precision: |1.1 On the basis of an interlaboratory study of this test 0.0002 % absolute. 11.2 Bias--Bias has not been determined for this test method. Supporting data are available, from ASTM Headquarters.. Request RR:D01- 12. Keywords 12.1 acetone; alkalinity test; alkalinity test, acetone The American Society for Testing and Materials lakes no position respecting the validity of any patent rights assertedjo connection with any Item mentioned In this standard. Users 6/fhys 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 invitedeither for revision ofthis standard or for additional standards and should bb addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, Which you may-aUend.lf you feel that your comments have not received a-fair hearing you should make your views.known to the ASTM Committee on Standards,,1936 Race St., Philadelphia, PA 19103. 225 DUP050295890 Designation: D 1617 - 90 Standard Test Method for Ester Value of Solvents and Thinners1 This standard is issued under the fixed designation D 1617; the number immediately following the designation indicates the year of original adoption or, in the case o. revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (f) 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 die Department ofDefense. 1. Scope 1.1 This test method covers the determination ofthe ester value of solvents and thinners used in lacquers and other coatings. 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 a specific hazard statement, see Note 2. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water12 3. Summary of Test Method 3.1 The specimen is reacted with a measured excess of aqueous potassium hydroxide, using isopropanol as a mutual solvent if necessary. The amount of potassium hydroxide consumed, which is determined by titrating the excess with standard mineral acid, is a measure of the ester originally present. 3.2 Since this determination is based on an acidimetric titration, a suitable correction should be applied ifthe acidity of the sample exceeds the limit of the specification. 4. Significance and Use 4.1 This test method is useful in determining the assay of solvents and thinners which are esters or solutions ofesters of carboxylic acid. The ester value is calculated as percent ester. This test method has its greatest application where the solvent or thinner is not a pure ester. This test method may be used in assessing compliance to specification. 5. Interferences 5.1 Organic chlorides, nitriles, and amides may be hydro lyzed by the reagent, particularly at 98C, and are a possible source of error. Ketones interfere only slightly with this procedure. Aldehydes consume some , alkali, but the error introduced by small amounts is negligible. 6.. Apparatus 6.1 Pressure Bottle,3 200 to 350-mL capacity, made from heat-resistant glass. .4 6.2 Container for Pressure Bottle--A suitable safety de- : vice to. contain the pressure bottle. A metal container with i hinged top and perforated bottom, a strong synthetic fabric or canvas bag, or a safety shield may be used. 6.3 Ampoule, 1 or 2-mL capacity. - 6.4 Weighing Pipet, Lunge or similar type. ' -1 6.5 Erlenmeyer Flasks, 250-mL glass-stoppered. 6.6 Buret, 50-mL capacity. j 6.7. Boiling Water Bath. 7. Reagents j 7.1 Purity ofReagents--Reagent grade chemicals shall be % used in all tests. Unless otherwise indicated, it is intended J that all reagents shall conform to the specifications of the a Committee on Analytical Reagents of the American Chem- | ical Society, where such specifications are available.4 Other 1 grades may be used provided it is first ascertained that the .1 reagent is of sufficiently high purity to permit its use without 1 lessening the accuracy of the determination. ij 7.2 Purity of Water--Unless otherwise indicated, refer- \ ences to water shall be understood to mean reagent water j conforming to Type IV of Specification D 1193. ' 7.3 Hydrochloric Acid, Standard (0.5 N)--Prepare 0.5 N | hydrochloric acid (HC1) and standardize to four significant figures. 7.4 Isopropyl Alcohol (99 %). | 7.5 Phenolphthalein Indicator Solution--Dissolve 1 g of ` phenolphthalein in 100 mL of methanol, ethanol, or | isopropyl alcohol. I 7.6 Potassium Hydroxide, Standard Solution (1.0 : N)--Dissolve 66 g of potassium hydroxide (KOH) pellets in water and dilute to 1 L with water (see Note 1). j, III Sulfuric Acid, Standard (0.5 N)--Prepare 0.5 N sul- I furic acid (H2S04) and standardize to four significant figures. 8. Procedure 8.1 Prepare a sufficient number of 250-mL, glass-stop pered Erlenmeyer flasks to make all blank and test determi- 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published asD1617-58T. Last previous edition D 1617 - 85. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Bottles of this type, equipped with lever-type closures, can be obtained from Preiser Scientific, PO Box 1330,94 Oliver St., St, Albans, WV 25177. * "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." 226 DUP05 0295891 # D 1617 s in duplicate. Us? heat-resistant pressure bottles if glass ampoules are required or if the reaction is ucted at 98"C. Into each of the flasks or bottles, carefully introduce L of 1.0 N KOH solution (Note 1) by means of a Te transfer pipet.TJse the same pipet for each transfer.. I --Do not substitute sodium hydrcixide (NaOH) Solution. The -n conditions given fit Table 1 are valid only when 1.0 N KOH 'on is used. Add the amount' of isopropyl-alcohol prescribed in le 1 but never add more than 40 mL. Stopper and reserve of the flasks or bottles for the blank determinations. *4 Into each of the other flasks or bottles introduce an unt of sample containing not more than 0.016 mol (16 equivalents) of the ester. For substantially pure material, the specimen to the nearest 0.1 mg, using the amount procedure specified in Table 1. Stopper the flasks after ition of the specimen. 5 If a sealed glass ampoule is used, add several pieces of polished 8-mm glass rod to each bottle, stopper, and :e the bottle vigorously to break the ampoule. Reaction at 98C (Precaution--See Note 2.)--Place specimens and blanks as close together as possible in a fling water bath maintained at least at 98C for the time scribed in Table 1. Maintain sufficient water in the bath just cover the liquid in the bottles. Remove the bottles pm the bath and allow them to cool to room temperature, en the bottles have cooled, remove them from the safety ice and uncap them carefully to release any pressure, ntinue as described in 8.8. ! No t e 2: Precaution--Enclose each bottle securely in a suitable safety vice to restrain fragments of glass should the pressure bottle rupture. 8.7 Reaction at Room Temperature--Allow the specimen X stand together with the blanks at room temperature for the `ngth of time specified in Table 1. 8.8 If a white precipitate develops in the specimen flasks r bottles, add sufficient water to dissolve the salt. Add the 'ame amount of water to each of the blanks. Add 6 to 8 drops of the phenolphthalein indicator solution to each flask br bottle and titrate with 0.5 N H2S04 just to the disappear ance of the pink color. If more than 25 mL of isopropyl alcohol were added in accordance with 8.3, titrate with 0.5 N fHCl. TABLE 1 Specimen Size and Reaction Conditions Ester Specimen, gA Isopropyl Alcohol Added, mL Minimum Reaction Conditions Time, Tempera min ture, C Amyl acetate Dibutyl phthalate 2-Ethoxyethyl acetate Ethyl acetate Isobutyl acetate Isopropyl acetate Methyl amyl acetate Normal butyl acetate Normal propyl acetate sec-Butyl acetate 1.4 to 1.6 40 30 98 1.4 to 2.0 30 30 98 1.3 to 2.1 0 30 25 0.9 to 1.4s 0 30 25 1.2 to 1.9 25 45 25 1.0 to 1.6s 10 30 25 1.4 to 2.3 30 30 98 1.2 to 19 25 45 25 1.0 to 1.6s 10 30 25 1.2 to 1.9 25 45 98 A Use a suitable weighing pipet unless otherwise specified. 0 Use a sealed glass ampoule. 8.9 Measure the temperature of the acid" temperature of the reagent at the time the este^j_. tion is made is not the .same as it was at the time was standardized, apply a .temperature correu 0.00014/C to the normality. e , 9. Calculation 9.1 Calculate the percent of ester, E, as follows: = [(( - V)N x F)/S] x 100 where: V = 0.5 N H2S04 (or HC1) required for titration of the specimen (8.8); mL B = 0.5 N H2S04 (or HC1) required for titration of the blanks (8.8), avg, mL, N = normality of the H2S04 (or HC1) corrected for temper ature, F = factor specified in Table 2 for the ester being deter mined, and 5 = specimen used, g. No t e 3--If the acidity of the ester exceeds the limit of the specifica tion, it is recommended that a suitable correction be applied to the ester value. 10. Report 10.1 Report the following information: 10.1.1 All results to the nearest 0.1%. Duplicate determi nations that agree within 0.38 %, absolute, are acceptable for averaging (95 % confidence level). 11. Precision and Bias 11.1 Precision--The precision statements are based upon an interlaboratory study in which two analysts in each of four different laboratories analyzed one sample of ethyl acetate, 88 %, and one sample of dibutyl phthalate, 99 %, in duplicate on three different days. The within-laboratory coefficient of variation was found to be 0.154 % at 40 df, and the between-Iaboratory coefficient of variation was found to be 0.313 % at approximately 16 df. Based on these coeffi cients of variation, the following criteria should be used in judging the acceptability of results at the 95 % confidence level. 11.1.1 Repeatability--Two results, each the mean of du plicates, obtained by the same operator on different days should be considered suspect if they differ by more than 0.44 % relative. 11.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories TABLE 2 Ester Factors Ester Factor4 Amyl acetale Dibutyl phthalate 2-Ethoxyethyl acetate Ethyl acetate isobutyl acetate Isopropyl acetate Methyl amyl acetate Normal butyl acetate Normal propyl acetate sec-Butyl acetate 0.1302 0.1392 0.1322 0.0881 0.1162 0.1021 0.1442 0.1162 0.1021 0.1162 ' Factor = molecular weight of compound/number of reacting groups x 1000. 227 DUP050295892 # D1617 should be considered suspect if they differ by more than 0.94 % relative. 1.1.2 -Bias--Any material or contaminant (see Section 5 and Note 3) that will react with potassium hydroxide under the test conditions will affect the results. Keywords ' 12.1 ester value; solvents; thinner ` The American Society for Testing andMaterials takes no position respecting the validity of any patentrights Asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of me validity ofany such patent rights, amt the risk of Infringement of such rights, are entirely their own responsibility.' , ... This standard hi subject to revision atany time by the responsible technical committee and must be reviewed every five years and If notrevised, either reapproved or withdrawn. Your comments are invited either for revision 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 e fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 228 DUP050295893 Last ASTM Designation: D 1638 - 7461 An American National Standard Standard Methods of Testing Urethane Foarn Isocyanate Raw Materials ese methods cover procedures for testing the isocyanate raw materials used in preparing urethane foams. nerly under the jurisdiction of Committee D-20 on Plastics, these methods were discontinued in 1991. 229 DUP050295894 Designation: D 1718 - 90 Standard Specification for Isobutyl Acetate (95 % Grade)1 Y This standard is issued under the fixed designation D 1718; the number immediately following the designation indicate 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 rijapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This specification has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This specification covers isobutyl acetate (95 % grade). 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for material listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D1078 Test Method for Distillation Range of Volatile Organic Liquids2 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)3 D1296 Test Method for Odor of Volatile Solvents and Diluents2 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1476 Test Method for Heptane Miscibility of Laquer Solvents2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D3545 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 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 DO 1.3 5 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct 26, 1990. Published December 1990. Originally published as D 1718 - 60 T. Last previous edition D 1718 - 86. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 05.03. 5 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 6 Annual Book ofASTM Standards, Vols 06.03 and 15,05. * 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Properties 3.1 Isobutyl acetate shall conform to the following re quirements: Apparent specific gravity: 20/20"C 25/25'C Color Pt-Co units, max Distillation, "C at 760 mmHg Initial boiling point, min Dry paint, max Nonvolatile matter mg/100 mL, max Odor Water, vrt %, max8 Acidity (free acid as acetic), wt %, max Purity, wt %, min 0.868 to 0.873 0.864 to 0.869 10 112.0 119.0 5 nonresidual 0.1 0.01 95 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Method 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20C. See Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation thermometer having a range from 98 to 152C, and conforming to the requirements for thermometer 41C, as prescribed in Specification E 1. 5.1.4 Nonvolatile Matter--Test Method D 1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Method D 1364 and Method D 1476. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Purity--Test Method D 3545. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 8 This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20C. 230 S| * DUP050295895 iPackaging shall conform to applicable carrier rules gulations or when specified shall conform to Fed. PP-C-2020. vX- 7. Keywords 7_ i ester; isobutyl acetate; solvent 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 cf any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and It notrevised, eitherreapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your.comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 231 DUP050295896 Designation: D 1719 - 90 Standard Specification for Isobutyl Alcohol1'2 This standard is issued under the fixed designation D 1719; 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 specification has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. ~ 1. Scope 1.1 This specification covers isobutyl alcohol for use in paint, varnish, lacquer, and related products. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheets for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material13 2 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)4 D1296 Test Method for Odor of Volatile Solvents and Diluents3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1476 Test Method for Heptane Miscibility of Lacquer Solvents3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1719-60 T. Last previous edition D 1719 -86. 2 This compound is also known under the names 2-methyl-2-propanoi and isobutanol. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book cfASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. 6Annual Book ofASTM Standards, Vol 14.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05.8 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 Isobutyl alcohol shall conform to the following re quirements: Apparent specific gravity: 20/20C 25/25C Color, Pt-Co Scale, max Distillation range Nonvolatile matter, max, g/100 mL Odor Water, max, weight % Acidity (free acid as acetic), max, weight % 0.802 to 0.804 0.794 to 0.801 10 A 0.005 nonresidual 0.2s 0.003c A Shall distill entirely within a 2C range which shall include 107.9C. BThis quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20C. c Equivalent to 0.028 mg of KOH per gram of sample. 4. Sampling 4.3 This material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods. 5.1.1 Apparent Specific Gravity--Determine the apparent * specific gravity by any convenient method that is accurate to the third decimal piace, the temperature ofboth material and water being 20 or 25C. See Methods D 268 or Test Method ; D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 40C having a ' range from 72 to 126C and conforming to the requirements ' in Specification El. 5.1.4 Nonvolatile Matter--Test Method D 1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Methods D 1364 and D 1476. ! 5.1.7 Acidity-:Test Method D 1613. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 isobutyl alcohol 232 DUP050295897 D 1719 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 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 it not revised, eitherreapproved or withdrawn. Yourcomments 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 Stphdards, 1916 Race St., Philadelphia, PA 19103.233 233 DUP050295898 Designation: D 1720 -88 Standard test Method for > Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions1 - v This standard is issued under the fixed designation D 1720; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4204.1 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 the volume ratio of hydrocarbon diluent to active solvent required to cause persistent heterogeneity (precipitation) in a solution of cellulose nitrate. 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. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D301 Test Methods for Soluble Cellulose Nitrate12 D841 Specification for Nitration Grade Toluene3 3. Description of Term Specific to This Standard 3.1 dilution ratio--the maximum number of unit vol umes of a diluent that can be added to a unit volume of solvent to cause the first persistent heterogeneity (precipi tation) in the solution at a concentration of 8 g cellulose nitrate per 100 mL of combined solvent plus diluent and at a temperature of 25 3C. No t e .1--The dilution ratio decreases as the cellulose nitrate concen tration at the end point increases. It is, therefore, necessary to set an arbitrary concentration of cellulose nitrate as part of the dilution ratio term. For this purpose 8.0 g of cellulose nitrate per 100 mL of solvent plus diluent has been adopted. 4. Significance and Use 4.1 By use of standard or reference grade materials for any two of the three components, namely, oxygenated solvent, diluent, or cellulose nitrate, the effect of different batches or different types of the third component can be determined. - 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 25, 1988. Published May 1988. Originally published as D 1720 - 60 T. Last previous edition D 1720 - 84. .. 2 Annual Book ofASTM Standards, Vol 06.0Z 3 Annual Book ofASTM Standards, Vol 06.03. 4.2 This test method is applicable for the determination of a the following: , 4.2.1 The dilution ratio of toluene as the standard diluent to an oxygenated solvent under test, using as the solute | standard cellulose nitrate as defined in 5.2. 4.2.2 The dilution ratio of a hydrocarbon diluent under f test to n-butyl acetate as the standard solvent, using as a 1 solute standard cellulose nitrate as defined in 5.2. ; 4.2.3 The dilution ratio of toluene, as the standard diluent, to n-butyl acetate as the standard solvent, using as the solute cellulose nitrate of varying solubility characteris- if tics. H 5. Materials 5.1 n-Butyl Acetate (90 to 92 %). J No t e 2--This grade of n-butyl acetate contains 8 to 10 % n-butyl '' m alcohol. jS 5.2 Cellulose Nitrate, conforming to the Sampling section (Appearance, Ash, and Stability requirements) of Methods D 301 and of such quality that, when used in determining the toluene dilution ratios of n-butyl acetate and methyl -propyl ketone, it will give results between the following limits: I 1 ;J I 1 | Toluene Dilution Ratio re-butyl acetate methyl re-propyl ketone 2.73 to 2.83 3.80 to 3.90 5.3 Toluene (Toluol), conforming to Specification D 841. 1 ;i 6. Hazards 6.1 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. Do not store samples of dry cellulose nitrate at any time. Dry only that portion required for immediate test. Wear a face shield when the oven is opened after samples have been heated. Wet excess material and the samples left after testing with water and dispose of properly. ' 7. Drying Cellulose Nitrate 7.1 Dry not more than 20 g of cellulose nitrate at a time by spreading in a thin layer on a tray at room temperature for 12 to 16 h, or on top of a 100C oven where the j f f f !i I i! , j :j 234 DUP050295899 # D 1726' ture is 35 to 40C for about 8 h (Warning, see 6.1). jively, use a steam or hot water-heated oven mainat-45 to 50C todry specimens in about 8 h. For safety j ithe oven should have the latch removed. Another simple way to. dry small quantities of cellu- ate; is to use a drier assembled from common ory apparatus. The assembled drier is shown in Fig. 1. from a laboratory' electiic-oven is drawn through wet nitrate contained in a lt%ss.tube hooked up. through _e iube, or small funnel, and suction flask to a water tor or other vacuum source. The brass pipe should be ,1 '/2 in. (40 mm) in diameter and 8 in. (200 mm) long, ^lative dimensions having been found to give efficient Such a tube will hold about 25 g, dry weight, of wet : nitrate. The pipe is insulated to conserve1 heat. The Iff flask end ofthe brass tube is fitted with a thistle tube, Small funnel, over themouth ofwhich is tieda silk cloth iu An indentation made in the funnel edge allows 'on of the thermometer. The funnel and thermometer eld in place by means of a rubber stopper. When using en temperature of 85C and vacuum supplied by a aspirator or other vacuum source, the alcohol?wet "ose nitrate will be dried in about 4 h. .'Iflarger quantities of celiulcise nitrate are required, the .g equipment described In the Procedure section of ng Samples of Methods D 30 i may be used. . eparation of Solution .1 When testing either a solvent pr diluent, first estimate ipirdbiable dilution ratio fijf the unknown component in Jon to the .other to determine the amount of solvent 'ted to dissolve the cellulose nitrate (Table T). This jlume of solvent should be such that there will be approx imately 10 g of cellulose nitrate present per 100 mL of veht plus diluent at the end point. fit! " . ' ' ' 'No t e 3--Reference to published data on similar types ofsolvents or 'ents will provide a.good approximation of the. amount of solvent uirgd. If data are not available, several solutions with varying Bunts of solvents may be required to arrive at a suitable volume to |ii|j8,2 On ah analytical balance, weigh, 5 , 0.01 g of the ellulose nitrate into a 125-mJL cork-stoppered, preweighed " lennieyer flask,,or other suitable container. From a buret !add the volume of solvent indicated in Table 1. Swirl the ask until the cellulose nitrate is completely dissolved. When `a high concentration of cellulose nitrate in solvent is re- uired, dispersion may be more quickly accomplished by adding a measured portion of the diluent to the flask. This reduces the solids concentration and thus lowers the viscosity of the solution, making it easier to dissolve the cellulose nitrate. TABLE 1 Volume of Solvent Required to Dissolve Cellulose Nitrate Probable Dilution Ratio, volume of diluentvolume of solvent mL of Solvent per 5 g of Cellulose Nitrate at:23C 1 25.0 2 16.7 3 12.5 4 10.0 5 - 8.3 9. Procedure 9.1 Add the diluent, maintained at 25 3.0C, to the flask from a buret in small additions. Five-millilitre increments riiay be added at first, but these shall be decreased to about 0.5 mL as the end point is approached. After each addition, stopper the flask and swirl vigorously to disperse any gel or precipitate thrown down by local overconcentration of diluent (Note 4). When precipitation persists after at least 2 min of vigorous `swirling, the initial end point has been reached, as indicated by the presence of gel particles in the solution or on the sides of the flask (Note 5). Determine the total volume of diluent added to the flask at this point .JSfosTE 4--Take care, to prevent loss of volatile components by evaporation. Avoid contact of the solution, with the stopper, No t e 5--Presence of a uniform fine haze that is usually formed when aliphatic hydrocarbons are used as dilu'ents must not be confused with the g^i end point. A ' ' u' 9.2 Determine a second end point using the same solu tion. This, requires addition of solvent to redissolve the cellulose nitrate. The amount of solvent to . add depends upon the amount of diluent used in the initial titration. The volume of solvent to be added is obtained directly from Fig. 2 and the volume of diluent used to reach the initial end point .< 9.3 After addition of the required volume of solvent, swirl the flask to redisperse the cellulose-nitrate. Then, continue the titration with diluent to the second end point, at which point there should be approximately 8 g of cellulose nitrate present per 100 mL of solvent plus diluent 10. Calculation 10.1 Calculate the dilution ratio and cellulose nitrate HOT AIR FROM OVEN INSULATION RUBBER STOPPER . THERMOMETER i RUBBER.---- STOPPER BRASS PIPE 1 j* X B SILK CLOTH OVER FUNNEL MOUTH FIG. 1 Assembled Drier 235 SUCTION DUP050295900 # D1720 Volume of Diluent at Initial End Paint, mL FIG. 2 Volume of Solvent to Be Added to Complete Titration versus Volume of Diluent lined to.Reach Initial End Point concentration at both the initial and the second end points as follows: ? Dilution ratio = A/B Cellulose nitrate concentration per 100 mL oF volatile matter = C/(A + B) where: A s= diluent for the titration, mL, B = solvent used, mL, and C = cellulose nitrate used, g, 10.2 Construct a graph for dilution ratio versus cellulose nitrate concentration. Plot as two points on the graph (Fig: 3) the two sets of values calculated as described in 10.1. One of the points will be very close to 8 g/100 mL of volatile matter. , ; Cellulose Nitrate, 9 per iOQmL of Volatile Matter . FIG. 3 Grams of Cellulose Nitrate per 100 mL of Volatile Matter versus Dilution Ratio The correct value at exactly 8 g/100 mL of volatile matter^ may be interpolated by drawing a straight line connecting t two experimentally determined points. While the ci showing the relationship between the dilution ratio cellulose nitrate concentration is not necessarily a s line, the error made by interpolating or extrapolating: the straight line connecting the two points is negligible iffi proximity of 8 1 g/100 mL of volatile matter. No t e 6: Example--Assuming a probable dilution ratio of appro;? mately 3, the following results are obtained; ' Initial End Point Solvent Added (from Fig. 2) g8f| Second EndPoint Cellulose nitrate, g Solvent, mL t Diluent, mL Solvent plus diluent, mL Dilution ratio : 5.00 12.5 35.0 47.5 35/12:5 = 2.8. .. 3 Cellulose nitrate per 100 mL of i0.5 ' volatile matter, g FromFig. 3 the dilution ratio at 8.0 g ofcellulose nitrate = 3.16 5.00. 15.5 49.6 65.1 49.6/155i,' , =3.2 7.7 isjji 11. Report 11.1. When testingsolvents, report the ratio of the volume of toluene to the volume of solvent at 8 g of cellulose nitrate . per 100 mL of volatile matter. 11.2 When testing diluents, report the ratio of the volume of diluent to the volume of n-butyl acetate at 8 g of cellulose nitrate per 100 mL of volatile matter. 11.3 When testing cellulose nitrate, report the ratio of the vbluitse of toluene to the volume of n-butyl acetate at 8 g of : cellulose nitrate per 100 mL of volatile matter. , '! 12. Precision and Bias 12.1 Precision--The following criteria should be used for judging the acceptability 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 0.1. 12.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 0.2. 12.2 Bias has not been determined for this test method. ' * The American Society for Testingand Materials takes no position respecting the validity of anypatent lightsasserted 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, etherreapproved or withdrawn. Yotir comments are invitedeither 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, if you feel thatyotir. 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. 236 DUP050295901 t designation: D 1721 - 84 (Reapproved 1988)*ii Standard Test Method for Permanganate Time of Tricresyl Phosphate1 This standard is issued under the fixed designation D 1721; 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. ei NOTE--Sections 1 and 6 were changed editorially in March 1988. m This test method covers the detection in tricresyl *ate of the presence of impurities that reduce potasermanganate. This standard may involve hazardous materials, oper and equipment. This standard does not purport to s all ofthe safety problems associated with its use. It is sponsibility of the user of this standard to establish Hate safety and health practices and determine the liability of regulatory limitations prior to use. For 'c hazard statements, see Section 6. . For hazard information and guidance, see the supMaterial Safety Data Sheet. 'erenced Document ) ASTM Standard: 1193 Specification for Reagent Water2 ignificance and Use .1 Impurities such as phenols, if present in tricresyl sphate, will- react with potassium permanganate, re;hg it to manganese dioxide. In the permanganate test, l color of the test solution is observed at the end of a min period, and if the pink color is still present, the -pie is considered substantially free of oxidizable impuri- 3.2 The results of this measurement can be used for ecification acceptance. Apparatus 4,1 Graduated Cylinders, glass-stoppered, 100-mL caacity. . Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be -*ed 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 Chemlical 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 ences to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 5.3 Potassium Permanganate Solution (0.316 g/L)--Dis solve 0.316 g of potassium permanganate (KMn04) in water and dilute to 1 L with freshly boiled water (Note). The solution should be stored in brown bottles and be freshly prepared weekly as required. No t e--Clean glassware is essential to the stability of the KMn04 solution. Clean graduated cylinders and permanganate storage and handling equipment with concentrated hydrochloric acid (HQ, sp gr 1.19) to remove residual manganese oxide (Mn02) which catalyzes reduction of KMn04. Remove the acid with not less than ten rinsings with water. 6. Hazards 6.1 Tricresyl phosphate is hazardous; take special precau tions when handling it. Avoid eye and skin contact and inhalation of vapors. 7. Procedure 7.1 Weigh 10 0.1 g of the sample to be tested into a 100-mL glass-stoppered graduated cylinder. To this, add 50 mL of the KMn04 solution. Vigorously shake the mixture for 2 min, noting the time when the shaking begins. Allow the test to stand for a period of 28 min following the shaking period and observe the color. 8. Report 8.1 If the color of the permanganate solution is still pink, report the sample as "passing." If no pink color is present, report the sample as "not passing." 9. Precision 9.1 No statement is made about the precision of assessing this test method, since the results of the test method are pass-fail. 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 DOI.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27, 1984. Published August 4984. Originally published as D 1721 - 60 T. Last previous edition D 1721 - 79. 2 Annual Book ofASTM Standards, Vols 06.03 and i 1.01. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc.t 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." 237 DUP050295902 # D 1721 TheAmerican Society tor Testingand 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 orwithdrawn. Your comments are invited either forrevision ofthis standardor 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. ~ 4 ` aiiiP i& s SffiaBsss&g I I | 4 238 DUP050295903 Designation: D 1722 - 90 Standard Test Method for Water Miscibility of Water-Soluble Solvents1 This standard is issued under the fixed designation D 1722; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year Oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval'. This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. ope iThis test method covers the determination of the bility of water-soluble Solvents with water. While specifically for testing; acetone, isopropyl alcohol lopanol), and methyl alcohol (methanol), the method is ble for testing most water-soluble solvents. This test method serves to detect water-immiscible aminants qualitatively; the level of detection of these unties varies widely with both the type of solvent and the f of impurity. |3 The level of detection of water-insoluble materials fends upon the solvent tested and the type of impurity or rities present, that is paraffin, olefin, aromatic, high cular weight alcohol, or ketone, etc. There is, therefore, Specific level of impurity detected by this procedure. JfOTE--This test method is normally performed at ambient, but other iperatures may be used as specified by the consumer and supplier. ft.4 This standard does not purport to address all of the /problems associated with its use. It is the responsibility the user ofthis standard to establish appropriate safety and faith practices and determine the applicability ofregulatory nitations prior to use. j, 1.5 For specific hazard information and guidance, consult |e supplier's Material Safety Data Sheet for materials listed t this test method. . Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 . Summary of Method 3.1 The specimen is diluted to 10 volumes with water and the resulting mixture examined for cloudiness or turbidity. ; 4. Significance and Use 4.1 Water-insoluble materials present in a solvent ex pected to be completely water miscible may interfere with many uses of the solvent. This test method provides a measure of the miscibility of water-soluble solvents with a polar medium-water. It also provides a qualitative indication 1 This test method is under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.3S on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as D (722 - 60. Last previous edition D 1722 - 86. 2 Annual Book ofASTM Standards, Vois 06.03 and 11.01. of the presence or absence of water-immiscible contami nants. 4.2 The results of this test method may be used in assessing compliance with a specification. Prior to agreeing to this test method as the basis of a specification require ment, it may be desirable that the interpretation of what constitutes cloudiness or turbidity be agreed upon between the supplier and the purchaser. 5. Apparatus 5.1 Cylinder, graduated, glass-stoppered, 250-mL. 6. Reagent 6.1 Water--References to water shall be understood to mean reagent water conforming to Type IV of Specification D1193. 7. Procedure 7.1 Transfer 25 mL of the sample to one of two clean 250-mL graduated cylinders, dilute to the mark with water, and mix thoroughly. Allow any bubbles to rise to the surface. 7.2 Add 250 mL of water to the second cylinder and reserve as a blank. 7.3 Compare the specimen solution with the water blank by viewing through the length of the column of liquid toward a dark background. When an artificial light source is used, position the light so that it passes transversely through the cylinders. 8. Report 8.1 If the specimen-water mixture is as free of cloudiness or turbidity as the blank, report the sample as "passes test." If any cloudiness or turbidity is detected after 30 min, report as "fails test." 9. Precision and Bias 9.1 Because of the pass-fail nature of this test procedure, no precision or bias statement is presented. 10. Keywords 10.1 solvents; water miscibility test 239 DUP050295904 D 1722 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 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 responsibly. - ... - y. This standerd 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 either for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful, consideration at a meeting ofthe 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 19103.240 240 DUP050295905 Last ASTM Designation: D 1728 - 83 Standard Test Method for Phthalate EsterColor of High-Gravity Glycerin is test method covers the determination of the color of the phthalate ester of high-gravity glycerin (glycerol). Werly under the jurisdiction txf Committee D-l on Paint and Related Coatings and Materials, this test method was ntinued in 1991. ` ................. 241 DUP050295906 Designation: D 1836 - 91 Standard Specification for Commercial Hexanes1 This standard is issued under the ftxed.,desigiiation D 1836; the number immediately following the designation indicate 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 specification covers the range of products com monly referred to as hexanes, which find uses in the preparation of adhesives, coatings, and printing inks, as raw materials in chemical synthesis operations, and as solvents in various kinds of extraction operations. 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. Specific hazard statements are given in Section 6. 1.3 For specific hazard information and guidance consult supplier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D156 Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method)21 D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint, and Related Coatings and Material3 D611 Test Methods for Aniline Point of Petroleum Products and Hydrocarbon Solvents4 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1133 Test Method for Kauri-Butanol Value of Hydro carbon Solvents3 D 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 D1296 Test Method for Odor of Volatile Solvents and Diluents3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D2710 Test Method for Bromine Index of Petroleum Hydrocarbons by Electrometric Titration5 D3I20 Test Method for Trace Quantities of Sulfur in Light Liquid Petroleum Hydrocarbons by Oxidative Microcoulometry5 D4367 Test Method for Benzene in Hydrocarbon Sol vents By Gas Chromatography3 1 This specification is under the jurisdiction of ASTM Committee 0-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 15, 1991. Published July 1991. Originally published as D 1836 - 61 T. Last previous edition D 1836 - 87. 2 Annual Book ofASTM Standards. Vol 05.01, 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 5 Annual Book ofASTM Standards. Vol 05.02. E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 . 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 3. Properties 3.1 Commercial hexanes shall conform to the following requirements: Aniline point, min Apparent specific gravity 15.6/15.6"C Bromine index, max Color Distillation range: Initial boiling point, min Dry point, max Kauri-butanol value, max Nonvolatile matter, mg/100 mL, max Odor Sulfur, ppm, max Benzene content, weight %, max 57"C ' 0.660-0.686 1000 not darker than +28 on the Saybolt Scale or 10 on the Pt-Co Scale 63C 71"C 33 1 nonresidual 10 0.1 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 5.1.1 Aniline Point--Test Method D 611. 5.1.2 Apparent Specific Gravity--Determine apparent specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 15.6C. See Methods D268. If measurement is by hydrometer, the instrument must be calibrated at the test temperature. 5.1.3 Benzene Content--Test Method D 4367. 5.1.4 Bromine Index--Test Method D 2710. 5.1.5 Color--Test Method D 156 or D 1209. In case of dispute, Test Method D 156 shall be the referee method. 5.1.6 Distillation--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 39C having a range from 48 to 102C and conforming to the requirements in Specifi cation El. 5.1.7 Kauri-Butanol Value--Test Method D 1133. 5.1.8 Nonvolatile Matter--Test Method D 1353. 6 Annual Book ofASTM Standards. Vols 05.03 and 14.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 8 Available from Standardization Documents, Older Desk, Bldg. 4 Section D, 700 Robbins Ave,, Philadelphia, PA 19111-5094, ATTN: NPODS. 242 DUP050295907 D 1836 Odor--Test Method D 1296. Samples of particular !bf products being tested, having odor characteristics pry to consumer and producer, are to be used as ce standards for comparison. 10 Sulfur--Test Method D 3120. ds Hexane may contain small amounts of benzene, is a carcinogen. Commercial hexanes contain ne, which is known to cause peripheral neuropathy. 7. Packaging and Package Marking 7.1 Package size shall be agreed upon by the purchaser and the supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 8. Keywords 8.1 commercial hexanes; hexanes; solvents 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 siibject to revision at any time by the responsible technical committee andmust be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard,or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 243 DUP050295908 Designation: D 1841 - 63 (Reapproved 1988)61 Standard Specification for ; Distilied Coconut Fatty Acids1 This standard is 'issued under the fixed designation D 1841; 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. el No t e--I'aragr.iph l.1.1 was editorially changed in October 1988. " 1. Scope 1.1 This specification covers distilled fatty acids derived from coconut oiL Two types are covered a follows: 1.1.1 Type /--Usually produced from raw1 coconut oil. 1.1.2 7S!pe//-r-tJiualiy produced from recovered coconut * oil. D1962 Test Method for Saponification Value of Drying Oils, Fatty Adds, and Polymerized Fatty Acids2 E> 1965 Test Method.for Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Acids2 D 1980 Test Method for Acid Value of Fatty Acids and Polymerized Fatty Acids2, D1982 Test Method for Titer of Fatty Acids2 2. Referenced Documents 2.1 ASTM Standards: D1467 Guide for Testing Fatty Adds Used in Protective Coatings2 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Adds2 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 DO1.32 on Drying Oils. Current edition accepted Sept. 30, 1963. Originally issued 1961. Replaces D1841-61 T. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3. Properties 3.1 Distilled coconut fatty adds shall conform to the requirements in Table 1. 4. Test Method 4.1 The properties enumerated in this spedfication shall be determined in accordance with Methods D 1467. TABLE 1 Requirements for Distilled Coconut Fatty Acids Acid value Saponification value Unsaponifiable matter, max, % Iodine value Color, Gardner, max Titer, C ASTM Test Method D 1980 D 1962 D 1965 01959 D 1544 D1982 Type 1 258 to 26S 260 to 272 1.00 8 to 15 3 22 to 26 Type II 255 to 266 257 to 268 1.00 8 to 15 5 22 to 28 The American Society ter 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, ere entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrewn. Your comments are Invited either lorrevision 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 Mend, tf you feeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 ftace St., Philadelphia, PA 19103. 244 DUP050295909 resignation: D 1842 - 63 (Reapproved 1988) Standard Specification for Distilled Corn Fatty Acids? This standardis issued under the fixed designation D 1842; 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 (r) indicates an editorial change'since the last revision or reapproval. specification covers distilled fatty acids derived m oil; recovered com oil usually is used. fenced Documents fes?TM Standards: 57 Guide for Testing Fatty Acids Used in Protective atings2 " . 44 Test Method for Color of Transparent Liquids Gardner Color Scale)3 1 Test Method, for. Iodine Value of Drying Oils -and Fatly Acids2 ' `1962 Test Method for Saponification Value of Drying .Oils, Fatty Adds, and Polymerized Fatty Acids2 specification is under thejurisdiction ofASTM Committee D-l on Paint ted Coatings and Materials and is the direct responsibility of Subcom- .32 on Drying Oils. it edition, accepted Sept 30, 1963. Originally issued. 1961. Replaced 1-61T. ,ual Book ofASTM Standards, Vol 06.03. !ual Book ifASTM Standards, Vols 06.01,06.02, and 06.03. D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Adds2 D1980 Test Method for Add Value of Fatty Adds and Polymerized Fatty Adds2 D1982 Test Method for Titer of Fatty Adds2 3. Properties , 3.1 Distilled com fatty acids shall conform to the require ments in Table 1. 4. Test Method 4.1 The properties enumerated in this specification shall be determined in accordance with Methods D 1467. TABLE 1 Requirements for Distilled Corn patty Adds -- ASTM Test Method Acid value Saponification value Unsaponifiable matter, max, % Iodine value, min Color, Gardner, max Titer, C D1980 D1962 D1965 D1959 D1644 D1982 195 to 205 197 to 207 1.50 110 8 26 to 32 The American Society for resting 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 of the validity of any such patent rights, and the risk of Infringement dt such rights, are entirelytheir 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, eitherreeppreved or withdrawn. Yourpomments are Invitedeither for revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting 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 19103.245 245 DUP050295910 Designation: D 1843 - 63 (Reapproved 1988)e1 Standard Specification for Fractionated and Distilled Cottonseed Fatty Acids1 This standard is issued under the fixed designation D 1843; 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 (t) indicates an editorial change since the last revision or reapproval. cl No t e--Paragraph 1.1.3 was editorially changed in Optober 1988. 1. Scope 1.1 This specification covers distilled acids derived from cottonseed ofl. Three types are covered as follows: 1.1.1 Type /--Highly fractionated fatty acids usually produced from recovered cottonseed oil. 1.1.2 Type //--Fractionated fatty acids usually produced from recovered cottonseed oil. 1.1.3 Type III--Usually produced from recovered cotton seed oil. 2. Referenced Documents 2.1 ASTM Standards: D1467 Guide for Testing Fatty Acids Used in Protective Coatings12 1 This specification is under the juriiidiction ofASTM Committee CM on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.32 on Drying Oils. Current edition accepted Sept. 30, 1963. Originally issued 1961. Replaces D 1843 - 61 T. . 2 Annual Book ofASTM Standards Vol 06.03. D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Adds2 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and PolymerizedFatty Adds2 D1980 Test Method for Acid Value of Fatty Acids, and Polymerized Fatty Acids2 D1982 Test Method for Titer of Fatty Adds2 si i J ^ | - 3. Properties 3.1 Fractionated and distilled cottonseed fatty acids shall conform to the requirements in Table 1. f ;i 4.. Test Methods 4.1 The properties enumerated in this specification shall be determined in accordance withMethods D 1467,. # 3 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. Acid value Saponification value . Unsaponifiable matter, max, % Iodine valueColor, Gardner, max Titer, C ' TABLE 1 Requirements for DistilledCottonseed Fatty Acid6 . ASTM Test Method Type 1 Type II D1980 D1962 D1965 D1959 D1544 D1982 ' 195 to 201 197 to 203 1.00 140 to 145 2 5 max 106 to 204 198 to 206 1.50 120 to 130 '5 25 max Type 111 199 to 205 201 to 207 1.50 9510110 8 32 to 38 The American Society for Testing andMaterials takes no position respecting the validity of any patent rights asserted In connection with any Hem menttoned 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 entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited eithertorrevision ofthis standardor tor additionalstandards and should be addressed to ASTM Headquarters. Your commsnts 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. DUP050295911 signation: D 1950 - 86 (Reapproved 1990) Standard Test Method for Acetone Tolerance of Heat-Bodied Drying Oils1 This standard is issued under the fixed designation D 1950; 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. e _ :His test method covers 'the determination of the ' tolerance of Heat-bodied drying oils when no rionterial is present, Ifcis standard does not purport to address all of the roblems associated with its use. It is the responsibility yer uses this standard, to consult and establish mte safety and health practices and determine the ' ility of regulatory limitations prior to use. Specific .`Statements are given in Section 6. scription of Term Specific to This Standard acetone tolerance--of a drying oil, the number of ; of acetone required to produce a persistent cloudiness ;-g ofthe oil at 25"C, under the conditions prescribed in : method. ignificance and Use 1 Unbodied drying Oils are miscible with acetone. As 'ng oils are heat-bodied, higher molecular weight species formed that are acetone insoluble. Therefore, addition of ' ne to a drying oil can be used as an indication of the of polymerization present in the oil. Since solubility . polymer is extremely temperature-dependent, the tem- re must be precisely controlled. This test method is tlicable to heat-bodied oils only when no other nonfatty terial is present 3.2There is no correlation between the acetone tolerance the usefulness of an oil, but, if acetone tolerance and Iher properties ofan oil are the same as those of an accepted aple, the two probably have been produced by the same hnique. . Apparatus 4.1 Balance, capable of weighing to an accuracy of 0.5 shall be fitted with a water pump for circulating water through the bath and the water jacket as shown in Fig. 1. No t e l--Details for the thermostatic control unit and heating element have been omitted from the drawing in Fig. 1, since the proper selection and construction of this unit may be left to the discretion of the analyst 4.B Volumetric Flask, 25-mL, glass-stoppered, for use as a specific gravity bottle. 4.9 Glass Beads, approximately Vt to V in. (1.5 to 3 mm) in diameter. 5. Reagents and Materials 5.1 Acetone (Warning--See 6.1); 5.1.1 Place a suitable quantity of acetone in a roundbottom, glass-stoppered flask and to it add 25 % of its weight of anydrous cupric sulfate (CuS04). Stopper the flask and allow the mixture to stand for at least 3 days. At the end of this period, attach the flask and its contents to an all-glass distillation apparatus that previously has been thoroughly dried and distill the acetone directly from the drying agent, using a steam bath for heating. Discard the first 10 % and the last 10 % of the distillate. During the distillation, protect the 4.2 Erlenmeyer Flasks, 250-mL, glass-stoppered. 4.3 Bath Clamp. 4.4 Ringstand, approximately 4 ft (1.2 m) high. 4.5 Buret, with a capacity of 50 mL, fitted at the top with a suitable drying tube. 4.6 Water Jacket Assemblyfor Buret, as shown in Fig. 1. 4.7 Water Bath--A constant-temperature water bath ca pable of maintaining a temperature of 25 0.1C. The bath 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 1.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as Sections 43-47 of Test Method D 555 - 58. Last previous edition D 1950-68(1984). 247 DUP050295912 D 1950 apparatus from atmospheric moisture by means of a trap containing anydrous CuS04. Collect and store the acetone in the same receiving bottle, fitted with a similar moisture trap. 5.1.2 Determine the specific gravity at 25/25'C and the percent of moisture in the acetone. The acetone shall be considered suitable for use if the specific gravity is between 0.7864 and 0.7872, equivalent to a water content of 0.00 to 0.24%. 5.2 Cupric Sulfate, Anhydrous--Technical grade, anhy drous, powdered cupric sulfate (CuS04). 6. Hazards s.... 6.1 Acetone is a flammable liquid. It is harmful if inhaled, use only with adequate ventilation. Avoid prolonged contact with skin or any contact with the eyes. See supplier's Material Safety Data Sheet. 7. Procedure , ,. 7.1 Weigh the glassrstoppered Erlpnmeyer' flask, con taining three or four glass beads, to 0.1 mg. Transfer about 30 g of the sample of the Erlenmeyer flask and weigh the flask and contents to 0.1 mg. Record the weight of the specimen by difference. 7.2 Immerse, the flask and .its contents in the constant- temperature bath so that the level of the water in the bath is above the level of the specimen. Clamp the flask , into position by means of the bath clamp. Fill the buret with acetone and attach the drying tube. Bring the flask and its contents, and the acetone, fo 25 0.1 C by allowing them to stand for at least 10 min. 7.3. Disconnect the flask from the'clamp, remove the. stopper, and run in the acetone.from the buret. Add the acetone in small portions, while keeping the flask immersed in the water bath. After the addition of each portion bf|| acetone, stopper the flask and swirl it gently to dissolve the '""'i contents properly. If it should become necessary to remote the flask from the bath to facilitate mixing, reimmerse the' stoppered flask in the bath and allow to stand for at least 5 min before continuing with the titration. Take care not to ' splash the contents over the upper part of the flask during the i titration. Each addition of acetone produces a dense cloudi- ` ness that will be discharged by agitating the mixture. As the end point is neared, the cloudiness will persist for longer periods of time. At this point, add the reagent dropwise until the addition of .1 drop of the reagent produces a persistent dense cloudiness. Stopper the flask immediately and wipe dry with a clean cloth. ' No t e 2--A suitable magnetic stirring apparatus may be used instead of the beads. 7.4 Weigh the flask and its contents to 0.1 mg. Record the weight of acetone by difference. 8. Calculation 8.1 Calculate the. acetone tolerance, T, as follows: . T = (AjS) x 100 where: ' w A = acetone required for titration of the specimen, g, and 5 = specimen used, g. 9. Precision and Bias 9.1 Precision and bias data were not established at the time this test method was written. An effort is being made to obtain the precision and, if obtainable, will be published in' future revisions. This test method has been in use for many years, and. its usefulness has been well established. The American Society tor Testing and Materials takas 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 ttielr own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either torrevision ofthisstandard 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. 248 DUP050295913 Jesignation: D 1951 - 86 (Reapproved 1990)V. p Standard"Test Method for Ash in Drying |)its and Fatty Acids1 This standard is issued under the fixed designation D 1951; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of iast revision, ^ npmbpr in parentheses indicates the year of last reapproval. A superscript epsilon (r) indicates aneditorial changesince;the last reyisiopjprreapproval. :; ,. This method has been approvedfor use by agendas ofthe Department ofDefense to replace Methads5262.5263.5265 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. Ids test method covers the determination of the | or ash resulting from ignition, under prescribed fans, of all natural and synthetic drying oils and their lids. This test method is not applicable to boiled oils. 1--Boiled oils do not give reproducible results. Lead driers are jLreduced by the carbon to give metallic lead and oxides of plcomposition, and zinc oxide is relatively volatile at the muffle ^temperature. Ash determinations on boiled oils consequently rical and not highly reproducible. This standard does not purport to address all of the problems associated with its use. It is the responsibility jtoever uses tkis standard to consult and establish jmate safety and health practices and determine the feability of regulatory limitations prior to use. Specific l statements are given in Section 4. Ificance and Use Most natural and processed oils contain small punts of ash, but the amount is insignificant. Certain, hetic drying oils may contain residual catalyst or other |erials, thus giving larger amounts of ash. Although the land metal content of boiled oils may be specified, the Id with new and improved driers is toward the specificai of drying time, allowing the manufacturer to obtain this ny way desired. 12 In this test method, ash is determined by igniting the fecimen under specified conditions and weighing the rese. Due to the volatility or the reduction of certain metal Ides, some inaccuracies may result. Wet ashing or extrac- methods may give more accurate results. Apparatus ,3.1 Crucible, porcelain or high-silica glass (Note 2), 50- , capacity. No t e 2--Platinum is not recommended. Boiled oils or oils contam(I'ttated with driers containing lead may ruin platinum by alloy forma tion. 3.2 Electric Muffle Furnace. P 3.3 Desiccator, containing an efficient desiccant. Anhyf drous calcium sulfate (CaS04), phosphorus pentoxide (P205) ' This test method is underthe jurisdiction of ASTM Committee D-l onPaint ' and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 1951 -61. Last previous edition D 1951 - 61 (1984). (Warning---see 4.1) or. concentrated sulfuric acid (Waming-MCe 4.2) (H?S04, sp gr 1.84} are satisfactory. No t e 3--Magnesium Perchlorate and Barium Perchlorate are also efficient desiccators and were previously listed in this section. However because of their explosive danger, and the availability of other safer materials, the recommendation for their use has been discontinued. 3.4 Oil Sample Bottle, 4-oz (120-mL). 3.5 Triangle, Nichrome or clay. 4. Hazards 4.1 Phosphorus Pentoxide is a strong oxidizer and reacts violently with water, reducing agents and organic matter. Causes bums. Avoid contact with skin or eyes, or clothing, or inhalation as dust. Refer to supplier's Material Safety Data Sheet. 4.2 Sulfuric Acid is corrosive to skin, eyes and mucous membranes in form of liquid, mist or fumes. It causes severe bums. Take care to prevent the contact of the arid with eyes, skin or on clothing. In making dilute solutions, always add the arid to water with care. See supplier's Material Safety Data Sheet. 5. Procedure 5.1 Ignite the crucible in the muffle furnace at 550 to 650C. Cool slightly, place in a desiccator for 1 h, and weigh to 0.1 mg. 5.2 Fill a 4-oz (120-mL) sample bottle with the sample and weigh to 0.05 g. Pour about 20 g of the sample from the bottle into the crucible supported on a triangle, using care so that no oil runs down the outside of the crucible or bottle. 5.3 Heat gently by moving a flame on the bottom and sides of the crucible until the oil ignites. Reduce the size of the flame until the heat is just sufficient to keep the sample burning. When the first batch of oil has burned out, add about 20 g more of the sample and continue in the same manner until all of the oil in the 4-oz bottle has been added. Reweigh the sample bottle to obtain the total weight of sample used, which will be somewhat over 100 g. 5.4 Continue heating the crucible until the oil is oxidized to a black char and transfer to a muffle furnace. Heat at 550 to 650"C for 1 h. Remove from the furnace, cool slightly, place in a desiccator, and cool to room temperature. Weigh and repeat heating in the furnace to constant weight (within 0.1 mg). 6. Calculation 6.1 Calculate the ash content. A, of the sample as follows: A, % = (R/Sj x 100 249 DUP050295914 or, A, ppm = (R/S) x 1 000 000 where: R = residue (5.4), g, and S = sample used, g. # D 1951 I 7. Precision and Bias 7.1 Precision and bias were not established at the time this ^ test method was written. An effort is being made to obtain * the precision and, if obtainable, it will be published in future revisions, tins method has been in use for many years, and its usefulness has been well established. The American Society for Testing and Materials takes no position respecting the validity ol any patent'rlghts asserted in connection with any Item mentioned in this standard. Users of this standard afe 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 ior additional standards and shoutct be addressed to ASTM Headquarters: Your comments wiii receive careful consideration at a meeting ol the responsible technicaicommiltee, which you may attend. If you fegl 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. *1 i ii 250 DUP050295915 Designation: D 1952 - 86 (Reapproved 1990) Standard Test Method for Quantitative Determination of Break in Drying Oils1 P| This standard is issued under the fixed designation; D 1952; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A Superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedJbr use by agencies ofthe Department ofDefense to replace Method 5161 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. lte I This test method covers the quantitative determinapfbreak in drying oils. This test method is applicable to ihd refined drying or fatty oils that have not been initially polymerized, oxidized, or chemically modified, jpr/us standard does not purport to address all of the %problems associated with its use. It is the responsibility moever uses this standard to consult and establish Wrriate safety and health practices and determine the of regulatory limitations prior to' use, Specific 1 statements are given in Section 8. . ieferenced Document l ASTM Standard: * 1 Specification for ASTM Thermometers2 of Term Specific to This Standard i break--in drying oils, that material rendered insoluble Ip an oil is heated to polymerization or varnish-making eratures. l^nmmary of Method 11.1 The oil under test is treated with hydrochloric acid Uted to 290C, allowed to cool, diluted with carbon achloride, and the resulting insoluble break is separated [ weighed. Significance and Use |5.1 This test method provides a quantitative determina|n of the. amount of non-oil material that will become oluble when the oil is heated. Break is not significant cept in oils that are to be heated, as in manufacture of lishes and alkyd resins. This test method is not applicable polymerized, oxidized, or chemically modified oils. The is rendered insoluble in the oil by the addition of |ydrochloric acid and heating to a specified temperature. nee the temperature must be specified, the results are Empirical. . Apparatus 6.1 Beaker, 100-mL capacity, tail-form. 6.2; Thermometer--An ASTM Open Flash Thermometer having a range from -6 to +400C and conforming to the requirements for Thermometer 11C as prescribed in Specifi cation El. 6.3 Filtering Crucible, porcelain bitumen-type, with top diameter of44 mm and depth of 25 mm prepared by matting with medium fiber asbestos (Warning--See 8.1), drying to constant weight (within 0.1 mg) at 105C, and cooling in a desiccator. 7. Reagents and Materials 7. i 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. 7.2 Carbon Tetrachloride (CCL,) (Warning--See 8.3). 7.3 Filter Aid--Diatomaceous silica4 dried at 105CC and stored in a desiccator. 7.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1) (Warning--See 8.2). 8. Hazards 8.1 Asbestos--Inhalation of asbestos fiber or dust has been found to be a cause of asbestosis and lung cancer. Handle dry asbestos in a suitable hood. Prewetting of asbestos with water or solvent can help reduce the concen tration of airborne particles. Use of a particulate filter face mask is recommended. See supplier's Material Safety Data Sheet for proper handling procedures. 8.2 Hydrochloric Acid--Concentrated hydrochloric acid is corrosive and may cause bums to the skin and eyes; the vapor is irritating to mucous membranes. Avoid contact with skin and eyes. Wash clothing before reuse. See supplier's Material Safety Data Sheet. 8.3 Carbon Tetrachloride is a very hazardous liquid. It is absorbed by the skin. Its vapor is hazardous through inhala tion. It is an irritant to skin and eyes; avoid breathing 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 D01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 1952-61. Last previous edition D 1952-61 <1984)*'. 2 Annual Book ofASTM Standards, Vote 05.03 and 14.03. 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 Nosuand Co., Inc., New York, NY, and the "United States Pharmacopeia." 4 Hyflo Super-Cel, produced by Johns-Manvilie Corp., has been found satisfac tory for this purpose. 251 DUP050295916 # D 1952 (TLV-10 PPM). It causes liver and kidney damage and has cumulative effects. Use with adequate ventilation (in a hood) and wear rubber gloves. See supplier's Material Safety Data Sheet. 9. Procedure 9.1 Weigh,toOvl g, 25 g ofthe well-mixed sample into the beaker on an' analytical balance. Add 0.15 mL of HCl from a measuring pipet and stir thoroughly with the thermometer. Suspend the thermometer in -the eenter of the mixture so that the bulb is completely immersed in the liquid but not ' touching the bottom of the beaker. Apply heat (Warning, Note) so;thatthe temperature'rises to 290 in 3 to 3.5 min. After heating to 29Q?G, withdraw..the flames No t e: Warning--Do not stir the Specimen after Keating Has begun. 9.2 Cool toppom temperature; then add, whilestirring, 50 mL of CCI4 followed by 0.2 g of diatomaceous filter, aid weighed to 0..1 mg> Xllp$ 49 stand for I h,. stirring at 15-min intervals:-.' .. ?. : ; ' 9.3 Filter, with the aid of vacuum, through the porqelaiji crucible previously prepared and weighed to 0.1 mg. Wash the residue with four 15-mL portions of CCl4l using a policeman to remove any traces of solids from the "beaker; and adding each portion as soon as the previous one has drained. 9.4 Dry the crucible audits contents at 105C to constant weight (within 0.1 mg), allowing it to cool in a desiccatoi piior to. weighing: 1 10. Calculation 10.1 Calculate the percent of break, B, as follows: , . , B, % = [04 - C-m/S] x 100 Where: " ' " A = total weight of dried crucible and its contents, g, C = filter aid added, g W = weight,of crucible and asbestos mat, g, and S ,= spjsciroen weight, g. fl.; Report , 11.1 Report .the results to the second'decimal place. 1'2. Precision and'Bias ' 12.1 Cooperative results indicate, that the reproducibility ofthis test method is approxinjately.0.02 %. relative. " 12.2 Bias--Bias has not been determined. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any.item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any svph ^ patent rlghts,,and the risk oflnfringementof such rigt\tjS, are entirely thefr own responsibility. . Jhfysiandard is subject to revision at any timeby the responsible technical committee and must.be reviewed every five years and if.not revised, either reapproved drwithdrawn. Your commentsareinvited either for revision ofthis standardorfor additional standards and-should, he addressed tolASTM Headquarters. ibdf Comments wiilregeive garefut consideration at a meeting of the responsible teclmicatfioriwffl6etw^ ydu..may attend If you feel thatiyour comments have not received a fair, hearing you shout'd make your viewsknom to the ASTMCommittaeon Standards, 1916 Race St., F*hliadeiphiatPA 19103!' '' ' ' s- \ : .. -* . * - ' = \> W - r. .. *? /* v .-- , ... .* t \ : V . . ; ... >- .. * ' . '' I 252 DUP050295917 esignation: D 1954 - 86 (Reapproved 1990) Standard Test Method for Foots in Raw Linseed OH (Volumetric Method)1 This standard is issued under the fixed designation D 1954; 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 chatige since the last revision or reapproval. This lest method has been approvedfor use by agencies ofthe Department ofDefense to replace Method5162 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. e This test method covers the determination of foots in l oil. -Test Method D 1966,2 is a more reproducible method and Used in place of Test Method D 1954 upon mutual agreement n the purchaser and the seller. ; This standard does not purport to address all of the problems associated with its use. It is the responsibility jever uses this standard to consult and establish -riate safety and health practices and determine the bility of regulatory limitations'prior to use. Specific l statements are given-in Section 8. referenced Documents ,1 ASTM Standards: ]1193 Specification for Reagent Water2 ,1966 Test Method for Foots in Raw Linseed Oil (Gravimetric Method)3 -i _ ,1 Specification for ASTM Thermometers4 * Terminology .1 Definition: 3.1.1 foots--r& term that originally was used to describe *se solid impurities that precipitate from raw linseed oil mg storage and then settle to the bottom or "foot" of a ;e tank. `3.2 Description of Term Specific to This Standard:. 3.2.1 foots--a material insoluble in a mixture of equal of acetone and the oil under test, and insoluble in 'cium chloride solution, under specific conditions of the t. . Summary of Test Method 4.1 The oil to be tested is treated by mixing under defined conditions with an acid-calcium chloride solution and aceone. This mixture is allowed to settle in a graduated tube knd the foots content is determined volumetrically. 5. Significance and Use 5.1 This test method provides an empirical measure of the 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 D01.32 on Drying Oils. Current edition approved Match 21, 1986. Published May 1986. Originally published as D 1954 - 61. Last previous edition D 19 54 - 62 (1984). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.0!. 5 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 05.03 and 14.03. amount of solid impurities present in raw linseed oil. The impurities are usiially suspended in the oil. Addition of the reagents stratifies the impurities in a layer that is measured volumetrically. After addition of' the reagents, a period of time is provided to allow the impurities to stratify. The test method is empirical since the volume of the impurity stratum will increase over a period of time due to the hydration of the impurities. - 5.2 After heating a sample of the oil to 65C, it is divided into two parts. One part is cooled to about 25C and the other to 0C before the test is run. The test results run on the two samples are known as the heated foots and chilled foots respectively. 6. Apparatus 6:1 Beakers, 150-niL, made of chemically resistant glass. 6.2 Thermometer--An ASTM Partial Immersion Ther mometer having a range from -20 to +150C and con forming to the requirements for Thermometer 1C as pre scribed in Specification E 1. ' 6.3 Sample Bottles, 2-oz (60-mL). 6.4 Graduated Cylinders, 10 and 25-mL. 6.5 Graduated Tube--A buret or color comparison tube, having an internal diameter of 10 to 15 mm, and a capacity of not less than 70 mL. The graduations in 0.1-mL should extend at least from 10 to 50 mL above the bottom of the tube. . . 6.6 Water Bath, capable of being maintained at 25 0.5C. . ' 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 conforming to Type I of Specification D 1193. 7.3 Acetone. (Warning--See 8.1) * "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." 253 DUP050295918 r r r # D 1954 7.4 Acid-Calcium Chloride Solution--Dissolve 600 g of calcium chloride (CaCl2) or 800 g of CaCla-2H20 in a mixture of 80 mL of concentrated hydrochloric acid (HC1, sp gr 1.19) (Warning--see 8.2) and 500 mL of water. Dilute to 1 L and mix. Filter if not clear. 8. Hazards 8.1 Acetone is a flammable liquid. Harmful ifinhaled, use only with adequate ventilation. Avoid prolonged contact with skin or any contact with the eyes. See supplier's Material Safety Data Sheet. 8.2 Hydrochloric Acid--Concentrated hydrochloric acid is corrosive and may cause burns to the skin and eyes; the vapor is irritating to mucous membranes. Avoid contact with skin and eyes. Wash clothing before reuse. See supplier's Material Safety Data Sheet. 9. Preparation of Oil 9.1 Place 75 g of the oil in a 150-mL beaker, heat to 65C, and maintain at 65 1C for 10 min. At the end of the 10-min period, divide it into two equal portions by pouring one half into a clean, dry, 2-oz (60-mL) bottle. Stopper the 2-oz bottle and cool immediately as described in 10.2. 10. Procedure 10.1 Determination ofHeated Foots--Allow the oil in the beaker (Section 9) to cool to a temperature of 20 to 27C and maintain at this, temperature for 30 min. Measure 25 mL of the prepared oil into a graduate and at the same time measure out 25 mL of acetone and 10 mL of the acid-CaCl2 solution. All materials should be at 20 to 27C. Pour the oil into the graduated tube. Rinse the graduate used for oil measurement with the acetone. Transfer the acetone rinses and the acid-CaCl2 solution into the graduated tube. Stopper the tube. Mix for I min by completely inverting and1, reinverting the tube ten to twelve times. Clamp the tube in a vertical position and allow to stand 24 h at 25 0.5'c. Determine the volume of the stratum lying between the clear CaCl2 solution and the clear acetone and oil mixture to 0,1 mL. 'i 10.2 Determination of Chilled Foots--Place the 2-oz (60-* mL) bottle in an ice water bath (0C) for 2 h. Then place it in < a constant-temperature bath at 25 0.5C for 30 min. Continue as described in 10.1. 11. Calculation 11.1 Multiply the volume of the intermediate strata (10.1 and 10.2) by four to obtain the percent of heated and chilled foots. 12. Report 12.1 Report the results to the first decimal place. f 13. Precision f 13.1 The precisionof theheated foots andchilled foots test methods hasnever been formally adopted from a statistical analysis of historical cooperative tests by ASTM members. A 1961 examination of ASTM results published in 1927 shows: (1) Heated foots: 66 % coefficient of variation between observers, and (2) Chilled foots: 35 % coefficient of variation between , observers. i" 13.2 These very wide coefficients were calculated from single observations by seven observers, on each of six samples, of oil. Values reported ranged from 0.0 to 0.2 % heated foots and 0.4 to 2.6 chilled foots in the cleanest sample, to 3.3 to 17.2 % heated foots and 9.6 to 20.0 % chilled foots in the dirtiest sample of oil. 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 ofthis standard or toradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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 Sf., Philadelphia, PA 19103. 254 DUP050295919 Designation: D 1955 - 85 (Reapproved 1989)'ei Standard Test Method for Gel Time of Drying Oils1 This standard is issued under the fixed designation D 1955; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4441 cfFederal Test Method StandardNo. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. No t e--Editorial changes were made throughout in OctpbeM989. This test method covers the deteftriination of the gel of tang oil, oitidca oil, and, with modification of rature, other oils having gelling characteristics. This standard may involve hazardous materiab, oper5 and equipment. This standard does not purport to ~s all ofthe safetyproblems associated with,its use. Itis isponsibility of the user of this standard to establish note safety and health practices and determine the ability ofregulatory limitations prior to use. "erenced Document ASTM Standard: ;1 Specification for ASTM Thermometers2 rminology Definition: .1 gel time, of a drying oil---the time required for the form a solid gel under specified conditions of temper- --S 5ml of I j Sample --A -'D nificance and Use _ The gel time of an oil at elevated temperature is an Cation of its drying characteristics. Oils that have a high ee of unsaturation are classed as drying oils. Oils in % a high percentage of this unsaturation is conjugated the fastest. .2 At elevated temperatures, the conjugated oils will a a gel; therefore this test method can be used to detect iteration in highly conjugated oils such as tung and cica oil, whereas unconjugated oils do not show a sharp point. The method is empirical in nature since the gel e must be compared to a known standard. 'Apparatus 5.1 The apparatus shall be assembled as shown in Fig. 1 d shall consist of the following: :l This test method is under the jurisdiction ofASTM Committee D-t on Paint d Related Coatings and Materials and is the direct responsibility of Subcom- D0I.32 on Drying Oils. 'Approved May 31, 1985. Published July 1985. Originally published as 1955 - 58 to replace Sections 45-51 of D 555 - 58. Last previous edition 1955 - 61(1984). 2 Annual Book ofASTM Standards, Vols 05.03 and 14.03. A-- 1000-mL, tatt-form beaker, 90 mm in diameter by 190 mm In height B-- support plate about 65 mm in width, made of monel metal, aluminum, or stainless steel C--test tubes, 150 mm by 16 mm, with cork stoppers D--5 mL of reference standard ol E-- thermometer, range 90 to 370C F-- glass rods 3 mm in diameter G--guide to prevent cover from slipping FIG. 1 Apparatus for Gel Time Test 5.1.1 Bath--A 1000-mL, tall-fonn beaker, containing a hydrogenated oil or other suitable liquid to a depth of 110 mm. The beaker shall be covered with a Monel, aluminum, or stainless steel support plate for test tubes and thermom eter. 5.1.2 Glass Rods, approximately 170 mm in length. 5.1.3 Test Tubes, 150 by 16 mm with a mark to designate the 5-mL level. Each tube shall be closed with a cork having a hole through which a 3-mm glass rod can move freely. 5.1.4 Thermometer--An ASTM Pensky-Martens HighRange Thermometer having a range from 90 to 370C and conforming to the requirements for Thermometer 10C as 255 DUP050295920 prescribed in Specification E i. 6. Procedure 6.1 Heat the bath to 300 PC (Notes I and 2). When the bath temperature is 300C and rising slowly, insert the tube containing 5 mL of the oil to be tested and another tube containing 5 mL of an oil ofknown behavior. Note the time, Within 2 min the bath temperature will have fallen to 288 PC (Note 3), at which point it should be maintained as closely as possible for the duration of the test. NOTE 1--The recent change in immersion and running temperature for this test was made to compensate for the change made in the type of thermometer used. It is particularly important to use the specified ASTM Thermometer IOC. No t e 2--No stirrer shall be used in the bath. A screen around the bath enables the temperature to be reached and maintained more easily. When the bath becomes discolored and viscous it should be renewed, as heating becomes irregular when a tarry and viscid state is reached. No t e 3--The test may be run.at a higher temperature for use with dehydrated castor oil and other gelling oils where the gel times at 2SSC are excessively long. The temperature of the test should be included i the report in these cases. 6.2 When the tubes have been in the bath 9 min, raise i glass rods at intervals of 15 s. Note the time when the oil' firmly set.. This is the point when the oil becomes enough that the entire tube and contents may be raised by i the rod.. Record the elapsed time for the test oil and the standard. If the standard deviates more than 30 s from the assigned value, the test should be repeated with closer' temperature control. 7. Report 7.1 Report the mean of two tests, differing by no more than 30 s, as the gel time. 8. Precision and Bias 8.1 Within laboratory standard deviation was 5 s, and between laboratories, 25 s. , 8.2 Bias has not been determined. 9. Keywords 9.1 drying oils; gel time TheAmericanSoclety for Testing and Materials takas no position respecting the validity of any patentrights asserted'in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity ofany such patent rights, end the risk of Infringement ofsuch rights, are entirety their own responsibility. Ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or for additional standards and should he addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, whloh you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1 II -. ..... 256 DUP050295921 ( Designation: D 1957 - 86 (Reapproved 1990) Standard fast Method for Hydroxyl Value of Fatty Oils and Acids1 Tins standard is issued under the fixed designation D 1957; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last'revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. test method covers the determination of the content of castpr oil, dehydrated castor oil, and ivatives. This test method may also be used, for other lucts such as fatty alcohols, mono- and diglycerides, ydroxystearic/ acid, but the precision will not neces|be as indicated. $ This standard does not purport to address all of the mproblems associated with its us?., It is the responsibility jpioever uses this standard to consult and establish safety and health practices and determine the lability of regulatory limitations prior to use. -Specific id statements are given in Section 6. llferenced Document ASTM Standard: 1(193 Specification for Reagent Water2 " ilficance and .Use 1 Hydroxyl value is important in establishing reactivity acids and isocyanates. It is also a measure ofthe degree ydration of castor oil. This test method detennines the total amount of ual hydroxyl groups present in oils and- other fatty j-containing materials, reported as hydroxyl value. i.'3 This test method involves the acetylation of hydroxyh taining fatty oils and acids using pyridine as, solvent er groups that will react with acetic anhydride such as lary and secondary amines under the conditions of the thod will be reported as hydroxyl. The hydroxyl value is ressed as milligrams of potassium hydroxide equivalent : the hydroxyl content of 1 g of the oil. A correction is lied for.acid groups present. Apparatus 4.1 Erlenmeyer Flask, 250-mL, standard ground-glassitoppered. 1.2 Condensers, straight-tube, Liebig type, haying andard ground-glass joints.. |j5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be iused 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 ences to water shall be understood to. mean reagent water conforming to Type I of Specification D 1193. 5.3 Acetic Anhydride, (Warning--See 6.5) fresh. 5.4 n-Butyl Alcohol (Warning--See 6.1), neutralized with 0.5 N alcoholic potassium hydroxide (KOH) solution to a faint pink phenolphthalein end point. 5.5 Ethyl Alcohol or Denatured Alcohol, conforming to Formula No. 3A or 30 of the U. S. Bureau of Alcohol, Tobacco, and Firearms. Formula No. 3A is a mixture of 100 parts by volume of ethanol to 5 parts by Volume of methanol; Formula 30 is 100 parts by volume of ethanol and 10 parts by volume of methanol. 5.6 Phenolphthalein Indicator - Solution (10 g/L)--Dis solve 1 g of phenolphthalein in methanol, ethanol, or isopropanol, and dilute to 100 mL. 5.7 Potassium Hydroxide, Alcoholic Solution (0.5 N) (Warning--See 6.3)--Prepare and standardize a 0.5 N solu tion of potassium hydroxide (KOH) in ethanol. The strength should be not less than 0.5 N in order that the blank titrations will take less than 50 mL to avoid refilling the buret. 5.8 Pyridine (Warning--See 6.4), distilled at 114 to 115'C. 5.9 Pyridine-Acetic Anhydride Solution (3+1)--Mix 3 volumes of pyridine with 1 volume of acetic anhydride. Prepare, fresh before using. 6. Hazards ' 6.1 n-Butyi Alcohol is a flammable liquid. The liquid and vapor are irritants to the eyes, skin and mucous membranes. Use with adequate ventilation (hood), (TLV-100 PPM). See supplier's Material Safety Data Sheet. 6.2 Ethyl Alcohol (denatured) is a flammable liquid. Liquid and vapor are harmful, the severity depending upon the concentration of the alcohol and the nature and concen tration of the denaturant. Denatured alcohol containing benzene should not be used. Do not swallow. Avoid breathing vapor and contact with skin and eyes. See suppli er's Material Safety Data Sheet. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint 1 and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D 1957 - 61 T. Last previous edition D 1957 - 63 (1984). 2 Annual Book cfASTM 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." 257 DUP050295922 # D 1957 6.3 Potassium Hydroxide and its strong solutions are caustic to the skin and eyes. Avoid all contact with skin and eyes. Remove contaminated clothing and wash before reuse. See supplier's Material Safety Data Sheet. 6.4 Pyridine is a flammable liquid and hazardous by inhalation. It is an eye, skin, and respiratory irritant (TLV-5 PPM). May cause liver and. kidney damage. Use with adequate ventilation; perform all operations in a hood. See supplier's Material Safety Data Sheet. 6.5 Acetic Anhydride is corrosive and may cause burns to the skin and eyes; the vapor is irritating to mucous mem branes. Use in a hood. Remove contaminated clothing and wash before reuse. See supplier's.Material Safety Data She,et. 7. Procedure 7.1 Weigh, to 0.1 mg into a 250-mL Erienmeyer flask, the correct amount of sample for -acetylation determined as follows: Hydroxyl Value Specimen Weight, g 0 to 20 20 to 50 50 to 100 100 to 200 10 5' 3 2 7.2 Weigh 9.0 to 11.0 g of the sample into another flask for the acid value. If the test method is being used for fatty adds, such as hydroxystearic acid, the weight should be 0.9 to 1.1 g. 7.3 Pipet 5.0 mL oftbe pyridine-acetic anhydride solution into the flask containing the specimen for acetylation. For samples having 0 to 20 hydroxyl value, add an additional 5 mL of pyridine to the flask. Thoroughly mix the contents by gentle swirling. Pipet another 5.0 mL of pyridine-acetic anhydride solution into an empty flask for the reagent. Add 10 mL of pyridine, neutralized to phenolphthalein, to the specimen for the acid value blank. Thoroughly mix the contents by gentle swirling. 7.4 Insert reflux condensers into the Erlenmeyer flasks. Place the flasks on an opening of a steam bath and heat for 1 h. By this method of heating only slight, ifany, refluxing will occur. 7.5 Add 10 mL of water through the condensers to the flasks. Heat on the steam bath for an additional 10 min with !1 reflux condensers attached. Allow the flasks to cool to room -a temperature with condensers still attached. J 7.6 Add 25 mL of neutralized n-butyl alcohol to each J flask in the following manner. About half should be added J through the condenser, the condenser removed, and the *1 remaining alcohol used to wash down the sides of the flasks. 1 Add 1 mL of phenolphthalein indicator solution to each I flask and titrate to a faint pink end point with 0.5 N alcoholic | KOH solution. 1 8. Calculation and Report | 8.1 Calculate the hydroxyl value as the number of milij- | grams of potassium hydroxide equivalent to the hydroxyl j content of 1 g of sample as follows: v i Hydroxyl yalue = ^ U j\r x 56.1 | where: - J A -- KOH solution required for titration of the acid value, | mL, V*jl B = KOH solution required for titration of the reagent | blank, mL, | C = sample used for the acid value, g, | V = KOH solution required for titration of the acetylated ,;i| specimen, mL, and ,i S = sample used for acetylation, g. | 8.2 Report the results to the first decimal place. | No t e--For routine analysis, the ethanol add value may be substi- 'i tuted in most cases for the pyridine add value, and the calculation altered accordingly. as 9. Precision and Biais | 9.1 The following criteria should be used for judging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--Duplicate results by the same open ~i ator should be considered suspect ifthey differ by more than > 2;4- ' J 9.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different 1 laboratories should be considered suspect if they differ by , more than 3.0. " 9.2 Bias--Bias has not been determined. n The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ot the validity ot any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the.responsible technical committee and must be reviewed every five years and ffnot revised, eitherreapproved or withdrawn. Yourcomments are invitedeither for revision o! thisstandard 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, if you feeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 258 DUP050295923 Designation: D 1958 - 86 (Reapproved 1990) Standard Test {Method for Chloroform insoluble Matter in Oiticica Oil1 This standard is issued under the fixed designation D 1958; 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. pe this test method covers the determination of the in oiticica oil that is insoluble in chloroform. It may iihsed for other drying oils. This standard does not purport to address all of the Problems associated with its use. It is the responsibility yver uses this standard to cqnsidt and establish :iate safety and health practiced and determine the pility ofregulatory limitations prior to use. A specific ./statement is given in Section 4. tiificance and Use Mineral contamination in oiticica or other drying oils yluble in chloroform while the natural components of il are soluble. This test method provides a means to line the degree of contamination by mineral matter. eagent Chloroform (CHC13) (Warning--See 4.1). rds .1 Chloroform is a hazardous liquid that can be absorbed is test method is under the jurisdiction of ASTM Committee D-I on Paint Slated Coatings and Materials and is the direct responsibility of Subcom; DO 1.32 on Drying Oils. rrent edition approved August 29, 1986. Published October 1986. Originally ed as D 1958 - 58. Last previous edition D 1958 - 85. through the skin. Its vapor is hazardous through inhalation. It is a narcotic. Use only with adequate ventilation (in a hood). For further information, see supplier's Material Safety Data Sheet. 5. Procedure 5.1 Dissolve 10 g of the sample in sufficient chloroform to obtain a fluid solution. Filter through a dried and weighed Godch crucible, wash with chloroform until the oil is removed. Heat the crucible and residue, if present, at 105 2C, cool, and weigh. Repeat the heating and weighing until the weight is constant to 0.1 mg. 6. Calculation 6.1 Calculate the percent of insoluble matter, /, in chloro form as follows: I = (RjS) x 100 where: R - residue, g, and S = sample used, g. 7. Precision and Bias 7.1 Precision and bias data were not established at the time this test method was written. An effort is being made to obtain the precision and, if obtainable, will be published in future revisions, This test method has been in use for many years, and its usefulness has been well established. 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 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, 7316 Pace St., Philadelphia, PA 19103. 259 DUP050295924 (jjjjj^ Designation: D 1959 - 85 (Reapproved 1989)e1 Standard Test Method for Iodine Value of Drying Oils and Fatty Acids1 This standard is issued under the fixed designation D 1959; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revisioa A number in parentheses indicates the year of lastreapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use bp agencies ofthe Department ofDefense to replace Method 5061 ofFederal Test Method Standard No. MIA. Consult tfteDoD Index ofSpecifications and Standardsfor the specific pear ofissue which has been adoptedby the Department ofDefense. ei No t e--Editorial changes were made throughout in October 1989. 1. Scope 1.1 This test method covers the Wijs procedure for. determination of unsaturation (iodine value) in drying oils. It is applicable to all natural and synthetic drying, oils and their fatty acids. 1.2 When the iodine value is determined on oils or fatty acids having conjugated systems, the result is not a measure of total unsaturation, but rather is an empirical value that affords a comparison of total unsaturation. 1.3 To obtain the total iodine value on conjugated sam ples, use Test Method D 1541. No t e 1--This test method is essentially equivalent to Test Methods D 2075 and D 2078. 1.4 Tkis standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D1541 Test Method for Total Iodine Value ofDrying Oils and Their Derivatives3 D2075 Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines3 D2078 Test Method for Iodine Value of Fatty Quarter nary Ammonium Chlorides3 3. Terminology 3.1 Definition: 3.1.1 iodine value--a measure of the unsaturation of oils and fatty acids and is expressed in terms of the number of centigrams of iodine per gram of sample (weight percent of absorbed iodine). 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 D01.32 on Drying Oils. Current edition approved May 31, 1985. Published July 1985. Originally published as D 1959-61. Last previous edition D 1959 - 69 (1984). 2 AnnuaI Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 3.1.1.1 Discussion--Total unsaturatidn of conjugated sys tems may be measured in accordance with Test Method D 1541. The Wijs iodine value method is not reliable for tall oil fatty acids containing an appreciable quantity of rosin acids. 4. Summary of Test Method ^ 4.1 The, determination of the iodine value of oils cot- j taining isolated double bonds is based on the absorption of 3 halogen under conditions selected to promote stoichiomet- 1 * rical results. 5. Significance and Use 5.1 This test method measures the unsaturation as iodine value by addition of an iodine/chlorine reagent. The amount ofreagent absorbed is determined by back titrating the excess reagent and comparing it to a blank determination. 5.2 In samples containing conjugated double bonds, the iodine value obtained is empirical since the reagent does not react stoichiometrically with conjugated unsaturation. Where no conjugation is present, the iodine value obtained isa measure of the total unsaturation. By using proper spec imen weights, the empirical values obtained are useful for comparative purposes. 6. Apparatus 6.1 Bottles--Glass-stoppered bottles or wide-mouth (Note 2) Erlenmeyer flasks of 500-mL capacity. No t e 2--Wide-mouth bottles or flasks are essential if stirring is done by mechanical means. 6.2 Pipets, 20 and 25-mL capacity. 7. Reagents 7.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise specified. Unless otherwise indicated, it is intended that all reagents shall conform to the Specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.4 Other grades may be used provided it is first * "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." 260 DU P050295925 # D 1959 ned that the reagent is of sufficiently high purity to its use without lessening the accuracy of the determi- ZPurity of Water--Unless otherwise indicated, referto water shall be understood to mean reagent water ,ruling to Type I of Specification D 1193. Acetic Acid (Glacial) (Caution--see 8.1)--Verify the ce of substances reducing permanganate as follows: 2 mL of the acid with 10 mL of water and add 0.1 mL >1 N- potassium permanganate (KMn04) solution. The color should not be entirely discharged at the end of 2 4 Carbon Tetrachloride (CClf) (Caution--See 8.2). 15 Chlorine (99.8% Cl) (Caution--see 8.3)--Comiflergrades of chlorine available in cylinders may be used, ;ded the gas is dried by passing through concentrated n'c acid (H2S04, sp gr 1.84) before passing it into the ne solution (see 7.10). Alternatively, the chlorine may be red by allowing concentrated hydrochloric acid (HCI, 1.19)40 drop onto potassium permanganate (KMn04) ato a mixture of KMn04 and manganese dioxide 02). Dry the gas thus generated by passing it through ntrated H2S04. ` .6 Potassiurh Iodide Solution (150 g/L)--Dissolve 150 g otassium iodide (KI) in water and'dilute to 1 L. ;7 Sodium Thiosulfate, Standard Solution (6.1 --Dissolve 24.8 g of stidium thiosulfate (h|a2Sj[03V5H20) water and dilute to 1 L. Standardize'against potassium hromate (K2Cr207)56' as follows: Weigh to 0.1 mg, by " erence from a weighing bottle, 0.16 to 6.22 g of K2Cr207 "t has been finely ground and then dried to constant `ght at 105 to 110C prior .to use. Place the K2Cr207 in a 0-mL flask or bottle and dissolve in 25 mL ofwater. Add mL of concentrated hydrochloric arid (HCI, sp gr 1.19) d 20 mL of KI solution, and rotate to mix. Allow to stand 5 min and then add 100 mL of water. Titrate with the _2S203 solution, while shaking constantly, until the yellow ldr has almost disappeared. Add 1 to 2 mL of starch dicator solution and continue the titration, adding the ,a2S203 solution slowly until the blue color has just `sappeared. Calculate the normality, N, of the Na2S203 as llows: . N=(A X 20..39)/C ; here: = K2Cr207 used, g, and 1 = Na2S203 solution required for titration of the K2Cr207, mL. 7.8 Starch Indicator Solution: 7.8.1 Use soluble starch that will pass the following test for sensitivity: Make a paste with 1 g of starch and a small i amount of cold water. Add, while stirring, 200 mL of boiling , water. Dilute 5 mL ofthis solution with 100 mL ofwater and add 0.05 mL of 0.1 N iodine solution. The deep blue color 5 "Analytical Reagents, ACS Specifications," Am. Chemical Soc., Washington, DC (1960). 6 National Institute of Standards and Technology Standard Reference Material No. 136 of potassium dichromate is recommended for this purpose, and should be treated as directed in the certificate ofanalysis accompanying the standard sample. produced must be discharged by 0.05 mL of 0.1 N Na2S203 solution. 7.8.2 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. If long.storage is required, keep the solution in a refrigerator at 4 to 10C (40 to 50F). Prepare fresh indicator when the end point of the titration from blue to colorless fails to be sharp. 7.9 Wijs Solution (Caution--rsee 8.4) (Note 3)--Dissolve 13.0 g of iodine in 1 L of acetic acid. Gentle heat may be necessary to promote solution. Cool and remove a small quantity (100 to 200 mL) and set aside in a cool place for future use. Pass dry chlorine gas into the iodine solution until the original titration is not quite doubled. A characteristic color change takes place in the Wijs solution when the desired amount ofchlorine has been added; this may be used to assist in judging the end point. A convenient procedure is to add a small excess of chlorine and bring back to the desired titration by addition of some of the original iodine solution that was taken out at the beginning. Determine the strength of theoriginal iodine-solution and the finished Wijs solution by titration against 0.1 N Na2S203 solution, as directed in 9.4. No t e 3--Iodine monochloride (Wijs solution) can be purchased commercially from various laboratory supply houses. The halogen ratio should be checked prior to use. The halogen ratio, that is, the ratio of iodine to chlorine, can be determined by the Graupner-AIuise method,7 as. follows: Reagents: (1) Potassium Ioddte Solution (0.04 A/)--Dry potassium iodate (KI03) for 1 hat 105 to 110C. Weigh 2.1402 g ofthe dried salt, dissolve in'water, dilute to 1 L in `a volumetric flask, and mix. (2) Hydrochloric Acid (l+l)--Dilute concentrated HCI (sp gr 1.19) with an equal volume of water. (3) Potassium Iodide Solution (150 g/L) (See 7.6). Procedure: (1) Measure 50 mL of HCI (1+1) and 50 mL of CC14 into a 500-mL iodine flask. By means ofa pipet, transfer 25.00 mL of the Wijs solution to the flask, and shake. Titrate the free iodine in the violet-colored CCL, layer With the KI03 solution to a colorless end point using vigorous shaking. (2) On a second 25.00-mL portion of the Wijs solution, determine the total halogen by adding ISO mL of water, 15 mL ofKJ solution, and titrating with standard Na2S203 solution to a starch end point. Calculation--Calculate the iodine to chlorine ratio, R, as follows: R = (V,Nt + V2N2)/(Vj W, - V2N2) where. Vl = Na^C^ solution required for total halogen, mL, N, ~ normality of Na2S203 solution, V2 = KI03 solution required for free iodine, mL, and N2 = normality of the KI03 solution. 8. Hazards 8.1 Acetic Acid, Glacial is corrosive and may cause bums to the skin and eyes. Wash clothing before reusing. See suppliers' Material Safety Data Sheet for further informa tion. 8.2 Carbon Tetrachloride is a very hazardous liquid. It is absorbed by the skin. Its vapor is hazardous through inhala- 7 Graupner, A. }., and Aluise, V. A., "A New Rapid Titration Method for Determining the Halogen Ratio of Wijs Solution and of Iodine Monochloride," Journal, Am. Oil Chemists' Soc., February 1966, p. 81. 261 DUP050295926  D 1959 tion. It is an irritant to the skin and eyes; avoid breathing (TLV-10 PPM). It causes liver and kidney damage and has cumulative effects. Use with adequate ventilation (in a hood) and wear rubber gloves. See suppliers' Material Safety Data Sheet. 8.3 Chlorine is a poisonous, strongly irritating gas. Exer cise care in dispensing chlorine from a cylinder or in manufacture of chlorine by the action of hydrochloric acid on potassium permanganate. Wijs and other similar solu tions should be prepared in a hood. For further information, see the Chlorine Manual of the Chlorine Institute8 or suppliers' Material Safety Data Sheet. 8.4 Wijs Solution iodine monochloride dissolved in gla cial acetic acid, is corrosive and may cause bums to the skin and eyes. Wash clothing before reusing. Wijs solution should not be heated above 30C as it may liberate chlorine, which is a strong, irritating gas. Wijs solution can be purchased commercially or prepared in a hood. 9. Procedure 9.1 Melt the sample if it is not already liquid (the temperature during melting and filtering should not exceed 10 to 15C above the melting point of the sample) and filter (drying oils of high viscosity should not be filtered) through filter paper to remove any solid impurities and the last traces of moisture. The sample must be absolutely dry. 9.1.1 All glassware used in this test must be absolutely clean and completely dry. 9.2 Place in a 500-mL flask or bottle, to which has been added 20 mL of CC14, an amount of sample such that there will be an excess of Wijs solution of 125 10 % for conjugated oils or fatty acids and 125 25 % for normal or nonconjugated oils or fatty acids. Specimen weights meeting this requirement are shown in Table 1. No t e 4--For dehydrated castor oil and fatty acids use a specimen weight between 0.11 to 0.13 g. 9.3 Pipet 25 mL of Wijs solution into the flask containing the specimen and also into each of at least two additional flasks to be carried through as blanks. Stopper the flasks, and swirl the flask containing the specimen to ensure an intimate mixture. Store the flask in a dark place for 1 h at a temperature of 25 5C. For conjugated oils or fatty acids such as tung, oiticica, and dehydrated castor, allow the absorption to proceed for 1 h at 25 1C. 9.4 Remove the flasks from storage and add 20 mL of KI 8 Available from Chlorine Institute, 342.Madison Ave., New York, NY 10173. Iodine Value Less than 3 3 5 10 20 40 60 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 TABLE 1 Specimen Weights t ........... Normal Oils and Fatty Adds, Conjugated Oils and 100 to 150 % Excess of Fatty Adds, 115 to 135 % Reagent, g Excess of Reagent g 10 8.46 to 10.57 5.08 to 6.35 2.54 to 3.17 0.85 to 1.59 0.64 to 0.79 0.42 to 0.53 0.32 to 0.40 0.28 to 0.35 0.25 to 0.32 0.23 to 0.29 0.21 to 0.26 0.20 to 0.24 0.18 to 0.23 0.17 to 0.21 0.16 to 0.20 0.15 to 0-19 0.14 to 0.1B 0.13 to 0.17 0.12 to 0.16 0.12 to 0.15 0.12 to 0.14 0.34 to 0.37 0.30 to 0.33 0.27 to 0.30 0.245 to 0.27 0.225 to 0.25 0.21 to 0.23 0.19 to 0.21 0.18 to 0.20 0.17 to 0.18 0.16 to 0.17 "'0.15 to 0.16 0.14 to 0.16 0.135 to, 0.15 0.13 to 0.14 0.12 to 0.135 : solution and 100 mL of water. Titrate with Na2S203 solution, adding it gradually and with constant and vigorous shaking (Note 5). Continue the titration until the yellow color has almost disappeared. Add 1 to 2 mL of starch indicator solution and continue the titration until the blue color has just disappeared. No i e 5--Mechanical stirring is very satisfactory for agitating during the addition of the Na2S203 solution. 10. Calculation 10.1 Calculate the iodine value, I, as follows: /=[(- V)N x 12.691/5 where: . V = Na2S203solution required for titration ofthe specimen, mL, : B - Na2S203 solution required for titration of the blank, mL, N - normality of the Na2S203 solution, and S = sample used, g. ' ; j i 11. Precision and Bias 11.1 Precision and bias have not been determined. 12. Keywords 12.1 drying oils; fatty acids; iodine value TheAmerican Society tor Testing and Materials takes noposition respecting the validity ofany patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised 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 fs subject to revision a( any time by the responsible technical committee and must be reviewed every live years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision 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 Pace St., Philadelphia, PA 19103. 262 DUP050295927 Designation: D 1960 - 86 (Reapproved 1990) Standard Test Method for Loss an Heating of Drying Oils1 This standard is issued under the fixed designation D1960; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use byagencies, ofthe Department ofDefense to replace Method 4461 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. pe This test method covers the determination of moisture -y other material that is volatile under the conditions ' test. It is applicable to all natural drying oils. l_For solutions of drying oils in volatile organic solvents it is ended that Test Methods D 1259 or D 1644 be used. }This standard may involve hazardous materials, oper and equipment. This standard does not purport to ps all ofthe safety problems associated with its use. It is responsibility ofwhoever uses this standard to consult and fish appropriate safety and health practices and deter' the applicability of regulatory limitations prior to use. !:1Ic hazard statements are given in Section 5. eferenced Documents 1 ASTM Standards: 1259 Test Methods for Nonvolatile Content of Resin Solutions2 1644 Test Methods for Nonvolatile Content of Var nishes3 Significance and Use .1 Drying oils may contain small amounts of residual tion solvent, moisture or other volatile adulterants that ht interfere with their use. This test method provides a is to measure the amount of volatile components at 'C. Oxidation of the oil could cause a weight gain at this mperature, and this is minimized by blanketing the specen with inert gas. 1 This test method is under thejurisdiction ofASTM Committee D-l on Paint I Related Coatings and Materials and is the direct responsibility of Subcomittee D01.32 on Drying Oils. , Current edition approved March 27, 1986. Published May 1986. Originally bjished as D 1960 - 61. Last previous edition D 1960-85. 7 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. 4. Apparatus and Materials 4.1 Air Oven, maintained at 105 2C. 4.2 Desiccator, containing efficient desiccant. 4.3 Carbon Dioxide or Nitrogen Gas, (Warning- -see 5.1) under pressure in cylinders. 5. Hazards 5.1 Carbon Dioxide and Nitrogen Gas--Gas supplied in cylinders is dangerous because of its extremely high pressure. Take care to prevent damage to cylinders, valves, and pressure regulators. Consult supplier's Material Safety Data Sheet. 6. Procedure 6.1 Weigh 10 g of sample to 0.1 mg, into a tared 50-mL flask. Heat in an air oven at 105 2C for 30 min, while passing a gentle stream of carbon dioxide or nitrogen into the neck of the flask. No t e 2--Care must be taken to keep the surface of the oil blanketed with inert gas throughout the test to prevent oxidation of the oil. 6.2 Remove the flask from the oven, cool in a desiccator, and weigh to 0.1 mg. 7. Calculation 7.1 Calculate the percent loss on heating, L, as follows: = S-R x 100 where: S = specimen weight before heating, g, and R = residue weight after heating, g. 8. Precision and Bias 8.1 Precision and bias were not established at the time this test method was written. An effort is being made to obtain the precision and, if obtainable, will be published in future revisions. This method has been in use for many years, and its usefulness has been well established. 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, eitherreapproved or withdrawn. Your comments are invited Other torrevision ofthis standard orlor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fee/ that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 263 DUP050295928 Designation: D 1962 - 85 (Reapproved 1989)1 Standard Test Method for Saponification Value of Drying Oils, Fatty Acids* and Polymerized Fatty Acids1 ; This standard is issued under the fixed designation D 1962; 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 lest method has been approvedfor use by agencies ofthe Department ofDefense to replace Method S081 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. ' ei No t e--Editorial changes were made throughout in .October 1989. 1. Scope 1.1 This test method covers the determination of the saponification value.of drying oils, bodied oils, fatty acids, and polymerized fatty acids. . ,, _ 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 1, 2. Referenced Documents 2.1 ASTM Standards: D305 Test Method for Solvent-Extractable Material in Black Pigments12 D1193 Specification for Reagent Water3 3. Terminology 3.1 Definition: 3.1.1 saponification value--& measure of the alkali reac tive groups in oils and fatty acids and is expressed as the number of milligrams of potassium hydroxide that react with 1 g of sample. 4. Significance and Use 4.1 The saponification value of oils.and fatty acids is a measure of the content of ester linkages. For an oil, provided it' is not significantly oxidized, the number of ester' linkages per molecule (for example, three in a triglyceride), Can be used to calculate the molecular weight of the oil. 4.2 A saponification value higher than normal indicates that the oil has been oxidized (blown) or chemically modi fied, for example, with other acids such as maleic, fumaric, orphthalic. 1 This test method is under the jurisdiction of ASTMCommittee D-l on Paint and Related Coatings and.Materials and is the direct-responsibility of Subcom-. mittee D01.32 on Drying Oils. Current edition approved May 31, 1985. Published July 1985. Originally published as D 1962 - 61. Last previous edition D 1962 - 67 <1984). 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4.3 Saponification value alone is not a measure of the .! quality of the oil.' 4.4 Chemically modified oils may require saponification times longer,,than 1 h for complete reaction. , 5.. Apparatus . . V* sj 5.1 Erlenmeyer Flasks, wide-mouth, alkali-resistant, 250, or 300-mL capacity. ni 5.2 Condenser.Loop. . - .. jj No t e 1--Suitable condenser loops are shown in Figs. I and 2 of Test Method D 305; ... 5.3 Steam Bath. t, 6. Reagents" `j 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 sufficiency high purity to penmt its use vtithout - 1 lessening the accuracy ofthe determination. ' ' 6.2 Purity of Wdfer---Unless otherwise indicated, refer- j erices to Water shall be understood to mean reagent water ''ij conforming to Type I of Specification D 1193. 6.3 Phenolphthalein Indicator Solution--Dissolve 1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol or ; isopropanol. I No t e 2--A "masked phenolphthalein indicator" may be used with off-color materials. Prepare by dissolving 1.6 g of phenolphthalein and 2,7 g of methylene blue in 500 ml/ of alcohol. Adjust the pH with sodium hydroxide (NaOH) or KOH solution'so that the greenish blue color is faintly tinged with purple. The color change is from green to purple when going from add to alkali. | j J | 6.4 Potassium Hydroxide, Alcoholic Solution--Place 5 to 10 g of potassium hydroxide (KOH) (Caution--see 7.1) in a 2-L flask and add 1 to 1.5 L of ethyl alcohol (95 %) or denatured alcohol conforming to Formula No. 30 or 3A of J I " "Reagent Chemicals, American Chemical Sodety Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 264 DU P050295929 S. Bureau of Alcohol, Tobacco and Firearms. Boil on ; bath under a reflux condenser for 30 to 60 min. d collect the alcohol. Dissolve 40 g of KOH in 1 L tilled alcohol, keeping the temperature below 15C ' e alkali is being dissolved/ This solution should "clear. %vlfuric or HydrochloricAcid, Standard (0.5 N)--Add ;! 15 mL of concentrated sulfuric acid (H2S04, sp gr 'Caution--see 7.2) or 45 mL of concentrated hydroacid (HQ, sp gr 1.19) (Caution--see 7.3) to about 900 t water, cool, and dilute to 1 L. Standardize against ,y standardized sodium hydroxide (NaOH) solution or r other accurate method. Potassium Hydroxide and `its strong solutions are c to the skin and eyes. Avoid all contact with skin and ;,in case of contact, immediately flush eyes for 15 min ash hands with plenty of cbld water. Call a physician, oye contaminated clothing and wash before reuse. See fliers' Material Safety Data Sheet for further informa- Suljuric Acid is corrosive to skin, eyes and mucous branes in the form of liquid,, mist, or fumes. It causes . j bums. Care should be taken to prevent the contact of acid with eyes, skin or on clothing. In making dilute ions, always add the add to water with care. In case of ct, immediately flush eyes with copious amounts of r for 15 min; flush skin with water (use shower if able); wash contaminated clothing before reuse, Imme,ly call a physician. See suppliers' Material Safety Data et. ,3 Concentrated Hydrochloric Acid is corrosive and may se bums to the skin and eyes; the vapor is irritating to ;cpus membranes. Avoid contact with skin and eyes. In of contact, wash skin and flush eyes with cold water for 15 min. Remove contaminated clothing. Call a physician. Wash clothing before reuse. See suppliers' Material Safety Data Sheet 8. Procedure 8.1 To an Erlenmeyer flask, transfer a specimen weight of such size, Weighed to 1 mg, that the back titration is 45 to 55 % of the blank. Add 25 mL of alcoholic KOH solution to the flask and to one or more additional flasks to be carried through as blanks. Place a condenser loop inside the neck of each flask and heat on the steam bath for 1 h. No t e 3--Certain synthetic oils are not completely saponified in 1 h. Run chemically modified drying oils in duplicate, using 1 and 2-h heating periods to establish completeness of saponification. If the 2-h heating gives appreciably higher results than the 1-h run, additional determinations using 4 and 6-h heating periods should be run to establish the time required for complete reaction. 8.2 Cool the solutioh, add phenoiphthalein indicator (Note 2), and titrate with 0.5 N H2S04 or HC1 until the pink color has just disappeared. 9. Calculation 9.1 Calculate the saponification number, P, as follows: P=[(B- V)Nx%.l]/S where: V -- H2S04 or HQ required for titration of the specimen, mL, B - H2S04 or HQ required for titration of the blank, mL, N -- normality of the H2S04 or HC1, and S = specimen weight, g. 10. Precision and Bias 10.1 Precision and Bias have not been determined. 11; Keywords 11.1 drying oils; fatty acids; saponification value The American Society tor Testing anti Materials takes no position respecting the validity of any patent rights asserted in connection with any Rem mentioned in this standarti. Users of this standard are expressly advised that determination of the validity of any such patent rights, anti the risk of infringement of such rights, are entirety their own responsibility. This standard Is sub/ect to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Yourcomments are Invited eitherforrevision 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 feat 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. 265 DUP050295930 Designation: D 1963 - 85 (Reapproved 1989)L'C1 Standard Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 1 This standard is issued under the fixed designation D 1963; 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. No t e--Editorial changes were made throughout in October 1989. 1. Scope 1.1 This test method covers the determination of the specific gravity of drying oils, varnishes, alkyd resins, fatty acids, and related materials. 1.2 This test method is recommended where precision is required in the determination of specific gravity, such as establishing specifications or referee work. 1..2.1 For materials with a kinematic viscosity of 40 stokes or less, use the Leach type pycnometer. 1.2.2 For materials with a viscosity in excess of 40 stokes, use the Hubbard-type pycnometer. 1.2.3 For materials that are solid or semisolid at 25C but liquid at slightly higher temperatures, use the Hubbard-type pycnometer. No t e 1--The weight per gallon cup method is satisfactory for most routine laboratory work although the precision does not equal that of the pycnometer method. The test method described herein for use with the Hubbard-type pycnometer is applicable to the weight per gallon cup method, or Test Method D 1475 may be used. No t e 2--Hydrometers also provide a rapid method for checking specific gravity and are generally satisfactory for routine control work. However, the precision of the hydrometer method is not adequate where accurate results are required. Test Method D 1298 covers the use of the hydrometer in the determination of specific gravity. Most ASTM Hydrometers (See Specification E 100) are calibrated to read specific gravity at 15.5/15.5C(60/60F). Information on sources of hydrometers calibrated at 25/25C is available at ASTM Headquarters. 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 safely 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: D1298 Test Method for Density, Relative Density (Spe cific Gravity) or API Gravity of Crude Petroleum and Liquid Petroleum Products by Hydrometer Method2 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 1.32 on Drying Oils. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 1963 - 61. Last previous edition D 1963 -74 (1984). 2 Annual Book ofASTM Standards, Vol 05.01. D1475 Test Method for Density of Paint, Varnish, Lac- M quer, and Related Products3 . E 100 Specification for ASTM Hydrometers4 3. Terminology 3.1 Definition: 3.1.1 specific gravity, of drying oils and varnishes--the ratio of the mass of a given volume of material at 25C to that of an equal volume of water at 25C, expressed as follows: Specific gravity at 25/25C ------- 4. Significance and Use 4.1 Specific gravity is a useful measure, since conversion from volume to weight, or vice versa, is often required. For this reason it should be determined with care. 4.2 Specific gravity is very sensitive to temperature, and the temperature of measurement must be controlled, or at least known, with high precision. If the specific gravity at some temperature other than the standard is required, temperature correction factors for this purpose are provided. These factors may also be used to correct die specific gravity from some other temperature to the standard 25/25C. 4.3 In addition, various procedures are outlined in this test method so that specific gravities of materials with widely II varying viscosities can be accurately measured. 4.4 Specific gravity is not a measure of the quality of the oil, and an oil that deviates slightly from the specified limits, but otherwise conforms, is usually completely satisfactory. Specific gravity increases with polymerization or oxidation in a regular manner, and for every bodied or blown oil of a given viscosity there is an appropriate specific gravity. 4.5 Determine the specific gravity in accordance with this test method, which is capable of high precision and is the referee method. If less accurate results (3 significant figures) are adequate, "weight-per-gallon" cups as described in Test Method D 1475 may be used. 5. Apparatus 5.1 Leach-Type Pycnometer--A glass pycnometer, con ical in shape and vente 1 by a side arm that has a cap with a standard-taper No. 5/12 joint. A thermometer shall be sealed in the neck by a standard-taper No. 10/18 interchangeable joint. The thermometer shall have a range from 12 to 38"C in 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 266 DUP050295931 D 1963 pivisions. Either 25 or 50-tnL capacity is satisfactory, pycnometers have also been found suitable. rJlubbard-Type Pycnometer--A glass pycnometer, or cylindrical in shape, and fitted with a ground glass 22 to 26 mm in diameter. The stopper shall have a 2.0-mm vertical hole in the center. The top of the irfhall be a plane, smooth surface. The under surface Mopper shall be concave (approximately 5 mm at the f) to let the air escape when it is inserted. The capacity i about 25 to 30 mL and the weight not more than 40 Water Bath, capable of being maintained at 25 rds vChromic Acid Cleaning Solution is based on concen|sulfuric acid that is corrosive to skin, eyes and mucous lies in the form of liquid, mist, or fumes. It causes 'i bums. Take care to prevent contact of the acid with ?skin, or clothing. In making dilute solutions, always he acid to water with care. In case of contact, immediI flush eyes with copious amounts of water for 15 min; (.'skin with water (use shower ifavailable); wash contam- clothing before reuse. Immediately call a physician. Sulfuric acid, chromic acid cleaning solution is a strong izer and should not be brought into contact with organic (glueing agents as a fire or explosion can result. Consult liter's Material Safety Data Sheets. yfalibration of Leach-Type Pycnometer Carefully clean the pycnometer by first soaking all in potassium dichromate (K2Cr207) dissolved in conated sulfuric acid (H2S04) (Caution--see 6.1) and then ing thoroughly with water. Dry the pycnometer thorily and place it with all its parts in a desiccator for at 1 h before weighing. Weigh the pycnometer with all its i to 0.1 mg. Record this weight as A. I Fill the pycnometer to overflowing (by holding on its in such a manner as to prevent the entrapment of air bbles) with cooled, just previously boiled, distilled water at bmperature of 20C. Insert the thermometer by holding I bottle 45 from the horizontal, being careful no air bbles are included. 7.3 Transfer the pycnometer to a 25C bath so that the pter in the bath will be Vi6 in. (1.5 mm) lower than the top the capillary vent tube and hold it'in the bath for proximately 1 h or until the pycnometer-thermometer has itched 25C. r.4 Carefully remove excess water from the capillary with sorbent materials, and cap immediately. Remove the ycnometer from the bath. Dry the outside of the ycnometer by wiping dry with an absorbent material. Take are not to handle the pycnometer so as to raise the bmperature markedly or leave fingerprints. Immediately eigh to 0.1 mg and record the weight as B. Calibration of Hubbard-Type Pycnometer if- 8.1 Clean and weigh the pycnometer as described in 7.1. 8.2 Fill the pycnometer with freshly boiled, distilled water : a temperature of approximately 20C. Insert the stopper, Baking care that no air bubbles are entrapped. 8.3 Immerse in the water bath at 25 0.1C to a level of Vi6 to Vs in. (1.5 to 3.2 mm) above the water until constant temperature is reached (approximately 1 h). 8.4 Seat the stopper firmly in the pycnometer and blot the water from the surface so that the level in the bore is flush with the surface. Remove the pycnometer from the bath, wipe dry with a clean cloth, and weigh immediately, re cording the mass as B. (The pycnometer may be cooled slightly before weighing to prevent loss of water through the capillary.) Calibrate until consistent results are obtained. 9. Procedure Using Leach-Type Pycnometer 9.1 Fill a clean, dry pycnometer with the material to be tested at a temperature of approximately 20C, in the same manner as described in 7.2. If necessary, centrifuge the material to remove air bubbles either before or after filling the pycnometer. 9.2 Bring the material to a temperature of 25C, dry with absorbent material moistened with toluene, and weigh as described in 7.3 and 7.4. Record the weight as C. No t e 3--When using the Leach-type pycnometer for routine work it is not necessary to bring the flask and contents to exactly 25C. The thermometer temperature can be read when the vent cap is put in place and a temperature correction applied to the calculated specific gravity. 10. Procedure Using Hubbard-Type Pycnometer 10.1 When determining specific gravity on materials that are very viscous, semisolid, or solid at 25C, use the following procedure: 10.1.1 Fill a clean, dry pycnometer one half full of the material to be tested. No t e A--Precautions must be taken to keep the material from touching the sides of the flask above the final level and to prevent the inclusion of air bubbles. It is advisable to warm the bottle before filling. 10.1.2 Permit the bottle with its contents to cool to room temperature and then weigh with the stopper. Record the weight as C. 10.1.3 Remove the pycnometer from the balance and fill it with freshly boiled distilled water of approximately 20C. Insert the stopper and place the pycnometer in the constant temperature bath for at least 30 min. At the end of this time firmly seat the stopper and then carefully blot the top of the stopper, being careful not to draw water from the stopper opening. No t e 5--When difficulty with bubble release is encountered in making the determination, refer to a procedure in which water is replaced with odorless mineral spirits.5 10.1.4 Remove the pycnometer from the bath and par tially immerse it in cold distilled water until the contents recede from the stopper opening. Wipe dry and weigh at once to 0.1 mg. Record this weight as D. 11. Calculation 11.1 Calculate the specific gravity, S, determined as de scribed in Sections ..7 through 9, where the pycnometer is completely filled with the material to be tested as follows: S = {C - A)l(B -A) 5 Ashton, H. E., "Measuring Specific Gravity of Viscous Materials," Materials. Research and Standards, Vol 1, No. 7, July 1961. 267 DU P050295932 .... ........................... j-- ---- <*" where: A = weight of pycnometer, g, B = weight of pycnometer plus water, g, C - weight of pycnometer plus material, g. 11.2 When the Leach pycnometer is used and the temper ature ofthe pycnoifaeter plus material, C, is not exactly 25C, a correction must be made using the thermal coefficient of the material tested: For most vegetable oils this is approxi mately 0.00068/C: Sc = *+ 0.00068 Y where: ^c= corrected specific gravity, X = uncorrected specific gravity, and Y = temperature difference, plus or minus, C. 11.3 Calculate the specific gravity, S, determined as de scribed in 11.1, where the pycnometer is only partially filled with the material to be tested, as,follows: S=(C-A)/[(B-A)-{D-Q] where: A = weight of empty pycnometer, g, B - weight of pycnometer plus water, g, and C = weight of pycnometer plus 'material plus water, g. 11.4 Using 0.00068 as the thermal coefficient of drying oils approximate corrections to other temperatures can be made as follows: To correct from 25/25`C to 25/15.5C, subtract 0.0018. To correct from 25/25C to 15.5/15.5C, add 0.0047. 12. Precision and Bias 12.1 Fourteen laboratories participating in the AOCS Smalley check series reported single results on six oils for a total of 84 results and a calculated standard deviation of 0.0049. 12.2 Repeatability--(95 % confidence level) Duplicate re sults by the same1 operator should be considered suspect if they differ by more than 0.0011. 12.3 Reproducibility--Single determinations made in two different laboratories should not differ by more than 0.0013. 12.4 Bias has not been determined. 13. Keywords 13.1 drying oils; resins; specific gravity; varnishes 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 cl 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 fiveyears and if not revised, eitherreapproved or withdrawn. Yourcomments 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. II you feel this your comments have not received a fair hearing you should make your views known to the ASTM Committee on Stoddards, 1916 Race St., Philadelphia, PA 19103. 268 DUP050295933 Designation: D 1964 - 85 (Reapproved 1989}' Standard Test Method for Tung Oil Quality1 This standard is issued under the fixed designation D 1964; 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'revisioh or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4442 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 No t e--Section 7 was added editorially in October 1989. ope This test method covers the determination of the of rang oil by distinguishing between pure and ated oil. The test method is not applicable to oils Jthan tijng oiL , i This standard may involve hazardous materials, oper- J| and equlpMent. This standard does. mot purport to jfs$ all qfthe safety problems associated with its Use. It is Responsibility of the. user of this standard, to establish1 ' oridte safety and-health practices - and determine the ability ofregulatory limitations prior !to use. ferenced Document Jl ASTM Standard: ' '', pi Specification for ASTM Thermometers2 Significance and Use 111 Since tung oil contains a high degree of conjugated saturation, it will form a dry gel when subjected to feted temperatures. for a relatively short time. This test *%od is desighda to delect adulteration oftung oil with less jugated oils, since an adulterated tung oil will require a 6iger gel time and will give a gel that is soft and sticky. fi3.2 This test method is extremely temperature sensitive therefore the temperature must. be accurately controlled. Apparatus yi.l Casserole--An ordinary vitreous-enameled iron caspole having a bottom diameter of 3 in. (75 mm). j. 1 This test method is under the jurisdiction of ASTM Committee D- l ou Paint pid Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.32 on Drying Oils. Current edition approved May 31, 198S. Published July 1985. Originally Spuhlished as D 1964 - 61 to replace Sections 52-55 of D 555 - 58. Last previous e<jitionD.1964 - 61 (1984). ' 2 Annual Book pfASTM Standards, Vols 05.03 and 14.03. 4.2 Tripod, wide-flange, with a 3-in. (75-mm) opening. No t e--The object of the flange is to prevent supeiheating of the sides of the casserole. 4.3 Thermometer--An ASTM Low .Distillation Ther mometer havinga range from -2 to 300C and conforming to the requirements for Thermometer 7C as prescribed in Specification E 1. 5. Procedure 5.1 Weigh 150 g of the oil into the casserole and heat so that the temperature reaches 282C in 4 min 30 s while stirring with the thermometer. Turn down the flame and maintain the temperature at 282 1C. Stir with the thermometer until, on lifting the thermometer, the oil drops with a pronounced string, showing that polymerization has started. The time required after reaching 282 1C until the string is. noted is the time of the heat test. For pure tung oils this will not exceed 8 min. 5.2 As soon as the oil strings, fum off the . flame and remove the thermometer. Stir with a stiffspatula until the oil is solid. After stringing, a pure tung oil will require not over 40 s to become solid. 5.3 When the oil has solidified, allow to stand exactly 1 min. Turn out upside down on clean paper and cut at once with a clean spatula. Pure tung oil gives a gel that is dry, not adhering to the spatula when cut. It is firm, crumbling under pressure of the spatula, without sticking. The crumbs .should have an appearance like dry bread crumbs. Adulterated tung oil gives a gel that is soft and sticky and does noi crumble. 6. Precision and Bias 6.1 Precision and bias data were riot established at the time -this test method was written. This test method has been in use for many years and its usefulness has been well established. 7. Keywords 7.1 tung oil 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 patentrights, and the risk of infringement of such rights, are entirely their own responsibility. t This standard is subject to revision at any time by the responsible technical committee andmust.be reviewed every five years and Ifnot revised, either reapproved orwithdrawn. Yourcomments are invited either forrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you May attend.` If you feel that your comments have not received a fair hearing you should make your views knbwn to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 269 DUP0502 95934 01965 t its use without lessening the accuracy of the determi- Purity of Water--Unless otherwise indicated, referto water shall be understood to mean reagent water Eforming to Type II of Spedficatipn D 1193. B Ethyl Alcohol, Neutral (95 %)--Use 95 % ethyl al ii or neutral denatured alcohol conforming to Formula |30 or 3A of the U. S. Bureau of Alcohol, Tobacco and ns. Boil and neutralize to the phenolphthalein fend t with alkali just before using. j'4 Ethyl Alcohol (1 + 9)--Mix 1 volume of alcohol storming to 5.3 with 9 volumes of water. i5 Phenolphthalein Indicator Solution (10 g/L) (Note ^Dissolve 1 g ofphenolphthalein in 100 mL ethanol (6.3), hand, or isopropanol. |6t e 2--A "masked phenolphthalein indicator" may be used with materials. Prepare by dissolving 1.6 g of phenolphthalein and |g of methylene blue in 500 mL of denatured alcohol conforming to Adjust the pH with sodium hydroxide (NaOH) or potassium oxide (KOH) solution so that the greenish-blue color is faintly I with purple. The color change is from green to purple when going I acid to alkaline. (5.6 Petroleum Ether conforming to the requirements i in Methods D 460. <fpTE 3--Petroleum ether conforming to the requirements of AOCS fication H 2-41 also meets these requirements. |6.7 Potassium Hydroxide Solution (50 %)--Dissolve posium hydroxide (KOH) in an equal weight of water. f6.8 Sodium Hydroxide, Standard Solution (0.02 N)-- asfer 40 mL of.0.5 N sodium hydroxide (NaOH) solution a 1-L volumetric flask. Adjust to volume with recently Idled and cooled water. Standardize by titrating against potassium acid phthalate, using phenolphthalein indicator elution. Sampling 7.1 The sampling of the material and sample preparation ad handling shall be in accordance with Test Method > 1466. |fl. Procedure 8.1 Transfer about 5 g of the well-mixed sample, weighed Jto 10 mg, to an Erlepmeyer or Soxhlet flask. Add 30 mL of jplcohol and 5 mL of KOH solution. Boil gently but steadily funder a reflux condenser for a minimum of 1 h and until 1 completely saponified. Complete saponification is essential. 8.2 Transfer to the extraction cylinder and wash to the 40-mL mark with alcohol. Complete the transfer with warm and then cold water until the total volume is 80 mL. Wash out the flask with a little petroleum ether and add to the cylinder. Cool the cylinder and contents to room tempera ture (20 to 25*Q and then add 50 mL of petroleum ether. 8.3 Insert the stopper and shake vigorously for at least l. min and allow to settle until both layers are clear. Use a glass siphon to remove the upper layer as completely as possible without including any of the lower portion. 8.4 Draw the petroleum ether fraction into a 500-mL separately funnel containing 5 mL of ethyl alcohol (1 + 9) in order to minimize the possibility of leakage of petroleum ether. 8.5 Repeat the extraction at least six mbre times using 50-mL portions of petroleum ether each time, and, shaking vigorously with each extraction. No t e 4--There are some cases in which seven extractions may not be sufficient. This is best judged by making another extraction and evaporating this separately. Extraction should be discontinued when a single extraction shows less than 5 mg of residue. 8.6 Wash the combined extracts in a separatory funnel with 25-mL portions of alcohol (1 + 9), shaking vigorously and drawing off the alcohol layer after each wash. Discon tinue washing when the wash solution is neutral to phenolphthalein. Be careful not to remove any of the ether layer. 8.7 Transfer the ether extract to a tared beaker and evaporate to dryness on a water bath under a gentle stream of clean, dry air. Complete the drying to a weight constant to 1 mg, preferably in a vacuum oven at 75 to 80C and an internal pressure ofnot more than 200 mm of mercury, or in an air oven at 105C for 15-min intervals. Cool in a desiccator and weigh. 8.8 After weighing, take up the residue in 50 mL of warm (about 50C) ethyl alcohol (95 %) containing approximately 1 mL of indicator solution and previously neutralized to a faint pink color. Titrate with 0.02 N NaOH solution to the same color. 9. Calculation 9.1 Calculate the percent of unsaponifiable matter, M, as follows: A -- VNx 0.282 M, % = P - A)/S] X 100 where: A = fatty acids in the extract, g, V -- volume of NaOH solution required for titration of the fatty acids (see 8.8), mL, N= normality of the NaOH solution, R = residue (see 8.7), g, and S = specimen weight, g. 10. Precision and Bias 10.1 Precision and bias were not established at the time this test method was written. An effort is being made to assemble this information and if obtainable it will be published in future revisions. This test method has been in use for many years and its usefulness has been well es tablished. 11. Keywords: 11.1 drying oils; fatty acids; unsaponifiable matter 271 DU P0502 95935 D 1965 ' 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 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 ifhoirevised, hither reapproved or Withdrawn. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters.1 Your comments will receive careful consideration-at a meeting of the responsible technical committee, which you may attend, It you feel that your comments'have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1! 272' DUP050295936 Designation: D 1966 - 69 (Reapproved 1991).'61 Standard Test Method for Foots in Raw Linseed Oil (Gravimetric Method)1 This standard is issued under the fixed designation O 1966; 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 editorialchange since the last revision or reapproval. <1NotE--Keywords were added editorially in August 1991. This method covers the determination of foots in raw led oil by the , gravimetric method. The procedure is fonly known in Europe as the PAT foots method. ; This standard does not purport to address all of the, 11,problems, if any,, associated with its use. It is the mibility of the user ofthis standard to establish approsafety and health practices and determine the applioaofregulatory limitations prior to use.. Referenced Document 11 ASTM Standards 11193 Specification for Reagent Water2 Summary .of Test Method 13.1 The oil to be tested is refined with 85 % phosphoric |d The precipitated material is settled by centrifuging and thed free of oil with acetone. It is dried and weighed to mine the foots content gravimetrically. Terminology fM.l Definition: ' iji.1.1 foots--those solid impurities that precipitate from ' linseed oil during storage and which then settle to the bttom or "foot" of a storage tank. 4.2 Description of Term: 4.2.1 foots--in this method, the material that is precipiated from the oil by phosphoric acid and which is insoluble ii acetone under the specific conditions of the test. speeds; a slow speed of 16 2 rpm and a fast speed of 32 2 rpm. 5.3 Centrifuge Tube, pear-shaped conforming to dimen sions given in Fig. 1, and made ofthoroughly annealed glass,, The graduations, numbered as shown in Fig. 1, shall be clear and distinct and the mouth shall be constricted in shape for closure with a stopper. 5.4 Centrifuge--Capable of whirling two or more filled tubes at a speed that can be controlled to . give a relative centrifugal force of between 500 to 800 g at the tip of the tubes. Calculate the speed of the rotating head as follows: . rpm = 265 Vrcf/d where: ref = relative centrifugal force, g, and d - diameter of swng, in., measured between tips of opposite tubes when in rotating position. 5.4.1 If d is given in millimetres, use the following equation: . rpm -- 1346 dref/d No t e 1--A list'of applicable rotational speeds is given in Table 1. 5.5 Pipet, 1-mL measuring type graduated in 0.01-mL subdivisions. 5.6 Desiccator, containing an efficient desiccant. Anhy drous calcium sulfate is satisfactory. 6. Reagents 6.1 Purity ofReagents- -Reagent grade chemicals shall be Apparatus 5.1 Fritted Glass Filtering Crucibles, having a medium porosity (10 to 15 |xm) and a capacity of 30 mL. 5.2 Agitator--The agitator shall consist of a horizontal shaft suitably supported and fitted with clamps or a clamping device for holding pear-shaped centrifuge tubes. The tubes shall be held in such fashion that when the shaft rotates, the tubes will be tipped end over end, thus allowing the liquid content ofthe tube to mix as it flows from one end oftube to the other. The shaft shall be rotated mechanically by any means desired that allows one to choose either of two fixed 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 D01.32 on Drying Oils. Current edition effective Oct. 3, 1969. Originally issued 1964. Replaces D 1966 - 64 T. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 273 FIG. 1 Pear-Shaped Centrifuge Tube DUP050295937 TABLE 1 Rotational Speeds Applicable for Centrifuges of Various Diameters of Swing the oil and the tip of the tube empties of oil at each revolution. A speed of 16 r/m is adequate when using the Diameter In. (mm) 12(305) 13(330) 14(356) 15(381) 16(407) 17(432) 18(458) 19(483) 20(508) 21(533) 22(560) 23(584) 24(610) rpm at 500 ref 1710 1650 1590 1530 1480 1440 1400 1360 1330 1300 1270 1240 1210 rpm at 800 ref 2160 2080 2000 1930 1870 1820 1770 1720 1680 1640 1600 1560 1530 above agitator. Adjust the speed of the agitator so tha intimate mixing without separation takes place; 32 rpm is satisfactory. Mix at this rate for 25 min. 9.4 Place the tube in the centrifuge and spin for 1 h with a relative centrifugal force of at least 500 g at the tip or until the deposit stays in position as a compact mass when the tube is inverted. The temperature should be maintained at approximately 25C. This may be accomplished by admitting air to the centrifuge casing. 9.5 Decant or siphon the supernatant oil as completely as possible into a clean centrifuge tube and allow time for drainage. Ifthe foots layer is liquid, extra care must be taken 1 8 1 1 I f ^ to remove the oil without disturbing the foots layer A j used in all tests. Unless otherwise indicated, it. is intended modified siphon can be used to advantage. that all reagents shall conform to the specifications of the 9.6 Add 25 mL of acetone to the precipitate in the first | Committee on Analytical Reagents of the American Chem tube and mix until the gummy material is dispersed. Use a ical Society, where such specifications are available.3 Other wire to loosen them from the tip of the tube if necessary. grades may be used, provided it is first ascertained that the Dilute to 100 mL with more acetone and shake. f reagent is of sufficiently high purity to permit its use without 9.7 Prepare fritted glass crucibles as follows: Add 0.3 tp ^ lessening the accuracy of the determination, 0.6 g of diatomaceous silica to the empty crucible. With I i 6.2 Purity of Water--Unless otherwise indicated, refer- experience this can roughly be measured on the tip of a | S ences to water shall be understood to mean reagent water spatula. Slurry with approximately 15 mL of acetone, f | conforming to Type II of Specification D 1193. ! 6.3 Acetone. I 6.4 Filter Aid, diatomaceous silica.4 Remove the acetone by applying a vacuum to the filter. Dry the crucible in an oven at 100 5C for 1 h or to constant weight (0.01 mg). Cool for 1 h in a desiccator and weigh to j t 1 6.5 Phosphoric Acid (85 %) (H3P04). the fourth decimal place. Store prepared crucibles in a \ 7. Hazard 7.1 This standard may involve the use of hazardous materials, operations, and equipment. It is the responsibility of whoever uses this standard to establish appropriate safety practices to determine the applicability of regulatory limita tions prior to use. desiccator until they are to be used. 9.8 Filter the mixture prepared in accordance with 7.6 through a weighed, fritted glass crucible. Use a moderate vacuum and always maintain some acetone in the crucible. Thoroughly wash the centrifuge tube and precipitate on the filter with four, 15-mL portions ofacetone. Since oil tends to creep up the sides of the crucible care must be exercised. A wash bottle containing acetone should be used to ensure J | f | 8. Preparation of Sample thorough washing of the centrifuge tube and crucible. After the crucible is exhausted of acetone, dry it at 100C,.cool to I 8.1 Allow the sample to come to room temperature (25 room temperature in the desiccator, and weigh to nearest 0.1 i 1C) and shake or mix thoroughly. Be sure that all sediment mg. has been thoroughly dispersed. If the oil is damp, dry by heating at 100C under vacuum or by sparging with dry No t e 2--The fritted glass filters must be cleaned periodically with cleaning solution. It is well to test the filtration rate of each crucible with carbon dioxide or nitrogen at 100C, cool the oil to 25C, pure acetone and then to discard any that cannot be cleaned to give and proceed with test. satisfactory rates. 9. Procedure 9.9 Treat the supernatant oil obtained in 9.5 with a second portion of phosphoric acid in accordance with 9.1 to 9.1 Weigh into the centrifuge tube 50.0 0.01 g of the 9.8. j sample and then add 0.5 0.05 mL of phosphoric acid (85 %) with a pipet. 10. Calculation 9.2 Stopper the tube and tilt it so that the acid runs out of 10.1 Calculate the percent of gravimetric foots as follows: the tip and into the oil. Shake vigorously for a few seconds. Gravimetric foots, % -- 2(A + B) Repeat the tilting and shaking twice more. 9.3 Place the tube on the agitator and mix for 5 min at such a speed that the acid dispenses completely throughout where: A -- weight of sediment from 50 g of original oil on first phosphoric treatment, g, and B = weight of sediment from 50 g of supernatant oil on 3 "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,, lnc,, New York, N. Y,, and the "United States Pharmacopeia." 4 Hyflo Super-Cel, produced by Jolans-Manville Corp. has been found satisfac tory for this purpose. second phosphoric treatment, g. 11. Report 11.1 Report the results to the second decimal place. 12. Precision 12.1 At the 95 % confidence level, assays run in the same 274 DUP050295938 it* D 1966 IJtory should not differ by more than 0.017 %. Assays jin two different laboratories, each of which is the mean jjto determinations, should not differ by more than 13. Keywords 13.1 foots; linseed oil The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent,rights, and the risk of Infringement of such rights, are entirely their cmn responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if notrevised, either reapproved or withdrawn. Yourcomments are Invitedeither for revision ofthis standard or for additional standards and should be addressee1 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. 275 DU P050295939 4KR Designation: D 1967 - 86 (Reapproved 1990) Standard Test Method for Measuring Color After Heating of Drying Oils1 * . . -' - This standard is issued under the fixed designation D 1967; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon () indicates an editorial change since the fast revision or reapprovai. j .;i :i if 1 1. Scope 1. i This test method covers the measurement of the color of drying oils after heating under specified conditions. 1.2 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility qf whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 4. Apparatus .. 1 4, V Heater1*--A high-temperature gas burner or other ; suitable gas burner. 4.2 Thermometer--An ASTM Partial Immersion Ther mometer having a range from 20 to 760F (-5 to +400"C) and conforming to the requirements for Thermometer 3F (3C) as prescribed in Specification El. ; 4.3 Color Standards--A set of permanent color standards as described in Test Method D 1544. 2. Referenced Documents 2.1 ASTM Standards: >1544 Test Method for Color of Transparent Liquids (Gardner Color Scaled E 1 Specification for ASTM Thermometers3 276 3. Significance and Use 3.1 When oil is heated to polymerization temperature, soine darkening may occur rendering the oil unsuitable for use where light coloris essential. Excessive darkening may be an indication of residual soap content from the alkali refining process rendering the oil unsuitable for use where light color is essential. 3.2 Some oils that are low in soap content may actually bleach when heated to polymerization temperature, which is beneficial. 3.3 This test method is indicative of the color developed when the oil is heated to polymerization temperatures. 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.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally published as D1967 - 66 T. Last previous edition D1967 - 85. 1 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 5. Procedure 5.1 Place 100 mL of the oil sample in a 250-mL heatresistant Griffin low-form beaker on a ring stand with an asbestos wire pad. Immerse the thermometer in the center of the oil so that the end of the bulb is from 'A to 5/i6 in. (6 to 8 mm) from the bottom of the beaker. Heat to 550F (288"C) in 5 to 10 min, and hold at this temperature 5F (3C) for 5 min. Remove the beaker from the stand and allow to cool to room temperature. Determine the color of the sample in accordance with Test Method D 1544. 6. Precision and Bias 6.1 The following criteria should be used forjudging the acceptability of results at the 95 % confidence level. 6.1.1 Repeatability--Duplicate results by the same oper ator should be considered suspect ifthey differ by more than one-third color unit. 6.1.2 Reproducibility--Two results obtained in different laboratories should be considered suspect if they differ by more than two-thirds color unit. No t e--These precision statements are based on results obtained in a collaborative study involving six laboratories with two operators in each laboratory and four samples of drying oils. 6.2 Bias--Bias has not been determined. 4 The Fisher heater has been found satisfactory for this purpose. 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 ofwithdrawn. Your comments areInvited eitherfor revision ofthis standardorfor additionalstandards and should be addressed to ASTM 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 notreceived a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 276 DUP0502 95940 Designation: D1969 - 91 Standard Specification for 2-Ethylhexanol (Synthetic)1 This standard.is.issued under.the fixed designation.D 1969; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of lastRevision. A number in parentheses indicates the year of last reapprovaL A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ope This specification covers regular and monomer grade ylhexanol. : For specific hazard information and guidance, see the ier's Material Safety Data Sheet for materials listed in specification. -ferenced Documents ASTM Standards: 1078 Test Method for Distillation Range of Volatile Organic Liquids2 , 2119 Test Method for Aldehydes in Styrene Monomer2 4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 4 5008 Test Method for Ethyl Methyl Pentanol and Purity "Value of 2-Ethylhexanol by Gas Chromatography2 1 Specification for ASTM Thermometers'' 300 Practice for Sampling Industrial Chemicals5 : 852 Test Methods for C4-CI3 Plasticizer Grade Alco hols5 ;.2 U.S. Federal Specifications: 1PP-C-2020 Chemicals, Liquid, Dry and Paste: Packaging 5 of6 Properties 3.1 The physical and chemical properties of 2-ethylhex; ol shall conform to the requirements specified in Table 1. % 'Sampling 4.1 The material shall be sampled in accordance with actice E 300. Test Methods: 5.1 The properties enumerated in this specification shall 1 This specification is under the jurisdiction of ASTM Committee D-01 on aint and Related Coatings and Materials and Devices and is the direct ponsibility of Subcommittee DO1.35 on Solvents, Plasticizers, and Chemical intermediates. Current edition approved May 15, 1991. Published July 1991. 1 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. 4 Annual Book ofASTM Standards, Vol 05.03 and 14.03. 5 Annual Book ofASTM Standards, Vol 06.03 and 15.05. 6 Available from Standardization Documents Order Desk, Bldg. 4 Section D, J700 Robbins Ave., Philadelphia, PA 19111-5094, ATTN: NPODS. TABLE 1 Physical and Chemical Properties of 2-Ethylhexanol Grade Monomer Grade Regular Acidity (free add as acetic add, max, weight % Apparent spedfic gravity 20/20C 25/25C Assay, weight %, min Color. Pt-Co scale, max Carbonyl (as 2-ethylhexanal), max, weight % Distillation range 760 mm Hg, C as Initial boiling point, min. Dry point, max. Distillation range Ethyl methyl pentanol, max, weight % Sulfuric acid color, Pt-Co scale, max Water, max, weight % 0.01A 0.8325 to 0.8345 0.8296 to 0.8318 99.6 6 0.06 182 186 entirely within a 2C range 0.4 20 0.10 0.01* 0.8325 to 0.8345 0.8298 to 0.8318 99.0 5 0.1 182 186 NA 0.5 30 0.10 A Equivalent to 0.093 mg of KOH per gram of sample. be determined in accordance with the following ASTM methods: 5.1.1 Acidity--Test Methods E 852. 5.1.2 Apparent Specific Gravity--Test Methods E 852 or Test Method D 4052 5.1.3 Assay--Test Method D 5008. 5.1.4 Color---Test Methods E 852. 5.1.5 Carbonyl--Test Method D 2119. Calculate the per cent aldehyde as 2-ethylhexanol in Reagent Section 6 by using 0.128 in place of 0.106. "C" is the density of specimen used. 5.1.6 Distillation Range--Test Method D 1078. Use ASTM Thermometer No. 104C. 5.1.7 Ethyl Methyl Pentanol--Test Method D 5008. 5.1.8 Sulfuric Acid Color--Test Methods E 852. 5.1.9 Water--Test Methods E 852. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keyword 7.1 2-ethylhexanol 277 DUP050295941 # D 1969 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 of Infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Yourcomments are invitedeither forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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. 278 DUP050295942 resignation: D 1980 - 87 (Reapproved 1991)61 Standard Test Method for Acid Value of Fatty Acids and Polymerized Fatty Acids1 Tbis standard is issued under the fixed designation D 1980; 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 teapprovai. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. elNOTE--Keywords were added editorially in August 1991. pe .This test method covers the determination of acid ;(a measure of the acidity or amount of free fatty acids) applicable to all fatty acids and polymerized fatty This standard does not purport to address dll of the problems, if any, associated with its use. It is the Visibility ofthe user; of this standard to establish approrsafety and health practices and determine the applicaofregulatory limitations prior to iise. ferenced Document 1 ASTM Standard: 1193 Specification for Reagent Water2 terminology :1 Definition: .1.1 acid value--the number of milligrams of potassium oxide required to neutralize the fatty acids in 1 g of pie. 'Significance and Use 4.1 Drying oils are composed primarily of triglycerides of acids, and normally contain low amounts of free fatty /ds. However they can be saponified to produce essentially 'y fatty acids. This test method is used to determine the 'dity (acid value) of the fatty adds and is therefore [icative of the amount of free fatty acids in a sample. ;4.2 This test method is not to be used as a quality luirement since it measures all acidic components and es not distinguish between fatty adds of different compo sition. 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 Sodety, where such specifications are available.3 Other 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 D01.32 on Drying Oils. Current edition approved June 26, 1987. Published August 1987. Originally published as D 1980 - 61. Last previous edition D 1980-85. 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 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 water con forming to Type II of Specification D 1193. 5.3 Ethyl Alcohol Neutral (95 %)--Use 95 % ethyl al cohol neutral denatured alcohol conforming to Formula No. 30 or No. 3A of the U.S. Bureau of Alcohol, Tobacco, and Firearms. Boil and neutralize to the phenolphthalein end point with alkali ju$t before using. 5.4 Phenolphthalein'indicator Solution (10 g/L) (Note 1)--Dissolve 1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol, or isopropanol. No t e 1--A "masked phenolphthalein indicator" may be used with off-color materials. Prepare by dissolving 1.6 g of phenolphthalein and 2.7 g of methylene blue in 500 mL ofalcohol conforming to 5.3. Adjust the pH with sodium hydroxide (NaOH) or potassium hydroxide (K.OH) solution so that the greenish-blue color is faintly tinted with purple. The color change is from green to purple when going from acid to alkaline. 5.5 Potassium Hydroxide or Sodium Hydroxide, Stan dard Solution (0.5 N): Prepare a stock concentrated solution by dissolving 560 g of potassium hydroxide (KOH) or 425 g of sodium hydroxide (NaOH) in 1 L of water. 5.5.1 Allow this 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 about 875 mL and dilute to 10 L with freshly boiled reagent water. Preserve in a stock bottle provided with a large drying tube filled with soda-lime. 5.5.2 Standardize by titrating against potassium acid phthalate (National Bureau of Standards Acid Potassium Phthalate No. 84), using phenolphthalein as indicator. This solution is approximately 0.5 Nbut instead of adjusting it to a specific value, determine the exact normality and use in the calculations. 6. Procedure 6.1 Transfer about 5 g of the sample, weighed to 1 mg to a 500-mL Erlenmeyer flask and add 75 to 100 mL of hot, ethyl alcohol. Agitation and further heating may be necessary to bring the fatty acids into complete solution. 6.2 Add 0.5 mL of the phenolphthalein indicator solution Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 279 DUP050295943 and titrate immediately, while shaking, with 0.5 iVKOH or NaOH solution to the first pink color that persists for 30 s. 7. Calculation 7 1 Calculate the acid Value as follows: ... . Aciavalu =( . )/ ... where: , V = KOH or NaOH solution required for the titration, mL, N= normality of the KOH or NaOH solution, and S = specimen weight, g. 8. Precision 8.1 On. the basis of an interlaboratory test of this test method in which two operators in four laboratories tested three samples of fatty acids the following criteria should be used for judging the acceptability of results at the 95 % confidence level: - 8.1.1 Repeatability--Two results by a single operator should be considered suspect if theydifferbymore than 2.3 in acid value. 8.1.2 Rjepwducibility--Two results, each the mean of two determinations, obtained by operators in-different laboratories should be considered suspect if they differ by more than 2.4. 9. Keywords 9.1 acid value; fatty adds i TheAmerican Society foe Testing end Materials lakes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this standard. Users cf 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 mustbe reviewed every five yea Ifnot revised, eitherreapproved or withdrawn. Yourcomments are Invited either lorrevision ofthis standard or for additional star and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting.pf the tespo technical committee, which you may attend. If you feel that.your comments have not received d'tkir hearing you should mak< views known to the ASTM Committee on Standards, ,191SPace St., Philadelphia, PA 19103. 28D DUP050295944 Designation: D 1981 - 86 (Reapproved 1990) Standard Test Method for Measuring Color After Heating of Fatty Acids1 This standard is issued under the fixed designation D 1981; 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. i>e ; i'This test method covers the measurement of the color nal fatty acids after heating under the: conditions L in the test and is applicable to all normal fatty adds. This standard does not purport to address all of the |problems associated with its use. It is the responsibility user ofthis standard to establish appropriate safety and i practices and determine the applicability ofregulatory itions prior to use. ferenced Documents ASTM Standards: Il544 Test Method for Color of Transparent Liquids (Gardner Color Scale)2 |l Spedfication for ASTM Thermometer3 Seance and Use U The color of a fatty acid is readily affected by heat and tion. Variations in degree of heat, time of heat, and to atmosphere during heating have a marked effect the color obtained; therefore, conformity to the equipfnt and procedure outlined in this test method is essential :y and predsion. Apparatus and Materials L1 Oil Bath--A 5-L stainless steel beaker equipped with a chanical stirrer and containing any fight-colored alkaliaed oil such as hydrogenated cottonseed oil, 4.2 Heat Source--Either three Tirrili burners or electric nersion heaters with suitable thermostatic control may be i. Burners or heaters shall be of sufficient capadty so that hen pladng several tubes in the bath, the bath temperature 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint jld Related Coatings and Materials and is the direct responsibility of Subcomnittee D01.32 on Drying Oils. Current edition approved March 27, 1986. Published May 1986. Originally ubJished as D 1981 -61. Last previous edition D 1981 -- 61 (1984). 2 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. J Annual Book ofASTM Standards, Vols 05.03 and 14.03. . does not drop more than 5C below the minimum bath temperature and the recovery time to reach 205C does not exceed 5 min. 4.3 Thermometer--An ASTM Partial Immersion Ther mometer, having a range from 95 to 255C, and conforming to the requirements for Thermometer 42C as prescribed in Specification El. 4.4 Tubes, 1 in. (25 mm) in diameter, 9xh in. (240 mm) in length with ground-glass joints4 (pig. 1). 4.5 Test Tube Holder (Fig. 2). 4.6 Timer, capable of registering up to 120 min. 4.7 Nitrogen--A source of nitrogen capable of being regulated to a pressure of 1 to 2 psi (7 to 14 kPa). 5. Procedure 5.1 Adjust the oil level so that the tubes will be immersed to a depth of 5 Vi in. (140 mm). Bring the bath to a temperature of 205 2C and maintain the temperature within the specified range. 5.2 If the sample to be tested is not liquid at room temperature, liquefy by heating on a water bath to a temperature not more than 20C above the melting point of the sample. Fill a clean, dry tube to a depth of 5.0 in. (127 mm) with the sample and place it in the oil bath. 5.3 Place a fitted stopper in each tube and adjust the flow of nitrogen so that the surface of the specimen is blanketed by inert gas at all times. Set the timer for 60 min if the sample has an iodine value greater than 15, or for 120 min if the sample has an iodine value of 15 or less. At the end of the applicable time remove the tubes from the bath and read the color immediately in accordance with Test Method D 1544. 6. Precision and Bias 6.1 Precision and bias were not established at the time this test method was written. An effort is being made to obtain the precision and, if obtainable, will be published in future revisions. This test method has been in use for many years and its usefulness has been well established. 4 Joints from Lab-Crest Scientific Glass Co., Div. of Fischer & Porter, East County Line Rd,, Warminster, PA J8974 have been found suitable for this purpose. 281 DU P0502 95945 # D 1981 No t e--1 in. 25.4 mm. FIG. 1 Details of Color-After-Heating Tube I ,I|!| Jflf Aluminum or Stainless Steel 3 Holes'rt" diom on 6" (Horn Bolt Circle 3 Rods /4udam 5 Long Threoded lVzM on Each End / 6-Whex hd a',t Nuls Hold Plotes 6 Holes l,/8"diam on 43/4'`diam Boll Circle 6 Holes Wdiam on 43/4"diam Bolt Circle T Holes ire" diom 'on 2" diom Bolt Circle 12 Holes 3/4" diom on 43/4,,diam Bolt Circle No t e--1 in. = 25.4 mm. 5 Lifer Stainless Sled Beaker Bottom Plata Some os Top Except as Noted FIG. 2 Tube Holder (Aluminum or Stainless Steel) for Color-After-Heating Test 282 I il. ____|_inrriiiMiiiMiiiTTnnnnrrriiniiillWTlllllllllWMMI^M DU P050295946 # D 1981 TheAmerican Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any 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 eitherforrevision 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 your views known to theASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 283 DUP050295947 Designation: D 1982 - 85 (Reapproved 1989)1 Standard Test Method for Titer of Fatty Acids1 This standard is issued under the fixed designation D 1982; the number immediately following the designation indicates theyear of original adoption or, m 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. el No t e--Editorial changes were made throughout in October 1989. 1. Scope 1.1 This test method covers the determination of the solidification (titer) point of fatty acids and is applicable to all fatty acids. 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 Standard: E 1 Specification for ASTM Thermometers2 2.2 AOCS Standard: Specification H 6-403 3. Significance and Use 3.1 Saturated fatty acids solidify at a higher temperature than unsaturated fatty acids. This test method provides a means of measuring the solidification temperature of a sample containing both unsaturated and saturated fatty acids by cooling the specimen and measuring the temperature at which solidification occurs. 3.2 Samples containing higher levels of saturated acids will have a higher titer (solidification temperature) than those with lower levels of saturated adds. 3.3 Water present in the sample will raise the titer, so provisions are made in the test method to remove traces of moisture. 4. Apparatus 4.1 Beaker, Griffin low-form, 2-L capatity. 4.2 Bottle, wide-mouth, 450-mL capacity, 190-mm height, inside diameter of neck 40 mm. 4.3 Test Tubes, 100 mm in length, 25 mm in diameter, with or without rim. These tubes may have an etched mark extending around the tube at a distance of 57 mm from the bottom to show the height to which the tube is to be filled. 1 This test method is under the jurisdiction of ASTM Committee D-l on Painl and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO!.32 on Drying Oils. Cuirent edition approved May 31, 1985. Published July 1985. Originally published as D 1982-61, replacing Sections 7-9 of D 1467 - 59 T. Last previous edition D 1982 -61 (1984)". 1 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 3 Available from American Oil Chemists' Society, 508 S. Sixth St., Champaign, IL 61820. 4.4 Stirrer, 2 to 3 mm in outside diameter, with one end bent in the form of a loop 20 mm in outside diameter. Glass, Nichrome,4 stainless steel, or Monel5 wire may be used. The upper end can be formed to accommodate hand stirring or to be attached to a mechanical stirrer. 4.5 Laboratory Thermometer, having a range from 0 to 150C. 4.6 Titer Test Thermometer--An ASTM Titer Test Thermometer having a range from -2 to +68C and conforming to the requirements for Thermometer 36C as prescribed in Specification E 1. r ' No t e 1--Thermometers conforming to the requirements for the * AOCS Titer Thermometer (AOCS Specification H 6-40) meet these requirements. 5. Procedure 5.1 Heat the sample on a hot plate to 130C to remove traces of moisture, and fill a test tube (see 4.3) to a height of 57 mm from the bottom. 5.1.1 Do not hold the sample at 130C nor reheat to this temperature more than once. If excessive moisture is present, allow the water to settle, decant the fatty acids, and then refilter and reheat. The acids must be dry and free of suspended matter. 5.2 Fill the water bath to the designated level (Fig. 1) and adjust the temperature to 15 to 20C below the expected titer point. 5.3 Place the test tube containing the fatty acids in the assembly as shown in Fig. 1. Insert the titer thermometer to the immersion mark so that it will be equidistant from the sides of the tube. 5.4 Stir with the stirring rod through a vertical distance of about 40 mm at the rate of 100 complete up-and-down motions per minute (Note 2). Start the agitation while the temperature is at least 10C above the titer point. < No t e 2--Stirring may be performed mechanically by attaching a small motor with suitable speed-reducing mechanism to the stirring rod. 5.5 Stir at the specified rate until the temperature remains constant for 30 s or begins to rise in less than a 30-s interval. Discontinue stirring immediately, remove the stirrer or raise it out of the specimen, and observe the increase in tempera ture. The titer point is the highest temperature indicated by the thermometer during this rise. 4 Nichrome is a trademark of the Driver-Hams Co. 5 Monel is a trademark of Inco Alloys Inc., 3800 Riverside Drive, P.O. Box 1958, Huntington, WV 25720, 24 DU P0502 95948 # D 1982 M-3of ' WSpecimen 'resf Tube these located atequaldis tances apart between the bottle and beaker wit! hold the <r-Wiife Mouth--* form rigid Bottle 1 /LeadShoT-\ Flat f or Weight \ Cork msm FIG. 1 iApparatus Assembly for Titer Test Precision and Bias K.1 Duplicate detehfiihsitions by the same operator should ee within 0.2C. 6,2 Bias has not been determined. 7. Keywords 7.1 fatty adds; saturated fatty acids; solidification point; titer TheAmerican Society for Testing and Materials takes rio position respecting the validity ofany patent rights asserted In connection with any Bern mentioned In this standard. Users of this standard are expressly advised that determination of the validity of anysuch patent'.rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard la subject to revision atany time by therespcnslble technical committee and must be reviewed every five years and ifnotrevised, either reapprovedor withdrawn. Your comments are invited either forrevision ofthis standard or foradditionalstandards and should be addressed to ASTM Headquarters. Yota 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 tothe ASTM Committee on Standards, 191d Baca St., Philadelphia, PA 19103. 285 DUP050295949 Designation: D 1983 - 90 An American National Standard Standard Test Method for Fatty Acid Composition by Gas-Liquid Chromatography of Methyl Esters1 This standard is issued under the fixed designation D 1983; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 7501 of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1, Scope 1.1 This test method establishes standard conditions for the separation and identification of methyl esters by gasliquid chromatography. 1.2 This test method is applicable to animal and vegetable fatty acids and oils having 8 to 24 carbon atoms. The use of the polyester liquid phase facilitates the separation of both the saturated and various unsaturated fatty acid methyl esters on the chromatogram obtained. 1.3 The conditions' specified in this`test method are not suitable for determining epoxy and oxidized fatty acids nor to fatty acids that have been polymerized. See also Test Methods D 2800 and D 3457. 1.4 This standard does no} 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: D2800 Test Method for Preparation of Methyl Esters from Oils for Determination of Fatty Acid Composition by Gas-Liquid Chromatography*2 D3457 Test Method for Preparation of Methyl Esters from Fatty Acids for Determination of Fatty Acid Composition by Gas-Liquid Chromatography2 3. Significance and Use 3.1 This test method provides, a means for identifying vegetable oils as to type by comparing to known standards. It can also be used to detect adulteration of one vegetable oil by another. 3.2 The amount or the proportion of one specific add can be used for specification purposes, for example, the amount of linolenic acid in linseed oil or the percent of linoleic acid in sunflower oil. 3.3 By measuring the amount of total eluted acids by use of an internal standard, an estimation may be made of the 3 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials, and is the direct responsibility of Subcommittee DO 1.32 on Drying Oils. Current edition approved May 25, 1990. Published July 1990. Originally published as D 1983 - 64 T. Last previous edition D 1983 -75(1980)ei. 2 Annual Book ofASTM Standards, Vol 06.03. amount of polymerization of the fatty acids present in a I polymerized oil. ;.i 4. Apparatus j 4.1 Gas Chromatographic Instrument having the fob ,j lowing minimal characteristics: 4 4.1.1 Column Oven, operated at a constant temperature sj between 190 and 210C. 4.1.2 Sample Inlet Port, with the. heater characteristics i necessary for operation at 60C higher than the maximum necessary column oven temperature. ,f 4.1.3 Detector, ofthe flame ionization or therinal conduc- ij tivity type. If separately thermostatted, it should be main- ,j taincd at column temperature or hotter. 4.1..4 Column, 5 to 10 ft (1.5 to 3.0 m) long, 'A in. (6.4 ` mm) in outside diameter, made of glass, stainless steel, copper, or aluminum packed with 20 weight % of poly diethylene glycol succinate polyester (DECS) liquid phase on 80 to 100 mesh add washed calcined diatomaceous earth.3 4.1.5 Recorder, 0 to 1-mV range, 1-s full-scale deflection with a chart speed of V2 to 1 in. (13 to 25 mm)/min, and an attenuator switch to change the recorder range as required; the recorder should be equipped with an integrator if possible. 4.1.6 Helium Carrier Gas, pure. 4.2 Syringe for Injecting Specimens, fixed needle, 10-pL capadty or equivalent with a known and reproducible volume. 4.3 Electronic or Mechanical Integrator. 5. Reagents 5.1 Standard Fatty Acid Methyl Ester containing approx imately equal quantities of oleic and stearic methyl esters, for optimizing operating conditions. 6. Preparation of Apparatus 6.1 Start the flow of helium gas through the apparatus and adjust the inlet port, column, and detector, if individually thermostatted, to their operating conditions as given in 4.1. Record a base line to check for stability of the instrument. Normally a-new column with the DEGS liquid phase must be preconditioned by maintaining it at its operating temper ature with helium flowing through it for 24 h or until the 3 Chromosorbs W and P manufactured by Manville Sales Corp., available from gas chromatography suppliers, have been found satisfactory for this purpose. 286 DUP050295950 D1983 er base line is stable at the most sensitive attenuation g to be used. 1--At no time should the detector filament current (TC I be turned on when helium gas is not flowing through the 2 The proper gas flow rate should permit elution of enic and shorter chain methyl esters in 30 min or less, inlet pressure and gas flow necessary to accomplish this . between columns and instruments used but are ively constant for a single apparatus. It should not be y to exceed. 40 psi (280 kPa) for the gas pressure at ilet of the flow control capillaries. A constant gas flow [ be maintained throughout the duration of an analysis aintain linearity of signal response. Polyester stationary ses are very susceptible to oxygen damage and hydrolysis, use of gas purifiers and oxygen removers is recomded for the earner gas. ,3 Take up 0.5 to 3 pL of fatty acid ester standard (see | into the syringe. Wipe the needle tip, pierce the septum ':e sample inlet port, quickly discharge the specimen, and ' draw the needle immediately. Note on the recorder chart .small peak , caused by air which marks the sample eduction reference point. This will be followed immedfly by the ether solvent peak if there is some residual "vent left in the sample. The specimen size must be Iso that the major peak does not exceed the linearity ge of the detector. Check manufacturer's specification. To t e 2--The specimen must be discharged rapidly so that uniform vaporization occurs or the phenomenon' of "tailing" may occur "ich precludes the possibility of sharp separations. !6.4 Having determined the optimum conditions, inject a eond specimen of the methyl ester standard (see 5.1} and itch the recorder pen to see that the peaks do not go off Je. Change the setting of the attenuator if necessary to p the peaks on the chart paper. Note the attenuation on 6 chart at the point that changes ire made. 6.5 Determine the instrument and column performance noting the separation of the oleate and stearate peaks (see ;4). This separation is expressed as peak resolution, R, as Mows: R-2YKS+ O) here: = distance between the peak maxima for stearate and oleate, S = base width of the stearate peak, and O = base width of the oleate peak. No t e 3--These values should be determined on a sample containing approximately equal quantities of oleate and stearate esters using a specimen size such that these peaks axe 25 to 50 % ofthe chart width. If the peak resolution is equal to or greater than 1.0 the column and instrument are in satisfactory condition. All columns when used will show a gradual loss in peak resolution. When the value becomes less than 1.0, a new column should be installed.7 7. Calibration 7.1 Calibration factors should be determined to correct for nonlinearity of instrument response due to molecular weight differences. In most cases the standard mixtures are not made up with exactly the same weights of each ester. The units of area per weight percent must be calculated by TABLE 1 Relative Retention and Relative Response Values for Methyl Esters of Fatty Acids Ester Relative Retention Relative Response Myristate Palmitate Margarate Stearate Oleate Linoleate Linolenate 0.56 1.00 1.32 1.70 1.94 2.31 3.00 1.03 1.00 0.99 0.97 0.95 0.92 0.90 dividing the area of each peak in the standard mixture by its weight percent. Then relative response values can be calcu lated by dividing this number by the units of area per weight percent obtained for the palmitate. The calculated values should be compared with those listed in Table I; they should be nearly the same. No t e 4--Careful workers in the field have reported variations in relative response when the ratio of one fatty acid to another in a standard mixture is greatly changed. The magnitude of the variation is generally considered, close enough to the precision of the test method that it does not appear practical to use these small corrections in routine work. However, for precise analysis the corrections may be desirable. 8. Procedure 8.1 Using the same condition as for the standard record the chromatqgram of the fatty acid methyl esters prepared in accordance with Test Methods D 2800 or D 3457 using attenuation settings that provide peak heights of principal components between 15 and 85 % of full scale. Observe the usual cautions described in 6.1 through 6.5 in the chromatogramming of the standard methyl ester. No t e 5--High-boiling constituents, polymers, unsaponifiables, and rosin acids that may be present in appreciable amounts in certain types of fatty acids are likely not to be eluted from the column and thus cause errors. By using an internal standard, these errors can not only be eliminated, but ifthe interest is in only certain of the fatty adds present, these can readily' be calculated on the original sample basis without measuring all the peaks. 8.2 After all the peaks have been traced and the pen has returned to the base line, remove the chart for identification. 8.3 Identify the peaks by relative position on the chart. Identities must be established with known mixtures under the same conditions and either before or after the unknown samples are analyzed if in doubt. The esters appear in order of increasing number of carbon atoms and of increasing uhsaturation for the same number of carbon atoms, that is, C-16 is ahead of C-17, and the C-18 esters appear in the order: stearate, oleate, linoleate, and linolenate. The C-20 saturated (arachidic) ester usually appears after C-18:3A (linolenic) ester but may be reversed on some columns or the positions may change with column usage. In the case of tall oil, the suggested order of identified peaks is palmitate, palmitoleate, margarate (if added as an internal standard), stearate, oleate, linoleate, cis-trans conjugated linoleate (not linolenate, which is absent in tall oil fatty acids) and trans-trans linoleate. Insufficiently identified minor peaks appear, one after the oleate, one after the linoleate, another between the cis-trans and the trans-trans linoleate, and several after the trans-trans linoleate peaks. While the identity of these has not been definitely established, the presence of esters of the following acids has been suggested: 287 DUP050295951 ......... # b 1983 isomers of oleic and linoleic acids as well as saturated C-19 and saturated, unsaturated, and polyunsaturated C-20 acids. 8.4 In case of doubt, the peaks can be identified by comparison with chromatograms obtained under the same test conditions with one or more known mixtures, such as described in Test Method D 3457. The component peaks are usually identified by relative retention times, which are the ratios of retention times (chart distances) from the air/ solvent peak to each component peak relative to the same time (distance).for the palmitate peak, the first peak observed when palmitate is present (or another peak when palmitate is not present). Compare the values obtained experimentally with thpse listed in Table 1; they should be nearly the same. No t e 6--Known mixtures should* be run periodically under the same, test conditions to. build up a reference file of chromatograms and retention data and for checking the operation of the instrument: 9. Calculation 9.1 Determine the relative area, compensated for attenu ation, under each methyl ester peak on. the chromatogram. If the recorder is equipped wittian integrator, this can be conveniently done by following the manufacturer's instruc tions. If no integrator is used, the `results will be most reproducible between operators by utilization of .a pla7 nimeter. Alternatively, the peak area can be measured by multiplying the peak height times the width at ride half the height using a calijper to obtain accurate measurements. Good correlation has been found between arda percent obtained by tiring the'method Of peak height tiines the width at one half the height as compared to those obtained by means ofa planimeter. A fourth arid less desirable method is to measure the area ofa triangle constructed by drawihg lines tangent to the sides of-the peak and intersecting the baseline. For attenuated peaks it requires drawing tangents to the outer side of the peak two thirds of the chart paper width. The area ofthe resulting triangle is found by multiplying the height by one half the base. The .fourth method is less desirable because alteration of the original chromatogram may introduce considerable error resulting from the fact that the exact angle at which the lines are drawn may involve some judgment. 9.2 The apparent true area may beobtained by multi plying 'the observed greas by their respective attenuator setting?. The areas of all peaks may then be summed and the percent of each reported as area percent. This is. not equivalent, to either weight percent or mole percept and may be in error by as much as 20 : No t e 7--The areas of each peak can be corrected for variations in relative detector response by ciiyiding the apparent true area obtained in accordance with 9.2 by the relative response, value, obtained experimen tally in accordance with Section. 7 or by,use of those listed in Table 1. Summing and calculating the area so obtained as a percent of fatty acid will give values quite close to true weight percent from which mole percent can-readily be determined. 9.3 If an internal standard was used because ofdoubt that the sample would be completely volatilized and eluted with its conditions of analysis specified, then an additional step is required in calculation. Calculate the percent of each fatty acid, F, (omit margaric arid or heptadecanoic, acid) as follows: E = (A</Ajx (M/W) x 100 where: Af = corrected area for the fatty arid (as the methyl ester) peak, Am = corrected area for the margarate (as the methyl ester) peak, , M = weight of margaric acid, and W = weight of unknown fatty acids before addition of margaric acid. j '9.3.1 Determine thetotal eluted fatty acids(methyl esters) by adding the perceiits obtained by use of the equation given 1 in 9.3. : ! 9.3.2 Calculate the noneluted portion of the specimen, if I so desired, by subtracting the total percent of eluted fatty 1 acids (methyl esters) obtained in 9.3.1 from TOO %. 10.Precision and Bias 10.1 Precision--The following criteria should be used for f judging the acceptability of results at the 95 % confidence j . 10.1.1 Methyl Esters from Fatty Acids- (Test Method ?i D3457):- ' f 10.1.1.1' Repeatability--Two determinations of major | components, Which are defined as components in excess of J 5 %, performed by the same operator should be considered | suspect, if they differ bytmore than 2.2 % absolute. \Q.\A.2. Reproducibility--Two results, each the mean of | two determinations of major -'components, obtained by 1 operators in different laboratories should be considered : suspect if they differ by more than 6.1 % absolute. No t e 8--The use of relative response presupposes precision ofabout 5 % of the amounts present for the other.steps in. the test method. tO.\.2 Methyl Estersfrom Oils (Test Method D 2800): ' 10.1.2.1 Any Individual Fatty Acid: ..(/) Repeatability--Two determinations by the same oper ator should be considered suspect ifthey differ by more than 1.7%. absolute.' (2) Reproducibility--Two results, each the mean of dupli cates, obtained by operators in different laboratories should be considered suspect if they differ by more than the following: Difference, %, absolute Saturated acids Oleic Linoleic Linolenic 1.5 2.4 2.2 6.) 10.1.2.2 Total Eluted Fatty Acids: (7) Repeatability--Two determinations by the same.oper ator should be considered suspect if they differ by more than 4.2 % absolute, (2). Reproducibility--Two results, each the mean of dupli cates, obtained by operators in different laboratories should be considered suspect if they differ by more than 13.2 % absolute. 10.2 Bids--Because of the complexity of oils and the difficulty in obtaining a standard, bias has not been estab lished. 11. Keywords 11.1 fatty acids; gas-liquid chromatography; methyl esters 288 DUP050295952 D 1983 The American Society for To3tlng and Materials lakes no position respecting the validity of any patent rights asserted In connection with any Hem mentioned In this standard. Users of this standard are expressly advised thef determination of the validity of any such patent rights, and the risk of infringement ot such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years end ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional 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., Ptlitadelphia, PA 19103. 289 DUP050295953 Designation: D 1984 - 69 (Reapproved 1988) I* Standard Specification for Tail Oil Fatty Acids1 This standard is issued under the fixed designation D 1984; 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 lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 4 1. Scope 1.1 This specification covers distilled fatty acids derived from tall oil. Three types are covered as follows: 1.1.1 Type I, having a minimum of 98 % fatty acids (by difference) and a maximum of 1 % rosin acids. 1.1.2 Type II, having a minimum of 96 % fatty acids (by difference) and a maximum of 2 % rosin acids. 1.1.3 Type III, having a minimum of 90 % fatty acids (by difference) and a maximum of 10 % rosin acids. 2. Referenced Documents 2.1 ASTM Standards: D1240 Test Method for Rosin Acids in Fatty Acids2 D1467 Guide for Testing Fatty Acids Used in Protective Coatings2 D 1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D 1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 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 DO1.32 on Drying Oils. Current edition effective Oct 3, 1969. Originally issued 1965. Replaces D 1984-65 T. 2 Annual Book ofASTM Standards, Vol 06.03, 3 Annual Book ofASTM Standards, Vois 06.01, 06.02, and 06.03. D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Acids2 D 1980 Test Method for Acid Value of Fatty Acids and Polymerized Fatty Acids2 D1983 Test Method for Fatty Acid Composition by Gas-Liquid Chromatography of Methyl Esters2 1 3. Properties 3,1 Tall oil fatty acids shall conform to the requirements given in Table 1. :I||| 4. Test Methods 1 4.1 The properties enumerated in this specification shall be determined in accordance with Methods D 1467. iNo t e--Tall oil fatty adds are produced with various specifications Ithat lie outside of the specifications given herein. Such specifications should be agreed upon between the purchaser and the seller. TABLE 1 Requirements for Tali Oil Fatty Acids s i ASTM Type 1 Test Methods Min Max Type II Min Max Type III Min Max Add value D1980 197 192 190 Rosin acids, % D1240 Unsaponlfiables, % D 1965 1.0 1.0 2.0 10.0 2.0 .. . 10.0 Fatty adds, % D1983 98 96 90 Color. Gardner D1644 4 5 10.0 Iodine value 01959 125 135 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 subfect to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should he addressed to ASTM Headquarters. Your comments witI 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. 290 DUP050295954 Designation: D 2071 - 87 (Reapproved 1991),'ei Standard Test Methods for Fatty Nitrogen Products1 This standard is issued under the fixed designation D 2071; 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 revirion or reapproval. These test methods were preparedjointly by ASTM and the American Oil Chemists' Society. ` No t e--Keywords were added editorially in August 1991. ope 'These test methods cover the testing of fatty nitrogen Jucts. They specify the use of other ASTM methods that fpublished separately. The test methods included are '. in Table 1. ;.2 The test methods cover the following compounds; .1 Fatty Amines--Fatty primary amines, difatty secamines, trifatty tertiary amines. jff.2.2 Fatty Quaternary Ammonium Chloride--Trimethyl ' quaternary ammonium chloride, dimethyl difatty quaaary ammonium chloride. *.2.3 Fatty Amidoamines--Reaction products of fatty [ with an excess of polyamines. . 1.4 Fatty Diamines--//-fatty- 1,3-propylene diamines. 1,3 .This standard does not purport to address all of the fety problems, if any, associated with its use. It is the ^ponsibility ofthe user of this standard to establish appro bate safety and health practices and determine the applica bility ofregulatory limitations prior to use. Referenced Documents 1 ASTM Standards: D 56 Test Method for Flash Point by Tag Closed Tester?'5 D 88 Test Method for Saybolt Viscosity3 4 D 92 Test Method for Flash and Fire Points by Cleveland Open Cup2 : D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2,5 D i 209 Test Method for Color ofClear Liquids(Platinum` Cobalt Scale)4,5 D1310 Test Method for Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus4,5 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials5 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4,5 D2072 Test Method for Water in Fatty Nitrogen Compounds5 D2073 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines, Amidoamines, and Diamines by Referee Potentiometric Method5 D2074 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method5 D 2075 Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines5 D 2076 Test Methods for Acid Value and Amine Value of Fatty Quaternary Ammonium ChIoridess D 2077 Test Method for Ash in Fatty Quaternary Ammo... nium Chlorides5 D 2078 Test Method for Iodine Value of Fatty Quaternary Ammonium Chlorides5 D2079 Test Method for Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides5 . D2080 Test Method for Average Molecular Weight of Fatty Quaternary Ammonium Chlorides5 D2081 Test Method for pH of Fatty Quaternary Ammo nium Chlorides5 D 2082 Test Method for Percent`of Non-amines in Fatty Nitrogen Compounds5 D 2083 Test Method for Calculation of Percent of Pri mary, Secondary, and Tertiary. Amines, in Fatty Amines5 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus5 3. Terminology 3.1 Definition: 3.1.1 fatty nitrogen products--nitrogen containing com pounds derived from vegetable and animal fatty acids. No t e 1--Vegetable and animal fatty acids include coconut, cotton, soya, tallow and tall oil fatty acids, fatty acid fractions thereof, and hydrogenated fatty acids. 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 D0I.32 on Drying Oils. Current edition approved June 26, 1987. Published August 1987. Originally published as D 2071 - 62 T. Last previous edition D2071 - 75 {]980>< 1. 1 Annual Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 04.04. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual'Book ofASTM Standards, Vol 06.03. 4. Significance and Use 4.1 These test methods list the methods used to test fatty amines, fatty quaternary ammonium chlorides, fatty amidoamines and fatty diamines. The results of the tests can be used to determine the purity of these materials and therefore can be used for establishing specifications. 291 DUP050295955 # D2071 TABLE 1 List of Test Methods Test Method Definition All Fatty Nitrogen Products: Sampling Color by the Gardner Method Color by the APHA Method Water by the Karl Fischer Method Fatty Amines: Amine values Iodine value Percent non-amine Primary, secondary, tertiary amines Fatty Quaternary Ammonium Chlorides: Add value and amine value Ash Flash point Iodine value Nonvolatile matter Average molecular weight PH Fatty Amidoamines: Amine values Iodine value Fatty Diamines: Amine values Iodine values Percent non-amines Sections 4 ASTM Designation of Test Method 5 D1466 e D 1544 7 D1209 8 D 2072 g D2073 D 2074 10 D2075 ii D2082 12 D2083 13 D2076 14 D 2077 15 D 56 D88 D92 D93 D 1310 D3278 16 D2078 17 D2079 16 02080 ig D2081 20 D2Q73 21 D2075 22 D 2073 23 D2075 24 D 2082 ALL FATTY NITROGEN PRODUCTS 5. Sampling 5.1 The techniques outlined in Test Method D 1466, should be generally suitable with the following additions: 5.1.1 Fatty amines and diamines can sensitize and irritate. Wash from clothing and body surfaces immediately on contact. Protect from air to prevent absorption of carbon dioxide and formation of carbonates. Prolonged storage at elevated temperatures will discolor and degrade. 5.1.2 Fatty quaternary ammonium chlorides usually con tain volatile alcohols. Avoid losing these components during sampling and analysis. Prolonged storage at elevated temper atures will discolor and degrade. 6. Color by the Gardner Method 6.1 Gardner color is determined by matching a standard color in an empirical series graduated from 1 (pale yellow) to 18 (dark brown). 6.2 Determine color in accordance with Test Method D 1544, but report the color as 3-, 3, 3+, A--, and so on. When the color is Gardner 2+ or less, determine the platinum-cobalt color also. 6.3 The precision of the method in the range of values of 1 to 18 is as follows: 6.3.1 Repeatability--Two single determinations per formed in one laboratory should be considered suspect if they differ by more than 0.6 unit. 6.3.2 Reproducibility--Single determinations per formed in two different laboratories should be considered suspect if they differ by more than 1.4 units. 7. Color on the Platinum-Cobalt Scale 7.1 Color on the platinum-cobalt scale (sometimes re ferred to as platinum-cobalt or Hazen Color) is determined by matching a standard color in an empirical series graduated from 0 (colorless) to 500 (pale yellows). 7.2 Determine color in accordance with Test Method D 1209, but report one of the following values: 0, 10, 20, 30, 40,50,60,70, 80,90,100,150,200, 300,350,400,450,500, DT 500. 7.3 The precision of this test method has not yet been determined for fatty nitrogen products. 8. Water by the Karl Fischer Method 8.1 Water is determined by reacting with an excess ofKarl Fischer reagent, which is then back-titrated with watermethanol solution. The usual direct titration with Karl Fischer reagent results in high values for these products. 8.2 Determine the percent of water in accordance with Test Method D 2072. FATTY AMINES 9. Amine Values 9.1 Total, primary, secondary, and tertiary amine values are defined as the milligrams of potassium hydroxide equiv alent to the total, primary, secondary, and tertiary amine basicities in 1 g of sample. These empirical values may be converted to percent total, percent primary, percent sec ondary, and percent tertiary amines, if the average molecular weights of these components in the sample are known. 9.2 Procedure; 9.2.1 Determine the amine values in accordance with Test Methods D 2073. 9.2.2 Alternatively, determine the amine values in accor dance with Test Methods D 2074. II 5 II 10. Iodine Value 10.1 The iodine value is a measure of the unsaturation of the alkyl groups, defined as the percent by weight equivalent of iodine absorbed per gram of sample. 10.2 Determine the iodine value in accordance with Test Method D 2075. This test method is a modified Wijs method using acetic acid as the solvent and mercuric acetate as catalyst. 11. Percent of Non-amine 11.1 The non-amines are fatty amides, nitriles, alcohols and unsaponifiable matter normally present in small amounts in these products. 11.2 Determine the percent non-amine in accordance with Test Method D 2082. 12. Percent of Primary, Secondary, and Tertiary Amines 12.1 The percent of primary, secondary, and tertiary amines present in the sample can be calculated from the 292 DU P0502 95956 # D 2071 secondary, and tertiary amine values and the t in accordance with Test Method D 2083, FATTY QUATERNARY AMMONIUM CHLORIDES kdd Value and Amine Value id Acid Value is the number of milligrams of potassium jpxide needed to neutralize 1 g of sample, arid is usually f|o amine hydrochloride. 2--Most industrial quaternaries contain a small amount of yl chloride,, slow hydrolysis of which causes an increase in acid s in a sample and a corresponding decrease in its amine,value. 3.2 Amine Value is the number of milligrams of potast hydroxide equivalent to the fatty amine basicity in 1 g aple. 1.3 Determine the ,acid and amine values in accordance i Test Methods D 2076. The test method covers converi ofacid and amine values to percent ofamine hydrochloi and percent of amine for standard industrial quaterna- Ash Il4.1 Ash in quaternaries is essentially sodium chloride, mess free caustic material is found as described in Test fethod D 2076. 14.2 Determine the percent ash in accordance with Test fethod D 2077. Flash Points 15.1 Flash points are run on quaternaries to determine 'hether they must be classified as flammable under govern ment regulations. The flash point of a liquid is defined as the west temperature, corrected to a pressure of 760 mm Hg <101.3 kPa) 1013 m bar of the sample at which application of .n ignition source causes the vapor ofthe specimen to ignite ider specified conditions of test. 15.2 Determine flash point of quaternaries having a Mscosity less than 45 SUS at 100F (9.5 cSt at 77F) (Test Method D 88) by Test Method D 56 and flash point of quaternaries having a viscosity of 45 SUS at 100F or more by Test Methods D 93. In addition, test suspensions of solids or liquids that tend to skin by Test Methods D 93. 15.3 Regulatory: 15.3.1 Determine the flash point by Test Method D 56 or by Test Method D93 for liquid storage regulations of Occupational Safety and Health Administration of U.S. Dept, of Labor and for classification of hazardous liquids for shipments by all common carriers under the regulations of U.S. Dept, of Transportation. 15.3.2 Determine flash point of liquids regulated by the U.S. Consumer Product Safety Commission by Test Method D 1310. JB 15.4 Test Method D 3278, which gives comparable results iiV to Test Method D 56 and Test Method D 93 but requires less sample and less time to run than the latter methods, may be used to check flash point of quaternaries. The U.S. Depart ment of Transportation specifies its use as an alternative method to the methods specified in 14.3.1. 16. Iodine Value 16.1 Iodine value is a measure of the unsaturation of alkyl groups, 16.2 Determine the iodine value in accordance with Test Method D2078. This test method is a modified Wijs method, using chloroform as the solvent and sodium lauryl sulfate to keep the free iodine in the nonaqueous phase. 17. Nonvolatile Matter 17.1 Industrial quaternary products normally contain quaternary, water, alcohol, and minor amounts of salt, amine, and amine hydrochloride. The simplest method of determining the quaternary content of a sample is to determine the percent nonvolatile which for most purposes is equivalent to fine percent of quaternary. 17.2 Determine the percent of nonvolatile matter in accordance with Test Method D 2079. 18. Average Molecular Weight 18.1 The average molecular weight of an industrial qua ternary varies from lot to lot and from producer to producer because of small variations in the alkyl groups. Where this variation is important the average molecular weight of the quaternary can be calculated by titrating the quaternary with perchloric acid, determining the percent nonvolatile, and correcting both for amine, amine hydrochloride, and salt (percent ash). 18.2 Determine the average molecular weight in accor dance with Test Method D 2080. 19. pH 19.1 The pH of quaternaries is dependent upon the fatty amines and fatty amine hydrochlorides present in the material. Most industrial quaternaries exhibit a slow drop in pH with time because of hydrolysis of methyl chloride dissolved in the product. 19.2 Determine the pH in accordance with Test Method D 2081. FATTY AMIDOAMINES 20. Amine Value 20.1 Amine value is defined as the milligrams of potas sium hydroxide equivalent to the amine basicity of 1 g of sample. 20.2 Determine the total amine value in accordance with Test Methods D 2073. The procedures described therein for primary, secondary and tertiary amine values are not appli cable to fatty amidoamines. 21. Iodine Value 21.1 The iodine value is a measure of the unsaturation of the alkyl groups, defined as the percent by weight equivalent of iodine absorbed by 1 g of sample. 21.2 Determine the iodine value in accordance with Test Methods D 2075. FATTY DIAMINES 22. Amine Values 22.1 Total, primary, secondary and tertiary amine values are defined as the milligrams of potassium hydroxide equiv- 293 DUP050295957 D 2071 alent to the total, primary, secondary and tertiary amine basicities in 1 g of sample. 22.2 Determine the amine values in accordance with Test Methods D 2073. Test Methods D 2074 are not applicable to the fatty diamines. 23. Iodine Value 23.1 Determine the iodine value in accordance with Test Methods D 2074. 24. Percent of Non-amine 24.1 The non-amines are fatty amides, nitriles, alcohols, and unsaponifiable matter normally present in small amounts in these products. 24.2 Determine the percent non-amine in accordance with Test Methods D 2082. 25, Keywords 25.1 fatty amidoamines; fatty amines; fatty diamines The American Society lor Testing and Materials takes ho 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 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 of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 294 DUP050295958 esignation: D 2072 - 66 (Reapproved 1987),'1 Standard Test Method for Water in Fatty Nitrogen Compounds1 This standard is issued under the fixed designation D 2072; 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 lest method was preparedjointly by ASTM and the American Oil Chemists'Society. 41 No t e --Editorial changes were made throughout in October 1987. pe This test method covers the determination of water in Nitrogen compounds by titration with a water-methanol n after addition of an excess of Karl Fischer reagent. T.The procedures appear in the following order: Sections ~mary Amines, Diamines, and Amidoamines `Secondary Amines i Ammonium Chlorides 4 to 8 9 to 12 13 to 16 | This standard may involve hazardous materials, oper and equipment. This standard does not purport to ess all ofthe safety problems associated with its use. It is 'esponsibility of the user of this standard to establish opriate safety and health practices and determine the icability of regulatory limitations prior to use. Specific d statements are given in 5.3, 6.1, and 11.2. eferenced Documents . 1 ASTM Standards: 1193 Specification for Reagent Water2 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 or otherwise (Note 1). The titration should be performed in a closed system to avoid the absorption of water. The electrode and buret shall be mounted through a close-fitting stopper, and provision made for mechanical stirring by means of a magnetic stirrer. No t e 1--It is essential that the Karl Fischer reagent, water-methanol solution, and anhydrous methanol be protected from atmospheric moisture at all times. In humid seasons or climates, the drying tubes used to protect the reagents against moisture in the air must be watched closely. The silica gel must be changed as soon as there is evidence of color change in it. Care also must be taken to minimize the exposure of the sample and solutions to atmospheric moisture during the determi nations. 4.2 Magnetic Stirrer, that can be used with the closed titration beaker with inert plastic-coated stirring bar. 4.3 Pipet, automatic, 25-mL. 4.4 Pipet, weighing, or equivalent for weighing water, for standardization of reagent. 4.5 Electrometric Titrator of the "dead stop" type, equipped with platinum electrodes. On operation a small electrical potential is imposed across the electrodes. At the end point there is a change in the flow of current due to the change in polarization of the electrodes.4 , Summary of Test Method $3.1 An excess of Karl Fischer reagent is added to the aen dissolved in the prescribed solvent. After reaction 1th the water in the specimen, the excess Karl Fischer agent is back-titrated with water-methanol solution. The d point is best detected electrometrically, but with practice may be satisfactorily determined visually. FATTY PRIMARY AMINES, DIAMINES, AND AMIDOAMINES |4. Apparatus 4.1 Buret and Bottle Assemblies (or other convenient arrangement), protected with silica gel so as to maintain Karl Fischer reagent and water-methanol solutions free from contamination with moisture either through the atmosphere 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 D01.32 on Drying (Mis. Current edition approved Sept. 30,1966. Published November 1966. Originally published as D2072 - 65 T. Last previous edition D 2072 - 66 (1981)41. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 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 reagent water conforming to Type II of Specification D 1193. 5.3 Acetic Acid. Glacial (CH3COOH). Warning--(see 6.2). 4 A number of different instruments of this type have been found suitable for this purpose and are~commercially available; including those manufactured by Beckman Instruments, Inc., Fullerton, CA; E. H. Sargent Co., Chicago, 1L; Precision Scientific Co., Chicago, IL, and Wilkens-Anderson Co., Chicago, lL 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listedby the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 295 DU P0502 95959 # D 2072 5.4 Karl Fischer Reagent--Suitable reagent is available from most chemical supply houses or see Test Method D 1364. 5.5 Methanol, anhydrous, water content less than 0.05 %. 5.6 Water-Methanol Solution--Prepare by weighing ap- proximately 10 g of water with the aid of a weighing pipet into a 2-L volumetric flask. Dilute to the mark with methanol and mix well. This solution will contain approxi mately 5 mg (weighed) of water per millilitre plus the amount of water normally present in the methanol. Stan dardize as described in Section 7. .6 Precautions 6.1 Fatty amines and diamines can sensitize and irritate. Wash from clothing and body surfaces immediately on contact. r 6.2 Warning---Glacial acetic acid will cause bums,of the skin and eyes. Use care in hahdling the acid! In case of contact, immediately flush skin or eyes with plenty of water. 6.3 Warning--The U. S. Food and Drag Administration has declared that chloroform is injurious to health. Care should be used in handling chloroform as it can be absorbed through the skin. ' 7. Standardization of Reagents . 7.1 Deliver from a buret 25 mL of Karl Fischer reagent in a dry,. 300-mL Berzelius beaker. Titrate (see 4.1) with the water-methanol sqlutipn, adding it slowly but steadily, so that it is thoroughly dispersed by the stirrer, until the end point is approached. Add dropwise when nearing the end point which is indicated by the change in color from dark reddish-brown to golden .yellow. Titrate to completion electrometrically. No t e 2--Test Method D 1364 describes the visual endpoint, but in that method the titration is direct, not a back-titration. - 7.2 Deliver from a buret 25 mL of Karl Fischer reagent into a dry, 300-mL beaker. Pipet 25 mL of methanol into the beaker. Repeat the titration as described in 7.1. 7.3 Calculate the water lacfor,'as follows: . F=JgL-M)_ + Ar ' . r 25 +M--L'*" where: F = water per millilitre of water-methanol solution, mg, i L = water-methanol solution required for titration of25 mL of Karl Fischer reagent, mL, M = waterTmethanol solution required for titration of25 mL of Karl Fischer reagent plus 25 mL of absolute , meth anol, mL, and N = water added per millilitre to the water-methanol solu tion described in 5.6, mg. 8. Procedure 8.1 Melt the sample, if it is not already liquid, in a water bath. Mix thoroughly and weigh into a dry beaker 10 g of sample or enough to give 5 to 25 mg of water. 8.2 Pipet 25 mL of glacial acetic acid and stir to dissolve. 8.3 Deliver from a buret 25 mL of Karl Fischer reagent. Back-titrate with water-methanol solution slowly but steadily, stirring so that it is, thoroughly dispersed by the stirrer until the end point is approached. Add dropwise when nearing the end (point which is indicated by the change in color from dark reddish-brown to golden yellow. Titrate to the same end point used in standardization. 8.4 Prepare a blank using 25 mL of Karl Fischer reagent and 25 mL of glacial acetic add. Carry through the proce dure separately and in an identical manner as for the spedmen. 9. Calculation 9.1 Calculate the percent of water as follows: Water, % = [( -- V) x F]/{S x 10) where: B = water-methanol solution required for titration of the j blank, mL, V = water-methanol solution required for titration of the spedmen, mL, F = water factor determined in accordance with Section 7, >i and S = specimen weight used, g. ' , DIFATTY SECONDARY AMINES 10. Apparatus 10.1 See Section 4. 11. Reagents 11.1 The reagents used in this procedure are the same as those listed in 5.1, 5.2, 5.4, 5.5, 5.6, and 11.2. 11.2 Chloroform (CHCI3). Warning--See 6.3. 12. Procedure 12.1 Proceed in accordance with Section 8, except in 8.2 use 25 mL of CHC13 heated to not over 30C instead of acetic add. Also, in 8.4 substitute CHC13 for acetic add when preparing the blank. 13. Calculation 13.1 See Sectidn 9. QUATERNARY AMMONIUM CHLORIDES 14. Apparatus 14.1 See Section 4. I f 15. Reagents 15.1 The reagents used in this procedure are the same as | those listed in 5.1, 5.2, 5.4, 5.5, and 5.6. `j 16. Procedure 16.1 Proceed in accordance with Section 8 except to omit i 8.2. In 8.3, stir to dissolve after addition of the Karl Fischer j reagent. In 8.4 omit the acetic acid when preparing the | blank. 17. Calculation I j 17.1 See Section 9. DUP050295960 < D 2072 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirety their own responsibility. This standardis subject to revision atany time by the responsible technical committee and mustbe reviewed every five yearn and itnotrevised, either reapprovedor withdrawn. Ypurcomments are Invited eitherfor revision ofthis standard or for addltkmalstandards 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. 297 di DUP050295961 Designation: D 2073 - 66 (Reapproved 1987)e1 | Standard testMethods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines, Amidoamines^ranct Diarrtiijes by Referee Potentiometrlc Methpd"1 This standard is issued under the fixed designation D 2073; 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. These methods were preparedjointly by ASTM and the American Oil Chemists' Society. el No t e--Editorial changes were made throughout in October 1987. I 1. Scope 1.1 These referee test methods cover the potentiometric determination of the total, primary, secondary, and tertiary amine values of fatty amines and diamines, and the total amine value of fatty amidoamines. Test methods for pri mary, secondary, and tertiary amine values are not appli cable to fatty amidoamines. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Notes 1 and 2 and 6.1. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water12 D2080 Test Method for Average Molecular Weight of Fatty Quaternary Ammonium Chlorides3 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 3. Definitions 3.1 total amine value--the number of milligrams of potassium hydroxide (KOH) equivalent to the basicity in 1 g of specimen. 3.2 primary amine value--the number of milligrams of potassium hydroxide (KOH) equivalent to the primaiy amine basicity in 1 g of specimen. 3.3 secondary amine value--the number of milligrams of potassium hydroxide (KOH) equivalent to the secondary amine basicity in 1 g of specimen. 3.4 tertiary amine value--the number of milligrams of potassium hydroxide (KOH) equivalent to the tertiary amine basicity in l g of specimen. 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and arc the direct responsibility of Subcommittee DO 1.32 on Drying Oils. Current edition approved Sept. 20,1966. Published November 1966. Originally published as D 2073 - 62. Last previous edition D 2073 - 66 (1981)*'. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. * Annual Book ofASTM Standards, Vol 15.05. 4. Apparatus 4.1 Air Condenser, minimum length 650 mm. 4.2 Erlenmeyer Flask, wide-mouth, alkali-resistant, borosilicate-glass, 250-mL capacity. 4.3 Glass Electrode pH Meter, conforming to the require ments of Test Method E 70 or similar potentiometric titrator. 4.4 Hot Plate, with variable heat control. 4.5 Magnetic Stirrer, with inert plastic-coated stirring bar. 4.6 Microburet, graduated to 0.02 mL and having a capacity of 10 mL. 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended j 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 ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 5.3 Acetic Acid, Glacial (CH3COOH). (Warning--See 6.2). 5.4 Acetic Anhydride. 5.5 Chloroform (CHC13). (Warning--See 6.3). 5.6 Hydrochloric Acid, Standard Solution (0.5 N)--Add 85 mL of concentrated hydrochloric acid (HC1, sp gr 1.19) to 1000 mL of isopropyl alcohol in a 2-L volumetric flask, Dilute to volume and mix. Standardize with sodium car bonate to a pH of 3.5. 5.7 Isopropanol (1 + 19)--Add 5 mL of water to 95 mL of isopropyl alcohol (99 %). 5.8 Perchloric Acid, Standard Solution (0.1 N)--Prepare and standardize in accordance with Test Method D 2080. 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 "Reagents Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 298 DUP050295962 TABLE 1 Specimen Weights specimen size into a 250-mL beaker for the secondary plus Specimen Weight tertiary amine value, and into a 250-mL flask for the tertiary ` of Fatty Amine Secondary plus Tertiary Amine Value, g Tertiary Amine Value, g amine'value. Mark the beaker S and the flask T. 9.3' To beaker S add 90 mL of CHC13 and boil for 1 min to drive off any free ammonia that may be present. Cool to t amine fatty amine tty amine room temperature. Add 5 to 6 mL of salicyiaidehyde and allow to'staiid for`30 miti. After 30 min '^dd 10 mL of isppropanol solution-Insert the. stirring bar into the beaker ^Salicyiaidehyde'ey and adjust the beaker so that the lower half of each electrode ,, of the pH meter is immersed in the sample. Start the stirrer cautions (Fatty amities and diamines can sensitize and irritate, from clothing and body surfaces immediately on it. Warning--Glacial acetic acid, concentrated hydros acid, 70 to 72 % perchloric acid, and acetic anhydride use bums of skin and eyes; the vapor of each is ng to mucous membranes. Use care in handling these substances. In case of contact flush skin or eyes with of water. The perchloric add may form explosive res if allowed to come in contact with oxidizable 'als (organic substances). Flush spills to drain with ; of water. ` Warning--The U. S. Food and Drug Administration ideclared that chloroform is injurious to health. Care 'd be used in handling chloroform as it can be absorbed ;gh the skin. and adjust the speed so that there is vigorous stirring without .spattering. Titrate with 0'Sji HCI using the millivolt scale. Record the millivolt'readings'every 1 mL, but in the vicinity of the end point record the millivolt readings every 0.1 mL. Plot a graph showing the millivolts against the millilitres required for titration. The end point is the midpoint of the inflection on the titration curve. 9.4 To flask T add 25 mL of acetic anhydride, 2 mL of acetic acid, and 2 or 3 glass beads to the flask. Attach an air condenser, and reflux on a hot plate for 45 min allowing the condensate to rise only 2 in. (50 mm) in the condenser. Rinse down the condenser and quantitatively transfer the solution with 50 mL of glacial acetic acid into a 250-mL beaker. Cool to room temperature. Insert the stirring bar into the beaker and adjust the beaker so that the lower half of each electrode of the pH meter is immersed in the sample. Start the stirrer and adjust the speed so that there is vigorous stirring without spattering. Titrate with 0.1 N HC104 using tandardization of pH Meter the millivolt scale. Record the millivolt readings every 1 mL, i.l Carefully follow the manufacturer's instructions for particular meter used and standardize at pH's of 4.0 and but in the vicinity of the end point record the millivolt readings every 0.1 mL. Plot a graph showing the millivolts against millilitres required for titration. The end point is the mid-point of the inflection on the titration curve. Procedure for Total Amine Value .1 Melt the sample, if it is not already liquid, in a water b. Mix thoroughly, and weigh 0.5 g to the nearest 0.1 mg a 250-mL low-form beaker. Add 90 mL of CHC13, 10 , of isopropyl alcohol solution and boil for 1 min on a hot te. Cool to room temperature. 8.2 Insert the stirring bar into the beaker and adjust the aker so that the lower half of each electrode of the pH -ter is immersed in the sample. Start the stirrer and adjust e speed so that there is vigorous stirring without spattering. 8.3 Titrate with 0.5 N HCI using the millivolt scale, ecord the millivolt readings every 1 mL, but in the vicinity f the end point record the millivolt readings every 0.1 mL. 'i'Lot a graph showing the millivolts against the millilitres required for titration. The end point is the mid-point of the inflection on the titration curve. . Procedure for Primary, Secondary, and Tertiary Amine Values 9.1 Determine the specimen size in accordance with Table 1. 9.2 Melt the sample, if it is not already liquid, in a water bath. Mix thoroughly and accurately weigh the designated 6 Eastman No. 225 salicyiaidehyde (from the bisulfite compound) has been found satisfactory for this purpose. 10. Calculations 10.1 Calculate the total amine value as follows: Total amine value -- {VxNx 56A)/S where: V = HCI required for titration of the specimen (8.3), mL, N = normality of the HCI solution, and S = specimen weight used, g. 10.2 Calculate the value of the secondary and tertiary amine groups as follows: Titration S amine value of secondary and tertiary amine groups = (Vx N x 56A)/S where: V -- HCI required for titration of the specimen (9.3), mL, N = normality of HCI solution, and S = specimen weight used, g. 10.3 Calculate the value of the tertiary amine groups as follows: Titration T amine value of tertiary amine groups = (V x N x 56A)/S where: V = HC104 required for titration of the specimen (9.4), mL, N = normality of the HC104 solution, and S = specimen weight used, g. 299 DUP050295963 10.4 Primary amine value equals total amine value minus the amine value of the secondary and tertiary amine group. 10.5 Secondary amine value equals amine value of the secondary and tertiary amine groups minus the amine value 10.6 Tertiary amine value equals OIUUIC ValUC tertiary amine groups. The American Society for Testing and Materials fakes noposition respecting the validity ofany patent rights assertedIn connection with any item mentioned In this standard. Users of this standard are express// advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard orforadditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. I 300 DUP050295964 resignation: D 2074 - 66 {Reapproved 1987).'1 Standard Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method1 This standard is issued under the fixed designation D 2074; 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 test methods were preparedjointly by ASTM and the American Oil Chemists' Society. " No t e--Editorial changes were made throughout in October 1987. pe ' These alternative test methods cover the indicator ure for determining the total, primary, secondary, and amine values of fatty amities. These procedures are plicable to fatty amidoamines and fatty diamines. This standard may involve hazardous materials, oper and equipment. This standard does not purport to s all ofthe safety problems associated with its use. It is sponsibility of the user of this standard to establish jpriate safety and health practices and determine the 'cability ofregulatory Imitations prior to use. efereiiced Document ASTM Standard: *1193 Specification for Reagent Water2 pfinitiojis .1 total amine value--the number of milligrams of ssium hydroxide (KOH) equivalent to the basicity in 1 g ..mple. .2 primary amine value--the number of milligrams of assium hydroxide (KOH) equivalent to the primary ine basicity in 1 g of sample. 3.3 secondary amine value--the. number of milligrams of tassium hydroxide (KOH) equivalent to the secondary ine basicity in 1 g of sample. (.3.4 tertiary amine value--the number of milligrams of atassium hydroxide (KOH) equivalent to the tertiary amine deity in 1 g of sample. . Apparatus 4.1 Erlenmeyer Flasks, wide-mouth, alkali-resistant, boosilicate-glass, 250-mL capacity. 4.2 Magnetic Stirrer, with an inert plastic-coated stirring bar. 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 ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 5.3 Bromphenol Blue Indicator Solution--Dissolve 0.2 g of bromphenol blue in 100 mL of methanol, ethanol, or isopropanol. 5.4 Bromcresol Green Indicator Solution--Dissolve 0.1 g of bromcresol green sodium salt in 100 mL of water. 5.5 Chloroform (CHC13). 5.6 Hydrochloric Acid, Standard Solution (0.1 N)--Add 17 mL of concentrated hydrochloric acid (HCI, sp gr 1.19) to 1000 mL of isopropyl alcohol'in a 2-L volumetric flask. Make up to volume after cooling to room temperature. Standardize with sodium carbonate using bromcresol green as the indicator. 5.7 Hydrochloric Acid, Standard Solution (0.2 N)--Add 34 mL of concentrated HCI (sp gr 1.19) to 1000 mL of isopropyl alcohol in a 2-L volumetric flask. Make up to volume after cooling to room temperature. Standardize with sodium carbonate using bromcresol green as the indicator. 5.8 Isopropyl Alcohol (99 %). 5.9 Phenyl Isothiocyanate. 5.10 Salicylaldehyde. 6. Procedure for Total Amine Value 6.1 Melt the sample, if it is not already liquid, in a water bath. Mix thoroughly, and accurately weigh 1 to 4 g to 0.1 mg into a 250 mL flask. Add 50 mL of alcohol and boil for 1 min to drive offany free ammonia that may be present. Cool to room temperature. 6.2 Add 5 drops ofbromphenol blue indicator and titrate, while swirling, with 0.2 N HCI to the yellow end point. 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 D 01.32 on Drying Oils. Current edition approved Sept. 20, 1966. Published November 1966. Originally published as D 2074 - 62 T. Last previous edition D 2074 - 66 <198l)el. 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." 301 DUP050295965 D 2074 7. Procedure for Primary, Secondary, and Tertiary Amine Values 7.1 Determine the specimen size as follows: Amine Value Specimen Weight, g 10 or less Over 10 5 2 7.2 Melt the sample if it is not already liquid. Mix thoroughly and accurately weigh the designated specimen size into two 150-mL beakers or 250-mL flasks. Mark them S and T. Add 50 mL of CHC13 to each flask (or beaker) and boil for 1 min on a hot plate to drive off any free ammonia. Cool to room temperature. 7.3 To beaker S add 3 mL of salicylaldehyde and allow to stand for 30 min. Add 1 mL of bromphenol blue indicator solution and titrate while swirling (or by using the magnetic stirrer if beakers are used) with 0.2 N HQ to a yellow end point (Note 1). The yellow may fade back to green upon standing, but this is to be disregarded if the yellow color is bright and the addition of another millilitre of 0.2 N HC1 does not change the yellow color. No t e 1--In the case of titrating the tertiary amine content of a primary amine, it is advisable to use a microburet as the titration will be extremely small. Errors in titration are greatly magnified because ofthe high molecular weights involved. 7.4 To flask T add 5 mL of phenyl isothiocyanate and allow to stand for 30 min. Add 1 mL of bromphenol blue indicator solution and titrate while swirling (or by using the magnetic stirrer, if beakers are used) with 0.2 N HC! to the yellow end point (Notes 1 and 2). The yellow may fade back to green upon standing, but this may be disregarded if the yellow color is bright and the addition of another millilitre of 0.2 N HC1 does not change the yellow color. No t e 2--Instead of 0.2 N HQ, 0.1 N HC1 may be used if the quantity of tertiary amine is very low. 8. Calculation 8.1 Calculate the total amine value as follows: Total amine value = (Kx N x 56.1)/S where: | V = HQ required for titration of the specimen (7.2), mL, I N = normality of the HQ solution, and 5 = specimen weight used, g. j 8.2 Calculate the amine value of secondary and tertiary amine groups as follows: Titration S amine value of secondary and tertiary amine groups = (Vx IV x 56.i)/S i where: V = HQ required for titration of the specimen (7.3), mL, N = normality of the HQ solution, and S = specimen weight used, g. 8.3 Calculate the amine value of tertiary amine groups as follows: ( | Titration T amine value of tertiary 1 amine groups = (V x IV X 56.1)/5 i where: V -- HC1 required for titration of the specimen (7.4), mL, N = normality of the HQ solution, and S = specimen weight used, g. 8.4 Primary amine value equals total amine value minus the amine value of the secondary and tertiary amine groups. 8.5 Secondary amine value equals amine value of the secondary and tertiary amine groups minus the amine value of tertiary amine groups. 8.6 Tertiary amine value equals amine value of the tertiary amine groups. I f 1 TireAmerican Society tor 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 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 fjve years and ifnotrevised, eitherreapproved or withdrawn. Yourcomments are invited eitherfor revision ofthis standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 302 DUP050295966 Designation: D 2075 - 89 Standard Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines1 This standard is issued under the fixed designation D 2075; 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. This method was preparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists'Society. (Scope .1 This test method (Note 1) covers the determination of 'odine value offatty amines, diamines, and amidoamines die Wijs procedure. 'ore 1--This test method is essentially equivalent to Test Methods 078 and D 1959. Use of mercuric acetate permits reduced reaction e compared to Test Methods D 2078 (30 min) and D 1959 (1 h). |.2 This standard may involve hazardous materials, oper' ns, and equipment. This standard does not purport to 'dress all ofthe safetyproblems associated with its use. It is e responsibility of the user of this standard to establish ipropriate safety and health practices and determine the iplicability ofregulatory limitations prior to use. , Referenced Documents ,2.1 ASTM Standards: D1193 Specification for Reagent Water2 H D1541 Test Method for Total Iodine Value ofDrying Oils 41 and Their Derivatives3 'D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids3 t- D 2078 Test Method for Iodine Value ofFatty Quaternary Ammonium Chlorides3 3. Terminology 3.1 Definition: 3.1.1 iodine value--a measure of the unsaturation of the alkyl group or groups, expressed in terms of percent iodine absorbed. . 4. Significance and Use 4.1 This test method measures the unsaturation of the alkyl groups as iodine value by addition of an iodine/ chlorine reagent 4.2 Where no conjugated double bonds are present, the iodine value obtained is a measure of the total unsaturation, and the values obtained are useful for comparative purposes. 4.3 If conjugated unsaturation is known to be present, use Test Method D 1541. 5. Apparatus 5.1 Bottles--Glass-stoppered bottles or wide-mouth Erlenmeyer flasks of 500-mL capacity. No t e 2--Wide-mouth bottles or flasks are essential if stirring is done by mechanical means. 5.2 Pipets, 20 and 25-mL capacity. 6, Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Acetic Add (Glacial)--Verify the absence of sub stances reducing permanganate as follows: Dilute 2 mL of the acid with 10 mL of water and add 0.1 mL of 0.1 N potassium permanganate (KMn04) solution. The pink color should not be entirely discharged at the end of 2 h.s 6.4 Chlorine (99.8 % Cl)--Commercial grades of chlorine available in cylinders may be used, provided the gas is dried by passing through concentrated sulfuric acid (H2S04, sp gr 1.84) before passing it into the iodine solution (see 6.10). Alternatively, the chlorine may be prepared by allowing concentrated hydrochloric acid (HQ, sp gr 1.19) to drop onto potassium permanganate (KMn04) or onto a mixture of KMn04 and manganese dioxide (Mn02). Dry the gas thus generated by passing it through H2S04 (sp gr 1.84). 6.5 Chloroform. 6.6 MercuricAcetate Solution--Dissolve 2.5 g of mercuric acetate (Hg (C2H302)2) in glacial acetic add (CH3COOH) and make up to 100 mL. 6.7 Potassium Iodide Solution (150 g/L)--Dissolve 150 g of potassium iodide (KI) in water and dilute to 1 L. 6.8 Sodium Thiosulfate. Standard Solution (0.1 N)-- Dissolve 24.8 g of sodium thiosulfate (Na2S203-5H20) in water and dilute to 1 L. Standardize against potassium 1 This method is under the jurisdiction ofASTM Committee D-1 on Faint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.32 on Drying Oils. Current edition approved March 31, 1989. Published May 1989. Originally published as D 2075 - 62. Last previous edition D2075 - 66(1981)ei. 1 Annual Book 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 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." 3 "Analytical reagents, ACS Specifications," Am. Chemical Soc., Washington, DC, 1950. 303 DUP050295967 D 2075 dichromate (K2Cr207)6 as follows: Weigh to the nearest 0.1 mg, by difference from a weighing bottle, 0.16 to 0.22 g of K2Cr207 that has been finely ground and then dried to constant weight at 110C prior to use. Place the K2Cr207 in a 500-mL flask or bottle and dissolve in' 25 mL'of water. Add 5 mL of concentrated hydrochloric acid (HC1, sp gr 1.19) and 20 mL of KI solution, and rotate to mix. Allow to stand for 5 min and then add 100 mL of water. Titrate with the Na2S203 solution, while shaking constantly, until the yellow color has almost disappeared. Add 1 to 2 mL of starch indicator solution and continue the titration, adding the Na2S203 solution slowly until the blue color has just disappeared. Calculate the normality N of the Na2S203 as follows: N' = (A X 20.39)/ where: A = weight of K2Cr207 used, g. and . B = volume of the Na2S2C>3 solution required for ti tration of the K2Cr207, mL. 6.9 Starch--Use soluble starch that will pass the following test for sensitivity:. Make a paste with 1 g of starch and a small amount, of cold water. Add, while stirring,. 200 mL of boiling water. Dilute 5 mL of this solution with 100 mL of water and add 0.05 mL of 0,1 N iodine solution. The deep blue color produced must be discharged by 0,05 mL of0.1 N Na2S203 solution. 6.10 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. If long storage is required, the solution shall be kept in a refrigerator at 4 to 10C (40 to 50F). Fresh indicator shall be prepared when the end point of the titration from blue to colorless fails to be sharp. 6.11 Wijs Solution (Note 3)--Dissolve 13.0 g of iodine, in 1 L of acetic acid. Gentle heat may be necessary to promote solution. Cool and remove a small quantity (100 to 200 mL) and set aside in a cool place for future use. Pass dry chlorine gas into the iodine solution until the original titration is not quite doubled. A characteristic color change takes place in the Wijs solution when the desired amount of chlorine has been added; this may be used to assist in judging the end point. A .convenient procedure is to add a small excess of chlorine and bring back to the desired titration by addition of some of the original iodine solution that was taken out at the beginning. Determine the strength of the original iodine solution and the finished Wijs solution by titration against 0.1 N Na2S203 solution, as directed in 7,6 and 7.7. Nora 3--Iodine monochloride (Wijs solution) can be purchased commercially from various laboratory supply houses. The halogen ratio should be checked prior to use. The halogen ratio, that is, the ratio of iodine to chlorine, can be determined by the Lopez Method,7 as follows: (1) Iodine Content--Pour W0 mL of saturated chlorine water into a 500-mL Erlenmeyer flask and add some glass beads. Pipet 5 mL of Wijs solution into the flask containing the saturated chlorine water. Shake and heat to boiling. Boil briskly for 10 min, cool, and add 30 mL of2 % 6 National Institute ofStandards and Technology Standard Reference Material 136 (potassium dichromate) is recommended for this purpose and should be treated as directed in the certificate ofanalysis accompanying the standard sample. 7 Journal. American Oil Chemists' Society, September 1951, p. 390. sulfuric arid (H2S04) and 15 mL of Ki solution. Mix well and titrate immediately with 0.1 N sodium thiosulfate (Na2S203) solution to a starch end point. (2) Total' Halogen Content--Pour 150 mL of recently boiled water into a clean, dry 500-mL Erlenmeyer flask. Add 15 mL of KI solution. Pipet 20 mL of Wijs solution into the flask and mix well. Titrate immediately with 0.1 jVNa2S203 solution to a starch end point. (3) Calculation ofHalogen Ratio: R = 2AK3B - 2A) where: R = halogen ratio, A = volume of Na^Oj required for titration of the iodine, mL, and B = volume of Na2S203 required for titration of total halogens, mL The halogen ratio, that is, the ratio of iodine to chlorine, should be 1.10 0.10. 7. Procedure, 7.1 Melt the sample, if it is not already liquid, in a water bath. Mix thoroughly, then weigh to 0.1 mg into two 500-mL flasks specimehs of the size given in Table 1. 7.2 Add 20 mL of glacial acetic acid. No t e A--If the specimen does not go into solution, the flask can be slightly wanned at this point until the specimen, is dissolved, but the flask must be allowed to cool to room temperature before proceeding to the next step. 7.3 Pipet 25 mL of Wijs solution into each specimen flask and two flasks to be used as blanks, allowing the pipet to drain in the same manner for both specimens and blanks. Add 10 mL of Hg(C2H3d2)2 solution directly after adding the Wijs solution. 7.4 Stopper the flasks immediately and moisten the stopper with KI solution so as to prevent the loss of iodine or Chlorine, but guard against the use of a quantity sufficient to run down the inside of the flask. Swirl the flask to obtain a good mixture. 7.5 Store the flasks in a dark place for, 3 min at a temperature of 25 5C. Swirl the flasks occasionally being careful not to allow the solution to crawl up the side of the flask over halfway. 7.6 Remove the flask from storage, and add 20 mL of KI solution, 50 mL of water, and 30 mL of chloroform. 7.7 Titrate with Na2S203, adding it gradually and with constant vigorous shaking until the yellow color has almost disappeared. TABLE 1 Iodine Value Less than 10 20 40 60 80 90 100 -110 120 130 140 160 ISO 200 Specimen Weights Specimen Wright, g 1.5 0.85 to 1,06 0.64 to 0.79 0.42 to 0.53 0.32 to 0.40 028 to 0.35 0325 to 0.32 0.23 to 029 021 to 027 020 to 024 0.18. to 023 0.16 to 020 0,14 to 0.18 0.13 to 0.16 304 DUP050295968 D 2075 --Mechanical stirring is very satisfactory for agitating during Add 2 mL of starch indicator solution, rinsing the :lor begins to disappear. Near the end ofthe titration Ir to free any iodine that dissolved so that it may be 8. Calculation 8.1 Calculate the iodine value I of fatty amines as follows: I = [(B - V)N x 12.69]/S where: V = volume of Na2S203 solution required for titration of the specimen, mL, B - volume of Na2S203 solution required for titration of the blank, mL, S' = specimen weight used, g, and N -- normality of the Na2S203 solution. The American Society for Testing and Materials fates no position respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, 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 reapprovedor withdrawn. Your comments are invited eitherforrevision of this standard or foradditionalstandards end should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which youmay 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. 305 DUP050295969 Designation: D 2076 - 64 (Reapproved 1987)' Standard Test Methods for Acid Value and Amine Value of Fatty Quaternary Ammonium Chlorides1 This slandard is issued under the fixed designation D 2076; 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 sia'ce the last revision or reapproval. These test methods were preparedjointly by ASTM and the American Oil Chemists' Society. 11. Nore:--Editorial changes were made throughout in October 1987.- 1. Scope 1.1 These test methods cover the deteimination of add value and amine value in fatty quaternary ammonium chlorides. 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: D1193 Specification for Reagent Water2 3. Definitions 3.1 acid value--the number of milligrams of potassium hydroxide needed to neutralize 1 g of sample, and is usually due to amine hydrochloride. 3.2 amine value--the number of milligrams of potassium hydroxide equivalent to the fatty amine basicity in 1 g of sample. 4. Apparatus 4.1 Erlenmeyer Flasks, wide-mouth, alkali-resistant, bo- rosilicate glass, 250-mL capacity. 4.2 Micro Buret, 10-mL capadty graduated to 0.02 mL. 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 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 D01.32 on Drying Oils. Current edition approved Aug 3.1, 1964. Published October 1964. Originally published as D 2076 - 62 T. Last previous edition D 2076 - 64 (1981 )'*. 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." grades may be Used, provided it is first ascertained that the rqagent 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 D 1193. 5.3 Bromphenol Blue Indicator Solution--Dissolve 0.2 g of bromphenol blue in 100 mL of methanol, ethanol, or isopropanol. 5.4 Hydrochloric Acid, Standard Solution (0.1 N)--Add 17 mL of concentrated hydrochloric acid (HC1, sp gr 1.19) to 1000 mL of isopropyl alcohol in a 2-L volumetric flask. Make up to volume after cooling to room temperature. Standardize with sodium carbonate using 0.1 % bromcresol green as the indicator. 5.5 Hydrochloric Acid, Standard Solution (0.2 N)--Add 34 mL of concentrated HC1 (sp gr 1.19) to 1000 mL of isopropyl alcohol in a 2-L volumetric flask. Make up to volume after cooling to room temperature. Standardize with sodium carbonate using 0.1 % bromcresol green as the indicator. 5.6 Isopropyl Alcohol (99 %)--Neutralize to the phenolphthalein end point with 0.1 N methanolic sodium hy droxide (NaOH) just before running the acid value test. 5.7 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in 100 mL of methanol, ethanol, or isopropanol. 5.8 Sodium Hydroxide, Standard Solution (0.1 N)--Dissolve 4.0 g of sodium hydroxide (NaOH) in 1000 mL of cold methyl alcohol. Allow to stand overnight in a cold room. Siphon the supernatant liquid into a clean bottle. After coming to room temperature, standardize the material with acid potassium phthalate using 1 % phenolphthalein as the indicator. 6. Procedure for Acid Value 6.1 Melt the specimen, if it is not already liquid, in a water bath, mix thoroughly, and weigh 5 to 20 g to 1 mg into a 250-mL flask,-Add 100 mL of neutralized alcohol and swirl to dissolve. Heat if necessary. 6.2 Add 1 mL of phenolphthalein indicator. If the solu tion remains colorless, titrate with 0.1 N NaOH solution to the appearance of the first persistent pink color of the same intensity as that of the neutralized alcohol before addition. If the solution turns pink, the presence of free caustic material 306 DUP050295970 # D 2076 Seated. If free caustic material is present proceed in dance with Section 8. reedure for Amine Value Weigh 5 to 20 g of sample to 1 mg into a 250-mL i, Add 100 mL of alcohol and swirl to dissolve. Heat if sary. Add 1 mL of bromphenol blue indicator and titrate 0.2 N HCI to a yellow end point. 1--If the amine value is very low, 0.1 N HCI should be used "er accuracy. ocedure for Free Caustic Material Titrate the specimen with 0.2 AT HCI until the solution colorless. | Add 1 mL ofbromphenol blue indicator and continue ration to a yellow end point. Iculation Calculate the acid value and amine value as follows: Add value or amine value = (Kx Nx 56.1)/5 ere: t= titrant used, mL, normality of titrant used, and = specimen weight used, g. ..2 If free caustic material is present, calculate the percent lee sodium hydroxide and the amine value as follows: Free sodium hydroxide, % = (A x N X 4)/S Amine value = {V x N x 56.1)/S ere: = HCI required for titration of the solution to the phenolphthalein end point, rpL, TABLE 1 Molecular Weights Fatty Quaternary Ammonium Chloride (QAC) Amine Molepular Weight Lauryl trimethyl QAC Myrlstyl trimethyl QAC Palmityl trimethyl QAC Stearyl trimethyl QAC Oleyl trimethyl QAC Tall oil fatty trimethyl QAC Coco trimethyl QAC Tallow trimethyl QAC Cotton trimethyl QAC 184 215 248 274 268 282 210 260 268 Amine Hydrochloride Molecular Weight 220 252 284 310 304 318 246 296 304 Dilauryl dimethyl QAC Dfmyristyl dimethyl QAC Dipalmityl dimethyl QAC Distearyl dimethyl QAC Dltalt oil fatty dimethyl QAC . > . Dlcoco dimethyl QAC Dlhydrogenated tallow dimethyl QAC Furftiryl hydrogenated tallow dimethyl QAC 350 401 454 539 504 387 505 354 386 438 490 576 .540 424 542 390 V = HCI required for titration of the solution from the phenolphthalein end point to the bromphenol blue end point, mL, N - normality of the HCI used, and S = specimen weight used, g. 9.3 Calculate the percent of amine hydrochloride and free amine as follows (Note .2): . t Amine hydrochloride or free amine,%- (A x V)/56l where: A = acid value or amine value, and V = molecular weight of the amine hydrochloride or free amine (Table l). No t e 2--Molecular weights listed in Table 1 are averages of prod- ucts from several processors. They are suitable for use with this test method only, since normal variations between different products do not seriously affect the calculated percent. They are not suitable in other tests, such as the determination of the percent ofquaternary ammonium chlorides by titration. The American Society for Testing and Materialstakes 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 of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at eny time by the responsible technicalcommittee and must be reviewed every five years and ifnot revised, eitherreapproved ofwithdrawn. 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 making 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. 307 DUP050295971 Designation: D 2077 - 64 (Reapproved 1987) Standard Test Method for Ash in Fatty Quaternary Ammonium Chlorides1 This standard is issued under the fixed designation D 2077; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. This test method was preparedjointly by ASTM and the American Oil Chemists' Society. 1. Scope 1.1 This test method covers the deterriiination of the nonvolatile matter remaining after a specimen of fatty quaternary ammonium chloride is completely burned and ignited. 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 Crucible--A porcelain or high-silica content glass of 250-mL capacity. 2.2 Electric Muffle Furnace. 2.3 Triangle, Nichrome q t clay. 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 D01.32 on Drying Oils. Current edition, approved Aug. 31, 1964. Published October 1964. Originally published as D 2077 - 62 T. Last previous edition D 2077 - 64 {1981). 3. Procedure 3.1 Ignite a crucible in the muffle furnace at 550 to 600C. Cool slightly, place in a desiccator for 1 h and weigh. Melt the sample if it is not already liquid, in a water bath. Mix thoroughly and weigh 20 g to 0.1 mg into the crucible. Heat gently by moving a flame on the bottom and sides of the crucible until the specimen ignites. Reduce the size of the flame until the heat is just sufficient to keep the specimen burning. Continue the heating of the specimen to a black char and transfer the crucible to the muffle furnace, heat at 550 to 600C for 1 h. Remove the crucible from the furnace, cool slightly, place in a desiccator, and cool to room temperature. Weigh and repeat the heating in the muffle furnace to constant weight. 4. Calculation 4.1 Calculate the percent of ash (Note) as follows: Ash, % =.(R/S) X 100 where: R = residue, g, and S = specimen weight used, g. ' <. No t e--Unless free caustic is found, the ash can be concluded to be essentially sodium chloride. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their, own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If notrevised, eitherreapproved or withdrawn. Your comments are invitedeither lorrevision 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. DUP050295972 Designation: D 2078 - 86 (Reapproved 1990) Standard Test Method for Iodine Value of Fatty Quaternary Ammonium Chlorides*1 This standard is issued under ibe fixed designation D 2078; 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 its parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ., This test method was preparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists' Society. scope This test method covers, the determination of die Bpe value of fatty quaternary ammonium chlorides by the |s procedure. UfoTE 1--This test method is essentially equivalent to Test Methods *959 and D2075. , v [.2 This standard does not purport to address all of the fty problems associated with its use. It is the responsibility user ofthis standard to establish appropriate safety and IIth practices and determine the applicability ofregulatory imitations prior to use. Specific hazards statements are given Section 7. [Referenced Documents (2.1 ASTM Standards: jpD 1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 |D2075 Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines2 Definition 3.1 iodine value--a measure of the unsaturation of the yl group or groups expressed in terms of percent iodine ibsorbed. Significance and Use 4.1 This test method measures the unsaturation as iodine alue in fatty quaternary ammonium chlorides by addition f an iodine/chlorine reagent. The amount of reagent abirbed is determined by back titrating the excess reagent and [Comparing it to a blank determination. 4.2 This determination is an indication of the source of le fatty component or, if the source is known, the number of the fatty components (for example, 1, 2, 3, or 4), in the quaternary ammonium chloride. |5. Apparatus 5.1 For apparatus used in this test method, see Test Method D 2075. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint 1 and Related Coatings and Materials and: is the direct responsibility of Subcom- I mittee D01.32 on Drying Oils. | Current edition approved Aug. 29, 1986. Published October 1986. Originally 8 published as D 2078 - 62 T. Last previous edition D 2078 - 85. I 2 Annual Book ofASTM Standards, Vol 06.03. 6. Reagents 6.1 For reagents used in this test method, see Test Method D 2075. 6.2 Sodium Lauryl Sulfate.3 7. Hazards . 7.1 Chloroform s a hazardous liquid that can be absorbed through the skin. Its vapor is hazardous through inhalation. It is a narcotic. Use only with adequate ventilation (in a hood). For further information; see supplier's Material Safety Data Sheet. 7.2 Wijs Solution, iodine monochloride dissolved in gla cial acetic acid, is corrosive and may cause burns to the skin and eyes. Wash clothing before reusing. Wijs solution should not be heated above 30C as it may liberate chlorine, which is a strong, irritating gas. Wijs solution can be purchased commercially or prepared in a hood. See Test Method D 2075 for instructions. 8. Procedure 8.1 Melt the sample, if not already liquid, in a water bath. Mix thoroughly, and weigh into the flask 1.5 g of sample to 0.1 mg by difference. Add 20 mL of chloroform (Warning-- See 7.1) and swirl to dissolve the material. 8.2 Pipet 25 mL of Wijs solution (Warning--See 7.2) into the.flask, allowing the pipet to drain in the same manner for both specimens and blanks. 8.3 Stopper the flasks immediately and moisten the stopper with the KI solution so as to prevent the loss of iodine or chlorine, but guard against the use of a quantity sufficient enough to run down the inside of the flask. Swirl the flask to obtain a good mixture. 8.4 Prepare and conduct at least two blank determina tions with each group of specimens simultaneously and similar in all respects. 8.5 Store the flasks for 30 min in a dark place at a temperature of 25 5C. Swirl the flasks occasionally, being careful not to allow the solution to crawl up the side of the flask more than half-way. 8.6 Remove the flasks from storage and add 20 mL KI solution followed by approximately 2.2 g of sodium lauryl sulfate and 40 mL of water. No t e 2--Sodium lauryl sulfate is added to prevent the free iodine from being tenaciously held by the nonaqueous phase, thus giving a sharper end point. 3 Sodium lauryl sulfate manufactured by K & K Laboratories, inc,, 121 Express St., Plainview, NY 11803 has been found suitable for this purpose. 309 DUP0502 95973 # D 2078 8.7 Titrate with 0.1 N Na.2S203 solution, adding it gradu ally and with constant vigorous shaking until the tannish color has almost disappeared. Add 2 mL of starch indicator solution, rinsing the neck ofthe flask therewith and continue the titration until the blue to brown color begins to disap pear. Near the end of the titration it is necessary to shake violently, with the stopper inserted, in order to free any iodine that is dissolved so that it may be taken up with the KI solution. Only allow the stopper to come into contact with the liquid at this stage. Titrate to disappearance ofblue color. 9. Calculation 9.1 Calculate the iodine value of fatty quaternary ammo nium chlorides, /, as follows: J-(B-V)[(Nx 12.69)/5] where: V = volume of Na2S203 solution required for titration of the specimen, mL, B = Na2S203 solution required for titration of the blank, mL, S -- specimen weight, g, and N - normality of the Na2S203 solution. 10. Precision and Bias 10.1 Precision and bias data were not established at the time this test method was written. An effort is being made to obtain the precision and, if obtainable, will be published in future revisions. This test method has been in use for many years, and its usefulness has been well established. The American Society for 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 entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invitedeither for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting 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, 7975 Race St.. Philadelphia, PA 19103. ' : a 310 DUP050295974 Designation: D 2079 - 82 (Reapproved 1987) Standard Test Method for Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides1 This standard is issued under the fixed designation D 2079; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovaL A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This method waspreparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists' Society. IScope jf.l This method covers the determination of nonvolatile ter (solids) in fatty quaternary ammonium chlorides. |jj.2 This standard may involve hazardous materials, operjpis, and equipment. This standard does not purport to ` dress all ofthe safety problems associated with its use. It is Ejf responsibility of the user of this standard to establish mropriate safety and health practices and determine the |pliability ofregulatory limitations prior to use. 'Summary of Method [2.1 Volatile matter is evaporated under heat and vacuum ad the nonvolatile matter determined. a, Apparatus 13.1 Vacuum Oven, with suitable controls for maintaining j temperature of 105 2C. '1 This method is under the jurisdiction ofASTM Committee D-l on Paint and ited Coatings and Materials and is the direct responsibility of Subcommittee 01.32 on Drying Oils. : . Current edition approved June 25, 1982. Published September 1982. Originally [^published as D 2079 - 62 T. Last previous edition D 2079 - 64 (1976). 3.2 Air Oven, with suitable controls for maintaining a temperature of 105 2C. 4. Procedure 4.1 If not a liquid, melt the sample using a water bath. Mix the sample thoroughly and accurately weigh 0.7 to 1.0 g to 0.1 mg into a 50-mL narrow-mouth Erlenmeyer flask. Place the flask in the air oven for 1 h at 105 2C. After about 15 min of oven time, rotate the flask gently to coat the specimen over the entire bottom of the flask. Place the flask in a vacuum oven for 8 h at 105 2C and a vacuum (negative gage pressure) of 27 to 29 in. Hg (absolute pressure of 25 to 35 mm Hg). Cool in a desiccator for xh h and reweigh. 5. Calculation 5.1 Calculate the percent of nonvolatile matter (solids) as follows: Nonvolatile matter (solids), % -- (R X 100)/S where: R = grams of residue, and S = specimen weight used, g. 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 reWetved every five years and ifnot revised, either reapproved or withdrawn. Yourcomments 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. 311 DU PO 50295975 Designation: D 2080 - 64 {Reapproved 1987) Standard Test Method for Average Molecular Weight of Fatty Quaternary Ammonium Chlorides1 This standard is issued under the fixed designation D 2080; 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 (0 indicates an editorial change since the last revision or reapprovai This method was preparedjointly by the American Societyfor Testing and Materials and the-American Oil Chemists'Society. 1. Scope 1.1 This method covers the determination of the average molecular weight of a fatty quaternary ammonium chloride by converting to the acetate, titrating potentiometrically, and correcting for the nonquaternary components. 1.2 This standard may invoke hazardous materials, oper ations, and equipment. 'This- standard does not purport to address all ofthe safety problems associated with its Use. It is the responsibility of the'user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: <: D 1193 Specification for Reagent Water2 D2076 Test Methods for Acid Value and Amine Value of Fatty Quaternary Ammonium Chlorides3 D 2077 Test Method for Ash in Fatty Quaternary Ammo nium Chlorides3 D2079 Test Method for Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides3 : E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 3. Apparatus . ; 3.1 Buret, having a capacity bf 25 mL. 3.2 Glass Electrode pH Meter, conforming to the require ments of Method E 70 or similar potentiometric titrator, and carefully standardized in accordance with the manufacturer's instructions. 3.3 Magnetic Stirrer, with inert plastic-coated stirring bar. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available3 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 confoqning to Specification D 1193, Type II. 4.3 Acetic Acid (Glacial) (CH3COOH). 4.4 Acetic Anhydride (CH3CO)20. 4.5 Chloroform (CHQ3). 4.6 Mercuric Acetate Solution--Dissolve 6 g of mercuric acetate [Hg(C2H302)2] in 100 mL of glacial: acetic acid. Prepare fresh for each determination. Caution--Mercury compounds are harmful and accumulate in the aquatic environment. Mixtures containing mercury compounds should not be flushed down a drain but disposed of as a hazardous waste. 4.7 Perchloric Acid, Standard Solution (0.1 N): 4.7.1 Add 28.4 g of 70 to 72 % perchloric acid (HCIO4) to 1000 mL of glacial acetic acid in a 2-L beaker while stirring. Carefully add 46.6 g of acetic anhydride while stirring. Carefully pour the solution through a glass funnel into a 2-L volumetric flask and dilute to mark with glacial acetic acid. Mix the solution and allow to stand for 24 h before standardizing. 4.7.2 Standardize against acid potassium phthalate (HKQH4O4).6 Weigh 0.31 to 0.39 g to the nearest 0.1 mg of finely ground and dried HKC8H4(Vinto a 200-mL beaker. Add 50 mL of glacial acetic acid arid warm; gently to dissolve. Cpol and add an additional 50 ihL of glacial acetic acid so as to wash down the sides of the beaker. Insert the stirring bar into the beaker and adjust the beaker so that the lower half of each electrode of the pH meter is immersed in the solution. Start the stirrer and adjust the speed so that there is vigorous stirring without spattering. Titrate with the HC104 solution using the millivolt scale. Record the millivolt readings every millilitre, but in the vicinity of the end point, record the millivolt readings every 0.1 mL. Plot a graph showing the millivolts against the millilitres required for titration. Calcu late the normality of the HC104 solution as follows; Normality = (4.8967 X A)/V ! 1 This method is under thejurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.32 on Drying Oils. Current edition accepted Aug. 31, 1964. Originally issued 1962. Replaces D 2080-62 T. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 15.05. 3 "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 "Reagents Chemicals and Standards," by Joseph Rosin, D.Van Nostrand Co., Inc., New York, N.Y., and the "United States Pharmacopeia." 6 National Bureau of Standards standard sample No. 84f of HKC8H40 is recommended for this purpose and should be treated as directed in the certificate of analysis accompanying the standard sample. 312 DUP050295976 # D 2080 grams of HKCgH404 used, and !l millilitres of the HC104 solution required for titration of the KHCgH404. ecaution ,1 This standard may involve the use of hazardous terials, operations, and equipment It is the responsibility hoever uses this standard to establish appropriate safely dices to determine the applicability of regulatory Iimitas prior to use. rocedure 1 Determine the acid value, amine value, percent of free ae, and percent amine hydrochloride in accordance with Methods D 2076. Determine the percent of ash in rdance with Test Method D 2077. Determine the perof nonvolatile matter in accordance with Test Method 079. .2 Melt the sample if not liquid, in a water bath, mix Lroughly, and weigh 1.0 to 1.5 g to the nearest 0.1 mg. The lit will vary somewhat 'with the average molecular it. .3 Add- lOO mL of glacial acetic acid and heat gently, if pessary to affect solution. Add 15 mL of Hg(C2H302)2 ution. Insert the stirring bar into the beaker and stir for 5 in. 6.4 Add 20 mL CHC13 and adjust the beaker so that the lower half of each electrode of the pH meter is immersed in the solution. Adjust the speed of the stirrer so that there is vigorous stirring without spattering. Titrate with 0.1 N HCI04 using the millivolt scale. Record the millivolt read ings every millilitre, but in the vicinity of the end point, record the millivolt readings every 0.1 mL. Plot a graph showing the millivolts against titration. 7. Calculation 7.1 Calculate the average molecular weight as follows: Average molecular weight =-------------------- ^ fVxN\ A E F where: Wx 10/ 58.5 561 561 L = percent of nonvolatiles, A = percent of ash, C -- percent of amine hydrochloride, D -- percent of free amine, E != acid value, F = amine value, N = normality of the HC104 solution, S = specimen weight used, g, and V = millilitres of HC104 required for titration of the solu tion. TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any lime by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Yourcomments areinvited either forrevision of this standard or for addiional 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. 313 DUP050295977 Designation: D 2081 - 64 (Reapproved 1987) Standard Test Method tor pH of Fatty Quaternary Ammonium Chlorides1 This standard is issued under trie fixed designation D 2081; 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 revirion or reapproval. This method was preparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists' Society, 1. Scope 1.1 This method covers the preparation of 5 % solutions of fatty quaternary ammonium chlorides and the determina tion of their pH. 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 ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: ' D1193 Specification for Reagent Water2 D2079 Test Method for. Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides2 E 70 Test Method for pH of Aqueous Solutions with the' Glass Electrode3 3. Apparatus 3.1 Glass Electrode pH Meter, conforming to the require ments of Method E 70. 3.2 Magnetic Stirrer, with inert plastic-coated stirring bar. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the 1 This method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.32 on Drying Oils. Current edition accepted Aug. 31, 1964. Originally issued 1962. Replaces D2081 -62 T. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 15.05. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, D. C. 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, N. Y,, and the "United States Pharmacopeia." reagent is of sufficiently high purity to permit its use without lessenmg the accuracy of the determination. 4.2 'Purity' of Water--^Unless otherwise indicated, refer-: ences to water shMl be understood to meali reagent water conforming to Specification D 1193, Type II. 4.3 ISopropyl Alcohol Solution (l41)--Mix. equal volumes of isopropyl alcohol (99 %) and water. 5. Precaution 5.1 This standard may involve the use of hazardous materials, operations, and equipment. It is the responsibility'' of whoever uses this standard to establish appropriate'safety practices to determine the applicability of regulatory limita tions-prior to use. 6. Standardization of pH Meter 6.1 Carefully follow the manufacturer's instructions for the particular meter used and standardize at a pH of 7.0. 7. Procedure 7.t Determine the percent of nonvolatile matter (solids) as directed in Method D 2079. > 7.2 Determine the specimen weight based on the percent of nonvolatile matter heeded to make 200 g ofa 5 % solution as follows: Grams of sample = (200 x 5) % of nonvolatile matter 7.3 Melt the sample if it is not already liquid, in a water bath. Mix thoroughly, and weigh the proper amount into a 250-mL low-form beaker. Add 100 g of isopropyl alcohol solution and warm, if necessary, to dissolve the specimen. Cool to room temperature and add enough isopropyl alcohol solution into the beaker to make a total of 200 g of isopropyl alcohol solution and specimen. 7.4 Adjust the beaker so that the lower half of each electrode of the pH meter is immersed in the solution. Start the stirrer and adjust the speed so that there is vigorous stirring with no spattering. Read the pH as soon as the instrument shows a steady reading. No t e--Most commercial fatty quaternary ammonium chloride prod ucts contain small amounts ofdissolved methyl chloride that hydrolyzes to hydrochloric acid which gradually decreases the pH of a given material on storage. Differences in pH values determined at different times or in different laboratories may be due in part to this factor. 8. Report 8.1 Report the results to the nearest 0.1 pH unit. 314 DUP050295978 D 2081 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 (he responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Yourcomments are Invited either forrevision ofthis standard ortoradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, 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. 315 DUP050295979 Designation: D 2082 - 82 (Reapproved 1987) Standard Test Method for Percent of Non-Amines in Fatty Nitrogen Compounds1 This standard is issued under the fixed designation D 2082; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This method was preparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists' Society. 1. Scope 1.1 This method covers the determination of the per centage of non-amine components in fatty amines and diamines. 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: D1193 Specification for Reagent Water2 3. Summary of Method 3.1 A specimen of the fatty amine compound is dissolved in alcohol and passed through an ion exchange column. The amine components of the specimen are retained on the column and the nonamine components pass through the column and are collected and weighed. A correction factor is applied to correct for any amine components that pass through the column. 4. Apparatus 4.1 Chromatographic Columns, made by attaching 500- mL bulbs with 24/40 joints to chromatographic tubes and with attached fritted-glass disks inside a 19/22 joint (Fig. 1). 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 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.33 on Drying Oils. Current edition approved June 25, 1982. Published September 1982. Originally published as D 2082 - 65 T. Last previous edition D 2082 - 66 (1976). 2 Annual Book ofASTM Standards, Vols 06.03. and 11.01. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, D. C. 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, N. Y., and the "United States Pharmacopeia." 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 Bromphenol Blue Indicator Solution--Dissolve 0.2 g of bromphenol blue in 100 mL of methanol, ethanol, or isopropanol. 5.4 Hydrochloric Acid, Standard Solution (0.2 N)--Add 34 mL of concentrated HC1 (sp gr 1.19) to 1000 mL of isopropanol in a 2-L volumetric flask. Make up to volume after cooling to room temperature. Standardize against sodium carbonate using brotncresol green as the indicator. 5.5 Methanol, Ethanol, or Isopropanol (99 %). 5.6 Resin, Cationic, Ion-Exchange,4 500 to 100 mesh. 4Dowex 50W-X4 resin obtainable from the Dow-Coming Corp., Midland, Mich., has been found satisfactory for this purpose. 316 DUP0502 95980 D 2082 preparation of Chromatographic Columns Jl Place the resin in a 250-mL beaker, pour 100 mL of hand, ethanol, or isopropanol on the resin, and stir. Filter with suction through a 350-mL coarse sinteredfunnel. Repeat until there is no residue left upon poration of the alcohol used to wash the resin. Transfer washed resin to a bottle and add enough isopropyl hoi to just cover the resin. 1.3 To fill the chromatographic column first place apximately 10 mm of glass wool oh top of the fritted-giass then pour a slurry of resin in methanol, ethanol, or propanol on top of the glass wool: For fatty amines use a i-mm column and pour in enough resin to just fill the limn after the resiii has settled. For fatty diamines a >mm column'should be packed with 450 mm of resin. |ce the resin has been placed in the column, keep it ered with alcohol at all times. tore 1--Blanks should be run on each new batch ofresin. Use 80 g sin for duplicate determinations of fatty amines using 200-nun tins and 200 g ofresin for duplicate determinations using.500-mm Ohs for fatty diamines. Experience has shbwn that the total-quantity hethanol, ethanof -or isopropanol required for washing the resin is l mL for 80-gibatches and 900 mL for 200-gbatches of resin. Procedure 7.1 Accurately weigh into a 150-tnL beaker approxiitely 5 g of the sample for fatty amines or 2.5 g of the iple, for fatty diamines. Add 75 mL of alcohol and warm dissolve the specimens. if No t e 2--Since some amines arb not veiV soluble in alcohol, it is |ecessary to heat the chromatographic column`bulb so that the amine elution is maintained at 55 to 6QC until it has passed-onto the resin, he heating can be discontinued when the 500 mL ofalcohol are added. bulb can be conveniently heated by suspending the bulb through a eating mantle top, of a size to fit a 500-mL flask, which is connected to autotransformer. 1. > 7.2 Allow the alcohol to fall to the top of the resin column and quantitatively transfer the amine solution onto the column so as not to disturb the resin. Wash the beaker with a small quantity of hot (55 to 60X1) alcohol and add to the column. 7.3 Place a j-L beaker under the column to collect the eluate. When the specimen solution has: run down to the top of the resin, slowly add 500 mL of alcohol so as not to disturb the resin. When the alcohol level is low enough, add another 200 mL of alcohol to the bulb. Collect the eluate until the flow stops. 7.4 Evaporate the eluate on the steam bath to about 75 mL and quantitatively transfer it to a tared 250-mL beaker containing several glass beads. Evaporate the concentrated eluate to dryness on the steam bath. Dry the residue in a vacuum oven at 70C for 2 h at a vacuum (negative gage pressure) of 27 to 29 in. (absolute pressure of 25 to 35 mm Hg). 7.5 Weigh the beaker containing the dried residue. Dis solve the residue in 50 mL of alcohol. Add 5 to 10 drops of bromphenol blue indicator solution and, while swirling, titrate to a yellow end point with 0 to 2 N HC1 from a microburet. No t e 3--The titration is performed to determine the small amount of fatty amine that may be present in the residue. It is assumed that amines that pass through the column have the same mean molecular weight as those in the original sample. 8. Calculation 8.1 Calculate the percent of nonamine as follows: Nonamine, % = [1.00 - (VxNx 56A)/(R X Q] x (R/S) X 100 where: V = millilitres of HC1 required for titration of the solution, N = normality of the HC1, R = weight of residue, g, C = amine value of the sample, and S == specimen weight used, g. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any /ton mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised^either reapprcnred or withdrawn. Your comments are invited either forrevision ofOtis standard orfor additionalstandards and should be addressed to ASTM Headquarters, Your comments wHI 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. 317 DUP050295981 Designation: D 2083 - 66 (Reapproved 1987) Standard Test Method for Calculation of Percent of Primary, Secondary, and Tertiary Amines in Fatty Amines1 This standard is issued under the fixed designation D 2083; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This method was preparedjointly by the American Societyfor Testing and Materials and the American Oil Chemists Society. 1. Scope 1.1 This test method covers calculation of the percent of primary, secondary, and tertiary amines in the sample from determinations of primary, secondary, and tertiary amine values and percent of non-amine. 1.2 This test method is applicable to materials containing only fatty primary amines, difatty secondary amines, trifatty tertiary amines, and nonamines. This method is not appli cable to blends such as a mixture of coco primary amine and tallow difatty secondary amine. 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: D2073 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines, Amidoamines, and Diamines by Referee Potentiometric Method2 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 D0I.32 on Drying Oils. Current edition approved Sept. 20,1966. Published November 1966. Originally published as D 2083 - 65 T. Last previous edition D 2083 - 65 T. 1 Annual Book ofASTM Standards, Vol 06.03. D2074 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method2 D2082 Test Method for Percent of Non-Amines in Fatty Nitrogen Compounds2 3. Procedure 3.1 Determine primary, secondary, and tertiary amine values in accordance with Test Methods D 2073 or D 2074.: 3.2 Determine the percent of non-amines in accordance with Test Method D 2082. 4. Calculation 4.1 Calculate the percent of amines as follows (Note): where: Let X = average molecular weight of the primary amine, PAV = primary amine value of the sample, SAV = secondary amine value of the sample, TAV = tertiary amine values of the sample; and PNA ~ % non-amine. then: ,, 561(100 - PNA) + Y1{SAV) + M(TAV) A PAV+ 2(SAV) + %TAV) i ` j and Primary amine, % = PAV(X)j561 Secondary amine, % = SA V(2X -- 17)/561 Tertiary amine % = TAV(3X- 34)/561 No t e--The equations given in 4.1 are based upon the assumption that the alkyl chain lengths in the monofatty, difatty, and trifatty amines are the same average length. TheAmerican Society tor Testingand Materials takes noposition 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, eitherreapprovedor withdrawn. Your comments are invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 318 DUP050295982 Designation: D 2086 - 89 Standard Test Method for Acidity in Vinyl Acetate and Acetaldehyde1 This standard is issued under the Fixed designation D 2086; 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 oflasl neapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ope 'T This test method covers the determination of total 'ty as acetic acid in refined vinyl acetate and acetalde- p- This standard may involve hazardous materials, oper as, and equipment. This standard does not purport to ess all ofthe safety problems associated withits use. It is responsibility of the user of this standard to establish iopriate safety and health practices and determine the licability of regulatory limitations prior to use. For Be hazard statements, see Section 8. ;3 For hazard information and guidance, see the sup er's Material Safety Data Sheet. referenced Documents 2.1 ASTM Standards: t> 1193 Specification for Reagent Water2 1200 Practice for Preparation, Standardization, and Stor age of Standard Solutions for Chemical Analysis3 Summary of Test Method 3.1 The specimen is mixed with either an equal volume of "'ed water or an equal volume of ethyl alcohol and titrated reduced temperature with aqueous sodium hydroxide 'ution to a phenolphthalein end point. Significance and Use j, .4.1 This test method provides a measurement of total 'dity in vinyl acetate and acetaldehyde. The results ofthese easurements can be used for specification acceptance. . Interferences 5.1 Any material or contaminant' that will react with TaOH under the test conditions will affect the results. { 5.2 Vinyl acetate will decompose on storage, typically by way of hydrolysis, to form acetic acid. 5.3 Acetaldehyde will react with oxygen, either dissolved or in a storage container, to form acetic acid. 5.4 Various acids or other acidic materials may be present. Common practice, including the method used here, calculates these as acetic acid. The actual weight percent of 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 31, 1989. Published May 1989. Originally published as D 2086 - 62 T. Last previous edition D 2086 - 84. 1 Annual Book ofASTM Standards. Vois 06.03 and 31.0). 3 Annual Book ofASTM Standards, Vol 15.05. acidic materials may be different. 6. Apparatus 6.1 Buret, 10-mL, graduated in 0.05-mL subdivisions. 6.2 Erlenmeyer Flask, 250-mL capacity. 6.3 Graduated Cylinder, 50 or 100-mL capacity. 6.4 Cold Bath, maintained at 0C or below. 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.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. 7.2 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; 7.3 Ethyl Alcohol (Ethanol), 95 volume %, minimum. No t e 1--Denatured ethyl alcohol conforming to Formula No. 3A of the U.S. Treasury Department, Bureau of Industrial Alcohol, is suitable for use as a solvent. 7.3 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in 100 mL of methanol, ethanol, or isopropanol. 7.4 Sodium Hydroxide, Standard Solution (0.05 N)-- Prepare and standardize a 0.05 2V sodium hydroxide (NaOH) solution (Note 2) in accordance with the Sodium Hydroxide Solution sections of Practice E 200. No t e 2--Alternatively, potassium hydroxide (KOH) solution may be used. 8. Hazards 8.1 Vinyl acetate and acetaldehyde are flammable and hazardous as their vapors form explosive mixtures with air. 8.2 Acetaldehyde boils at 21"C; therefore, store in pres sure containers or refrigerate ifkept in glass containers. Wear safety goggles or a full face shield when handling acetal dehyde. 9. Procedure for Vinyl Acetate (Warning--see Section 8) 9.1 Measure into a 250-mL Erlenmeyer flask 50 mL of ethanol. 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." 319 DU P050295983 # D 2086 9.2 Add 0.5 mL of pfaenolphthalein indicator solution. Titrate with 0.05 N NaOH solution to the first perceptible pink color. 9.3 Add 50 mL ofthe specimen from a graduated cylinder and cool the solution to approximately 0C in the cold bath. 9.4 Titrate with the 0.05 N NaOH solution to the same first perceptible pink color originally obtained in 9.2. 10. Procedure for Acetaldehyde (Warning--see Section 8) 10.1 Measure into a 250-mL Erlenmeyer flask 50 mL of water and add sufficient crushed ice (prepared from reagent water) so that some ice will remain at the end of. the determination. ( 1 \ . No t e 3--Titration at low temperature avoids interference and is required because of the low boiling point of acetaldehyde., 10.2 Add 0.5 mL of iphenolphthaleSn indicator solution and titrate with 0.05 N NaOH solution to the first perceptible pink color. 10.3 By means of a graduated cylinder add 50 mL of the acetaldehyde specimen that jirevidusly has been chilled to 0 to 5C. 10.4 Titrate immediately with the 0.05 N NaOH solution to the same first perceptibleTtink color originally obtained in 10.2. ' - ' 11., Calculation 11.1 Calculate the acidity A of the specimen as follows: 11.1.1 Acidity as weight %. acetic acid: . , A '--(VN x 0.060 x 100)/50 Z> = (Wx 0.12)/D or 11.1.2 Acidity as milligrams KOH per gram of specimen;1 = (Wx 0.056 X 1000)/50 D = (VN x \A2)/D where: , . V = volume of NaOH solution required for titration of the specimen, mL, N - normality of the NaOH solution, . . D,, - specific gravity of th.e specimen, 0.060 = milliequivalent weight of acetic acid, and 0.056 = milliequivalent weight of KOH. 12. Report i 12.1 Report the following information: 12.1.1 The percent of acetic acid to the nearest 0.001 %. 12.1.2 Vinyl Acetate--Duplicate determinations that | agree within 0.004 %, absolute, are acceptable for averaging f (95 % confidence level). 12.1.3 Acetaldehyde--Duplicate determinations that agree within 0.010 %, absolute, are acceptable for averaging (95 % confidence level). 13. Precision and Bias 13.1 The following criteria should be used for determining the acceptability of results at the 95 % confidence level. 13.2 Vinyl Acetate: . 13.2.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same analyst should be considered suspect if they differ by more than 0.006 %, absolute. >: 13.2.2 Reproducibility--Two results, each the * mean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 0.008 % absolute. . . No t e 4--The above precision estimates are. based upon an intcriab- oratory study on four samples of vinyl acetate containing 0.006, 0.013, 0.026, and 0.037 % acetic acid. Each sample was analyzed in duplicate : by two analysts in each of four different laboratories on two different days. - 13.3 Acetaldehyde: 13.3.1 Repeatability--Two results, each the mean pf du plicate determinations, .obtained by the same analyst should be considered suspect if they differ by more than 0.014 % absolute. 13.3.2 Reproducibility--Two results, each the mfean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 0.035 %, absolute. < No t e 5--The above precision estimates'ate based on an inteflaboratory study on samples of acetaldehyde containing 0.034 and 0.146 % acetic acid. Each sample was analyzed in duplicate by two analysts in each of five different laboratories on two different days. ' 13.4' Bias--Bias has not been determined for this test method (see Section 5). The American Society for Testing and Materials takes no position respecting the validity of any patent rlghta asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any tittle by the responsible technical committee and must be reviewed every five years end ifnot revised, either reapproved or withdrawn. Your comments are Invited'either for revision of this standard Or for additionalstandards' and should be addressed to ASTM Headquarters. Your comments will receive 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, 19!6-Race St., Philadelphia, PA 19103. 320 DUP050295984 Designation: D 2087 - 89 Standard Test Method for Iron in Formaldehyde Solutions*1 This standard is issued under the fixed designation D 20S7; 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. cope ,1 This test method covers the determination of the total content of formaldehyde solutions. ,2 This standard may involve hazardous materials, oper as, and equipment. This standard does not purport to fess all ofthe safety problems associated with its use. It is responsibility of the user of this, standard to establish fopriate safety and health practices and determine the licability of regulatory limitations prior to use. For ic hazard statements see Section 7. j.3 For hazard information and guidance, see the sup er's Material Safety Data Sheet. Referenced Document .1 ASTM Standard: ,D 1193 Specification for Reagent Water2 j Summary of Test Method '3.1 The specimen is evaporated and ashed; the iron, duced to the divalent state by the addition of hydroxylane hydrochloride, is reacted with o-phenanthroline to velop a color that is measured at 510 nm. { Significance and Use 4.1 This test method provides a measurement of iron ntent of formaldehyde solutions. The results of these tasurements can be used for specification acceptance. Apparatus 5.1 Spectrophotometer, capable ofmeasuring light absorp'on at 510 nm. 5.2 Absorption Cells, minimum light path, 10 mm. 5.3 Evaporating Dishes, 90-mm diameter, high-silica glass. . Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be ed in all tests. Unless otherwise indicated, it is intended hat 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 ^ 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 31, 1989. Published May 1989. Originally 1 published as D 2087 - 62 T. Last previous edition D 2087 - 84. 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." reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. 6.3 Ammonium Acetate Solution (100 g/L)--Dissolve 100 g of ammonium acetate (NH4C2H3O2) in 100 mL of water. Add 200 mL of acetic acid (CH3COOH), dilute to 1 L with water, and mix. 6.4 Ammonium Hydroxide (1+1)--Mix equal volumes of concentrated ammonium hydroxide (NH4OH, sp gr 0.90) and water. 6.5 Congo Red Paper. 6.6 Hydrochloric Acid (1+1)--Mix equal volumes of con centrated hydrochloric acid (HQ, sp gr 1.19) and water. 6.7 Hydroxylamine Hydrochloride Solution (100 g/L)-- Dissolve 10 g of hydroxylamine hydrochloride (NH2OHHQ) in water and dilute to 100 mL. 6.8 Iron, Standard Solution (1 mL = 0.05 mg Fe)-- Dissolve 0.3510 g of ferrous ammonium sulfate (FeS04(NH4)2S04-6H20) in 50 mL of water and 20 mL of concentrated sulfuric acid (H2S04, sp gr 1.84). Dilute with water to 1 L in a volumetric flask and mix. 6.9 o-Phenanthroiine Solution (1 g/L)--Dissolve 0.1 g of o-phenanthroline in 10 mL of iron-free ethyl alcohol4 and dilute to 100 mL with water. 7. Hazards 7.1 Formaldehyde and formaldehyde solutions are toxic and exposure to them should be minimized to avoid acute effects and possible sensitization. 7.2 The reagents acetic acid, ammonium hydroxide, hy drochloric acid, and sulfuric add are hazardous; they may cause severe bums to the skin and eyes. 8. Calibration 8.1 Prepare a series of standards by adding the reagents described in 9.3 to 0.2, 0.5, 1.0, 2.0, 3.0, 4.0, and 5.0-mL of standard iron solution in 100-mL volumetric flasks, and diluting to volume. 8.2 Make spectrophotometer comparisons in the absorp tion cells and prepare a calibration curve by plotting the absorbances of the standard iron solutions against the milligrams of iron per 100 mL of solution. This curve must be determined for each instrument and should be checked periodically. 4 Specially denatured ethyl alcohol conforming to Formula No. 30 ofthe U. S. Treasury Department, Bureau of Industrial Alcohol has been found satisfactory for this purpose. 321 DU P0502 95985 3 9. Procedure # D 2087 I 11 r|Bcontamination in the reagents. Correct the results obtained 9.1 Clean a high-silica glass3 evaporating dish as follows: in 9.4 accordingly. Add 10 mL of HC1 (1+1), cover with a watch glass, and digest on a steam bath for about 20 min. Then discard the HC1 solution, rinse the dish with water, and dry. 9.2 Weigh 50 g of sample into the cleaned dish and evaporate to dryness on an electric hot plate in a hood: Ifany organic matter remains^ ignite for 5 min over a high- 10. Calculation 1 10.1 Calculate the parts per million of iron I as follows: I -- (1F/5) x 1000 / where: W -- weight, of iron found mg, and s temperature gas burner. S = weight of sample used, g. 9.3 Add 10 mL of HOi.(l+l), cover with a watch glass, and digest on the steam bath for 15 min. Transfer quantita tively to a 100-mL volumetric flask. Add the following reagents in order, mixing after the addition of each: 1 mL of NH2bH*HCl solution, 5 mL of o-phenanthroline solution, enough NH4OH (1+1) as required to make the solution just alkaline to Congo red paper (approximate pH range 3.0 to 5.0), and 5 mL of NH4C2H3O2 solution. Dilute to the mark with water and mix thoroughly. 9.4 Allow to stand for 5 miri, fill an absorption cell, and measure the absorbance at 510 nm with the spectrophotom eter. From the calibration curve, read the milligrams of iron present. 9.5 Carry a blank containing no added iron through all steps of the procedure in order to correct for any iron 11. Report 11.1 Report the mass of iron to the nearest parts per million. 12. Precision and Bias 12.1 Repeatability--The difference between two detern&,, nations by the same operator is normally about 0.6 ppm. Two such results should be considered suspect if they differ by more than 0.16 ppm. 12.2 Reproducibility--The difference between two results obtained by operators in different laboratories is normally about 0.11 ppm. Two such results should be considered suspect if they differ by more than 0.3 ppm. 12.3 Bias--Bias has not been determined for tliis test method. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are 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, eitherreapproved 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, 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. ms 322 DUP050295986 Designation: D 2090 - 88 Standard Test Method for Clarity and Cleanness of Paint and Ink Liquids1 This standard is issued under the fixed designation D 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 parenthesesindicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. pScope .1 This test method covers a procedure for the visual lamination of any unpigmented liquid for use in paints and including fatty oils and acids, drier.solutions, solvents, *cellaneous chemicals, varnishes, resin solutions, clear alters, and other clear coatings for the presence or absence fundesirable components. 1.2 This standard may involve hazardous materials, operfjons, and equipment. This standard does not purport to ress all ofthe safety problems associated with its use. It is W responsibility of the user., of this standard to, establish wropriate safety and health practices and determine the |plicabilily ofregulatory limitations prior to use. g Referenced Documents 12.1 ASTM Standards: D1003 Test Method for Haze and Luminous Transmit tance of Transparent Plasties2' D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 < D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method4 . Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 There are various terms for clarity or cleanness of iquids, which are established as trade vernacular in de scribing undesirable components of a liquid. The following Vseven are preferred over the other terms (in bold face) related to them: ; 3.1.2 foreign matter--way 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--& relatively great amount of nonsettling Hoc, 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 D-l 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 December 198$. 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, Vo! 08.01. 3 Annual Book ofASTM Standards. Vo! 06.01. 4 Annual Book ofASTM Standards, Vols 06.03, 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 con tainer, in the specified sample containers, and then in a film thin enough to show any nonumformity. 5. Significance and Use 5.1 The results of the clarity arid cleanness examinations are used as controls in production, and for specification acceptance of any nonpigmetited 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 phosphatides, waxes, 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 and for "making the examination. When not stated otherwise, the sample is presumed to have been stable for any period of time and observedat 77F (25C). 8. Procedure 8.1 Examine all parts of the sample and its container under at least 50 fit-candles (53.8 lx) of light for any nonuniformity. 323 DUP050295987 # D 2090 8.2 Transfer some of the sample to fill a clean GardnerHoldt tube as specified in Test Method D 1545 to leave an air bubble under a clean stopper. Tilt the tube at a small angle from the horizontal so that the air bubble will move slowly and permit observation in the moving liquid of any fine particles that may produce a haze in the specimen. 8.3 Drain the tube of 80 to 90 % of its contents, replace the stopper, let stand vertically for 15 min or other time specified to allow a highly viscous specimen to complete its flow to the bottom, while leaving a very thin film of the specimen over the upper walls of the tube, and while still protected from extraneous dust and from evaporation. Examine the drained, vertical tube by both transmitted and reflected strong light to detect particles ofany sort in the thin film. A liquid may appear clear in mass, yet not clean in a thin film. No t e--Many variables influence the choice of details of specimen conditioning and examination, such as: Highly colored bitumen solutions; driers, varnishes, etc., that never theless may be judged to be clear and clean when examined in a very thin film. Relative pure fatty adds may have narrow melting ranges of temperature, and their cleanness is easily observed at a temperature of 50F (27.8"C) above their melting point, whereas gross or dark mixtures of fatty adds may have such a wide range of melting temperature that specification oftime and temperature for specimen conditioning and for passing a clean test may constitute'a convenient, proximate method of limiting their composition. Glyceride oils may contain small amounts of fatty adds, phosphatides, waxes, and high melting glycerides, for example, stearin in fish oil; specification of time, temperature, and air and moisture exposure for spedmen conditioning and for pasting a clean 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 particles which spoil the appearance of high gloss paints and enamels made from them. The drained tube technique is particu larly useful in detecting these particles 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 dther 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 ASTM test method to fill a recognized need. It is published as information only and offered without prejudice against dther test methods. XI.1 Summary of Test Method XI. 1.1 A specimen of liquid is placed in a curette and a parallel beam of light shining through it is measured at the normal (sere) angle of emergence and also at an angle 10 from normal. The ratio of intensities of the emergent beams is a measure of clarity. X1.2 Procedure X1.2.1 Test the specimen in accordance with Procedure A 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 XI.3.1 Calculate percent haze Has follows: H = (TJT;) x 100 where: Td = diffuse transmittance, and Tt = total transmittance. 324 DUP050295988 # D 2090 REFERENCES Nimeroff, I., "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. ) Billymer, Jr., F. W., "Measurement of Optical Clarity by Low- Angle Light Scattering," Journal, Optical Soc. Am., Vol. 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. <3., "Light.Scattering 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 fuller's 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 Committee D-l, Subcommittee II, Group II, on Gum Determina tions in Linseed Oil. ' The American Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such . patent rights, and the risk of infringement of such rights,, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and mustbe reviewed every five years and ifnotrevised, either reapproved or withdrawn. Yourcomments are Invited either for revision of this standard or for additional standards : and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may'.attend., if you feel that your comments have not received a fafr hearing you should make your views known to the ASTM Committee on Standards, 1916:ftace St., Philadelphia, PA 19103. 325 DUP050295989 Designation: D 2190 - 89 Standard Specification for Vinyl Acetate1 Has standard is issued under the fixed designation D 2190; the number immediately following the designation indicates tbe year of original adoption or, in.the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers vinyl acetate. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D1078 Test Method for Distillation Range of Volatile Organic Liquids2 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D2086 Test Method for Acidity in Vinyl Acetate and Acetaldehyde2 D2191 Test Method for Acetaldehyde Content of Vinyl Acetate2 D2193 Test Method for Hydroquinone in Vinyl Acetate2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Standard: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 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 DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2190 - 63 T. Last previous edition D 2190 - 84. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4 Annual Book cfASTM Standards, Vol 05.03. 5 Annual Book ofASTM Standards, Vols 14.03 and 05.03. 6 Annual Book qfASTM Standards, Vols06.03and 15.05. 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Sampling 3.1 Sample the material in accordance with Practice E300. 4. Properties 4.1 The vinyl acetate shall conform to the following requirements: Distillation range, 'C Apparent specific gravity, 20/20"C Color (HQ grade only), Pt-Co scale, max Water content, weight %, max Acetaldehyde content, weight %, max Acidity, as acetic acid, weight %, max Inhibitor content (HQ) 71.8 to 73.0 0.9335 to 0.9345 10 0.10 0.03 0.02 A A As agreed upon between tbe purchaser and the manufacturer. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the fourth decimal place, the temperature of both specimen and water being 20C. (See Methods D 268 or Test Method D 4052.) 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 39C having a range from 48 to 102C, and conforming to the requirements in Specification E1. 5.1.4 Water--Test Method D 1364. 5.1.5 Acetaldehyde--Test Method D 2191. 5.1.6 Acidity--Test Method D 2086. 5.1.7 Inhibitor Content--Test Method D 2193. .6 Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 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 at arty time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, either reapproved or withdrawn. Your comments ere invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that yow 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. 326 DUP050295990 Designation: D 21911 - 89 Standard Teat Method for Acetaldehyde Content of Vinyl Acetate1 This standard is issued under the fixed designation D 2191; 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 (s) indicates an editorial change since the last revision or reappro. al. eope |i. This test method covers the determination of trace jatities ofacetaldehyde, in the range from 0.00 to 0.05 %, fined in 99 % grade vinyl acetate. This standard may involve hazardous materials, oper- s, and equipment. This standard does not purport to 'ress all ofthe safety problems associated with its use. It is Iresponsibility of the user of this standard to establish hfpriate safety and health practices and determine the Mcability of regulatory limitations prior to use. For 3c hazard statements see Section 8. j3 For hazard information and guidance, see the supr's Material Safety Data Sheet. Referenced Document H>.1 ASTMStandard: 1193 Specification for Reagent Water2 'Summary of Test Method P'3.1 The acetaldehyde present in the specimen is reacted ||th a measured excess ofsodium bisulfite. The amount of idium bisulfite consumed, determined by titrating the |tcess with a standard iodine solution, is a measure of the cefaldehyde present in the vinyl acetate. Significance and Use 4.1 This test method provides a measurement of acealdehyde content in vinyl acetate. The results of these aeasurcments can be used for specification acceptance. Interference 5.1 Ketones and other aldehydes, if present, cause a positive interference. |-6, Apparatus ,, 6.1 Buret, 50-mL capacity, graduated in 0.1-mL subdivisions, with a funnel or flared top and a ground-glass 1 stopcock. 6.2 Erlenmeyer Flask, 500-mL capacity, glass-stoppered. 6.3 Bipet, 50-mL capacity. 6.4 Bipet, 100-mL capacity. 7.1 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.3 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 determination. 7.2 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. 7.3 Iodine, Standard Solution (0.1 N)--Dissolve 35.0 g of potassium iodide (KI) and 13.0 g of resublimed iodine in water, and dilute to 1 L with water. Store this solution in a dark bottle and standardize each day, as required, against a standard 0.1 N sodium thiosulfate (Na^O^ solution. (See standardization procedure, 9.3 and 9.4.) 7.4 Potassium Iodate (KT03), primary standard. 7.5 Sodium Bisulfite Solution (0.44 %)--Dissolve 4.4 g of sodium metabisulfite (Na2S205) in 1 L of water. This solution should be prepared fresh daily or just before using. 7.6 Sodium Thiosulfate, Standard Solution (0.1 N)-- Weigh to 0.1 g 24.8 g ofsodium thiosulfate (Na2S203 5H20) crystals and dissolve in 500 mL ofwater. Dilute this solution to 1 L with water. Add 0.5 mL of chloroform per litre of solution as a preservative, and store in a clean dark bottle. This solution should be standardized weekly, as required, against potassium iodate (KI03). (See standardization proce dure, 9.1 and 9.2.) 7.7 Starch Indicator--Make a paste of 6 g of powdered soluble starch in water, and dilute to 1 L with water, stirring to produce a suspension. While stirring, add 20 g of potassium hydroxide (KOH) pellets, and continue stirring until the KOH is dissolved. Let stand for 2 h and add 27.5 mL of hydrochloric acid (HQ). Adjust the mixture to a pH of 6.0 0.1 by adding small increments of HC1 or KOH as required. Add 6 mL of glacial acetic acid as a preservative. 7.8 Sulfuric Acid (1 N)--Place approximately 700 to 800 mL of water in a 1-L volumetric flask. Add slowly and with constant stirring 27.2 mL of concentrated sulfuric acid (H2S04, sp gr 1.84). Allow the solution to cool to room temperature, and adjust the volume to the 1-L mark with additional water. 8. Hazards 8.1 Vinyl acetate is flammable and hazardous; use special precautions when handling it. Avoid eye and skin contact 1 This test method is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DOi .35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 31, 1989. Published May 1989. Originally published as D 2191 - 63 T. Last previous edition D 2191 - 84. 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." 327 DUP050295991 # D 2191 and the inhalation of its vapors. 9. Standardization 9.1 To standardize the 0.1 NNa2S203 solution, first dry. for 6 h approximately 3 g of the KI03 primary standard in a drying oven maintained at a temperature of 110 5C. Place the dried KI03 in a desiccator until cool. Weigh 0.14 to 0.15 g of the dried KI03 to 0.1 mg, and transfer to a 250-mL Erlenmeyer flask. Add 25 mL ofwater to the flask to dissolve the KI03. To this solution, add 2 g of KI crystals and 10 mL of the 1 N H2S04, and thoroughly mix. Fill, a 50-iiiL buret with the'Na^S2b3 solution to be standardized and titrate the KK)3 solution until the brown colpr of the iikfinp bas been reduced to a pale yellow color. At this point, add 0.5 mL of the starch indicator, and continue the titration until the color changes sharply from blue to colorless. No t e 1--When titrating excess iodine with sodium thiosulfate, the starch indicator should be added .only when near the end point as noted by the fading of.die brown colpr of the iodine. Starch reacts \yith iodine in the presence of iodide to form an intensely blue color absorption complex,'and if added to a solution containing free .iodine, a stable complex is formed, that would give erroneous results. 9.2 Calculate the normality N of the Nq2S203 solution as follows: ' ... N - (W X P)/{Vx 0.035669) where: W = weight of KI03 used, g r P = correction for purity of KI03 standard, and V = volume of Na2S203 required for titration of the KI03, mL. 9.3 Fill the funnel-topped 50-mL burdt with the 0.1 N iodine solution to be standardized. Measure approximately 40 mL of the iodine solution into a 250-mL Erlenmeyer flask, and read the buret to the nearest 0.1 mL. Add approximately 50 mL of wafer to the flask containing the iodine solution, and titrate with the standardized 0.1 N Na2S203 solution as described in 9.1. 9.4 Calculate the normality -A, of the iodine solution as follows: Nl=(VxN)/Vl where:. , V - volume of Na2S203 required for titration of the iodine solution, mL, N = normality of. the.Na2S203 solution, and Vt = volume of iodine , solution used for standardization, mL. 10. Procedure 10.1 Pipet 50 mL of Na2Si205 solution (7.5) into each of two glass-stoppered 500-mL Erlenmeyer flasks. Add approx imately 25 g of dean chipped ice to each flask and into one ofthe flasks pipet 100 mL ofthe sample. Grease the stoppers and place, the flasks on: a mechanical shaker, allowing them to shake for 10 1 min. 10.2 At the end ofthe 10-min reaction period, add 0.5 mL of starch indicator to the blank and specimen. Titrate the excess sodium bisulfite with the standard iodine solution. The end point is when the first permanent blue color is obtained. No t e 2--In order to maintain good drainage of the iodine solution, care should be taken to always use a clean buret which should be filled with the iodine solution just before beginning each series of titrations. 11. Calculation 11.1 Calculate the weight percent aldehyde content of the vinyl acetate, as acetaldehyde, A, as follows: A = [((R - V2) X W, x 0.02202)/(> X M)} X 100 where: . , B ~ volume ofiodine required for the titration of the blank, mL, V V2 = volume of iodine required for titration ofthe specimen, mL, Ni ~ normality of the iodine solution, D -- specific gravity of the sample, and M = volume of sample used, mL. 12. Report 12.1 Report the following information: weight percent acetaldehyde to the nearest 0.001 %. Duplicate runs that agree within 0.003 % are. acceptable for averaging (95 % confidence level). 13. Precision and Bias 13.1 Precision--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 analyst should be considered suspect if they differ by more than 0.006 % absolute. 13.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 0.008 % absolute. No t e 3--The above precision estimates are based upon, an interlab oratory study on four samples of vinyl acetate containing 0.01, 0.02, Q.Q3, and 0.05 % . acetaldehyde. Two analysts, in each of three different laboratories performed duplicate determinations on each sample on two successive days making a total of 96 determinations. 13.2 Bias--Bias has not been determined for this test method. See Section 5 for interferences. 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 edvised that determination of the validity of any such patent rights, and the risk of infringement of suoh rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, 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. 328 DUP050295992 Designation: D 2192 - 89 Standard Test Method for Purity of Aldehydes and Ketones1 This standard is issued under the fixed designation D 2192; 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. cope 1 This test method covers the determination of the ty of certain commercially available aldehydes and nes. >2 In addition to all aldehydes and ketones, all comnds such as vinyl alkyl, ethers, acetals, and ketals, that ilyze under the conditions of the reaction to form free onyl groups, react with the reagent and consequently rfere. Water, alcohols, saturated esters, and hydrocarbons not react with: the reagent, but large amounts of inert nic solvents are undesirable because of the effect on the ator.. This standard may involve hazardous materials, opergns, and equipment.. This standard does not purport to 'ms all ofthe safetyproblems associated with its use. It is responsibility of the user of this standard to establish propriate safety and health practices and determine the fplicability of regulatory limitations, prior to use. For 1c hazard statements, see Notes 1 and 2. 1,4 For hazard information and guidance, see the sup er's Material Safety Data Sheet. ..Referenced Documents '2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and . Related Coatings and Material2 D1193 Specification for Reagent Water3 ; , E 200 Practice for Preparation, Standardization, and Storage of Standard Solutions for Chemical Analysis4 E 222 Test Methods for Hydroxyl Groups by Acetic Anhydride Acetylation4 ;3. Summary of Test Method 3.1 Hydroxylamine hydrochloride is converted in part to free hydroxylamine by reaction with a known amount of aqueous triethanolamine. NH2OH HC1 + (HOCH2CH2)3N fn NH2OH + (HOCH2CH2)3N-HCl The free hydroxylamine reacts with the aldehyde or ketone to form the corresponding oxime. 1 This test method is under the jurisdiction of ASTM Committee EX-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2192-63. Last previous edition D 2192 -84. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. " Annual Book ofASTM Standards, Vol 15.05. RRjG-O + NH2OH -> RR,C=H=NOH + H20, (2) where: R = alkyl group and R, = alkyl group or hydrogen. The amount of hydroxylamine consumed, which is deter mined by titration of the excess base with standard sulfuric acid, is a measure of the aldehyde or ketoiie originally present. 3.2 Since the determination is based on an acidimetric titration, a suitable correction must be applied if the sample is not neutral to bromophenol blue indicator. 4. Significance and Use 4.1 This test method provides a measurement of purity (assay) of aldehydes and ketones. The results of these measurements can be used for specification acceptance. 4.2 The precision of this test method is applicable only to material having a purity of 98 to 100 %. 5. Apparatus 5.1 Pressure Bottle, 200 to 350-mL capacity, with lever type closure and made of heat-resistant glass. 5.2 Container for Pressure Bottle--A suitable safety de vice to contain the pressure bottle. A metal container with a hinged top and perforated bottom, a strong synthetic fabric or canvas bag, or a safety shield may be used. 5.3 Ampoule, 1 or 2-mL capacity. 5.4' Weighing Pipet, Lunge or similar type. 5.5 Burets, 50-mL capacity. 5.6 Transfer Pipet, 50-mL capacity. 5.7 Glass Rod, 8-mm, several pieces approximately 1 in. long. 5.8 Boiling Water Bath. 6. Reagents and Materials 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.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 Purity of.Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water 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." 329 DUP050295993 D 2192 conforming to Type IV of Specification D 1193. 6.3 Bromophenol Blue Indicator (0.04 % Alcoholic Solu tion)--Dissolve 0.04 g of bromophenol blue (tetrabromophenolsulfonphthalein) in 100 mL of methyl alcohol. Titrate this solution with 0.1 N sodium hydroxide (NaOH) solution to a reddish-bronze color. If an off-color is obtained at this point, it is probably due to the age of the indicatorand fresh indicator should be used to prepare a new solution. 6.4 Cylinder Nitrogen. 6.5 Hydroxylamine Hydrochloride, Standard (0.5 N Alco holic Solution)--Dissolve 35 g of hydroxylamine hydrochlo ride (NH2OH HC1) in 150 mL of water and dilute to 1 L with 99 % isopropanol. 6.6 Isopropanol (99%). 6.7 Sulfuric Acid, Standard (0.5 N)--Prepare and stan dardize 0.5 N sulfuric acid (H2S04) in accordance with Practice JE 200, Sections 24 through 27. 6.8 Triethanolamine, Standard (0.5 N Aqueous Solu tion)--Dissolve 65 mL (74 g) of 98 % triethanolamine in water and dilute to 1 L with water. Adjust the normality of this solution so that it is slightly below the normality of the H2S04 being used. 7. Procedure 7.1 Sample, the material in accordance with Methods D 268. 7.2 Add 15 mL of a 0.04 % alcoholic solution of bromo phenol blue indicator to 500 mL of the hydroxylamine hydrochloride solution. From a buret add 0.5 N trieth anolamine until the solution appears greenish-blue by trans mitted light. Prepare the solution fresh before each series of analyses. 7.3 Prepare a sufficient number of heat-resistant pressure bottles to make all blank and sample determinations in duplicate. Replace the rubber gaskets if necessary and make sure the caps can be fastened securely. 7.4 Using a graduated cylinder, add 65 mL of the neutral ized hydroxylamine hydrochloride to each bottle. Using a transfer pipet, add 50.0 mL of the 0.5 N- triethanolamine solution to each bottle. . . 7.5 Before capping, purge the bottles for 2 min with a gentle stream of cylinder nitrogen. This is best accomplished by means of a glass tube inserted through the neck of the bottle and clamped so that the opening is just above the surface of the liquid. 7.6 Reserve two of the bottles for the blank determina tion. Into each of the other bottles introduce an amount of sample containing not more than 0.015 mol of aldehyde or ketone. For substantially pure material, weigh the specimen to the nearest 0.1 mg, using the amount and procedure specified in Table 1. No t e 1: Precaution--Acetaldehyde is a highly volatile, flammable material; observe all necessary safety precautions. Handle samples only in a fume hood that is free from open flames, electric heaters, and other sources of ignition. Cool all samples in an ice bath before the containers are opened. Weigh the acetaldehyde in a sealed glass ampoule. The actual procedure for filling and sealing the ampoule will vary somewhat with the type of ampoule being used. One convenient method is to pack commercially available ampoules in powdered, solid carbon dioxide, introduce the specimen by means of a chilled hypodermic syringe, and seal the ampoule with a gas torch. 7.7 If a sealed glass ampoule is used to weigh the TABLE 1 Specimen Size and Reaction Conditions Compound Specimen, g* Minimum Reaction Conditions Time, Tempera min ture, c Acetaldehyde (Precaution, Note 1) Methyl isobutyl ketone Methyl isoamyl ketone Isophorone 0.5 to 0.7s 1.1 to 1.4s 1.1 to 1.7 1.4 ta.2.0 30 60 30 60 25 25 25 98 A Use a suitable weighing pipet unless otherwise specified. 3 Use a sealed glass ampoule. specimen, add several pieces of 8-mm glass rod and shake the bottle vigorously to break the ampoule. i 7.8 React the solutions at room temperature or at 98C according to the directions in Table 1. 7.8.1 Reaction at 98C (Precaution--See Note 2.)--Place f the specimen and blank bottles as close together as possible 1 in a boiling water bath maintained at least at 98C for the t time specified in Table 1. Maintain sufficient water in the : bath to just cover the liquid in the bottles. Remove'the j bottles from the bath after the specified time and allow them to cool in air to room temperature. When the bottles have ? cooled, remove them from the safety device and continue as \ described in 7.9. No t e 2; Precaution--Enclose each bottle securely in a suitable i container (metal or strong fabric) to restrain fragments of glass should the pressure bottle rupture. 7.8.2 Reaction at Room Temperature--Allow the speci mens and the blanks to stand together at room temperature for the length of time specified in Table f. Swirl the bottles occasionally. 7.9 Cool each of the bottles slightly with tap water and uncap carefully to prevent loss of the contents. Allow the contents to return to room temperature. No t e 3--Bromophenol blue indicator is temperature sensitive, and a difference of 10C at the end point causes a discrepancy of approxi mately 0.3 mL of 0.5 N H2S04. To achieve the best precision, it is imperative that the blank and the specimen be at the same temperature at the end point. A water bath at room temperature is a convenient means of conditioning the specimen and the . (flanks prior to the titration. 7.10 Titrate each of the blanks with standard 0.5 N H2S04 to a greenish-blue end point. Titrate each of the specimens with standard 0.5 N H2S04 to the color of the blanks, approaching the end point dropwise until the colors match by transmitted light. . No t e A--If the solution becomes cloudy upon titration, add suffi cient isopropanol to the specimen solution to effect homogeneity and add an equal amount ofisopropanol also to the blank. 7.11 Measure the temperature of the acid titrant. If the temperature of the reagent at the time the analysis is made is not the same as it was when the reagent was standardized, apply a correction to the normality. Use a AN/T of 0.00014 per degree Celsius in making the temperature correction.6 8. Calculation 8.1 Calculate the weight percent of aldehyde or ketone, A, as follows (Note 5): 6 See Table I of Practice E 200. 330 DUP050295994 # D 2192 TABLE 2 Aldehyde and Ketone Factors Factor* 0.04405 0.1002 0.1142 0.1382 TABLE 3 Within-Laboraiory Deviations Acetalde hyde Methyl Isoamyl Ketone Isophorone Standard deviation Degrees of freedom Repeatability 0.33. 20 1.0 0.22 42 2.6 0.18 42 0.6 A = [((5 -V)Fx N)fS[ X 100 (3) *2SC>4 required for titration of the specimen (see 7.10), ;L ? J2S04 required for titration of the blanks (see 7.10), Average, mL , normality of the H2S04, factor specified in Table 2 for the compound being .'determined, and sample used (see 7.6), g. ie 5--If the sample is acidic to bromophehd blue indicator, it is mended that a suitable correction be applied to the purity value, to Test Method E 222. eport 1 Report all results to the nearest 0.1 , Precision and Bias 0.1 In interlaboratory studies of this test method, the '^laboratory and between-laboratory standard 'deviawere found to be as shown in Tables 3 and 4. Based on deviations, the following criteria should be used for ng the acceptability at the 95 % confidence level of "ts obtained on materials having a purity of 98 to 100 %. 0.2 Repeatability--Two results, each the mean of dupli TABLE 4 Between-Laboratory Deviations Acetalde hyde Methyl Isoamyl Ketone Isophorone Standard deviation 0.33 0.41 0.63 Degrees of freedom 20 19 19 Reproducibility 1.0 1.2 1.9 cates, obtained by the same operator on different days, should be considered suspect ifthey differ by more than the amount shown in Table 3. 10.3 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories, should be considered suspect if they differ by more than the amount shown in Table 4. No t e 6--The preceding precision statements for acetaldehyde are based upon two separate interlaboratory studies using two different samples having purities above 99%. In the first study duplicate determinations were made on each sample by two analysts on two different days in each of three laboratories. The second study included the same test program in each of four laboratories. The precision statements for methyl isoamyl ketone and isophorone are based upon two separate interlaboratory studies using two different samples of each chemical. In both studies, one analyst in each of eleven different laboratories made duplicate determinations on each sample on two different days. The American Society for Testing and Materials takes no position respecting the validity of any patentrights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity at 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 live years and If not revised, either reapproved or withdrawn. Your comments are invited either for ravlslon 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 feei 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. 331 DUP050295995 Designation: D 2193 - 89 Standard Test Method for Hydroquinone in Vinyl Acetate1 This standard is issued under the fixed designation D 2193; 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 hydro- quinone in the range from 1 to 20 ppm in refined, com mercially available, vinyl acetate. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Document 2.1 ASTM Standard: D119.3 Specification for Reagent Water2* 3. Summary of Test Method 3.1 The vinyl acetate is evaporated at room temperature in a stream of inert gas or clean air to minimize the lo$s of hydroquinone by evaporation. The hydroquinone is dis solved in water and titrated with dilute standardized ceric acid sulfate using diphenylamine as indicator. 4. Significance and Use 4.1 This test method provides a measurement of inhibitor level in vinyl acetate. The results of these measurements can be used for specification acceptance. 5. Apparatus 5.1 Buret, 25-mL, graduated in 0.1-mL subdivisions. 5.2 Beakers, 50 and 600-mL capacity. 5.3 Volumetric Flask, 1000-mL capacity. 5.4 Erlenmeyer Flasks, 100 and 250-mL capacity. 5.5 Nitrogen Cylinder, or source of clean air. 5.6 Pipets, 10 and 50-mL capacity. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.3 Other grades may be used provided it is 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 IV of Specification D 1193. 6.3 Ceric Acid Sulfate, Standard Solution (0.002 N)-- Dissolve 1.096 g of ceric ammoniuni nitrate ((NH4)2Ce(N03)6) in 28.0 mL of concentrated sulfuric acid (H2S04, sp gr 1.84) contained in a 50-mL beaker. Slowly pour the ceric solution, while stirring, into 200 mL of water contained in a 600-mL beaker. When solution is complete, transfer this mixture to a 1000-mL volumetric flask and dilute to the mark with water. 6.4 Diphenylamine Indicator Solution--Dissolve :0.1 g of diphenylamine in 100 mL of H2S04 (sp gr 1.84) and store this solution in a brown glass bottle. 6.5 Hydroquinone Standard--Dissolve 200.0 mg of hy droquinone, weighed to the nearest 0.1 mg, in water and dilute to 1000.0 mL in a volumetric flask. This solution is unstable and should be discarded after 1 week of normal use. 7. Standardization 7.1 Pipet 10-mL portions of the hydroquinone standard (see 6.5) into each of two 100-mL Erlenmeyer flasks. Add 3 drops of diphenylamine indicator solution to each flask. . Using a 25-mL buret, titrate the contents of each flask with ceric acid sulfate solution to a faint blue end point that is permanent for 15 s. The titrations should be approximately 20 mL and should agree within 0.5 mL. Average the two values and use in the calculations (Section 9). 8. Procedure 8.1 Pipet 50 mL of the vinyl acetate sample into each of two 250-mL flasks. 8.2 Evaporate the specimens at room temperature by passing a stream of cylinder nitrogen gas or clean air into the flasks. Bench-line air should be passed through a fiberglass filter before entering the specimen flasks. Maintain the flow ofgas just short ofa level causing splattering ofthe specimen. That part of the delivery tube in the flask must be of metal, glass, or an inert plastic, such as polyethylene or polytetrafluoroethylene (PTFE). 8.3 After complete evaporation, which requires 45 to 60 a II ' 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 DOi.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D2I93 - 63 T. Last previous edition D 2193 - 84. 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 Nosliand Co., Inc., New York, NY, and the "United States Pharmacopeia." 332 DUP050295996 .remove the gas stream and dissolve the hydroquinone ,mL of water. Add 3 drops of diphenylamine indicator solution to sk using the same dropper as in the reagent standardn. Titrate each solution with the ceric add sulfate nt to a light blue end point that is permanent for 15 s. eolation Calculate the parts per million of hydroquinone, H, in iple as follows: H = l(V x F)/S] x 1000 e: millilitres of ceric add sulfate reagent required for titration of the spedmen, (see 8.4), factor (Section 7) = milligrams of hydroquinone in 10-mL aliquot/average millilitres of ceric add sulfate reagent, and grams of sample used = 50 x specific gravity. 10. Report 10.1 Report the concentration of hydroquinone to the nearest 0.1 ppm. 11. Predsion and Bias 11.1 The following criteria should be used forjudging the acceptability of results at the 95 % confidence level: l l.i.i Repeatability--Two results, each the mean of du plicate determinations, obtained by the same analyst should be considered suspect if they differ by more than 0.3 ppm. 11.1.2 Reproducibility^-Two results, each the mean of duplicate determinations, obtained by analysts itf different laboratories should be considered suspect if they differ by more than 1.0 ppm. No t e--The preceding precision statements are based upon an interlaboratory study on two,samples of vinyl acetate containing 4.6 and f 5.3 ppm hydroquinone. Each sample was analyzed in duplicate on two different days by one analyst in each of five different laboratories." The American Society lor Testing and Materials takes no positron respecting the validity ofany patent rights asserted in connection, with any Item mentioned In this standard. Users ofthis standard are expressly advised that determination of the validity ofany 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 theresponsible technical committee and must be reviewed every live years and Ifnotrevised, eitherteapproved or withdrawn. Your comments are invited eithertorrevision 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 your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 333 DUP0502 95997 Designation: D 2194 - 89 Standard Test Method for Concentration of Formaldehyde Solutions*1 This standard is issued under the fixed designation D2194; 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 covers the determination of the formaldehyde content of commercially available formalde hyde solutions ranging in concentration from 36 to 55 weight %. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTMStandard: D 1193 Specification for Reagent Water2 3. Summary of Test Method 3.1 The specimen is reacted with an excess of sodium sulfite solution and the resulting sodium hydroxide is titrated with sulfuric acid using thymolphthalein indicator. 3.2 The sample should be essentially neutral; 0.1 % acidity (as formic add) is equivalent to 0.065 % formalde hyde. 4. Significance and Use 4.1 This test method provides a measurement of formal dehyde content (assay) of formaldehyde solutions. The results of these measurements can be used for specification acceptance. 5. Apparatus 5.1 Buret, calibrated, 100-mL, with a 50 or 75-mL reser voir on top of a lower portion calibrated in 0.1 -mL divisions. A TFE-fluorocarbon resin stopcock is suitable for this purpose. 5.2 Erlenmeyer Flask, 500-mL capadty. 5.3 Vials, specimen, short, style, 1 to 1 `/2-dram (4 to 6-mL) capadty. 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 conforming to Type IV of Spedfication D 1193. 6.3 Sodium Sulfite Solution (125 g/L)--Dissolve 125 g of anhydrous sodium sulfite (Na2S03) in water and dilute to 1 L. No t e 1--Sodium sulfite gradually oxidizes to sodium sulfate on exposure to air and therefore should be kept in a tightly closed container. For best results freshly prepared Teagent should be used. 6.4 Sulfuric Acid (0.5 N)--Prepare and standardize 0.5 N sulfuric add (H2S04) against 0.5 N sodium hydroxide (NaOH) solution which has been standardized against potas sium acid phthalate to a thymolphthalein end point. 6.5 Thymolphthalein Indicator (0.1 % Alcohol Solu tion)--Dissolve 1.0 g of thymolphthalein in 100 mL of methanol, ethanol, or isopropanol and dilute to 1 L with additional alcohol. 7. Hazards 7.1 Formaldehyde and formaldehyde solutions are toxic and exposure to them should be minimized to avoid acute effects and possible sensitization. 8. Procedure 8.1 Add 100 mL of Na2S03 solution to a sufficient number of 500-mL Erlenmeyer flasks to make all blank and specimen determinations in duplicate. 8.2 Weigh a 2-g specimen to the nearest 0.1 mg in the weighing vials and transfer the vials to the Erlenmeyer flasks, being careful to avoid getting any of the sample on the sides of the flasks. 8.3 Add 3 to 5 drops of the thymolphthalein indicator solution to each of the flasks containing specimens as well as the blanks and titrate to a colorless end point 9. Calculation 9.1 Calculate the weight percent of formaldehyde, W, as follows: 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 27, 1989. Published December 1989. Originally published D 2194 - 63 T. Last previous edition D 2194 - 84. 1 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." 334 DUP050295998  D2194 W=[(V-B)xNxF]/Sx 100 H2S04 required for titration of the specimen, mL, H2S04 required for titration ofthe blank, average, mL, normality of the H2S04, ' 0.03003 (the milliequivalent weight of formaldehyde), and sample used, g. jeport .1 Report the percent formaldehyde to the nearest %. Duplicate runs that agree within 0.12 % are acceptfor averaging (95 % confidence level). Precision and Bias 1.1 The following criteria should be used for judging the acceptability of results at the 95 % confidence level. 11.1.1 Repeatability--The difference between two results, each the mean of duplicate determinations, obtained by the same analyst on different days is normally about 0.05 % absolute. Two such results should be considered suspect if they differ by more than 0.12 % absolute. 11.1.2 Reproducibility--The average difference between two results (each the mean of duplicate determinations) obtained by analysts in different laboratories is normally about 0.08 % absolute. Two such results should be consid ered suspect if they differ by more than 0.23 % absolute. No t h 2--The above precision estimates are based on two interlaboratory studies involving five and nine laboratories, respectively, using two different samples in each case with a single analyst performing duplicate results on each of two days. The formaldehyde levels studied were as follows: 36.85 %, 36.98 %, 37.15 %, and 37.23 %. The American Society for Testing andMaterials fakes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity 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-fiveyears and ifnot revised, eitherrSepproved or withdrawn. Yourcomments are Invited either for revision 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 hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 335 DUP050295999 Designation: D 2195 - 89 Standard Test Methods for Pentaerythritol1 ' This standard is issued-under the fixed designation DT195; the number immediately following the designation indicates the year of original adoption or, in the Case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the testing ofpentaerythritol for use in the manufacture -of alkyd resins and other synthetic resins. ' : ... 1.2 The test procedures appear in the following sections: Section Sulfate ash Moisture Hydroxyl Assay (by dibenzal) .Assay (by gas chromatography) Phthalate ester color 5 to 10 11 to 16 17 to 22 23 to 29 30 to 41 42 to 49 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 34. 1.4 For hazard information and guidance, see the sup plier's Material Safety Data Sheet 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D1209 Test Method for Color ofClear Liquids (Platinum- Cobalt Scale)3 D1615 Test Methods for Glycerol, Ethylene Glycol, and Pentaerythritol in Alkyd Resins4 D1728 Test Method for Phthalate Ester Color of High- Gravity Glycerin5 D2593 Test Method for Butadeine Purity and Hydro carbon Impurities by Gas Chromatography6 E 1 Specification for ASTM Thermometers7 E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals8 E 200 Practice for Preparation, Standardization, and Stor age of Standard Solutions for Chemical Analysis* E 203 Test Method for Water Using Karl Fischer Reagent8 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 D01.35 on Solvents, Plasticizers, and Chemicals Intermediates. Current edition approved Oct 27, 1989. Published December 1989, Originally published as D 2195 -63 T. Last previous edition D2195 -84. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 06.02. 5 Discontinued, see J990 Annual Book QfASTM Standards, Vol 06.03. 6 Annual Book ofASTM Standards* Vol 05.02. 7 Annual Book ofASTM Standards*Vols 05.03 and 14.03. * Annual Book ofASTM Standards, Vol 15.05. E 222 Test Methods for Hydroxyl Groups by Acetic Anhydride Acetylation* E 260 Practice for Packed Column Gas Chromatography9 3. Significance and Use 3.1 These test methods provide a measurement of sulfate,, ash, moisture (water), hydroxyl content, assay by dibenzal and gas chromatograiihy, and phthalate ester color ofperitaerythritol. The results of these measurements can be used for specification acceptance.. 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 sucii specifications are available.10 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 IV of reagent water conforming to Specification D 1193. SULFATE ASH 5. Summary of Test Method 5.1 The organic matter is burned off, the residue treated with sulfuric acid, ignited, and the ash weighed. 6. Apparatus 6.1 Crucible or Dish--A silica, quartz, or platinum cru cible or dish having a capacity of 50 to 60 ml. 6.2 Bunsen Burner. 6.3 Electric Muffle Furnace, maintained at 600 25C. 7. Reagents and Materials 7.1 Sulfuric Acid (1+1)--Carefully mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84) with 1 volume of water. 8. Procedure 8.1 Preignite the crucible or dish at 600'C, transfer to a desiccator, and when cool, weigh to 0.1 mg. Place approxi mately 20 g ofthe sample in the crucible or dish and weigh to 9 Annual Book ofASTM Standards, Vol 14.01. 10 "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." I i :|j 336 DUP050296000 # D 2195 mg. Heat gently with a gas flame and ignite the specimen, wing it to bum completely. Cool somewhat, and then ten the residue with 10 to 20 drops of H2S04 (1+1). tiously ignite until the carbon is completely consumed, ally, ignite in the muffle furnace at 600C (dark red heat) instant weight, cool, and weigh to 0.1 mg. Calculation "l Calculate the percent of sulfate ash, A, to three ;'mal places as follows: A = (R/S) x 100 (1) +e: residue, g, and ; = sample used, g. \2 Duplicate determinations that agree within 0.005 % acceptable for averaging. Precision and Bias 10.1 The following criteria should be used for judging the "ptability of results at the 95 % confidence level: 10.1.1 Repeatability--Two results, each the mean of dupate determinations, obtained by the same analyst should considered suspect if they differ by more than 0.008 %, 'olute. 10.1.2 Reproducibility--"two results, each the mean of `iiplicate determinations, obtained by analysts in different 1 oratories should be considered suspect if they differ by ore than 0.008 %, absolute. f No t e 1--The above precision estimates are based on an interlaborary study involving seven laboratories using three samples with one `lyst performing duplicate runs on each oftwo days. The average level Tthe ash content of the samples studied was 0.01%. MOISTURE 11. Summary of Test Method 11.1 The loss in weight on heating at 105"C for 3 h is etermined. 12. Preparation of Sample 12.1 Grind a 25-g portion of the sample in a mortar and `pestle, to pass a 40-mesh sieve, and use portions for the subsequent tests. 13. Apparatus 13.1 Weighing Dish, aluminum, 70 by 30 mm, with cover. 13.2 Oven, gravity convection, maintained at 105 + 2C. 14. Procedure 14.1 Dry the aluminum dish at 105 C. Cool in a dessicator and store until ready for use. 14.2 Weigh, to 0.1 mg, a 5-g portion ofthe ground sample into a tared-aluminum dish, and place in the 105 2C oven for 3 h. Remove, cover, cool in a desiccator, and weigh. 15. Calculation 15.1 Calculate the percent of moisture content, M, as follows: M=[(A -- B)/W] x 100 (2) where: A = weight of dish + specimen before heating, g, B = weight of dish + specimen after heating, g, and W - sample used, g. 15.2 Duplicate determinations that agree within 0.15 % are acceptable for averaging. 16. Precision and Bias 16.1 The following criteria should be used for judging the acceptability of results at the 95 % confidence level: 16.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same analyst should be considered suspect if-they differ by more than 0.20 %, absolute. 16.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 0.30 % absolute. No t e 2--The above precision estimates are based on an interlabora tory study involving seven laboratories using three samples with one analyst performing duplicate runs on each of two days. The mean level of the moisture content of the samples studied was 0.3 %. HYDROXYL CONTENT 17. Summary of Test Method 17.1 The hydroxyl content is determined in accordance with Test Methods E 222. 18. Apparatus 18.1 Fiasks, Erlenmeyer, 300-mL with standard-taper 24/40 joint. 18.2 Condenser, 400-mm, standard-taper 24/40 joint with cooling extending into the joint, drip tip. 18.3 Hot Plates, with variable resistance for temperature control. 18.4 Buret, calibrated, 100-mL, with a 50 or 75-mL reservoir on top of a lower portion calibrated in 0.1 -mL divisions. A TFE-fluorocarbon resin stopcock is suitable for this purpose. 19. Reagents and Materials 19.1 Acede Anhydride. 19.2 Acetylation Reagents--Mix 105 mL of acetic anhy dride with 1 L of pyridine (see 19.4). The reagent shall be freshly prepared each day, and used and kept in a dark bottle. It should not be used if darker than a pale yellow color. 19.3 Phenolphthalein Indicator Solution (1 g/100. mL)-- Dissolve 1 g of phenolphthalein in 100 mL of aqueous pyridine solution (1+1). 19.4 Pyridine, containing 0.30 to 0.45 % water. Deter mine the water content of the pyridine using Test Method E 203 and add the required amount of water. Calculate the volume of water to add in millilitres per litre of pyridine, V, as follows: V = 4.0 - 9A (3) where + = water in pyridine, %. 19.5 Sodium Hydroxide, Standard Solution (0.5 N)-- Prepare and standardize in accordance with Practice E 200. Apply temperature corrections to the volumes of titrant so 337 DUP050296001 # D 2195 that the normality is for concentration at 20C. 20., Procedure 20.1 Weigh a 0.30 to 0.33-g portion of the ground sample into a small glass-stoppered weighing,bottle. Dry for 3 h at 105'C. Weigh accurately, transfer the portion to a 250-mL Erlenmeyer flask with groundjoint, and reweigh the bottle to obtain the specimen weight by difference. 20.2 Pipet 25 mL of the acetylation reagent into the flask using a uniform drainage time for all aliquots. Connect the flask to the condenser (Note 3), sealing the joint with 1 or 2 drops of pyridine, and place on a hot plate; if necessary, swirl the flask to dissolve the specimen. Heat at reflux.for 30 min, regulating the heat so that the vapors condense in the condenser. No t e 3--If the surrounding atmosphere is humid, connect the condenser to a drying trap containing a mixture of No. 2 mesh calcium chloride and indicating anhydrous calcium sulfate. 20.3 Allow the flask to cool somewhat, then rinse the condenser with 25 mL of water. Remove the condenser and rinse the joint of the condenser and the flask with water, collecting the rinsing in the flask. 20.4 Cool the flask in an ice-water bath so that the contents are below 20C, add 0.5 to 1.0 mL of phenolphthalein indicator solution, and titrate slowlywith the 0.5 N NaOH solution to the fust permanent, faint pink end point. The solution must be swirled or magnetically stirred during the titration, and the solution must be vigorously swirled as the end point is approached. Read the volume of the titrant to 0.02 mL (Note 4). Record the temperature of the 0.5 N NaOH solution. No t e 4--If the volume of 0.5 N NaOH solution required for the specimen is less than 80 % of that required for the blank, the specimen was too large and the analysis must be repeated with a smaller specimen weight. 20.5 Perform a blank determination in parallel by the same procedure, omitting only the addition of the specimen. 21. Calculation 21.1 Calculate the percent of hydroxyl content, H, as follows: H = [(B - V)N x 17.01]/[5 X 1000] X 100 (4) where: V -- NaOH solution required! for titration of the specimen, mL, B = NaOH solution required for titration of the reagent blank, mL, N - normality of the NaOH solution used, and S = specimen used, g. 21.2 Duplicate determinations that agree within 0.3 % are acceptable for averaging. 22. Precision and Bias 22.1 The following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 22.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same analyst should be considered suspect if they differ by more than 0.8 %, absolute. 22.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by analysts in different laboratories should be considered suspect if they differ by more than 1.2 %, absolute. No t e 5--The above precision estimates are based on an interlabora tory study involving seven laboratories using three samples with one analyst performing duplicate runs on each of two days. The mean level of the hydroxyl value of the samples studied was 48%. ASSAY (BY DIBENZAL) 23. Scope and Application- 23.1 This test method covers the determination of the monopentaerythritol content of pentaerythritol (PE) by the dibenzal method. It is applicable to material containing 75 % or more monopentaerythritol. Norma! amounts of dipentaerythritol do not interfere. Tripentaerythritol, etc, interferes, due to its insolubility in the reaction mixture. Refer to Tesf Methods D 1615. 24. Summary df Test Method 24.1 A weighed specimen is dissolved in water, a meth anol solution of bexizaldehyde is added, followed by hydro chloric acid, and the mixture cooled to 0CC. The pentaerythritol-dibenzal precipitate is filtered, dried, and weighed.' A solubility correction factor is added to the weight of precipitate found. 25. Apparatus 25.1 Crucibles, filtering, fntted-glass, medium-porosity. 25.2 Stirring Rods, about 70 mm long, preferably having one flat end. 25.3 Vacuum Pump or Water Aspirator--It is convenient to have at least two outlets, in order to make duplicate flltrations simultaneously. 26. Reagents and Materials 26.1 Benzaldehyde, N.F. grade, 98 % minimum purity. This material is easily oxidized by air. If it is to be used over a long period, transfer the contents of a 1-lb (0.5-kg) bottle to a number of 22-mL capacity screw-cap vials. 26.2 Benzaldehyde-Methanol Reagent--Add 20 mL of benzaldehyde to 100 'mL of methanol. Prepare fresh for each series of determinations. 26.3 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HC1). 26.4 Methanol. 26.5 Methanol-Water Wash Solution (I+I)--Mix equal volumes of methanol and water and cool to 20 to 25C. 27. Procedure 27.1 Weigh approximately a 0.5-g portion of. the ground sample into a small glass-stoppered weighing bottle. Dry for 3 h at 105C. 27.2 Weigh accurately, transfer the portion to a 125-mL Erlenmeyer flask, and reweigh the bottle to obtain the specimen weight by difference. 27.3 Add 5.0 mL of water, insert a stopper loosely, and heat to incipient boiling on a hot plate with swirling, until the specimen is dissolved. 27.4 To the hot solution, preferably in a hood, add 15 mL of benzaldehyde-methanol reagent and 12 mL of HC1. The 338 DUP050296002 # D 2195 a should be clear at this point. Insert the stopper and allow the flask to stand for 15 min at room ature. Swirl the flask occasionally to prevent the ,te from adhering to the bottom of the flask. Place in an ice bath at 0 to 2C for 1 h or more. Alsb, mL of 1+1 methanol-water wash solution in the ice (fbr later use. b Remove the flask from the ice bath and immediately ithe reaction mixture with suction through a weighed, Sglass crucible. Complete the transfer ofthe precipitate 25 mL of the cold (0 to 2"C) 1+1 methanol-water wash, 5n. J Wash the.precipitate with a total of 100 mL of 1+1- sl-water wash solution at 20 to 25C, in several pis, as follows; Disconnect the vacuum Une, pour a , portion of the methanol-water wash solution from a irate into the crucible, and stir the; precipitate to'form a geneous slurry; Connect the vacuum line and draw the ' solution through the crucible. Repeat this washing lation six times. With the last 30 mL of methanol-water solution, rinse the interior walls of the crucible, and i"and remove the stirring rod. Aspirate thoroughly and dry the precipitate at 105 for 2 h. Cool in a desiccator and weigh. ? PCalculation III Calculate the percent of pentaerythritol, E, as fol-. E = [fP + 0.0269) x 43.59J/5 (5) ire: = sample, used, g, . = precipitate, g, f>69 = solubility correction factor, and = (mol weight PE/mol weight PE-dibenzal) X 100. 3.1Duplicate determinations that agree within 0.3 % are. stable for averaging. gSR Precision and Bias - Ml 29.1 The following criteria should be used for judging the Acceptability of results at the 95 % confidence level: Mp!9.2 Repeatability--Two results, each the mean of dupli- HSte determinations, obtained by the same analyst should be Mfinsidered suspect if they differ by more than 1.2%, Absolute. . .- [[09.3 Reproducibility--Two results, each the mean of Implicate determinations, obtained by analysts in different pboratories should be considered suspect if they differ by jhorp than 3.3 %, absolute. No t e 6--The above precision estimates are based on an interlabora- ary study involving seven laboratories using three samples with one Bnalyst performing duplicate runs on each oftwo days. The.average level pf the monopentaerythritol content of the samples studied was 88 %. I ASSAY (BY GAS CHROMATOGRAPHY) 30. Summary of Test Method | 30.1 A solution of material in pyridine and containing mannitol as an internal standard is etherified with jtrimethylchlorosilane using hexamethyldisilazane as a pro moter. A portion of the etherified solution is injected onto a igas chromatography column consisting of 17 % silicone rubber on an acid-washed and dimethylchlorosilane-treated calcined diatomaceous earth support. The column is initially at 100C and is gradually heated to 350C to obtain the chromatogram. Programming to 350C is necessary in order that all impurities possibly present in .commercial pentaerythritol are removed in a reasonable length of time. - 30.2 The,.monopentaerythritol content is calculated from the .ratio of the peak areas of the internal standard and the monopentaerythritol. 31. Significance and Use 3h 1 This test method is* useful for determining the amount of monopentaerythritol in commercial grades of pentaerythritol by physical means. 31.2 The test results are calculated using an internal standard method. 32; Apparatus 32.1 Programmed Temperature Gas Chromatograph with thermal conductivity detectors (see Note 7) and capable of operating efficiently at temperatures up to 350C. No t e 7--Flame ionization detectors are too sensitive for this.test method and the reaction medium can contaminate the flame jetl 32.2 Column (Note 2), 4-ft (1.2-m) length, . Yie in. (4.8 mm) outside diameter stainless steel, packed with approxi mately 4 g of 17 % silicone rubber on 60/80 mesh acidwashed, dimethylchlorosilane-treated calcined diatomaceous earth support. The Vis to /A-in. (4.8 to 6,4-mm) Swagelok adapters should also be filled with packing and the glass wool plugs kept to a minimum volume in order tp minimize the dead volume during injection and thus prevent tailing of the peaks.. No t e 8--Useful information on column preparation may be found in Test Method D 2593 and Practice E 260. 32.3 Syringe, microlitre, 50-p.L capacity, with fixed needle. A, syringe with a removable needle may be. used but the fixed needle type is recommended. No t e 9--Immediate cleaning with water followed by a volatile solvent, such as acetone, is necessary to prevent blockage of.the needle \ by salts present in the reaction mixture. 32.4 Flask, Morton, ,500-mL capacity. 32.5 Evaporator, rotating vacuum. 32.6 Bottle, 1-oz (30-mL) wide mouth, fitted with screw cap having polytetrafluorpethylene liner (see Note 10). The bottle must be of such a shape it will maintain its upright position in a water bath, and tall enough to allow separation of enough supernatant liquid for sampling. No t e 10--The bottle caps from regular supply houses may not be available with polytetrafluoroethylene liners and it may be necessary to order the liners separately.11 Alternatively, they may be cut from polytetrafluoroethylene sheeting. 32.6.1 Alternatively, a 17-mL vial, 28-mm diameter, 60mm high, fitted -with screw cap having a poiytetrafluoroethylene liner has been found satisfactory. 32.6.2 Alternatively, in place of the screw cap bottle or 11 Liners provided by Erno Products Co., 65 N. 2nd St, Philadelphia, PA 19106, or by Arthur H. Thomas Co., P.O. Box 779, Philadelphia, PA 19105, have been found satisfactory for this purpose. 339 DUP050296003 D 2195 vial, a 50-mL Erlenmeyer flask may be used. 33. Reagents and Materials 33.1 Chloroform. 33.2 Diatomaceous Earth, calcined, acid-washed, dimethylchlorosilane-treated, 60 to 80 mesh. 33.3 Column Packing--Dissolve 20 g of silicone rubber in 300 mL of chloroform. Weigh 100 g of the treated solid support (33.4) into a 500-mL Morton flask and wet with about 75 mL of chloroform. Pour the silicone rubber solution into the flask, attach to the rotating evaporator, apply suction with a water aspirator, and allow the flask to rotate until a free-flowing powder results. A steam bath may be used to facilitate the final drying process. Remove the finished packing and store in a screw-capped bottle. No t e 11--Gas-Chrom Z has been used as the solid support. Other solid supports that give equivalent values may be used, such as Gas-Chrom Q and ABS. 33.4 Hexamethyldisilazane (HMDS).12 33.5 Mannitol (internal standard), C6H1406, melting point 167 to 169C. (Eastman white label grade is recom mended.) 33.6 Molecular Sieve 5A, `/te-in. (1.5 mm) pellets. 33.7 Monopentaerythritol of known assay. It is important that material relatively high in monopentaerythritol be used (greater than 95 % is suggested). 33.8 Pyridine. 33.9 Silicone Rubber (methyl silicone).13 33.10 Trimethylchlorosilane (TMCS), reagent grade,13 or distill technical grade material and use that boiling between 57 and 60C. This reagent is stable when stored under dry inert atmosphere in a glass bottle fitted with a screw-type cap having a chemically inert liner. 34. Hazards 34.1 Avoid contact of hexamethyldisilazane or trimeth ylchlorosilane with the skin or inhaling their vapors. Wear suitable rubber gloves and work in a suitable fume hood when handling these reagents. 35. Preparation of the Chromatographic Apparatus 35.1 Assemble the apparatus according to the manu facturer's instructions. 35.2 Make the following instrument settings: Sample inlet temperature, C Detector temperature, C Column temperature (programmed): Initial, *C Final, `C AT, `C/min Carrier gas Pressure, psi Flow rate, mL/min Detector current, mA Recorder range, mV Chart speed, mm/min 350 350 100 350 10 helium 50 so 150 (W-l filaments) Oto 1 25 12 Reagent from Pierce Chemical Co., P. O. Box 117, Rockford, IL 61105, has been found satisfactory for this purpose. 13 Silicone rubber SE 30 has been used as the liquid phase. Other silicone rubbers giving the same separation may be used, such as OV-1. 36. Column Conditioning 36.1 Attach one end of a freshly packed column to the inlet side of the instrument while the exit end of the column; remains unattached. With helium flowing through at 80d mL/min, heat the column from 100 to 350C at lOVmiB. % Then maintain at 350C for 1 h. This procedure willJ thermally strip the column of volatiles and prevent thenbuildup in the detector. Cool to 100C and couple the exit of the column to the detector. Inject two 40-p.L aliquots of TMS blank (7 mL of pyridine, 1 mL of HMDS, and 2 mL of TMCS). Reprogram the column at 10C/min to 350C and hold for 1 h. This procedure will thermally strip the column of additional volatiles that may have reacted with TMS. Recool to lOfTC and the column is ready for specimen analysis. Normally, injection of TMS blanks or specimens: onto a column at a temperature hotter than 200C acceler ates column deterioration and leads to extraneous peaks and peak tailing due to stripping of some of the liquid phase and exposure of the solid support. 37. Calibration of the Chromatograph " j|| 37.1 Use a material of known high assay monopen- I taerythritol to determine the instrument response factor 1 (Note 12). Very minor impurities may be present in the' 1 mannitol internal standard but are not usually significant.' f Run a blank on the mannitol using regular test reagents to determine impurities. Recalibrate for each new bottle of :| mannitol or other reagents used. I No t e 12--For normal use, a material of 95 % minimum mono- fl pentaerythritol is adequate for standardization. When purer material is 13 required for more accurate work, prepare it by reacting about 2 g of the available monopentaerythritol with 5 mL of hexamethyldisilazane, 10 mL of trimethylchlorosilane, and 25 mL of dry pyridine as in the : | normal sample preparation (this is a threefold excess of reagent). Isolate, the trimethylsilyl ethers by extracting the reaction mixture with 40 mL ofhexane and enough water to form two phases (about 5 mL). Separate and dry the upper hexane layer over anhydrous sodium sulfate. Decant j the hexane into a distillation flask and evaporate to dryness on a steam bath with aid ofa stream ofdry air. Vacuum distill the silyl ether residue j at 6 mm pressure. The pure monopentaerythritol derivative is a colorless s liquid at room temperature and has a boiling point of 128'C at 6 mm pressure. Apply a conversion factor of the molecular weight of the parent polyol divided by the molecular weight of its derivative to determine the specimen weight of the free polyol. (For Mono-PE this factor is 0.322.) 37.2 The monopentaerythritol peak temperature will be 200 to 210C and the mannitol peak temperature 250 to 260"C. Response factors of about 0.86 to 0.91 for the monopentaerythritol to 1.00 for mannitol have been found (Note 13). Repeat the determination of response factors until reproducible results are obtained Determine the factor (in duplicate) each day that analysis is run. 37.3 Calculate the response factor, F, as follows: F= {(Wc x F/100)/^] x (AJAC) x {SJSC) (6) where: We = weight of purest monopentaerythritol available, mg, P -- monopentaerythritol, weight %, Ws = weight of internal standard, mg, As = peak area for internal standard, mm2, Ac -- peak area for monopentaerythritol, mm2, Ss = sensitivity setting for internal standard, usually 2, and 340 DUP050296004 sensitivity setting for monopentaerythritol, usually 2 13--Lack of reproducible response factors or improperly eaks are indications of improper column condition, inadequate re control at the injection port, poor temperature programoducibility, or a combination ofthese factors. Each TMS series )sfart with a conditioning blank run to 350C. cedure Weigh, to 0.1 mg, about 120 to 150 mg of sample j[20 to 150 mg of mannitol into a 1-oz screw cap bottle mL vial) having a polytetrafluoroethylene cap liner. 7 mL of dry pyridine and 1 mL of hexamethylane into the bottle (or vial) and close it with the screw An open vial may be used, but close. attention, is to avoid overheating and loss of specimen or nts. (Alternatively, as noted in 32.6,2, a 50-mL 'hmeyer flask may be used. When using the flask, add the e amount of samples and reagents as when using the w cap bottle! Place the flask on a hot plate in a hood and just under boiling for. 10 min. With proper heating, the r'ring should be maintained about 0.5 in. (13 mm) from op of the flask neck.) ,2 Place the bottle in a bath of boiling water in a hood neat for 15 min with! intermittent gentle swirling. The r in the bath should be at about the same level as the 'd in the bottle and should not reach the bottle cap. After allow the bottle and contents to cool to room perature and wipe the outside of the bottle dry. It is imely important that the final solution be clear and free lid particles. 38.3 Pipet 2 mL oftrimetfaylchlorosilane into the bottle or and swirl for 2 or 3 min, . Then warm the solution in a Water bath maintained af 70 to 80C for 5 min (Note 14). 'before, the water in the bath should be at about the same el as the liquid in the bottle. Immediately remove the ttle from the bath and. swirl for 1 mill, Adequate agitation important to assure a suitable reaction. Dry and allow to olto roomtemperature. This preparation is stable and can stored for at least 24 h at room temperature in the :w-capped bottles. No t e 14--For specimens that; contain appreciable amounts of such purities as di- or tripentaerythritol, a 5-min reaction time may not be ufficient. A longer reaction time, up to about 15 min, has been found tisfactory and may be used as necessary. ; 38.4 At 350"C, the life of even commercially available silicone rubber septa is short. Replace the septa (on both channels even if the other one is not used) every day. The syringe! barrel should be tight (no back-flush) and injection should be rapid. For most operators, slow withdrawal of the ; needle appears best for preventing injection losses; however, some operators prefer rapid withdrawal. 38.5 With the chromatograph in operation and the column at 100C, inject about 15 pL of the supernatant liquid (Note 15) and obtain the chromatogram, program ming at about 10C/min until a temperature of 350C is reached. Use sensitivity setting (2x) or attenuate the sensi tivity setting as necessary for full scale major peaks. No t e 15--Never inject anything but clear supernatant liquid onto the column. If the NH4C1 precipitate has not settled, heat the solution until it does or centrifuge it. 38.6 Repeat the procedure using only 120 to 150 mg of mannitol to identify peaks due to impurities in the reagents. 38.7 After each run, cool the column to lOCTC for the next specimen. 38.8 Measure to 1 mm2, by triangulation or other suitable methods, thej peak areas for the mannitol (internal standard) and monopentaerythritol. 39. Calculation 39.1 Calculate the percent of monopentaerythritol, M, content as follows: ' ScXAcXlVsXFxm SsXAsx .mg of specimen where: Sc = sensitivity setting for monopentaerythritol, usually 2, Sg = sensitivity setting for internal standard, usually 2, Ac -- peak area for monopentaerythritol, mm2, As = peak area for internal standard, mm2, . F = appropriate response factor for the monopenta erythritol (see 37.2), and Ws = weight of internal standard, mg. 40. Report 40.1 Report the. following information:. 40.1.1 Monopentaerythritol content to the nearest 0.1 %. 41. Precision and Bias 41.1 The precision statements are based upon an interlatooratory study in which one operator, in 13 laboratories analyzed two saniples of technical pentaerythritol containing approximately 84 and 89 % monopentaerythritol, respec tively, in duplicate on two successive days. Results were analyzed in accordance with Practice E 180. The withinlaboratory standard deviation of results, each the mean of duplicates, was found to be 0,56 % absolute at 21 degrees of freedom. The between-laboratories standard deviation, each the mean of duplicates, appeared to vary with the mono pentaerythritol content and has been estimated for the two different levels to be as shown in Table 1. Based on these -' standard deviations, the following criteria should be used in judging the acceptability of results at the 95 percent confi dence level: 41.1.1 Repeatability--Two results, each the mean of du plicates, obtained by the same operator on different days should be considered suspect if they differ by more than 1.7 % absolute. 41.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than the values listed in Table 1. TABLE 1 Reproducibility Mean monopenta erythritol content, 56 _____________________ ____________________ 88.82 83.74 Degrees of freedom Standard deviation, % absolute Maximum acceptable range between laboratory means. % absolute 9 0.62 2.0 10 1.36 4.3 341 DUP050296005 D 2195 PHTHALATE ESTER COLOR 42. Summary of Test Method 42.1 The ester is prepared by reacting pentaerythritol (PE) with phthalic anhydride under controlled conditions; The resulting ester color is measured while warm by use of a spectrophotometer calibrated with platinum-cobalt stand ards. This method is similar to that in Test Method D 1728. 43. Apparatus 43.1 Oil or Wax Bath with stirrer and heating coil, thermostatically controlled, maintained at 225 l'C. No t e 16--An insulated metal bath of 5 to 6-gal (18 to 23-L) capacity, equipped with heating elements of 625 to 700-W capacity heat input, is satisfactory for preparing five to six esters simultaneously without an excessive temperature drop. 43.2 Test Tubes, borosilicate glass, 22 by 175 mm. 43.3 Clamps and Supports, for use with 22 by 175-mm test tubes. , 43.4 Thermometer, ASTM Solvents Distillation Ther mometer having a range from 95 to 255C, 100-mm immer sion, and conforming to the requirements for Thermometer 42C as prescribed in Specification E 1. 43.5 Timer, 60-min. 43.6 Spectrophotometer or Filter Photometer, capable of measuring the absorbance or transmittance of a sample at a wave-length of 450 nm. A spectrophotometer employing essentially monochromatic light of a half-band width at 450 nm of not more than 2.0 nm should be used for referee work. 43.7 Rectangular Cuvettes or Optical Cells, suitable for the instrument to be used for color measurement. The optical light path of the cuvette should be not less than 10 mm nor greater than 20 mm. The cuvettes used for calibration and for measurement must be matched optically, and light paths must not differ by more than 0.1 mm. 44. Reagents and Materials 44.1 Cobalt Chloride (CoCl2 6H20). 44.2 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HQ). 44.3 Phthalic Anhydride (QH4O3)--Solidification point 131!C min; melt color 15 platinum-cobalt, max, heat sta bility color 25, max. No t e 17--As a check on the heat stability of the phthalic anhydride, a specimen of the phthalic anhydride should be held at 225C for 45 min. The original melt color and the heat stability color should be measured, using a 50-mL long-form Nessler tube, and compared against the platinum-cobalt standards described in Test Method D 1209. Material of the specified quality should be procured by selection or by direct correspondence with the manufacturers. 44.4 Potassium Chloroplatinate (K2PtCl6). 45. Preparation of Standards 45.1 Platinum-Cobalt Stock Solution--Dissolve 1.245 g of K2PtCl6 and 1.000 g of CoCl2 6H20 in water. Add 25 mL of HC1 and dilute to 250 mL with water. This stock solution has a platinum-cobalt color of 2000. 45.2 Platinum-Cobalt Standards--From the stock solu tion, prepare color standards as given in Table 2 by diluting the required volumes to 20 mL with water. TABLE 2 Platinum-Cobalt Color Standards Color Standard Number Stock Solution, mL Color Standard Number Stock Solution, mL 200 2 1200 12 400 4 1400 14 600 6 1800 18 1000 10 2000 20 46. Calibration of Photometer 1 46.1 Calibrate the photometer against the platinum-cobalt | standards in cuvettes at a wavelength of 450 nm. Prepare a if calibration curve of absorbance or transmittance values versus the platinum-cobalt standards. | 47. Procedure 47.1 Bring the bath to 225 1C and maintain the t temperature within the specified range. 47.2 Weigh 20.0 g of phthalic anhydride into a clean, dry 22 by 175-mm test tube. Clamp the test tube in the bath (with the lip of the tube 20 5 mm above the level of the bath liquid). When the crystals have melted, add, from a . weighing scoop, 20.0 g of the pentaerythritol sample, in small portions, while stirring with a stirring rod. Set the timer for 45 min. 47.3 When the crystals have dissolved, remove the stirring rod and immediately cap the tube tightly with aluminum foil. Water formed in the reaction should reflux in the vapor space and thus wash down sublimed phthalic anhydride crystals. 47.4 After placing several specimens in the bath at one time, the bath temperature should not drop more than 5C, and the time required for the temperature of the bath to return to 225 1C should not exceed 5 min. 47.5 Remove the test tube from the bath at the end of 45 min. Ifappreciable phthalic anhydride crystals have collected on the inside ofthe test tube, rerun the esterification. Ifonly a few crystals are present, pour a portion of the ester melt into a waste receptacle to clear the lip and side of the test tube of any crystals that may interfere with the procedure described in 47.6. 47.6 Preheat the cuvette or optical cell at 100C. Pour the ester melt carefully into the cell or rectangular cuvette in which the measurement is to be made. If air has been entrained, heat the melt at 100 to 150'C so that the bubbles may rise clear of the optical light path. Do not attempt to determine the color of any ester that appears to contain any suspended matter or haze. Discard such an ester and prepare another. To obtain reproducible results, it is mandatory that all esters be perfectly clear. 47.7 While still warm, measure the absorbance or trans mittance ofthe ester at 450 nm and read the platinum-cobalt color from the previously prepared calibration curve. 47.8 The cells may crack if allowed to cool. To clean the cells, stand them upside down on a wire gauze, suspended by bending the comers, about 1 in. (25 mm) from the bottom of a beaker. Immediately place them in an oven at 125C for a few hours to melt the bulk of the ester. Complete the cleaning by placing the cells on a gauze in a beaker, add acetone or methyl ethyl ketone to a depth just below the 342 DUP050296006 # D 2195 Report the color of the ester as the platinum-cobalt i read from the instrument calibration curve. .1 Duplicate runs that agree within 70 platinumunits are acceptable for averaging. ecision and Bias The following criteria should be used forjudging the bility of results at the 95 % confidence level: 1.1 Repeatability--The usual difference between two results, each the mean of duplicate determinations, obtained by the same analyst on different days approximates 20 platinum-cobalt units. Two such values should be considered suspect if they differ by more than 60 units. 49.1.2 Reproducibility--The usual difference between two results, each the mean of duplicate determinations obtained by analysts in different laboratories, approximates 50 platinum-cobalt units. Two such values should be consid ered suspect if they differ by more than 150 units. No t e 18--The above precision estimates are based on an interlaboratory study on three samples, each from a different supplier, covering a color range of 400 to 700 platinum-cobalt units. One analyst in each of seven laboratories performed duplicate determinations and repeated these determinations one day later for a total of 84 determinations. The American Society for Testing and Materials takes no position respecting the validity olany patentrights 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 ths risk of Infringement of such rights, are entirely their own responsibility. This standard la 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 torrevision 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 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. 343 DUP050296007 Designation: D 2245 - 90 Standard Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints1 ' This standard is issued under the fixed de^igrjation D 224$; hfcie number immediately following the designation indicates the year of original adoption dr, in the case of teviiSoh, the year1 of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (4 indicates an editoriai.change since the last revision or reapproval. ' This standard has-been approvedfor use by agencies ofthe Department ofDefense to replace^ Method 7501 ofFederal Test Method - Standard No. MTConsult the DaD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the DeportmentofDefense. . ,, a tf > , tj ; i j 1. Scope 1.1 This test method covets the identificationofoils and oil acids in vehicles that have been separated from solvent- reducible paints. The test method is based on a gas chro matographic technique (of the methyl esters) applicable to products containing both saturated and udsaturated; animal and vegetable, unpolymerized or partially polymerized fatty acids having 8 to 20 carbon atoms. 1.2 This test method is not applicable to products con taining fatty acids that have been polymerized or oxidized to such an extent that no characteristic monomeric fatty acids remain. 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: D1398 Test Method for Fatty Acid Content of Alkyd Resins and Resin Solutions2 D1983 Test Method for Fatty Acid Composition by Gas-Liquid Chromatography of Methyl Esters3 D2372 Practice for Separation of Vehicle from Solvent- Reducible Paints4 D2800 Test Method for Preparation of Methyl Esters from Oils for Determination of Fatty Acid Composition by Gas Chromatography3 3. Summary of Test Method 3.1 This test method is based upon the differential migra tion and partitioning of constituent fatty acids in the form of vaporized methyl esters between a flowing gas phase and a supported liquid phase in a gas chromatographic column. The test method is based on isothermal operation of the gas chromatograph and a hot wire, thermal conductivity de tector. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paiut 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 25, 1990. Published July 1990. Originally published as D 2245 - 64 T. Last previous edition D 2245 - 72 (1984)C1. 2 Annual Book ofASTM Standards, Vo! 06.02. 3 Annual Book ofASTM Standards, Vo! 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 3.2 The test method consists in the separation of the Vehicle from thfe paint by . ceritriftigation, extraction of fatty acids from the vehicle after saponification, conversion of fatty adds and a measured addition of margaric add (internal standard) into methyl esters, preparation of the gas chromatogram; and interpretation of the chromatogram, The amount ofeach m.onoinetic fatty add .ester is calculated, totaled,', subtracted fern 100 % to yield polymerized fatty adds, reported as is, and interpreted by comparison with standards as being from specific oils or oil adds. ij f g -if] -S |j 4. Significance and Use 4.1 This test method provides a procedure to identify the fatty adds present in the vehicle of a paint. 5. Apparatus 5.1 Centrifuge, high-speed, capable of developing in excess of 10 000 g. 5.2 Separatory Funnels, with PTFE-fluorocarbon stop cocks. 5.3 Gas Chromatograph and Accessories, suitable for analysis of fatty acids as methyl esters (see Test Method D 1983). 3 I 1 1 I | g 11 i , 6. Reagent 6.1 Hydroquinone. 7. Calibration and Standardization 7.1 Establish optimum operating conditions on the gas chromatograph with known samples of methyl esters as described in Test Method D 1983. 7.2 Prepare working standards by running known paints or vehicles through the procedure described in Section 8. Indude particularly compositions with chemical or struc tural modifications that might be expected to alter the fatty add distribution or the apparent polymer content of the starting raw materials. - 8. Procedure 8.1 Separate the vehicle from the paint by direct high speed centrifuging (see Practice D 2372). 8.2 Extract the fatty adds from the separated vehicle after saponification and removal of the dicarboxylate salts and unsaponifiable matter in accordance with Test Method D 1398, but substitute separatory funnels with PTFE-fluoro carbon stopcocks when available. In cases involving un saturated fatty acids, add a crystal or diethyl ether solution 344 DUP050296008 # D 2245 irfc he pstdeic pTfitic Ipitolelc pric fjg": . pTeic gchidic ||#TlitiC Knitoieic igi&ric Ipc ll&tefc ipolenic Irachidic gfadoleic ppric ristic iyristoleic palmitic galmltoleic Stearic Xelc holds Linolenic tfachidonic Hupanodonic Nisinic iShiblc Unidentified unsaturate TABLE 1 Caster Oil, SS Coconut Oil, % Cottonseed Oil, % Linseed Oil, % Menhaden Oil, % Fatty Acid Composition of Oils Used in Paint Products4 Oitidca Oil, % 2 palmitic 1 Stearic 7 Oleic 87 licanic 3 Hydroxy adds Perilla Oil. % trace 6 6 44 18 11 6 7 2 trace trace trace 1 trace 29 2 4 24 40 trace 6 trace 4 22 16 52 trace trace trace 7 trace 16 16 2 15 7 2 17 11 4 1 2 Palmitic Stearic Oleic Linoleic Linolenic Myristte Myristolelc Palmitic Palmltoleie Stearic Oleic Unoleic Linolenic Araehidic Gadoleic Myristic Palmitic Stearic Oleic Linoleic Linolenic Araehidic Gadoleic Palmitic. Stearic Oleic Lholeic Linolenic Araehidic Palmitic Stearic Oleic Linoleic Linolenic Beostearic Safflower Oil, % Soybean Oil, % Tall Oil, X Tung OH, % 7 5 6 78 4 7 2 13 14 64 trace trace 8 trace 3 13 75 1 trace trace trace ii 4 25 51 9 trace trace 5 3 46 41 3 2 4 1 B 4 3 80 A The acids and percents presented in this table are taken from the "Composition and Constants of Fatty Acids" chart and used by permission of the ' Archer-Daniels-Midland Co. The percent rosin adds in tall oil may vary from 0 to 42 %, the percent terpenes from 0 to 13 %. Both variations depend on the grade and refining of the oil. of hydroquinone (equivalent to less than 0.05 weight % of . the fatty acids to the fatty acid fractions obtained in 6.8 of f Test Method D 1398. Swirl the flask containing the fatty 1 acids, some ether solvent, and the hydroquinone until the hydroquinone is well dispersed; evaporate off the remaining ether carefully under vacuum as described in Test Method D 1398. Analyze immediately or store for only a limited time in a small tall form vial under nitrogen in a dark cool place. 8.3 Prepare methyl esters of the extracted fatty acids in accordance with 6.2 through 6.5 of Test Method D 2800. 8.4 Determine the fatty acid composition in accordance with Test Method D 1983. (See Appendix, Fig. X 1.1, for a typical chromatogram prepared in accordance with Test Method D 1983). 8.5 Compare the chromatogram or fatty acid composi tion, or both, with the chromatograms or fatty acid compo sitions, or both, of suspected known materials (See Table 1, for typical fatty acid compositions of oils used in paint products). Consider the content of specific fatty acids char acteristic of specific oils. Consider the total saturates versus unsaturates and polymer content in relation to what the original starting oil or oil acids might have been. 345 DUP050296009 ~1 # D2245 1 I 9. Report 9.1 Report the type of oil or oil acid when the fatty acid distribution approximates a specific known distribution or combination, when the limit ofthe possibilities is known and when the polymer content can be explained. (See Appendix X1 for some ofthe considerations in interpreting the analysis results), 9.2 Even when the identification is positive, it is recom-. mended that the actual percent distributions of monomeric fatty acids and the polymer content be reported. In very numerous to allow an immediate identification, the percent breakdown figures should be recorded. Considered with*, other data that might subsequently be obtained, the fattys acid and polymerdistribution canbe important. jfj 10. Precision 7 10.1 Single-oil types have been correctlyidentified in*) collaborative work for seven round-robin samples. Repre sented were four linseed types, three soya types, one fish ofl: type, and one coconut type. 11. Keywords * complex systems where the possible combinations are too 11.1 fatty acids; oils; oil acids; solvent-reducible paints V APPENDIX (Nonmandatory Information) XI. CONSIDERATIONS IN THE INTERPRETATION OF FATTY ACID COMPOSITION X1.1 In the determination of the identity of pure natural percent polymer determinations for assistance in oil identififj oils, the percent breakdown ofthe fatty adds will many times cation. In most cases, the presence ofthese modifications can? suffice for oil identification. When a mixture ofoil or oil-acid be detected by running infrared spectra on a portion of the*) types is suspected, one can profit by comparing the content separated fatty adds. As more work is done using the of key fatty acids. For example, a high oleate content in what quantitative internal standard technique, it is expected that,, otherwise appears to be a soya-type composition would the data accumulated will aid everyone in interpreting what" suggest soya plus some tall oil. If, however, the palmitate is involved in some of the observed polymer content results. appears a little high, one would conclude that some cotton X1.4 Another more direct interference, which has not seed had been added to the soya-type acids. Theoretically, if been mentioned, is the presence of carboxylic acid esters it can be established that the system under study is derived other than fatty adds. Acids such as isophthalic and benzoic ! from a limited number of oil types on which exact fatty add acid are expected to be present in the fatty acid fraction due distributions are known, and polymerization or to the partial solubility of their potassium salts in the isomerization is not involved, a strictly mathematical ap saponification medium. This is the main reason for using proach to determining the quantity of each oil type is anhydrous reagents for the saponification of alkyds . or feasible. By means of a set of simultaneous equations polyesters. When unfamiliar peaks are observed in the involving key acids such as oleate, linoleate, linolenate, and chromatogram of fatty acid methyl esters from whole paint, stearate one should expect to be able to estimate mixtures of this type of interference should be considered. two or possibly three oil types. X1..2 In the event that chromatographic analysis suggests the presence of polymer, it must be known that the polymer composition is due solely to oil polymer if the calculation of polymer content is to be of value in oil identification. In such cases the polymer content of the oil-ester sample plus the percent of the polyunsaturated adds obtained from the chromatogram (see Fig. XI.l) can be used to determine the total polyunsaturates present in the original oil. Since the value for total polyunsaturates varies with the oil in question, the experimental value obtained is used as additional evi dence for oil identification. XI.3 The presence of oil polymer composed of reaction products of oil adds with cyclo- or dicyclopentadiene, maleic 80 % Linseed Type Fatly Acid* anhydride, styrene vinyltoluene, of other Diels-Alder 20% Heptadecanolc Acid adducts, or the presence of rosin adds' (in the case of tall oil fatty acids with high rosin content), negate the value of346 FIG. X1.1 Drying-Oil Methyl Esters 346 DUP050296010 # D 2245 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard ere expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your commentsare Invited either for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters: Your comments will recerve-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. DUP050296011 Designation: D 2373 - 85 (Reapproved 199Q)C1 Standard Test Method for Determination of Cobalt in Paint Driers by EDTA Method41 1 This standard is issued under the fixed designation D 2373; 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. 41 No t e--Section 12 was added editorially in May 1990. 1. Scope 1.1 This test method covers a titrimetric determination of cobalt in liquid paint driers that can be dissolved in glacial acetic acid and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA). 1.2 This test method is not applicable to drier blends. If driers other than cobalt are present, they may interfere by reacting with EDTA under the conditions used for analysis. 1.3 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D600 Specification for Liquid Paint Driers2 D1193 Specification for Reagent Water3 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals4 E 300 Practice for Sampling Industrial Chemicals5 3. Summary of Test Method 3.1 The liquid drier is dissolved in glacial acetic acid, diluted with isopropyl alcohol and water, and treated with an excess ofstandard EDTA solution. The excess is titrated with standard cupric sulfate solution using PAN as the metal indicator. 4. Significance and Use 4.1 The amount of cobalt drier used in oxidizing-type coatings significantly affects their drying properties. This test method may be used to confirm the stated cobalt content of a pure liquid cobalt drier soluble in glacial acetic acid and manufactured for use by the coatings industry. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 25, 1985. Published December 1985. Originally published as D 2373 - 65 T. Last previous edition D 2373 - 79. 2 Annual Book ofASTM Standards, Vol 06.03. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 5. Apparatus 5.1 Centrifuge, capable of developing 1000 to 2000 g. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended \ 1 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 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Ammonium Chloride <NH4C1). j 6.4 Ammonium Hydroxide (sp gr 0.90)--Concentrated ,' ! ammonium hydroxide (NH40H). i 6.5 Buffer Solution (pH 10.0)--Dissolve 67.5 g of NH4C1 in water, add 570 mL of concentrated NH4OH (sp gr 0.90), and dilute to 1 L. ,'i 6.6 Cupric Sulfate, Standard Solution (0.05 M)--Dissolve :|i 12.5 g of cupric sulfate pentahydrate (CuS04'5H20) in li water and dilute to 1 L. 6.7 Eriochrome Black-T Indicator--Triturate 0.20 g of . ; the concentrated dye with 100 g of sodium chloride (NaCl) ,j and store in a tightly stoppered jar. This mixture remains 1 stable for several years. 6.8 EDTA, Standard Solution (0.05 M)--Dissolve 18.62 i g ofEDTA in water and dilute to 1 L. Store in a polyethylene or borosilicate glass bottle. 6.9 Glacial Acetic Acid (sp gr 1.06). 6.10 Isopropyl Alcohol, 99.5%. 6.11 Methyl Red Indicator Solution--Dissolve 0.2 g of 1 methyl red in 100 mL of methanol, ethanol, or isopropanol. 6.12 PAN Indicator (l(2-Pyridylazo)-2-Naphthol)--Pre pare a dilute solution of the indicator by dissolving 0.10 g in 100 mL of ethanol or isopropanol. 6.13 Sodium Acetate Solution--Prepare a saturated aqueous solution of sodium acetate (NaC2H302) in water. 6.14 Sodium Chloride (NaCl). 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." 348 DUP050296012 P Sodium Hydroxide Solution (80 g/L)--Dissolve 80 g Bum hydroxide (NaOH) in water and dilute to 1 L. m Sulfuric Acid (8+l)-^-Carefu!ly mix' 8 yqlumes of pitrated sulfuric acid (H2S04, sp gr 1.84) with ! volume Jper. .... . Zinc Oxide {ZnO). . t .- pmpling p Take a small sample of liquid drier from bulk using Procedures in Practice E 300 appropriate for the size of ntainer: see the section on Bottle Sampling for tanks _nk cars, or the section on Tube Sampling for drums as. 1--Liquid driers are normally homogeneous so that only js physical tests, such as specific gravity or solids content, on top -ttom samples from tanks are required to confirm that separation -t occurred. Agitate drums in accordance with the section on Tube ling in Practice E 300. Examine the sample of drier for sediment or susded matter which, if present, is evidence of noncompli- with Specification D 600. js3 If the sample is homogeneous keep it in a stoppered ;el to prevent solvent evaporation prior to analysis. Itandardization .1 EDTA, Standard Solution (0.05 M)--Weigh to the rest 0.1 mg approximately 1.5 g of ZnO into a 100-mL '-erandadd 10 mLofH2SQ4 (8+1). Transfer the solution 1 a 500-mL volumetric flask and dilute to the mark with ter. Pipet a 50-mL aliquot into a 500-mL Erlenmeyer k, add 100 mL of water, 2 or 3 drops of methyl red dicator solution, and neutralize with NaOH solution (80 ). Add 5 mL of buffer solution, 0.2 g of Eriochrome ack-T indicator, and titrate with EDTA solution until the lor changes from red to blue, where the last red shade just appears. 8.1.1 Calculate the molarity, , of the EDTA solution as flows: M,= W (K, X 0.0814) (1) here: = ZnO used, g, = EDTA solution, mL, and 0.0814 = molecular weight of ZnO x 10~3 = millimolar weight of ZnO. 8.2 C2S04, Standard Solution (0.05 M)--Determine the titer of the CuS04 solution by titrating 50 mL ofthe standard EDTA solution with CuS04 as described in 9.4 using the PAN indicator solution. 8.2.1 Calculate the molarity, M2, of the CuS04 solution as follows: m2 = <^ (2) where: = molarity-of EDTA solution, V3 ,= 'EDTA solution, mL, ahd V2 - CuS04 solution, mL. 9. Procedure 9.1 Check the clarity of the drier. If not clear, centrifuge a portion of the sample unfil .it is dear. Keep the centrifuge tribe stoppered so that solvent will riot evaporate. 9.2 Weigh the following specimen amounts into a 500-mL Erlenmeyer flask and add 5 mL of gladal acetic acid: (i) for 6 % cobalt, 1.0 to 1.3 g, (2) for 8 % cobalt, 0.8 to 1.0 g, and (5) for more or less cobalt use proportionate specimen sizes. Warm on a hot plate at low heat, swirling the flask until the specimen is completely dissolved. 9.3 In a second flask (blank) put the same amount of glacial acetic acid but no sample. Add 200 mL of isopropyl alcohol, 100 mL of water, 6 mL of concentrated NH4OH (sp gr 0.90), 10 mL of NaC2H302 solution, and 50 mL ofEDTA solution to each flask. Swirl to ensure complete mixing and warm both flasks at steam bath temperature for 5 min. 9.4 To each of the flasks add 2 mL of PAN indicator solution and titrate with the standard CuS04 solution to a blue end point. No t e 2--Because the color ofthe metal indicators (and some oftheir complexes) is affected by pH changes, the pH must be kept constant during titration by the recommended buffer during titration. 10. Calculation 10.1 Calculate the percent of cobalt, A, present as follows: A = (B - Vi) x M2x -1* 100 (3) where: B = CuS04 solution required for titration of the blank, mL, V4 = CuS04 solution required for the specimen, mL, M2 -- molarity of CuS04 solution, F = millimolecular weight for the metal in the sample = 0.05894 for cobalt, and S = specimen used, g 11. Precision and Bias 11.1 Precision: 11.1.1 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 0.10 % cobalt. 11.1.2 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 0.05 % cobalt. 11.2 Bias--Bias has not been determined for this test method. 12. Keywords 12.1 cobalt drier analysis; EDTA method 349 DUP050296013 # D 2373 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 ttie risk of Infringement of Such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must ba reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your oomments will receive careful consideration at a meeting of tire 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 ihe ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.350 350 DUP050296014 Designation: D 2374 - 35 (Reapproved 1990)' Standard Test Method for Lead in Paint Driers by EDTA Method1 This standard is issued under the fixed designation D2374; 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. ei No t e--Section 12 was added editorially in May 1990. ope 1 This test method covers a titiimetric determination of liquid paint driers that can be dissolved in glacial jfc add and utilizes the disodium salt of ethyleneJinetetraacetic add dihydrate (EDTA). |2 This test method is not applicable to drier blends. If other than cobalt are present, they may interfere by Iting with EDTA under the conditions used for analysis. |3 All cations that can be titrated with EDTA in alkaline fea interfere and must not be present in the sample. |4 This standard does not purport to address the safety $>lems associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety and pIth practices and determine the applicability of regulatory mitations prior to use. IReferenced Documents .1 ASTM Standards: n >600 Spedfication for Liquid Paint Driers2 |p 1193 Specification for Reagent Water3 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals4 f E 300 Practice for Sampling Industrial Chemicals5 Summary of Test Method 1,3.1 The liquid drier is dissolved in glacial acetic acid, :ed with isopropyl alcohol and water, and treated with an ss of standard EDTA solution. The excess is titrated with ndard cupric sulfate solution using PAN as the metal adicator. Significance and Use 4.1 The amount of lead drier used in oxidizing-*type boatings significantly affects their drying properties. This test method may be used to confirm the stated lead content of pure liquid lead drier soluble in glacial acetic acid and manufactured for use by the coatings industry. 1 This test method is under the jurisdiction of ASTM Committee D-I on Paint j 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 Oct. 25, 1985. Published December 1985. Originally published as D 2374 - 65 T. Last previous edition D 2374 - 79. 2 Annual Book ofASTM Standards. Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 5. Apparatus 5.1 Centrifuge, capable of developing 1000 to 2000 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.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 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Ammonium Chloride (NH4G). 6.4 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 6.5 Buffer Solution (pH 10.0)--Dissolve 67.5 g of NH4C1 in water, add 570 mL of concentrated NH4OH (sp gr 0.90), and dilute to 1 L. 6.6 Cupric Sulfate, Standard Solution (0.05 M)--Dissolve 12.5 g of cupric sulfate pentahydrate (CuSO4-5H20) in water and dilute to 1 L. 6.7 Eriochrome Biack-T Indicator--Triturate 0.20 g of the concentrated dye with 100 g of NaCl and store in a tightly stoppered jar. This mixture remains stable for several years. 6.8 EDTA, Standard Solution (0.05 M)--Dissolve 18.62 g of EDTA in water and dilute to 1 L. Store in a polyethylene or borosilicate glass bottle. 6.9 Glacial Acetic Acid (sp gr 1.06). 6.10 Isopropyl Alcohol (99.5%). 6.11 Methyl Red Indicator--Dissolve 0.2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol. 6.12 PAN Indicator (l(2-Pyridylazo)-2-Naphthol)--Pre pare a dilute solution of the indicator by dissolving 0.10 g in 100 mL of ethanol or isopropanol. 6.13 Sodium Acetate Solution--Prepare a saturated aque ous solution of sodium acetate (NaC2H302) in water. 6.14 Sodium Chloride (NaCl). 6.15 Sodium Hydroxide Solution (80 g/L)--Dissolve 80 g 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." 351 DUP050296015 # D 2374 of sodium hydroxide (NaOH) in water and dilute to 1 L. 6.16 Sulfuric Acid (5+1)--Carefully mix 8 volumes of concentrated sulfuric acid (H2S04, sp gr 1.84) with 1 volume of water. 6.17 Zinc Oxide (ZnO). 7. Sampling 7.1 Take a small sample of liquid drier from bulk using the procedures in Practice E 300 appropriate for the size of the container: section on Bottle Sampling for tanks and tank cars, or section on Tube Sampling for drums and cans. No t e 1--Liquid driers are normally homogeneous so that only simple physical tests, such as specific gravity or solids content, on top and bottom samples from tanks are required to confirm that separation has not occurred. Agitate drums in accordance with the section on Tube Sampling of Practice E 300. 7.2 Examine the sample of drier for sediment or sus pended matter which if present is evidence of noncompli ance with Specification D 600. 7.3 If the sample is homogeneous, keep it in a stoppered vessel to prevent solvent evaporation prior to analysis. 8. Standardization 8.1 Weigh to the nearest 0.1 mg approximately 1.5 g of ZnOintoa 100-mL beaker and add 10 mL ofH2S04 (8 + 1).Transfer the solution to a 500-mL volumetric flask and dilute to the mark with water. Pipet a 50-mL aliquot into a 500-mL Erlenmeyer flask* add 100 mL of distilled water,, 2 or 3 drops of methyl red solution, and neutralize with NaOH solution (80 gfl). Add 5 mL of. buffer solution, 0.2 g of Eriochrome Black-T indicator,>pnd titrate with EDTA until the color changes from reel to blue, where the last red shade just disappears. 8.1.1 Calculate the molarity, Mu ofthe EDTA solution as follows: W M} = (Vl x 0.0814) (1) Where: W = ZnO used,, g, V, = EDTA solution, mL, and 0.0814 == molecular weight of ZnO x 10~3 = millimolar weight of ZnO.; 8.2 CuS04, Standard Solution (0.05 M)--Determine the titer of the CuS04 solution by titrating 50 mL ofthe standard EDTA solution with CuS04 as described in 9.4 using the PAN indicator. 8.2.1 Calculate the molarity, M2, ofthe CuS04 solution as follows: V2 -- EDTA solution, mL, and F3 = CuS04 solution, mL. 9. Procedure 9.1 Check the clarity of the drier. If not clear, centrifuge a portion of the sample until it is clear. Keep the centrifuge tube stoppered so that solvent will not evaporate. 9.2 Weigh the following specimen amounts into a 500-mL Erlenmeyer flask and add 5 mL of glacial acetic acid: (i) for 24 % lead, 1.0 to 1.5 g, (2) for 30 and 32 % lead, 0.7 to 0.9 g and (3) for more or less lead use proportionate specimen sizes. Warm on a hot plate at low heat, swirling the flask until the specimen is completely dissolved. 9.3 In a second flask (blank) put the same amount of glacial acetic acid but no specimen. Add 200 mL ofisopropyl alcohol, 100 mL ofwater, 6 mL ofconcentrated NH40H, 10 mL 0f NaiC2H3O2, and 50 mL of EDTA solution to each flask. Swirl to ensure complete mixing and warm both flasks at steam bath temperature for 5 min. 9.4 To each of the flasks add 2 mL of PAN indicator and titrate with the standard CuS04 solution to a blue end point] No t e 2--Because of the color Of metal indicators (and some of their complexes) being affected by pH changes, the pH must be kept constant during titration by the recommended buffer during titration. 10. Calculation . ...: jj 10.1 Calculate the percent of lead, A, present as follows: ' ' | (3> | where: ;j B = CuS04 solution required for titration of the blank, jj mL, . v' 1 V4 = CuS04 solution required for the specimen, mL, ? M2 = molarity of CuS04 solution, F = millimolecular weight of the metal in the sample = 0.2072 for lead, and | S = specimen used, g. ' | 11. Precision and Bias f 11.1 Precision: ; i 1.1.1 Repeatability--Tv/o results, each the mean of du- f plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by ! more than 0.10 % lead. j 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 0.50 % lead. 11.2 Bias--Bias has not been determined for this test method. where: Mi - molarity of EDTA solution, 12` Keywords 12.1 drier analysis; EDTA method; lead 352 DUP050296016 # D 2374 The AmericanSociety 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 standardis subject to revision et any time by the responsible technical committee andmust be reviewedevery live years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or foraddftional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. d- 353 DUP050296017 Designation: D 2375 - 85 (Reapproved 1990),'61 Standard Test Method for Manganese in Paint Driers by EDTA Method1 This standard is issued under the fixed1designation D 2375; the nurfiber immediately following the designation indicates the yeat of original adoption of.'in the case'bf revision, the year oflast revision. A number in parentheses indicates the year of last mapproval. A superscript epsilon {<) indicates an editorial change since the last revision or reapproval. ei No t e--Section 12 was added editorially in May 1990. 1. Scope 1.1 This test method covers a titrimetric determination of manganese in liquid paint driers that can be dissolved in a toluene-alcohol mixture and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA). 1.2 This test method is not applicable to drier blends. 1.3 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 600 Specification for Liquid Paint Driers2 D1193 Specification for Reagent Water3 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals4 E 300 Practice for Sampling Industrial Chemicals5 3. Summary of Test Method 3.1 The liquid drier is dissolved in toluene and ethyl alcohol and treated with an excess of standard EDTA solution. The excess is titrated with standard zinc chloride solution using Eriochrome Black-T as the indicator. 4. Significance and Use 4.1 The amount of manganese drier used in oxidizingtype coatings significantly affects their drying properties. This test method may be used to confirm the stated manganese content ofpure liquid manganese drier soluble in toluene-alcohol and manufactured for use by the coatings industry. 5. Apparatus 5.1 Centrifuge, capable of developing 1000 to 2000 g. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 2375 - 65 T. Last previous edition D 2375 - 79. 2 Annua! Book ofASTM Standards. Vol 06.03. 3 Annua! Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annua! Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Ammonium Chloride (NH4C1). 6.4 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). 6.5 l-Ascorbic Acid. 6.6 Buffer Solution--Add 350 mL of concentrated NH4OH (sp gr 0.90) to 54 g of NH4CI and dilute to 1 L with water. 6.7 Eriochrome Black-T Indicator--Triturate 0.2 g of Eriochrome Black-T and 100 g of NaCl, and store the mixture in a tightly stoppered bottle. This mixture remains stable for several years. 6.8 Ethyl Alcohol (95 %), pure or denatured. 6.9 EDTA, Standard Solution (0.05 M)--Dissolve 18.62 g of EDTA in water and dilute to 1 L. Store in a polyethylene or borosilicate glass bottle. 6.10 Hydrochloric Acid (sp gr 1.19)--Concentrated (hy drochloric acid (HC1): 6.11 Sodium Chloride (NaCl). 6.12 Toluene. 6.13 Zinc, Granular. 6.14 Zinc Chloride, Standard Solution (0.05 M)--Weigh 3.2690 g of zinc to the nearest 0.5 mg and dissolve in 50 mL of dilute HC1 (14 mL of concentrated HC1 (sp gr 1.19) to 36 mL of water). Warm if necessary. Dilute the zinc chloride (ZnCi2) solution to 1 L in a volumetric flask. Mx = 3.2690/65.37 (0 where: Mx = molarity of ZnCl2 solution, and 65.37 = zinc to produce a 1 M solution, g. 6 "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 Nostrand Co. Inc., New York, NY and the "United States Pharmacopeia." 354 DUP050296018 # D 2375 ampling si Take a small sample of liquid drier from bulk using procedures in Practice E 300 appropriate for the size of icontainer: section on Bottle Sampling for tanks and tank ", or section on Tube Sampling for drums and cans. 1--Liquid driers are normally homogeneous so that only le physical tests, such as specific gravity or solids content, on top bottom samples from tanks, are required to confirm that separation not occurred.. Agitate drams in. accordance with section on Tube pling in Practice E 300. .2 Examine the sample of drier for sediment or sus- nded matter which, if present, is evidence of noncompli- giwith Sjfecification D600. ^ 7.3 If the sample is homogeneous keep it in a stoppered ssel to prevent solvent evaporation prior to analyst Standardization s. 1 MDTA, Standard Solution (0.0.5 M)--Measure 40.00 , of the EDTA solution into a 250-mL flask that contains mL of toluene and 100 mL of alcohol. Add 15mL of ffen. solution .and .2;g;:pf indicator mixture, and mix oroughiy. Titrate with the standard zinc chloride solution the first permanent appearance of a red color. 8.1.1 Calculate the molarity of the EDTA solution. M2, as llows:v ' here:. ; m2 = ViM'i/Ab.o i 'r.; ' . /. s s. fr: ", ZnCl2 solution, mL, EDTA solution titrated, mL. ' (2) ^Procedure,, V 9.1 Check the clarity of the drier. If not clear, centrifuge a {portion of the* sample until it-is clear. Keep the .centrifuge tube stoppered so that solvent will not evaporate. * 9.2 From a buret place a few gtams of the drier in a 50-mL Erlenmeyer flask that is5 fitted with a cork through | which a dropping tube and rubber bulb (or eye dropper) pass ! and obtain'the total weight. Weigh by deference two or three 1-g specimens (10 drops weigh about 0.2 g) to the nearest 0.5 mg into 400-mL assay beakers or wide-mouthed flasks (Note 2). Add 10 mL of toluene to each specimen and swirl to mix. Add 100 mL of 95 % ethyl alcohol and swirl again until the specimen is dissolved and well dispersed. From a buret measure 40.0 mL of EDTA solution into each beaker. Add 0.3 g of ascorbic acid, 15 mL of buffer solution, and 0.2 g of the indicator .mixture. Mix thoroughly by swirling. Titrate with the standard ZnCl2 solution to the first permanent tinge of red. Maintain vigorous swirling during the titration to ensure thorough mixing of the two phases which may appear. . , No t e 2--If a magnetic stirrer is available, it is convenient to titrate in an ordinary beaker. Stirring magnetically ensures thorough mixing during the titration. .No t e 3--If.the end .point is overstepped, add 1,0 mL of the EDTA solution to the mixture and titrate again with standard Zn02 solution. Use total volume of each solution for the. calculation. ... 10. Calculation . 10.1 Calculate the percent manganese present, A, as follows:- r ' A = K( K2 x M2) - (r3 X Mi)) x 5.494)/S ' (3) where: . .. .... V2 -- EDTA solution, mL, V3 = ZnCl2 solution required for specimen, mL, S = specimen used, g, and 5.494 = miilimolar weight of manganese X 100. 11. Precision and Bias ii`H Precision: ' 11.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the-same operator on different days should be considered suspect if they differ by mote than 0.05 % manganese. 11.1.2 Reproducibility--Tvto results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.15 % manganese. . 1L2 Bias--Bias has not been determined for this test method. 12. Keywords 12.1 EDTA method; manganese; drier analysis TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection '' . with any item mentionedin this standard'; Users ot ttiis standard are expressly advisedthat 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 bereviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard ortor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a dieeting of the responsible technical committee, which you may attend, tf'you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ' 355 DUP050296019 Designation: D 2378 - 84 (Reapproved 1987) Standard Specification for Formaldehyde 50 % Grade Uninhibited and 37 % Grade Inhibited and Uninhibited1 This standard is issued under the fixed designation D 2378; 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 50% uninhibited formalde hyde and 37 % uninhibited and inhibited formaldehyde. 1.2 The material specified in this standard may be haz ardous if improperly handled. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses the material to consult and establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D891 Test Methods for Specific Gravity pf Liquid Indus, trial Chemicals2 D120? Test Method for Color of Clear Liquids.(Platinum- Cobalt Scale)3 D 2087 Test Method for Iron in Formaldehyde Solutions4 D 2194 Test Method for Concentration of Formaldehyde Solutions4 D2379 Test Method for Acidity of Formaldehyde So lutions4 D2380 Test Method for Methanol Content of Formalde hyde Solutions4 E 300 Practice for Sampling Industrial Chemicals5 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27, 1984. Published September 1984. Originally published as D 2378 - 65 T. Last previous edition D 2378 - 79. 1 Annual Book ofASTM Standards, Vd. 15.05. 3 Annual Book ofASTM Standards, Vols 06.0) and 06.03. 4 Annual Book ofASTMStandards, Vol 06.03. 5 Annual Book ofASTM Standards, Vols 06.03 and i 5.05. 2.2 U.S. Federal Standard: PPP-C-2020 Federal Specification For Packaging of Chemicals, Liquid, Dry, and Paste6 3. Properties 3.1 The physical and chemical properties of formalde hyde, 50 % uninhibited and 37 % uninhibited and inhibited, shall conform to the requirements specified in Table 1. 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Precautions 5.1 Formaldehyde and formaldehyde solutions are toxic and exposure to them should be minimized to avoid acute effects and possible sensitizing. Consult the supplier's Mate rial Safety Data Sheet for specific hazard information. 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: . 6.1.1 Apparent Specific Gravity--Test Method D 891. 6.1.2 Formaldehyde Content--Test Method D 2194. 6.1.3 Acidity--Test Method D 2379. 6.1.4 Color--Test Method D 1209. 6.1.5 Iron--Test Method D 2087. 6.1.6 Methanol Content--iTest Method D 2380. 7. Packaging and Package Marking 7.1 Package size to be agreed upon between the purchaser and supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 6 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 356 DUP050296020 specific gravity at 25/25sC iyde content, weight % D2378 TABLE 1 Physical and Chemical Properties of Formaldehyde Formaldehyde 50 % Grade Formaldehyde 37 % Grade 1.1470-1.1520 49.75 - 50.5 0.05 10 1.0 1.5 dear and free:of suspended matter ,: *.0749-1.1139 37.0 - 37.4 0.02 10 1.0 as agreed upon between the purchaser and seller clear and free of suspended matter with any' Item mentionedln this standard, Usersbt this standard are expressly advlsed that determination of the validity of any stich patent rights, and the risk of Infringement of slrch rights, are entirely their awn responsibility. . t Thjs standardIs subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and Ifnotrevised, eitherreapproved or withdrawn. Yourcomments are Invitedeither tor revision otthis standarddrfor additional standards and should be addressed to A&TM'Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may atterid. If you feet ttik'your comments have nob received a fair hearirig you should make your , views known to. the ASTM Committee on Standards,.391B Race St., Philadelphia, PA 19103. ,i. i. l - ' 'H J: 357 DUP050296021 Designation: D 2379 - 84 (Reapproved 1987) Standard Teat Method for Acidity of Formaldehyde Solutions1 This standard is issued under the fixed designation D 2379; 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 revirion or reapproval. 1. Scope 1.1 This test method covers the determination of the acidity of commercially available formaldehyde 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 of regulatory Imitations prior to use. Specific precautionary statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D2380 Test Method for Methanol Content of Formalde hyde Solutions3 E 200 Practice for Preparation, Standardization, and Stor age of Standard Solutions for Chemical Analysis4 3. Summary of Method 3.1 A specimen is titrated with standard alkali to the bromthymol blue end point. 4. Significance and Use 4.1 This test method provides a measurement of acidity (as formic acid) in formaldehyde solutions. The results of these measurements can be used for specification acceptance. 5. Apparatus 5.1 Buret, 25-mL, calibrated in 0.1-mL divisions. A TFE- fluorocarbon resin stopcock is suitable for this purpose. 6. Reagents and Materials 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.5 Other ' 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 D01.3S on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27,1984. Published December 1984. Originally published as D 2379 - 65 T. Last previous edition D 2379 - 79. * Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ifASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 15.05. s "Reagent Chemicals, American Chemical Society Specifications," American Chemical Society, Washington, D. C. For suggestions on the testing ofreagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Company, Inc., New York, N. Y., and the "United States Pharmacopeia." 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 IV of Specification D 1193. 6.3 Bromthymol Blue Indicator Solution (1.0 g/L)--Dis solve 0.1 g of the water-soluble form of bromthymol blue indicator powder ip 100 mL of water. 6.4 Sodium Hydroxide, Standard Solution (0.1 N)--Pre pare and standardize 0.1 N sodium hydroxide (NaOH) solution as described in Practice E 200. 7. Precautions 7.1 Formaldehyde and formaldehyde solutions are haz ardous and exposure to them should be minimized to avoid acute effects and possible sensitization. Consult your sup plier's Material Safety Data Sheet for specific hazard infor mation. 7.2 Sodium hydroxide solutions are corrosive and haz ardous. Exercise steps to prevent contact with the skin or eyes. Consult supplier's Material Safety Data Sheet for specific hazard. 8. Procedure 8.1 Measure 50 mL of the sample into a 250-mL Erlenmeyer flask, add 3 or 4 drops of bromthymol blue indicator solution, and titrate with 0.1 N NaOH solution to a blue end point. 8.2 Ifgood laboratory practice dictates that the concentra tion of NaOH be adjusted as a result of higher or lower acid levels, then adjust as necessary using Methods E 200, and titrate to a blue end point. 9. Calculation 9.1 Calculate the percent of formic acid as follows: Formic acid, weight % = [{VxNx 0.046)/(5' x D)J x 100 where: V = millilitres of NaOH solution, required for titration of the specimen, N = normality of the NaOH solution, 0.046 = the milliequivalent weight of formic acid, 5 = millilitres of sample used, and D = specific gravity of sample. The value of D from Test Method D 2380, may be used, although specific gravity estimated to the second decimal is adequate. 10. Report 10.1 Report the percent formic acid to the nearest 0.001 %. Duplicate determinations which agree within 358 DU P050296022 % absolute are acceptable for averaging (95 % confiIevel). a mj I DvAft 7 % absolute at 60 degrees of freedom, and the be' iboratories standard deviation 0.0031 % absolute at 9 of freedom. Based on these standard deviations, the wing criteria should be used for judging the acceptability ults at the 95 % confidence level: 11.1.1 Repeatability--Two results, each the mean of du plicates, obtained by the same analyst on different days should be considered suspect if they differ by more than 0.002 % absolute. 11.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by analysis in different laboratories, should be considered suspect if they differ by more than 0.010 % absolute. No t e--The above precision estimates are based on an interlaboratory study involving ten laboratories using three samples with two analysts performing' duplicate runs on each of two days. The mean level of the acidity value of the samples studied was 0.02 %. The American Society for Testing and Maiedals takes no position respecting the vaBdity of any patent rights assartedin 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 ofinfringement of such rights, are entirely their own responsibility. This standard IS subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and It notrevised, eitherreapproved or withdrawn. Your comments ere Invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Pace St, Philadelphia, PA 19103. 359 DUP050296023 Designation: D 2380 - 84 (Reapproved 1987) Standard Test Method for Methanol Content of Formaldehyde Solutions1 This Sandard is issued under the fixed designation D 2380; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflist revision. A number in parentheses indicatesthe year'-oflast reapproval, k superscript epsilon (e) indicates an editorial changesince the last revision or reapproval. ' . 1. Scope 1 ; 1.1 This test method'provides'for thd cafculdtibn of the methanol content of commercially available 37 % formalde hyde solutions and is based on the relationship of 'spedfic gravity to formaldehyde and methanol contest,2 Separate equations are given for three ranges of methanol: 0 to 2 %, 6 to 8 %, and 12 to 15 %. 1.2 This standard may involve hazardousnmefidls, oper ations, and equipment: foif 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 precautionary statements ares given in Section 4. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D2194 Test Method for Concentration of Formaldehyde Solutions3 3. Significance and Use 3.1 This test method provides a measurement of meth anol content of formaldehyde solutions. The results of these measurements can be used for specification acceptance. 3.2 This test method is applicable to 37 % formaldehyde solutions containing 0 to 2 %, 6 to 8 %, or 12 to 15 % methanol. 4. Precautions 4.1 Formalydehyde and formaldehyde solutions and con tact should be minimized to avoid acute effects and possible sensitizing. Consult the supplier's Material Safety Data Sheet for specific hazard information. 5. Procedure 5.1 Determine the apparent specific gravity of the mate rial by a method that is accurate to the fourth decimal place, 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 D0I.3S on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27,1984. Published September 1984. Originally published as D 2380 - 65 T. Last previous edition D 2380 - 79. 2 Walker, J. F., Formaldehyde, 3rd edition, 1964, pp. 86-91. 3 Annual Book ofASTM Standards, Vol 06.03. the temperature oFboth the spetimeri arid the water being 25C. See Methods D 268. 5.2 Determine the formaldehyde content of the material in accordance with T'eSTMethod D 2194; 6. Calculation 6.1 ..Calculate the methanol content as follows using the -.appropriate equation forthe.expected methanol range: 6.1.1 6 to 2% Methanol: .. : Methanol; wt % .w (1.0017 + 0.003F - C)/0.00253 6.1.2 6 to 8% Methanol: Methanol, wt % = (1.0015 + 0.003F - Z))/0.00250 6.1.3 12 to 15 % Methanol: Methanol, wt % = (1.0210 + 0.0025F - Z>)/0.00257 where: F = formaldehyde content, weight %, and D = specific gravity at 25/25C. No t e 1--The numerical factors were calculated from the slope ofthe methanol curve of a nomograph relating specific gravity at 25/25C to methanol-formaldehyde content. 7. Report 7.1 Report the methanol content to the nearest 0.1 %. 8. Precision and Bias 8.1 In an interlaboratory study of this test method, the !': within-laboratory standard deviation was found to be 0.10 % j absolute with 28 degrees of freedom and the between- 3 laboratories standard deviation 0.16% absolute with 12 h 1 degrees of freedom based on these standard deviations, the V following criteria should be used for judging the acceptability of results at the 95 % confidence level: < 8.1.1 Repeatability--Two results, each the mean of dupli cates, obtained by the same analyst on different days should be considered suspect if they differ by more than 0.3 % absolute. i 8.1.2 Reproducibility-- Two results, each the mean of J duplicates, obtained by analysts in different laboratories, should be considered suspect if they differ by more than 0.5 % absolute. No t e 2--The above precision estimates are based on two interlabo ratory studies involving five and nine laboratories respectively, using two different samples in each case, with a single analyst performing duplicate runs on each of two days. The methanol levels studied were 1.5, 6.5, and 14.3 %. smis 360 DUP050296024 The American Society for Testing and Materials takes no position respecting the validity ofan/ parent rights assertedin connection with any item mentioned in tills standard. Users of this standard are expressly advised that determination or 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, eitherreapprovedor withdrawn. Yourcomments 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 technics/. 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, PA19103. 361 DU P050296025 Designation: D 2575 - 70 (Reapproved 1991)1 Standard Methods of Testing Polymerized Fatty Acids1 This standard is issued under the fixed designation D 2575; the number mimcdiately following the designation indicates the year of original adoption or, in the case of revision, the year dflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapproval. *'No t b--Keywords were added editorially in August 1991. i 1. Scope 1.1 These methods cover selection and application of procedures for testing polymerized fatty acids specifying the use of other ASTM methods. 1.2 The procedures appear in the following sections: Section ASTM Method Terminology Sampling Acid Value Saponification Value Unsaponifiable Matter Water, (Karl Fischer) Color, Gardner 3 4 DM66 5 D 1980 6 D 1962 7 D 1965 8 D 1364 9 D 1544 2. Referenced Documents 2.1 ASTM Standards: D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Re lated Materials2 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids2 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Acids, and Polymerized Fatty Adds2 D1980 Test Method for Add Value of Fatty Adds and Polymerized Fatty Acids2 3. Terminology 3.1 Definition: 3.1.1 polymerized fatty acids--polycarboxylic adds pro duced by polymerizing acids from animal or vegetable fats and oils, in rither an ester or free add state, by means ofheat alone or catalytically. 1 These methods are under the jurisdiction of ASTM Committee D-l on Paints and Related Coatings and Materials and is the direct responsibility of D 01.32 on Drying Oils. Current edition effective Dec. 24, 1970. Originally issued 1967. Replaces D 2575 - 67 T. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01, 06.02 and 06.03. 4. Sampling | 4.1 Sample the material in accordance with Test Method D 1466. 5. Add Value 5.1 Determine add value in accordance with Method D1980. 5.2 The predsion of the method (95 % confidence level for polymerized fatty adds) in the range of values from 162 to 195 is as follows: repeatability, 1.5; reproducibility, 2.4. i ft ; 1 6. Saponification Value 6.1 Determine saponification value in accordance witb a Test Method D 1962. 6.2 The precision of the method (95 % confidence level) ft in the range of values from 187 to 197 is as follows: 4 repeatability, 10.7; reprodudbility, 11.1. ` ;i 7. Percent of Unsaponifiable Matter 7.1 Determine the percent of unsaponifiable matter in accordance with Method D 1965. 7.2 The precision of the method (95 % confidence level) in the range of values from 0.3 to 2.6 is as follows: repeatability, 0.53; reproducibility, 0.75. > ' 8. Water by the Karl Fisher Method 8.1 Determine moisture in accordance with Test Method D 1364. 8.2 The predsion of the method (95 % confidence level) in the range of values from 0.0 to 1.2% is as follows: repeatability, 0.16; reproducibility, 0.17. 9. Color by the Gardner Method 9.1 The Gardner color system was chosen as best suited for reporting the colors of these products. 9.2 Determine the color in accordance with Test Method D 1544. 9.3 The precision of the method (95 % confidence level) in the range of values from 1 to 18 is as follows: repeatability, 0.6 unit, reproducibility, 1.6 units. T 10. Keywords 10.1 fatty adds; polymerized fatty adds. 362 DUP050296026 # D 2575 The American Society for Testing end 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 technicalcommittee andmust be reviewed every five years and Ifnot revised, eitherreapproved or withdrawn. Your comments are invitedeither forrevision of this standard orfor additionalstandards and should beaddressed to ASTM Headquarters. Your comments will receive carebi! consideration at a meeting of the responsible technical cammittee. whlcfi you may attend. 'lf you fed 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.i, i, -v 363 DUP050296027 Designation: D 2613 - 85 (Reapproved 1990)'61 Standard Test Method for Calcium or Zinc in Paint Driers by EDTA Method1 This standard is issued under the fixed designation D 2613; 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 epsiion (c) indicates an editorial change since the last revision or reappiovai. ei No t e--Section 12 was added editorially in May 1990. 1. Scope 1.1 This test method covers a titrimetric determination of calcium in liquid calcium driers and zinc in liquid zinc driers that can be dissolved in a toluene-alcohol mixture and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA). 1.2 This test method is not applicable to drier blends. 1.3 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 600 Specification for Liquid Paint Driers12 D1193 Specification for Reagent Water3 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals4 E 300 Practice for Sampling Industrial Chemicals5 3. Summary of Test Method 3.1 The liquid calcium or zinc drier is dissolved in toluene and ethyl alcohol and treated with an excess of standard EDTA solution. The excess is titrated with a standard zinc chloride solution using Eriochrome Black-T as the indicator. 4. Significance and Use 4.1 This test method may be used to confirm the stated calcium or zinc content ofpure liquid calcium or zinc driers soluble in toluene-alcohol and manufactured for use by the coatings industry. 5. Apparatus 5.1 Centrifuge, capable of developing 1000 to 2000 g. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 2613 - 67 T. Last previous edition D 2613 - 79. 1 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Bock ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards Vols 06.03 and 15.05. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Buffer Solution--Add 350 mL of concentrated ammo nium hydroxide (NH4OH, sp gr 0.90) to 54 g of ammonium chloride (NH4C1) and dilute to 1 L with water. 6.4 EDTA, Standard Solution (0.05 M)--Weigh 18.62 g of EDTA, dissolve in water and dilute to 1 L. Store in a polyethylene or borosilicate glass bottle. 6.5 Indicator Mixture--Triturate 0.2 g of Eriochrome Black-T and 100 g of sodium chloride (NaCl) and store the mixture in a tightly stoppered bottle. This mixture remains stable for several years. 6.6 Zinc Chloride, Standard Solution (0.05 M)--Weigh 3.2690 g of zinc metal to 0.5 mg and dissolve in 50 mL of dilute hydrochloric acid (14 mL of concentrated HC1 (sp gr 1.42) to 36 mL of water). Warm if necessary. Dilute to 1 L in a volumetric flask. 7. Sampling 7.1 Take a small sample of liquid drier from bulk using the procedures in Practice E 300 appropriate for the size of the container Section 19 for tanks and tank cars or Section 23 for drums and cans. No t e 1--Liquid driers are normally homogeneous so that only simple physical tests, such as specific gravity or solids content, on top and bottom samples from tanks, are required to confirm that separation has not occurred. Agitate drums in accordance with the section on Tube Sampling of Practice E 300. 7.2 Examine the sample of drier for sediment or sus pended matter which if present is evidence of noncompli ance with Specification D 600. 7.3 If the sample is homogeneous keep it in a stoppered 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." 364 DUP050296028 / D 2613 |to prevent solvent evaporation prior to analysis, landardtzation ; Zinc Chloride Standard Solution (0.05 M)--Calculate pact molarity, Mt, of the solution as follows: ^ Mx = 5i/65.37 (1) = zinc used, g, and = zinc to produce a 1 M solution, g/L. EDTA, Standard Solution (0.05 M)--Measure 40.0 If the EDTA solution into a 250-mL flask that contains , of toluene and 100 mL of 95 % ethyl alcohol pine,or Jtured. Add 15 mL of buffer solution, 0.2 g of indicator pure, and mix thoroughly. Titrate with the Standard zinc Jpon to the first permanent appearance of a red color. 2.1 Calculate the molarity ofdie EDTA solution, as, aws: Mi =? (Ft x Mi)/40.0 (2) bre: -- ZnCl2 solution, mL, - EDTA solution titrated, mL. ( ' Procedure 9.1 Check the clarity of the drier. If not clear, centrifuge a tion of the sample until it is clear. Keep the. centrifuge. stoppered so that the solvent will not evaporate. , 1.2 From' a buret place a`few* grams of the`drier in a phL ErlenmeyCr flask that is fitted with a itork Through lich passes a dropping tube and rubber bulb or eye dropper Ip'Obtain the total weight. Weigh by differencfe two or three [specimens (10drops weigh-about 0.2 g) to the dearest 0.5 |`;itttp. 400-mL assay beakers or wide7mouth fldsks (Note | Add 10 !mL of toluene to each specimen arid swirl to mixl pdd 100 mL of 95 % ethyl alcohol and swirl again until the pecimen is dissolved and well dispersed; Front , a buret ifesufe 40.0 mL of EDTA splution into each beaker. Add p mL of buffer solution and 0.20 g of the indicator mixture (more or less can be added, if desired). Mix thoroughly by swirling. Titrate with the standard ZnCl2 solution to the first permanent .tinge of red.,hlaintain. vigorous swirling during the titration to ensure thorough mixing of the two phases which may appear. ''. No t e 2--If a magnetic stirrer is available, it is convenient to titrate in an ordinary beaker. Stirring magnetically ensures thorough mixing duringUhe titration. ` No t e 3--If the end point is overstepped, add 1.0 mL of the EDTA solution to the mixture and titrate again with standard ZnCJ2 solution. Use total volume of each solution for the calculation. 10. Calculation ! 10.1 Calculate the percent of Ca, A, or Zn, JB,;as follows: A = l[(V2M2) - (Vy\li)} 4.01J/S B = ll(V2M2) - (F3M,)] 6.54]jS (3) (4) where: V2 = EDTA solution, mL, V3 == ZnCl2 solution required for specimen, mL, S:- = specimen used, g, \ ` 4.01 = millimolar weight of Ca x 100, and` 6.54 = millimolarweight of Zn X 100. 11,. Precision and Bias 11.1 Precision: ILL1! 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 0.05 % calcium or zinc. 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 0.10'^calcium or zina' 11.2 Bias'--Bias' has not been determined Tor this test method. 12. Keywords 12.1 calcium; drier analysis; EDTA" analysis; zinc The American Society for Testing andMaterials takes noposition respecting the validity^ any patent rights asserted in connection with any Item mentioned-in thjs 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. ThisstandardIs subject to revision at any time.by theicesponsible technical committee and must be reviewed every five years and .if not revised, either reapprpved or withdrawn. Your comments are invited either for revision ofthis standard or for additionalstandards and should be addrossed.to.ASTM.Headquarters. Your.comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fed that your comments have not received a fair hearing you should make your views known to theASTM Committee on Standards. 1916 RaceSt., Philadelphia, PA 19103. , /, 365 DUP0502 96029 Designation: D 2627 - 91 Standard Specification for Diacetone Alcohol1 This standard is issued under the fixed designation D 2627; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers diacetone alcohol.2 1.2 For specific hazard information and guidance, consult the suppliers Material Safety Data Sheet. 1. Referenced Documents 2.1 ASTM Standards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings Mid Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)4 D1296 Test Method for Odor of Volatile Solvents and Diluents3 . D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D1722 Test Method for Water Miscibility of WaterSoluble Solvents3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 3. Properties 3.1 Diacetone alcohol shall conform to the following requirements: 1 This specification is under the jurisdiction of the ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO1.35 on Solvents, Plasticizer;, and Chemical Intermediates. Current edition approved Aug. 1:5, 1991. Published October 1991. Originally published as D 2627 - 67 T. Last previous edition D 2627 - 87. 2 This compound is also known as 4-hydroxy-4-methyl-pentanone-2. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annua! Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 8 Available firom Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. Apparent specific gravity 20/20*C 25/25"C Color, Pt-Co units, max Distillation, 760 mm Hg Initial boiling point, "C, min Dry Point, 'C, max Nonvolatile matter, g/100 mL, max Odor Water, wt %, max4 Acidity (free acid as acetic acid), wt %, max Water solubility 0.938-0.941 0.935-0.938 25 145. 172 0.01 nonresidual 0.1. 0.01 miscible with distilled water in all proportions * This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20'C. 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300.- 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20 C or 25C. (See Test Methods D 268 and D 4052.) 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D.1078, using an ASTM Solvents Distillation Thermometer 102C having a range from 123 to 177C and conforming to the require ments of Specification E 1. No t e--In order to avoid an erratic value for the initial boiling point the distillation flask should be clean and free of any residual carbon deposit. This exception to the suggestion in Note 1 of Test Method D 1078 is specifically applicable to diacetone alcohol. Particular care should also be given to the heating rate so that the initial boiling point is obtained within the specified time of 5 to 10 min. 5.1.4 Nonvolatile Matter--Test Method D1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Method D 1364. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Water Solubility--Test Method D 1722. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keyword 7.1 diacetone alcohol 366 DUP050296030 # D 2627 The American Society for Testing andMaterials takes no position respecting the validity ol anypatent rights asserted In connection with any item mentioned In this standard. Users ot this standard are expressly actWseof that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are antirely their own responsibility. This standard Is sobject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you, may attend. 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. 367 DUP050296031 Designation: D 2634 - 86 Standard Specification for Methyl Amyl Acetate (95 % Grade)1 This standard is issued under the fixed.'designation D 2634; the number immediately following the designation indicates the year of' original adoption or, in the case of revision,, the year of lait revision. A number in parentheses indioitesthe year oflasit reapproval. A superscript epsilon (f) indicates an editorial change since'the last revision or reawjroval. 1. Scope 1.1 This specification covers methyl amyl acetate2 (95 % grade) for use in paint, varnish, and related products. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)4 5 D1296 Test Method for Odor of Volatile Solvents and Diluents3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D1617 Test Method for Ester Value of Solvents and Thinners3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Packaging of Chemicals, Liquid, Dry, and Paste8 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coalings and Materials and is the direct responsibility of Subcom mittee DO 1.33 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Sept. 26, J986. Published November 1986. Originally published as D 2634 - 67. Last previous edition D 2634 - 81. 2 This compound is also known as 4-methyl-2-pentyl acetate. 3 Annual Book ofASTM Standards, Vo! 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05,03. 6 Annual Book ofASTM Standards, Vols 14.03 and 05.03. 1 Annual Book ofASTM Standards, Vols 06.03 and' 15.05. 8 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Are., Philadelphia, PA 19111-5094. 3. Properties 3.1 Methyl amyl acetate sh^U conform to the following requirements: Apparent specific gravity; 20/20C 25/25*C Color, Pt-Co units, max Distillation range Below 142.5"C Above 149.5C Nonvolatile matter mg/100 mL, max Water, wt %, max Acidity (free acid as acetic acid), wt %, max Ester value, wt %, min 0.856 to 0.859 0.852 to 0.855 15 none none 5 0.1 ' 0.01 95.0 4. Sampling 5.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 20C. See Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 102C having a range from 123 to 177C, and conforming to the require ments of Specification E 1, shall be used in connection with this test. 5.1.4 Nonvolatile Matter--Test Method D1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Method D 1364. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Ester Value--Test Method D 1617. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 368 DUP050296032 # D 2634 TheAmerican 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 patentrlghts, 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. Your comments are Invited either torrevision 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 theASTM Committee on Standards, 1916 Bace St., Philadelphia, PA 19103. 369 DUP050296033 Designation: D 2635 -91 Standard Specification for Methyl Isohutyl Carbinol1 This standard is issued under the fixed designation D 2635; the number immediately following the designation itidiciites the.'yhar of original adoption or, in the case ofrevi&oririlipyearoflastriyision. Antipnberin parentheses indicates the year of last reapprdvai. A superscript epsilon (<) indicates an editorial Change since the last revision dr reappfoval. r 1. Scope 1.1 This specification covers methyl isobutyl carbinol2 for use in paint, varnish, lacquer, and related products. 1.2 For specific hazard information and guidance, consult supplier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)4 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for use in Paint, Varnish, Lacquer, and Related Products3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D 3329 Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: 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 D 01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 15, 1991. Published July 1991. Originally, published as D 2635 - 67. Last previous edition D 2635 - 87. 2 This compound is also known its 4-methyl-pentanol-2 and methyl amyl alcohol. 3 Annual Book ofASTM Standards, Voi 06.03. 4 Annual Book ofASTM Standards, Vols 06.0] and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. "Annual Book ofASTM Standards, Vols 05.03 and 14,03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 3. Properties 3.1 Methyl isobutyl carbinol shall conform to the fol lowing requirements: Apparent specific gravity 20/20'C 25/25"C Color, Pt-Co units, max Distillation, 760 mm Hg Initial boiling point, "C, min Dry point, `C, max Water, wt%, max Acidity (free acid as acetic acid), wt %, max Nonvolatile matter, mg/100 mL, max Purity, wt %, min 0.806 to 0.809 0.803 to 0.806 10 130.0 133.0 0.1 0.005 5 98,0 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The material shall be sampled and the properties enumerated in this specification shall be determined in accordance with the following ASTM test methods.: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 20C or 25C. (See Test Methods D 268 and D 4052.) 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 41C having a range from 98 to 152C, and conforming to the requirements in Specification E 1. 5.1.4 Water--Test Method D 1364. 5.1.5 Acidity--Test Method D 1613. 5.1.6 Nonvolatile Matter--Test Method D 1353. 5.1.7 Purity--Test Method D 3329. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keyword 7.1 methyl isobutyl carbinol "Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 370' DU P050296034 # D 2635 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 suph patent rights, and the risk of infringement of such rights, are entirely their ovm responsibility. '' = , This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years Sad 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 ygu feel that your comments, have not received, a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. . , A ' Vrt, DUP050296035 Designation: D 2636 - 91 Standard Specification for Hexylene Glycol1 This standard is issued under the fixed designation D 2636; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers hexylene glycol2 for use in paint, varnish, lacquer, and related products. \ ,2 For specific hazard information and guidance, consult supplier's Material Safety Data Sheet. 2. Referenced Documents 2.1 .ASTM Standards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)4 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D 1722 Test Method for Water Miscibility of WaterSoluble Solvents3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 6 E 1 Specification for ASTM Thermometers E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 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 D 01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 15, 1991. Published July 1991. Originally published as D 2636 - 67. Last previous edition D 2636 - 87. 2 This compound is also known as 2-methyl pentanediol-2,4. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vols 14.03 and 05.03. 7 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 8 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3. Properties 3.1 Hexylene glyrol shall conform to the following requirements: Apparent specific gravity, 20/20'C 25/25"C Color, Pt-Co units, max Distillation range Acidity (free acid as acetic acid) wt %, max Water, wt %, max Water miscibility 0.921 to 0.924 0.918 to 0.921 15 3.0"C to include 197. PC 0.005 o.i passes test ' ! | i i 1 4. Sampling 4.1 The material shall be sampled in accordance with * Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall f be determined in accordance with the following ASTM i methods: 5.1.2 Apparent Specific Gravity--Determine the apparent f specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 20C or 25C. (See Method D 268 and Test Method D 4052). 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078 using an ij ASTM Solvents Distillation Thermometer 104C having a j range from 173 to 227C, and conforming to the require- i ments in Specification El. 5.1.4 Acidity--Test Method D 1613. 1 5.1.5 Water---Test Method D 1364. 5.1.6 Water Miscibility--Test Method D 1722. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keyword 7.1 hexylene glycol 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 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 is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, eitherreapproved or withdrawn. Yourcomments are 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. If you feeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 372 DUP050296036 Designation: D 2693 - 87 Standard Specification for Ethylene Glycol1'2 Tbis standard is issued underJhe fixed designation D 2693; the number immediately following the designation indicates the year of original adoption or, in. the case of revision, theyeai 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 specification covers ethylene glycol for use in the lation of surface coatings. eferenced Documents \ASTM Standards: 52 Test Method for Density and Relative Density of iquids by Digital Density Meter3 ,. 02 Method for Analysis of Ethylene Glycols and ropylene Glycols4 00 Practice for Sampling Industrial Chemicals5. U.S. Federal Specification: -C-2020 Chemical^ Liquid, Dry, and Taste: Packajging f6 operties Ethylene glycol'shall conform to the following require- Ijhis specification is under the jurisdiction ofASTM Committee D-1 on Paint Related Coatings and Materials ,and is the direct responsibility, of Subcora- ; D0I.35 on Solvents, Plasticizers, and Chemical Intermediates, ttent edition approved May.. 29, 1987. 'Published July 1987. Originally shed as D 2693 - 68, Last previous edition D 2693 - 83. This compound is also known as 1,2-ethanediol. Annual Book ofASTM Standards, Vol 05.03! ' `rnuat Book ofASTftt. Standards, Vol 15.05,/ 1 ' s Annual Book ofASTM Standards, Vols 06.03 and 15.05:- 6 Available from Standardization Documents Order Desk, Bldg. 4 Section D, Robbins Ave., Philadelphia, PA 19111-5094. Apparent specific gravity 20/20'C 25/25'C Color, Pt-Co units, max Distillation range, 769 mm Hg Initial boiling point, *C, min Dry point, "C, max Water, wt %, max Acidity as acetic acid, wt %, max Diethylene glycol, wt %, max Iron, ppm, max 1.1151 to 1.1156 1.1129 to 1.1134 15 193 204 0.2 0.005 1.0 1.0 4. Sampling 4.1 The material shall be sampled , in accordance with Practice E 300., 5.; Test Methods . . . ... 5.1 The properties enumerated in this specification shall be determined in accordance with Method E 202. 5.2 The specific gravity can also be determined in' accordance with Test Method D 4052. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon, by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. The American Society for Testing and Materials takes Reposition respecting the validity of,any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination ot the validity of any sueh patent right?, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time bythe responsible technical committee and must be reviewed.every five years end if not revised, eitherreapproved or withdrawn. Your comments are Invitedeither tor 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 technicalcommittee, whichyou may attend. If you feel that your commentshave hot receiveda fair hearing you should make your views known to'die ASTM Cofhiiiitthe on Standards, 1976 BacS St., Philadelphia, PA 19103. 373 DUP050296037 i Designation: D 2694 - 91 Standard Specification for Diethylene Glycol1'2 This standard is issued under the fixed designation D 2694; 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 revirion or reapproval. . 1. Scope 1.1 This specification covers diethyleae glycol for use in the preparation of surface coatings. 1.2 For specific hazard information and guidance, consult the suppliers Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 E 202 Method for Analysis of Ethylene Glycols and Propylene Glycols4 E 300 Practice for Sampling Industrial Chemicals5 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of6 3. Properties 3.1 Diethylene glycol shall conform to the following requirements: Apparent specific gravity 20/20'C 25/25C Color, Pt-Co units, max Distillation range, 760 mm Hg Initial boiling point, "C, min Dry point, "C, max Water, wt %, max Acidity as acetic acid, wt %, max Ethylene glyeoi; wt %,' max Triethylene glycol, wt %, max Iron, ppm, max . 1.1170 to 1.1200 1.1147 to 1.1177 15- 240 250 0.2 0.01 0.5 ' 1.0 ' 1.0 . 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with Method E 202. 5.2 The apparent specific gravity can also be determined in accordance with Test Method D 4052. 1 This specification is under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved May 15, 1991. Published July 1991. Originally published as D 2694 - 68. Last previous edition D 694-87. 2 This compound is also known as 2,2'oxydiethanol. 3 Annual Book ofASTM Standards, Vo! 05.03. 4 Annual Book ofASTM Standards, Voi 15.05. 5 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. > 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keyword 7.1 diethylene glycol 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 stendard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely Stair 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, eitherreapproved or withdrawn. Your comments are invited eitherforrevision 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 aSend. 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. 374 DUP050296038 Standard Specification for Propylene Glycol pecification covers propylene glycol for use in the preparation of surface coatings, ly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this specification was Lued in 1992 and replaced by ASTM Specification D 5164, for Propylene Glycol and Dipropylene Glycol.1 Book ofASTM Standards, Vol 06.03. 375 DUP050296039 Last ASTM Designation: D 2696 - 87 Standard Specification for Dipropylene Glycol This specification covers dipropylene glvco! for use in the.preparation of surface coatinRS. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this specification was discontinued in 1992 and replared by ASTM Specification D 5164, for Propylene Glycol and Dipippylene Glycol.1 1 Annual Book ofASTM Standards, Vol 06.03. 376 DUP050296040 Designation: D 2800 - 87 Standard Test Method for Preparation of Methyl Esters From Oils for Determination of Fatty Acid Composition by Gas-Liquid Chromatography1 This standard is issued under the fixed designation D 2800; 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 reapprova). A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 7501 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. Pe This test method covers a rapid procedure for converF animal and vegetable fatly oils into methyl esters of tty acids suitable for analysis by gas-liquid chromatog- This test method is believed to b& applicable to most g oils used in the paint industry including linseed, soya, wer, and cottonseed oils. Unsaturated oils with a ncy to undergo alkaline isomerization or to polymerize b presence ofboron trifluoride (BF3) may give erroneous ts. Unsaponifiables are not removed. This standard may involve hazardous materials, opers, and equipment. This standard does not purport to ess all ofthe safetyproblems associated with its use. It is responsibility of the user of this standard to establish ropriate safety and health practices and determine the licability of regulatory limitations prior to use. For cific hazard statements, see 5.4 and Note 1. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 : > 1983 Test Method for Fatty Acid Composition by Gas-Liquid Chromatography of Methyl Esters3 j D2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints3 D3457 Test Method for Preparation of Methyl Esters from. Fatty Acids for Determination of Fatty Acid Composition by Gas-Liquid Chromatography3 . Summary of Test Method 3.1 This test method is based upon a rapid saponification of the oil with methanolic sodium hydroxide followed by boiling the soaps with BF3-methanol in the same vessel to convert quantitatively the fatty acids to methyl esters. The methyl esters are floated out of the mixture upon addition of a saturated salt solution. 3.2 Methyl margarate may be added quantitatively to the oil prior to saponification and inethylation to serve as an internal standard and check on the recovery of monomeric methyl esters. For a discussion on the use of an Internal Standard see Test Method D 3457. 4. Significance and Use 4.1 This test method provides a means by which animal or vegetable fats and oils are converted into their methyl esters so that the fatty adds can then be analyzed by the use of Test Method D 1983. 5. Reagents and Materials 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise sperified. 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 sperifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi nation. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type IV of Spetification D 1193. 5.3 Boron Trifluoride, cylinder.5 5.4 Boron Trifluoride Reagent (125 g/L of Methanol)-- Add 1 L of methanol to a 2-L Erlenmeyer flask and weigh on a balance. Place in an ice bath and slowly bubble boron trifluoride (BF3) gas from a tank through a glass tube until 125 g are taken up. This operation should be performed in a good fume hood, and the gas should not flow so fast that white fumes emerge from the flask. The BF3 must be flowing through the glass tube before it is placed in and until it is removed from the methanol, or the methanol may be drawn into the gas cylinder valve system and cause an explosion. This reagent has an excellent shelf life and may be used up to four months from preparation. Refrigerate it in a glassstoppered bottle. No t e l: Caution--Handling BF3 gas is at best quite hazardous. It may be preferable to buy the reagent. 5.5 Methanol, anhydrous. 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 D 01.32 on Drying Oils. Current edition approved May 29, 1987. Published July 1987. Originally published as D 2800 - 70. Last previous edition D 2800-75{1980)el. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 1 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 Roan, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 5 Available from the Matheson Co., Box 966, Joliet, IL. 377 DUP050296041 # D 2800 5.6 Methyl Margarate--Methyl ester of margaric acid (heptadecanoic acid). 5.7 Petroleum Ether, redistilled, boiling point 30 to 60C. 5.8 Sodium Chloride, Saturated Solution--Prepare a sat urated solution of sodium chloride (NaG) in water. 5.9 Sodium Hydroxide, Methanol Solution (0.5 N)-- Prepare a 0.5 N solution of sodium hydroxide (NaOH) in ' methanol 6. Procedure 6.1 Weigh to 0.1 mg about 300 mg of oil into a 50-mL volumetric flask. Add to this specimen about 50 mg weighed to 0.1 mg of methyl margarate. If an internal standard or a check on the recovery of the methyl esters is not desired, the oil need not be weighed and the methyl margarate may be omitted. 6.2 Add 6 mL of 0.5 N methanolic NaOH solution, swirl, and heat the mixture on a steam bath until the oil globules go into solution. This step will take 5 to 10 min. No t e 2--With some lipid materials it may take somewhat longer, however, excessive reaction times should be avoided due to the possibility of alkali isomerization. 6.3 Add 8 mL of BF3-methanol reagent and boil for 2 min. Cool and add 1 mL of petroleum ether to the flask. 6.4 Add enough saturated NaCl solution to float the methyl esters up with the petroleum ether into the narrow neck of the flask 6.5 Withdraw the methyl ester layer by means of a syringe, and analyze immediately in accordance with Test, Method D 1983. The oils may usually be identified from their fatty acid composition in accordance with Method D 2245. TheAmerican Society for Testing andMaterials takes noposition respecting the validity atany patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical, committee and must be reviewed every five years end ifnot revised, either reapproved or withdrawn. Your comments are invited either for 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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, PA 19105. ; fi 1 1 f 378 DU P0502 96042 P Designation: D 2804 - 88 Standard Test Method for Purity of Methyl Ethyl Ketone Using Gas Chromatography1 This standard is issued under the fixed designation D 2804; the number immediately following the designation indicates the year of original adoption o.r, in the case of revision, the year of last revision. A number in parentheses indicates the year of Iasi reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. jScope |U This test method covers the determination of the jjity of methyl ethyl ketone by gas chromatography, purities including water, acidity, and nonvolatile matter | measured by appropriate ASTM procedures and the ilts are used to normalize the chromatographic value. 1.2 This standard may involve hazardous materials, oper- |ons, and equipment. This standard does not purport to wress all ofthe safety problems associated with its use. It is f responsibility of the user of this standard to establish propriate safety and health practices and determine the plicability ofregulatory limitations prior to use. El .3 For hazard information and guidance, see the sup|er's Material Safety Data Sheet. [ Referenced Documents |t2.1 ASTM Standards: D 1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re- if lated Products2 f D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer andRelated Products2 D2593 Test Method for Butadiene Purity and Hydro carbon Impurities by Gas Chromatography3 E 180; Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals4 p. Summary, of Test Method 3.1 A representative specimen is introduced into a gasIliquid partition column. The methyl ethyl ketone is sepaI rated from other impurities such as hydrocarbons, alcohols, acetone, di-jec-butyl ether, and ethyl acetate as the compo! nents are transported through the column by an inert carrier j gas. The separated components are measured in the effluent by a detector and recorded as a chromatogram. The chro matogram is interpreted by applying component-attenuation and detector-response factors to the peak areas, and the relative concentration is determined by relating individual 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 DDI.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 25, 1988. Published May 1988. Originally published as D 2804 - 69. Last previous edition D 2804 - 84. 2 Annual Book ofASTM Standards. Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.02. 4 Annual Book ofASTM Standards, Vol 15.05. peak response to the total peak response. Water, acidity, and. nonvolatiles are measured by the procedures listed in 3.2, and the results are used to normalize the results obtained by gas chromatography. 3.2 The appropriate ASTM test methods are: 3.2.1 Water--Test Method D 1364. 3.2.2 Acidity--Test Method D 1613. 3.2.3 Nonvolatile Matter--Method D 1353. 4. Significance and Use 4.1 This test method provides a measurement of com monly found impurities in commercially available methyl ethyl ketone. The measurement of these impurities and the results thereof can individually or when totaled and sub tracted from. J00 (assay) be used for specification purposes. 5. Apparatus 5.1 Chromatograph--Any gas chromatographic instru ment having either a thermal-conductivity or flame ioniza tion detector provided the system has sufficient sensitivity and stability to obtain for 0.01 weight % of impurity a recorder deflection of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The specimen size to be used in judging the sensitivity must be such that the column is not overloaded. 5.2 Column--Any column capable of resolving methyl ethyl ketone from the impurities that may be present. Possible impurities are paraffins, acetone, methanol, ethanol, propanol, isopropanol, tert-butanol, rec-butanol, di-^ec-butyl ether, and ethyl acetate. The peaks should be resolved, quantitatively in proportion to concentration, within a practical elapsed time. Columns that meet the requirements of this test method are listed in Table 1. Other columns may be used, provided the user establishes that a column gives the required separation and the precision requirements of Sec tion 13 are met. 5.3 Specimen Introduction System--Any specimen system capable ofintroducing a representative specimen into the column may be used. Systems that have been used successfully to introduce 1 to 10-jiL of methyl ethyl ketone specimens include microlitre syringes, micropipets, and liquid sampling valves. 5.4. Recorder--A recording potentiometer with a full-scale deflection of 5 mV or less, full-scale response time of 2 s or less, and sufficient sensitivity to meet the requirements of 5.1. 6. Reagents and Materials 6.1 Carrier Gas, appropriate to the type of detector used. Helium or hydrogen may be employed with thermal conduc tivity detectors, and nitrogen, helium, or argon with ioniza- ; 379 I DUP050296043 TABLE 1 Columns and Conditions Used Successlully in Cooperative Work Column: Liquid phase Liquid phase, weight % Support type Case) packed polyethylene glycol 1500* 10 TFE resinf Support mesh size Length, ft (m) Outside diameter, In. (mm) inside diameter, in. (mm) Column temperature, C Carrier gas Canter flow rate, mL/min Typical retention time, min methyl ethyl ketone Relative retention time (methyl ethyl ketone = 1.00): Propyl ether Octenes sec-Butyl ether Acetone Ethyl acetate Methyl ethyl ketone tert-Butanol Methanol Isopropano! Ethanol sec-Butanol n-Propanol " 40/60 12 (3.7) 0.25(6.4) 0.21 (5.3) 100 helium 60 6.9 0.19 0.54 0.78 0.61 0.81 1.00 1.00 1.10 1.20 1.30 2.12 2.35 Case 11 packed polyethylene glycol 4008, 28 Pink, diato maceous earth8 30/60 18(5.5) 0.25 (6.4) 0.21 (5.3) 80 helium 80 17.0 Casein packed polyethylene glycol 3008 20 Pink, diato- maceoys earth8 40/60 10 (3.0) 0.25 (6.4) 0.21 (5.3) 75 helium 35 11.0 Case IV packed poly&thylene glycol 200 20 White, diato maceous earth' 60/80 10 (3.0) 0.125 (3.2) 0.085 (2.2) 70 helium 60' 5,8 Case V packed polyethylene glycol 1500* 20 Pink, diato maceous earth8 60/80 20 (6.1) 0.25 (6.4) 0.21 (5.3) 100 helium 50 16.5 Case VI capillary polytrifluoro- propylsiloxane8 1.2 pm film none 32.8(10.0) 0.028 (0.72) 0.021 (0.53) 30 helium 3.7 8-8 0.14 0.21 0.45 0.54 1.00 1.12 1.32 2.28 0.64 0.82 1.00 1.27 1.36 1.73 2.73 3.27 0.34 0.47 0.67 0:78 1.00 1.71 1.71 2.03 2.21 3,50 3.97 ... 1.21 0.67 0.85 1.00 1.03 1.09 2.12 1.27 1.94 ft65 0.60 0.78 1.00 0.39 0.27 b.34 0.3f0.53 0.43 ` A Carbowax 540 (Carbowax, a registered trademark of Union Carbide Corp., 39 Old Ridgebury Road, Danbury, CT 06817-0001, has been found suitable for. this purpose). 8 Carbowax 400 (see Footnote A). c Carbowax 300 (see Footnote A). Carbowax 200 (see Footnote A). 8 RSL-400 (RSL, a registered trademark of Alltech Assoc., (2051 Waukegan Road, Deerfield, IL 60015, has been found suitable for this purpose), F Chromosorb T (Chromosorb', a registered trademark of Manriville Sales Corp, Filtration and Minerals, P.O. Box 5108, Denver, CO 80217 - 5108, has been found suitable for this purpose). 8 Chromosorb P,AW (see Footnote F). H Gas Chrom RA (see Footnote E). ' Chromosorb W-AW (see Footnote F)- tion detectors. The minimum purity of any carrier should be 99.95 mol %. 6.1.1 Warning--If hydrogen is used, take special safety precaution to ensure that the system is free of leaks and that the effluent is vented properly; 6.2 Column Materials: 6.2.1 Liquid Phase--The materials successfully used in cooperative work as liquid phases are listed in Table 1. 6.2.2 Solid Support--The support for use in the packed column is usually (PTFE)-fluorocarbon, crushed firebrick, or diatomaceous earth. Sieve size depends on the diameter of the column used and the liquid-phase loading, and should be such as to give optimum resolution and analysis time. Optimum size ranges cannot be predicted on purely theoret ical grounds. For some systems it has been found that a ratio of average particle diameter to column inside diameter of 1 to 25 will result in minimum retention time and minimum peak widths. Table 1 lists conditions used successfully in cooperative work. 6.2.3 Tubing Material--Copper, stainless steel, nickel copper alloy, aluminum, and various plastic materials have been found to be satisfactory for column tubing. The material must be nonreactive with the substrate, sample, and carrier gas, and of uniform internal diameter. 6.3 Standards for Calibration and Identification--, Standard samples for all components present are needed for identification by retention time; and for calibration for quantitative measurements. No t e 1--Mixtures bf components may be used, provided there is no uncertainty as to the identity or concentration of compounds involved. 7. Preparation of Apparatus 7.1 Column Preparation--The method used to prepare the column is not critical provided that the finished column produces the required separation (Note 2). Partitioning liquids, supports, and loading levels used successfully in cooperative work are listed in Table 1. No t e 2--A suitable method for column preparation is described in Test Method D 2593. 7.2 Chromatograph--Install the column in the chromato graph and establish the operating conditions required to give the desired separation. Relative component retention times, along with the typical retention time for methyl ethyl ketone are listed in Table 1. Allow sufficient time for the instrumenl to reach equilibrium as indicated by a stable recordei baseline. Control the detector temperature so that it i: constant to within 0.1C without thermostat cycling whicl causes an uneven baseline. Adjust the carrier-gas flow rate tc a constant value. 8. Calibration and Standardization 8.1 Identification--Select the conditions of column tem 380 DUP050296044 # D 2804 TABLE 2 Thermal Conductivity Detector*- ||thyl ethyl ketone Hit-butyl ether jpsopropyl ether hyi acetate p-Butanol If-Butanol getorte ppropanol fopanol gtianol Hthanbi" ' Thermal Mole Response 98 160 130 111 97 96 86 85 83 72 55 ' Weight Factor 0.74 0.81 0.79 . 0.79 0.76 0.77 0.68 0.71 0.72 0.64. 0.58 i data on the thermal conductivity response are based on data presented Issner, A. E. et al, Analytical Chemistry, Vol 31,1959, pp. 230-233, and fw. A., Journal of Gas Chromatography, Vol 5, No. 2, February 1967; pp jf(see Note 3 of this test method). for reference, hydrogen Same response data on all compounds except the i are presented m the above paper by W. A. Dietz. Jfture and carrier-gas. flow that will give the necessary gfponent resolution. Determine the retention time for component by injecting small amounts of the c6nt- Qd either separately or in mixtures. f` |2 Standardization--The area under the peak of the Imatogram is considered a quantitative measure of the punt ofthe corresponding compound. The relative area is |portional to the concentrations if the detector responds Uy to all of the sample components. Differences. in tor Response may be corrected by use of relative ionse factors obtained by injecting and measuring1 the Iponse to pure (99 weight % minimum) compounds or hwn blends! It is permissible to use the established ponse factors shown in Table 2 instead of standardization. S&3 In using literature values, area response front thermal- Inductivity detectors' is corrected by multiplying each pmponent area by the respective weight factor above. ;,No t e 3--It must be recognized that the u$e of published response ore serves qnly as a rough estimate, due. to, differences in equipment metry, condition, and types of detectors. It is preferable for each ilyst to determine-'actual response factors on his own instruthent No t e 4--When thermal-conductivity- detectors are used for the ilysis of high-purity methyl ethyl ketone, the difference between area ent is within the precision of the method. - . Procedure 9.1 Using a suitable method selected from 5.3 introduce Isufflcient representative liquid specimen into the; chromatof graph to ensure a minimum of 1,0 % recorder deflection for a r-0.1 % concentration of impurity at the most sensitive[ operating setting of the instrument. 9.2 Using the same conditions as for component identifi| cation and standardization, record the peaks of all com pounds at attenuation settings that provide maximum peak heights. 10. Calculation 10.1 Measure the area of all peaks (Note 5) and multiply by the appropriate attenuation factor to express the peak areas on a common basis. If a flame ionization detector was used, apply the appropriate detector-response factors to correct for the difference in response to, the components. (Calculate the weight percent composition by dividing the individual corrected component areas by the total corrected area. Make corrections to account for the water, acidity, and nonvolatile matter as determined by the ASTM procedures given in 3.1. ' ' No t e 5--Peak areas may be determined'by any method thit meets the precision limits given in Section 13. Methods found to be acceptable include planimetering, integration, and triangulation (multiplying the peak height by the width at the half-height). 10.2 Calculate weight percent as follows: Methyl ethyl ketone, weight % = {A(8) x (100 - C) whiere: " , \ A = corrected peak response, B;. =, sum of corrected peak responses, and C = sum of water, acidity, and nonvolatile impurities. 11. Report 11.1 Report the following information: percent ofmethyl ethyljcetone and* any impurities of interest to the nearest o.oi %. ; 12. Precision and Bias 12.1 Precision--The precision statements are based upon an interlaboratory study in which one operator in six different laboratories analyzed in duplicate on two days two specimens of methyl ethyl ketone from different manufac turers. The results were analyzed in accordance with Practice E 180, and the within-laboratory standard deviation was found to be 0.007 % absolute with 12 degrees of freedom and the between-laboratories standard deviation 0.033 % abso lute. with five degrees of freedom. Based* on these standard deviations the following criteria should be used for judging the acceptability at the 95 % confidence level, of results obtained on methyl ethyl ketone having a purity of 99 to 100%: 12.1.1 Repeatability--Two results each the mean pf two runs obtained by a single analyst on different days should be considered suspect if they differ by more than 0.02% absolute. . 12.1.2 Reproducibility--Two results each the mean of two runs obtained by analysts in differeht laboratories should be considered suspect if, they differ by more than 0.12% absolute. 12.2 Bias--Bias has not been determined for this test method. 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 (his standard are expressly advised that determination of the validity of arty such patent rights, arid the risk ofinfringement ofsuch rights, are'intirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapprovedor withdrawn. Your comments are Invited either for revision ofthis standardhr for additionalstandards avid 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'teel 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. 381 DUP050296045 Designation: D 2916 - 88 Standard Specification for Isophorone1 This standard is issued under the fixed designation D 2916; 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 specification covers isophorone2 (98 % grade) for use in paint, varnish, lacquer, and related products. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color ofClear liquids (PlatinumCobalt Scale)4 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used In Paint, Varnish, Lac quer, and Related Products3 D 2192 Test Method for Purity ofAldehydes and Ketones3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 25, 1988. Published Slay 1988. Originally published as D 2916 - 70. Last previous edition D 2916 - 84, 1 This compound is also known under the name 3,5,5-trimethyl-2-cyclohexene1-one. 3 Annual Book ofASTM Standards. Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.01 and 06.03. `Annual Book ofASTM Standards, Vol. 05.03. 6 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 1 Annual Book, ofASTM Standards, Vols 06.03 and 15.05. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. . 3. Properties 3.1 Isophorone shall conform to the following require- Apparent specific gravity; 20/20`C 25/25"C Color, Pt-Co scale, max Distillation Initial boiling point, min "C 95 % point, max "CPurity, weight % min Acidity as acetic add, weight %, max Water, weight %, max 0.921 to 0.923 0.918 to 0.920 100 210 218 98 0.02 0.1 4. Sampling 4.1 Sample the material in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25"C. See either the Specific Gravity section of Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 105C having a range from 198 to 252C and conforming to the require ments in Specification El. 5.1.4 Purity--Test Method D 2192. 5.1.5 Acidity--Test Method D 1613. 5.1.6 Water--Test Method D 1364. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging Shall conform to applicable carrier rules and regulations or when specified shall Conform to Fed. Spec. PPP-C-2020. The American Society for Testing and Materials takes 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 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 forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 Race St., Philadelphia, PA 19103. 382 DU P0502 96046 Designation: D 2917 - 91 Standard Specification for Methyl Isoamyi Ketone1,2 This standard is issued under the fixed designation i> 2917; the numberimmediately 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. This standard has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. Jope ! This specification covers methyl isoamyl ketone (98 % ) for use in paint, varnish, lacquer, and related prod- For specific hazard information and guidance, see the lier's Material Safety Data Sheet. eferenced Documents ASTM Standards: '268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material13 2 1078 Test Method for Distillation Range of Volatile Organic Liquids3 1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)4 1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer and Related Products3 >3893 Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyi Ketone by Gas Chromatography3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter5 E 1 Specification for ASTM Thermometers6 [ E 300 Practice for Sampling Industrial Chemicals7 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of8 1 This specification is under thejurisdiction ofASTM Committee D-1 on Paint I Related Coatings and Materials and is the direct responsibility of Subcomiittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 15,1991. Published December 1991. Originally published as D 2917 - 70. Last previous edition D 2917 - 87. 2IUPAC--approved name is 5-methyl-2-hexanone. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vois 06.01 and 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. 6 Annual Book ofASTM Standards, Vois 05.03 and 14.03. 1 Annual Book ofASTM Standards, Vois 06.03 and 15.05. 8 Available from Standardization Order Desk, Bidg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Properties 3.1 Methyl isoamyi ketone shall conform to the following requirements: Apparent specific gravity: 20/20C 25/25C Color, Pt-Co scale, max Distillation, *C Initial boiling point, min Dry point, max Water, wt %, max Acidity as acetic acid, wt %, max Purity, wt %, min 0.812 to 0.815 0.809 to 0.812 15 140 148 0.1 0.02 98 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25C. See Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 41C having a range from 98 to 152C and conforming to the requirements in Specification E 1. 5.1.4 Water--Test Method D 1364. 5.1.5 Acidity--Test Method D 1613. 5.1.6 Purity--Test Method D 3893. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon by the purchaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 ketone; methyl isoamyi ketone; solvents 383 DUP050296047 DUP050296048 Last ASTM Designation: D 2999 - 85 Standard Test Method for Monopentaerythritol in Commercial Pentaerythritot test method covers the determination by gas chromatography of monopentaerythritol in commercial grades of penta1. ! eriy under the jurisdiction of Committee D-1 on Paint and Related Coatings and Materials. test method was discontinued in 1989, and replaced by ASTM Test Methods D 2195, for Testing Pentaerythritol.1 I Book ofASTM Standards, Vol 06.03. 385 DUP050296049 Designation: D 3008 - 90 Standard Test Method for * i * h Resin Acids in Rosin by Gas-Liquid Chromatography1 This standard is issued under the fixed designation D 3008; the number immediately following the designation indicates the year of original adoption or, in the case ofrevisipn, the yea? of last revision. A number jmpareptbesesindicates.the year of last reapproval. A superscript epsilon (ej indicates an editorial change since the last revision of reapproval. ' . ' la , 1. Scope 1.1 This test method covers the determination of the resin adds in tall oil, gum, or wood rosin after conversion to their methyl esters. 1.2 The composition is calculated from the ratio of each peak area to the total area of all peaks obtained. Rosins generally contain nonvolatile or polymeric materials for which no peaks are obtained under the conditions used. On the other hand, volatile neutral materials elute in the general region of resin add methyl esters and can result in errors in the calculated composition. More reliable data is obtained by removal of neutral materials before gas chromatography.12 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. Specific hazards are given in Note 2. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water3 D 3257 Test Method for Aromatics in Mineral Spirits by Gas Chromatography4 E 260 Practice for Packed Column Gas Chromatography5 3. Summary of Test Method 3.1 A portion of the sample is prepared by either con verting it to the tetramethylammonium salts or esterifying it with diazomethane. A specimen of the prepared sample is injected into a 275C injection port to a 200C column of ethylene glycol succinate silicone copolymer (EGSS-X) or diethylene glycol succinate on silanized diatomaceous earth solid support. If added as the tetramethylammonium salt, the sample is pyrolyzed to the methyl ester. The pyrolyzed esters or the prepared esters are carried through the column with nitrogen or helium carrier gas and the chromatogram is obtained using a flame ionization detector. 3.2 The peak areas are obtained by any of the conven tional means and the percent of the respective resin in adds is calculated from the ratios of the areas of the individual peaks to the total area of all peaks. 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 1.34 on Naval Stores. Current edition approved May 25, 1990. Published July 1990. Originally published as D 3008 - 72. Last previous edition D 3008 - 82. 1 Zinkel, D. F., and Han, 3., Naval Stores Review, Vol 96(2), pp. 14-19(1986). 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 14.0). 4. Apparatus 4.1 Gas Chromatograph--Any gas-liquid chromatograph having a flame ionization detector that can be operated at ! the conditions given in Table 1. 4.2 Column--Six to 10 ft (1.8 to 3 m) of Vs-in. (3.2-mm) outside diameter, 0.085-in. (2.15-mm) inside diameter, 0.020-in. (0.52-mm) wall-thickness stainless steel tubing specifically tempered for easy handling and packed with the . material as described in 8.1. ) 4.3 Recorder--A recording potentiometer with a full-scale deflection of 0 to 1-mV full-scale response time of 1 s or less, 7 chart speeds of V2 to 1 in. (12 to 25 mm)/min, and sufficient < sensitivity and stability to meet the requirements of 4.1. 4.4 Specimen Introduction System--Any system capable of introducing a representative specimen into the column. - Microsyringes, 10-pL capacity, with fixed needle have been found satisfactory. 4.5 Integrating Equipment--In order of preferences based on accuracy, electronic, disk, planimeter, or rule. 5. Reagents and Materials 5.1 Purity ofReagents--Reagent grade chemicals shall be j used in all tests unless otherwise specified. Unless otherwise j indicated, it is intended that all reagents shall conform to the f 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 determi nation. 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 Toluene. 5.4 N-Methyl-N-Nitroso-p- Toluenesulfonamide.7 5.5 Diethyl Ether, Anhydrous. 5.6 2-Ethoxyethanol. 5.7 LiquidPhase--Diethylene glycol succinate (DEGS) or ethylene glycol succinate-silicon copolymer (EGSS-X, lowsilicone content). No t e I--EGSS-X is the preferred liquid phase because of its greater stability. 5.8 Methanol. 6 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on 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." 'Available from Aldrich Chemical Co., Inc., Milwaukee WI 53233 and Eastman Kodak, Rochester, NY 14650. 386 DUP050296050 TT EMPTY TRAP ETHf v_y v :t e--Connect four 25 by 200-mm test tubes in the hood as sho< FIG. 1 Apparatu ABLE 1 Typical Instrument Operating Conditions ( Method D 3257) i temperature. C ction port temperature, C ;tor temperature. C srgas: assure, psig ow rate, mL/mln _-tor gas (hydrogen) pressure, psig [Flow rate, mL/min r gas (air) pressure, psig Flow rate, mL/min 200 to 210 275 to 300 285 prepurified nitrog... 60 25 to 30 prepurified hydrogen 13 30 dried air 30 400 Resin Acid Methyl Ester Pimarate Sandaracoplmarate Communate . Levopimarate ' Palustrate Isopimarate Abietate Dehydroabietate Neoabietate Relative Retention'' DEQS EGSS-X 1.00 1.13 1.28 133 1.35 1.49 2.14 2.33 2.47 1.00 1.12 1.27 1.34 1.36 1.46 2.10 2.32 2.46 A See Zinkel and Han.2 5.9 Potassium Hydroxide Solutions, Aqueous--Dissolve i 300 g of potassium hydroxide (KOH) in 500 mL of water. 5.10 Solid Support--Acid-washed diatomaeeous earth,8 80 to 100 mesh, specially treated to minimum adsorption and tailing of polar compounds. 5.11 Tetramethylammonium Hydroxide Solution (24 %) in methanol. 5.12 Tetramethylammonium Hydroxide Solution (6 %) in methanol. Dilute 25 mL ofthe reagent described in 5.11 with 75 mL of methanol. 6. Reference Standards 6.1 Ahietic Acid,9 6.2 Dehydroabietic Acid.9 7. Preparation of Methyl Esters 7.1 Diterpene resin acids are more effectively chromatographed as the methyl esters. Either of the two * Chromosorb W-AW, manufactured by Manviile Sales Corp., Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108, has been found satisfactory for this purpose. Available from chromatography supply houses. 0 These and most other resin acids are available Grom Helix Biotech Ltd., 217-7080 River Rd,, Richmond. B. C,, Canada V6X 1X5. Between Laboratory Standard Deviation, Vc---------------- 1 ,'-5 o\ 7? Degrees o Freedom 15 29 83 Maximum Acceptable Differences 1.5 2.4 3.9 ng determined, and it solvent peak, resin acids more accun factors, as follows: Correction Factor (FIt. 1.00 1.07 1.04 00 injected inu,. tetramethylammom tu rn the injection port. 7.3 Esterification with Diazomethane: No t e 2--Diazomethane is explosive and an insidious poison, extreme care with the following esterification procedure, carrying out the reaction in a hood. 7.3.1 Weigh to 0.1 mg 50 to 60 mg of the sample into a 1-dram (4-mL) vial and dissolve in 1.0 mL of diethyl ether-methanol (9/1). 7.3.2 Connect four 25 by 200-mm test tubes as shown in Fig. 1. Use rubber stoppers in Test Tubes 1 and 4 and cork stoppers in Test Tubes 2 and 3. Connect the tubes with glass tubing as shown. Draw down the outlet end or the glass tube from Test Tube 4 to about a 1 to 2-mm diameter opening. 7.3.3 Leave Test Tubes 1 and 4 empty to serve as traps. Fill Test Tube 2 about one-half full with diethyl ether. 7.3.4 Add about 10 mL of the ICOH solution, 10 mL of 2-ethoxyethanol, and 20 mL of diethyl ester to Test Tube 3. 7.3.5 Place the vial with the specimen solution under the delivery tube from Test Tube 4 sq that the end of the tube dips beneath the surface of the liquid. Figure 2 shows an assembly of the esterification apparatus. 7.3.6 Add about 1 g of N-methyl-N-nitroso-p-toluenesuifonamide to Test Tube 3. Apply nitrogen gas to the inlet of Test Tube 1 at such a rate as to sweep the generated diazomethane through the solution of the sample at a moderate rate. 7.3.7 The esterification is complete when the yellow color of excess diazomethane is just apparent throughout the vial. 7.3.8 Evaporate the solution just to dryness under ni trogen on a steam bath in a hood. Dilute with toluene or methyl 7-butyl ether to approximately 1 to 2 mL, 8. Preparation of Apparatus 8.1 Prepare a 10 % mixture of DEGS or EGSS-X on the acid-washed, diatomaeeous earth and pack the column as discussed in Practice E 260. 8.2 Install the column in the chromatograph and establish 387 DUP050296051 DUP050296052 p Sbvei, % 1- !<3 ptoTO S>10 Checking Limits for Duplicates 0.7 22 3.9 Standard Deviation 0.2 0.7 1.4 0 3008 TABLE 2 Within Laboratory Degrees of Freedom 9 IS 35 Precision Maximum Acceptable Differences 0.7 2.2 3.9 Between Laboratory Standard Deviation . Degrees of Freedom 0.5 15 0.8 29 1.4 83 Maximum Acceptable Differences 1.5 2.4 3.9 Iperatiiig conditions given in Table 1. Allow sufficient ffor the instrument to reach equilibrium as indicated by Me recorder baseline. Control the detector temperature ant to within 1C without thermostat cycling which es an uneven baseline. Adjust the carrier gas flow rate to fetatit-value';- " ; bration ,, Jp Preparation of Test Blend--to i mg about 15 fof abietic add and 5 mg of dehydroabietic add into a (4-mL) vial Dissolve; in? 0.5 to 1 mL of solvent opriate for the methylation as described in 7.2 or 7.3. Inject a 1 to 3-pL portion of the test blend into the 3 If the resulting chromatogram shows good resolution abietic and dehydroabietic adds, it can be assumed the column is performing satisfactorily. Procedure , ).l Inject a; 1 to 3-p.L portion of the. tetramethylaonium salt or methyl ester solution prepared in accordr with 7.2 or 7.3 into the chromatographic column, ng the same conditions as. for. the test, blend, record the s of all components at alternating settings that .provide ximum peak heights. Figure 2 shows chromatograms for : American gum, wood, and tall oil rosin. 3.2 Measure the peak areas of all of the peaks (Note 3)., all the areas of the individual peaks exclusive of the fjjyeht peak to obtain the total peak area!. ' No t e 3--Peak areas are preferably measured with an electronic Integrator although other methods, such as disk integration, planimeter, r triangulation in decreasing order, may be used. II. Calculation ' ,1 1.1 Calculate the relative percent of each resin acid, R7 jlpresent, uncorrected for the amount of nonvolatile materials J present,' hs follows: , r *-(a -x . ioo)/r (i) where: A -- peak area for resin add being determined, and T = sum of areas of all peaks except solvent peak. 11.2 To quantify the individual resin adds more accu rately, apply the appropriate correction factors, as follows: in Acids MeihyJ Ester Correction Factor (FID); Pimarate Levopimarate Paiustrate Isopimarate Abietate Dehydroabietate Neoabietate .. 1.00 1.07 1.04 1.00 1.0S 1.01 1.04 12. Report ; 12.1 Report the percent of the individual resin acids to 0.1 weight %. Duplicate determinations that agree within the percent .absolute shown in Table 2 are acceptable for averaging (95 % confidence level). 13. Precision and Bias ' : 13.1 Precision--In an interlaboratory study of this jest method in which one operative in each of the laboratories analyzed on two days, the within laboratory and between- lafaoratory 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 the 95 % confidence level. 13.1.1 Repeatability--Two results, each the mean of du plicates, obtained by the same operator should be considered suspect if they differ by more than the percent absolute given in Table 2 for the appropriate level of resin acid content. 13.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by different laboratories should be considered suspect if they differ by more than the percent absolute given in Table 2 for the appropriate level of resin acid content. 13.2 Bias--Bias cannot be determined because there are no standard materials. 14. Keywords 14.1 gas chromatography; rosin adds analysis Th?American Society for Testing and Materials takes no position respecting the validity of any (talent 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 paienf tights, and the risk of infringement of such rights,'are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee end must be reviewed every five years and ifnot revised, either reapproved 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 feel that your comments have not received a iair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 389 DUP050296053 Designation: D 3009 - 72 (Reapproved 1981)f1 Standard Test Method for Composition of Turpentine by Gas Chromatography1 This standard is issued under the fixed designation D 3009; 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 file year of last reapproval. A superscript epsilon {<) indicates an editorial change since the last revision or reapproval. " No t e--Section 2 was added editorially and subsequent sections renumbered in April 1985. 1. Scope 1.1 This test method covers the determination of the composition, specifically a-pinene, /3-pinene, in wood, gum, and sulfate turpentine by gas chromatography. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 3. Summary of Method 3.1 A weighed mixture of the sample and of the internal standard is prepared, an aliquot injected into a 75C chro matographic column, and the temperature programmed to 240C to obtain the chromatogram. The peak areas for the components to be determined and also for the internal standard are measured. The percent of the components present are calculated from the product of the; peak area of the component, weight of internal standard, and the calibra tion factor divided by the product of the weight of sample and peak area of the internal standard. 4. Apparatus 4.1 Linear Programmed Temperature Gas Chromato graph--Any instrument with programming features with thermal conductivity or flame ionization detector and adapt able to the following operating conditions: Detector cell temperature, 'C Injection port temperature, X' Carrier gas flow at exit, cm3/min Programmed temperature details: Approximate column beating rate, *C/min Starting column temperature, "C 250 200 .50 3 to 4 75 4.2 Recorder---A 1-mV recorder with a full-scale response of 1 s and a chart speed of 30 in./h. 4.3 Column--A 12-ft length of lk to Vt-in. (3.18 to 6.35-mm) outside diameter, 0.085 to 0.210-in. (2.15 to 5.33-mm) inside diameter, 0.020-in. (0.51-mm) wall, stain less steel tubing specially tempered for easy handling and packed with 20 weight % of Carbowax 20M on 60 to 80 mesh Chromosorb W (nonacid washed). Condition at 240C for about 4 h before use. 4.4 Microsyringe, having a fixed needle, 10-p.L capacity. 1 This method is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.34 on Naval Stores. Current edition approved Jan. 4, 1972. Published March 1972. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents 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- ences to water shall be understood to mean reagent water conforming to Specification D 1193. 5.3 Calibration Liquid--a-pinene--Purify technical grade a-pinene by fractionation at a 10/1 reflux ratio taking a center cut4 Store at sub-zero temperature in tightly capped bottles under nitrogen gas. >. 5.4 Column Packing--Prepare a 20 weight % mixture of Carbowax 20M on 60/80 mesh Chromosorb W in accord ance with gas chromatographic practice. 5.5 Liquid Phase--Carbowax 20M. 5.6 Reference Standard--H-decane, at least 99 %. 5.7 Solid Support--Chromosorb W (non-acid washed), 60/80 mesh. 6. Calibration of Chromatograph 6.1 Weigh, to the nearest 0.001 g, 1 g of reference standard a-pinene and 1 g of n-decane into a small capped vial. Thoroughly mix and inject 1 to 5 jxL of the mixture onto the 75C column. The sample may be' diluted for use in flame ionization systems. 6.2 With the column at 75C and the chromatograph at equilibrium conditions (4.1), inject a 1 to 5-|xL portion ofthe calibration mixture. Allow the lower boiling fractions to elute and then program the temperature at about 3 to 4C/min until a column temperature of 240C is reached. Then turn off the programmer and allow the column temperature to return to 75C. 6.3 Measure the areas of the n-decane and the a-pinene peaks with a planimeter, by triangulation, or by any accepted method of integration. Correct the areas for any attenuation. f | | I | | [! | |! | | 4 | | j } | f jj 'II > 1 5 ; j 1 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 Yoric, NY, and the "United States Pharmacopeia." 4 Material with 99 % purity available from Chemical Samples, 4692 Kenny Road, Columbus, OH 43221. 390 DUP050296054 D 3009 Calculate the relative response factor for a-pinene as |ws: F=(A,x Ws x F)I(W, x As) \ peak area for internal standard, = weight of standard a-pinene, g, = purity of a-pinene, %/100, = weight of internal standard, g, and peak area for a-pinene. L5 Use this same response factor for a-pinene and (jinene. rocednre 1.1 Weigh, to the nearest 0.001 g, 1 g of sample and 0.5 g lk-decane into a small capped vial. Mix thoroughly with column, at 75C, inject a 1 to 5-pL portion of the fxture. Allow the lower boiling fractions to elute and then Igram the temperature at about 3 to 4C/min until a llumn temperature of 240C is reached. Attenuate as _ to keep the peaks on the chart. When the 240C aperature is reached, then turn off the programmer and low the column temperature to return to 75C. 7.2 Measure the areas of the peaks of the components of terest. Correct the areas for any attenuation. Calculation ,8.1 Calculate the? weight percents of a-pinene, and 0Bnene, as follows: I C% = (A, xWjXFx 100)/(^ X Aj) where: C = component being determined, a-pinene, /3-pinene, weight %, As -- peak area for a-pinene, or 0-pinene, Wj -- weight of internal standard, g, F = relative response factor, see 6.4, , Ws = weight of turpentine sample, g, and Aj - peak area for internal standard. 9. Report 9.1 Report the percentage of a-pinene, and /J-pinene to the nearest 0.1 weight %. Duplicate determinations that agree within a certain percent absolute as shown in Table 1 are acceptable for averaging (95 % confidence level). 10. Precision 10.1 The following criteria should be used forjudging the acceptability of results: 10.1.1 Repeatability (Single Analyst)--The standard devi ation of results (each the average of duplicates), obtained by the same analyst on different days has been estimated to approximate a specific percent absolute as shown in Table 1. Two such values should be considered suspect if they differ by more than the stated percent absolute. 10.1.2 Reproducibility (Multilaboratory)--The standard deviation of, results (each the average of duplicates) obtained by analysts in different laboratories, has been estimated to appropriate a specific percent absolute as determined in Table 1. Two sUch values should be considered suspect (95 % confidence level) if they differ by more than the stated percent absolute. F Component |t a-Pinene i /3-Pinene Checking Limits ter Duplicates 1.6 0.8 TABLE 1 Standard Deviation 0.S6 0.26 Precisian Limits Repeatability Degrees of Freedom 30 30 95% Range 1.6 0.8 Standard Deviation 1.9 1.1 Reproducibility Degrees of Freedom 12 12 95% Range 5.9 3.3 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and IInotrevised, eitherreapproved or withdrawn. Your comments are invitedeitherforrevision 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 tai1 hearing you should make your views known to the ASTM Committee on Standards, 191$ Race St., Philadelphia, PA 19103. 391 DUP050296055 Designation: D 3125 - 83 (Reapproved 1987) Standard Test Method for Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid1 This standard is issued under the fixed designation D 3125; the number immediately following the designation indicates the year of original adoption or, in the case of revision, die year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. I. Scope 1.1 This test method covers the determination of. monomethyl ether of hydroquinone2 3(MEHQ) in colorless monomeric acrylate esters and acrylic acid. The.test method is applicable to the determination of MEHQ in the concen tration range from 0 to 1200 parts per million. 1.2 This, standard mayinvolve hazardous materials, oper ations, and equipment itkis standard does not purport,,to 4.2 MEHQ effectiveness may decline with age and this decline in effectiveness may not be indicated by this test method. 5. Interferences 5.1 Hydroquinone (HQ), thioffiphenylamiite, diphenyl;* f pfienylene-diamihe and p-hydroxydiphenylamine interfere if present. '' _? ihe%sponsibility.ofwhoever, uses this standard to consult and establish appropriate sqfetyand health, practices and deterr mine the applicability of regulatory limitations'prior to use. Specific precautionary statements are given in Section 81, ' 2. Referenced Documents ' 2.1 ASTM Standards: D1193 Specification for Reagent Water?- , E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals4 3. Summary of Method 3.1 As shown in the equation, MEHQ reacts with nitrous ' acid (sodium nitrite in acidic media) to form the nitroso derivative which equilibrates between two structures. 6. Apparatus : - ':ij| 6.1 Spectrophotometer,, with borosilicate-glass cells for determining absorbance at 420 nm.f . '6.2 Volumetric Flasks', 50 and 100-mL capacity. 6.3 Measuring Pipets, 5 and 10-mL capacity. i i 7. Reagents ** ^ 7.1 Purity OfReagents--Reagbnt grade chemicals shall be used. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of. the Com mittee 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 f 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- ij: ences to water shall be understood to mean reagent grade jp water conforming to Type IV of Specification D 1193. | 7.3 Acetic Acid, glacial. 7.4 Mpnomeihyl Ether of Hydroquinone (MEHQ) (4- : methoxyphenol). .. 7.5 Sodium Nitrite Solution (2 %)--Dissolve 2 g of so dium nitrite (NaN02) in water and dilute to 100 mL. 3.2 The yellow color of the nitroso compound is mea sured spectrophotometrically at a wavelength of 420 nm. 4. Significance and Use 4.1 Acrylic acid and its esters are normally inhibited with MEHQ only. This procedure presents a rapid and accurate method of determining the MEHQ content of fresh acrylic acid and acrylate esters in the absence, of other inhibitors/ 8. Precautions .. ' 8.1 Samples of acrylic monomers should be stored in amber bottles or protected from light by other means to aid in preventing polymerization. Keep samples away from heat sources and chemicals which can cause free radical polymer ization. Acrylic monomers can polymerize violently, evolving considerable heat. Sample container size should be kept to a minimum. 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 1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 25, 1983. Published July 1983. Originally published asD3125-72. Last previous edition D 3125 - 78. 2 IUPAC-approved name is 4-methoxyphenol. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 15.05. 3 The Beckman models DU or B spectrophotometers with 20 mm cells and the Bausch and Lomb Spectronic 20 with 25 mm cells have been found satisfactory for this purpose. Equivalent apparatus may be used. 6 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, D. C. 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, N. Y., and the "United States Pharmacopeia." 392 DUP050296056 ibration Weigh 0.10 g of MEHQ to the nearest 0.1 mg into a L volumetric flask containing approximately 50 mL of acetic add. Mix well until solution is complete then to the mark with gladal acetic acid. Prepare a series of ards by pipetting 1, 2, 4, 6, and 10-mL portions of the Q solution into respective 50-mL volumetric flasks, each flask to the mark with glacial acetic add and mix A 10-mL aliquot of each of these standards contains 400, 800, 1200, and 2000 jig of MEHQ, respectively. Determine the absorbance of each of these standards pbtting 10-mL aliquots into 50-mL volumetric flasks 'ning 20-mL of gladal acetic acid. To each flask add of 2 % NaN02 solution and dilute to the mark with acetic acid. Mix well and allow to stand for 10 min. cells appropriate to the instrument, determine the rbance at 420 nm using acetic acid as the blank. 3 Construct a calibration curve on rectangular coordigraph paper by plotting the absorbances of the standards ;20 nm against the micrograms of MEHQ. . Procedure 0.1 Perform analyses in duplicate and carry a blank ough the analysis using 49 mL of glacial acetic -add in he of the spedmen solution. '10.2 Weigh the appropriate amount ofspecimen (Table 1) to a 50-mL volumetric flask containing 20-mL of gladal etic acid. 10,3 Add 1 mL of 2 % NaN02 solution to the specimen d dilute to the mark with glacial acetie acid. Mix well and 'ow to stand for 10 min. : 10.4 Using the procedure followed for the calibration, etermine the absorbance ofthe solution at 420 nm with the lank solution in the reference position. From the calibration qurve, determine the micrograms of MEHQ corresponding 'o the absorbance obtained. * 'it .. .' ;- 11. Calculation 11.1 Calculate the concentration of MEHQ in ppm as ; follows: TABLE 1 Amount of Specimen ' Expected MEHQ Content, ppm Amount of Specimen, g 0 to 25 25 to 100 100 to 250 250 to 550 550 to 1000 25* 10* 5s 2 Is * Weigh to the nearest 10 mg. 6 Weigh to the nearest 1 mg. TABLE 2 Reporting and Averaging of Duplicate Runs MEHQ Concentration, ppm Report ppm Duplicate Runs That Agree Within the Following Amounts Are Suitable for Averaging (95 % Confidence Level) 15 0.1 50 0.5 200 1 500 1 ppm 0.54 . 1.8 5.5 9.9 MEHQ, ppm = M/S where: M =' micrograms of MEHQ from calibration curve and S = grams of spedmen used in the test. 12. Report 12.i Report the concentration of MEHQ as indicated in Table 2. 13, Precision7 13.1 The precision statements are based upon an interlab oratory study in which one operator in each of twelve laboratories analyzed in duplicate on two different days each of the following samples: Acrylic Monomer Mean MEHQ Concentration, ppm Ethyl acrylate Ethyl acrylate . . 2-Ethylhexyl acrylate 2-Ethylhexyl acrylate Acrylic acid Acrylic acid 16:9' 48.2, 14.7 47.3 212 ' 499 The results were analyzed statistically in accordance with Recommended Practice E 180 and the within-laboratories coeffident of variation was found to be 1.4 % relative with 6 r degrees of freedom and the between-laboratOries cofeffident of variation was found to be 4.6 % relative with 9 degrees of freedom. Based on these coeffidehts of variation, the following criteria should be used for judging the accept ability of results at the 95 % confidence level: 13.1. T Repeatability--Two results, each the mean of du plicates, obtained by the same operator on different days should be considered suspect if they differ by more than 4.0 % relative. 13.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 15 % relative. 'Supporting data are available from ASTM Headquarters. Request RRD-01-1016. 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 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 arid must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of 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. 393 DUP050296057 i Designation:D 3128-89 Standard Specification for 2`Methoxyethanol1'2 This standard is issued under the fixed designation D 3128; 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. 1. Scope 1.1 This specification covers 2-methoxyethanol. 1.2. This standard may involve hazardous materials, oper ations, and equipment. Tfiis standard does hot 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. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet for materials listed in this specification. . 2. Referenced Documents 2.1 ASTM Standards: D 268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint, and Related Coatings and Materials3 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 D1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)3 D .1296 Test Method for Odor of Volatile Solvents and Diluents3 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 D 4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers4 E 300 Practice for Sampling Industrial Chemicals5 6 , 2.2 U.S. Federal Standard: PPP-C-2020 Specification for Packaging of Chemicals, Liquid, Dry, and Paste4 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 mittee DO!.35 on Solvents, Plasticizer, and Chemical Intermediates. Current edition approved March 31, 1989. Published May I9S9. Originally published as D 3128 - 72, Last previous edition D 3128 - 84. 2 Also known as ethylene glycol monomethyl ether (EGME). 3 Annual Book QfASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 05.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 6 Available from the Naval Publications and Forms Center, 5801 Tabor Avc., Philadelphia, PA 19120. 3. Properties 3.1 2-Methoxyethanol shall conform to the following requirements: Apparent specific gravity: . 20/20'C 2S/25"C Color, Pl-Co scale, max Distillation range: Below 123.0`C Above 126.0C Water, weight, % max Acidity (free acid as acetic acid), weight, % max Odor 0.963 to 0.967 0.960 to 0.964 15 none none 0.2 0.01, equivalent to 0.093 mg of KOH per gram of material nonresidua! 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Hazards 5.1 2-Methoxyethanol is hazardous. Avoid skin and eye contact mid inhalation of its vapors to prevent possible adverse health effects. s ; '. ' 6. Test Methods 6.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 61.1 Apparent Specific Gravity--Determine the apparent specific gravity by any method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25C. See Specific Gravity section of Methods D 268 or Test Method D 4052. 6.1.2 Color--Test Method D 1209. 6.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 41C having a range from 98 to 152C and conforming to the requirements in Specification E 1. 6.1.4 Water--Test Method D 1364, 6.1.5 Acidity--Test Method D 1613. 6.1.6 Odor--Test Method D 1296. 7. Packaging and Package Marking 7.1 Package size is to be agreed upon between the purchaser and supplier. 7.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 394 DUP050296058 D 3128 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 fnfringement of such rights, are entirety their own responsibility. This standardis subjectto revision at any time by the responsible technical committeeandmust be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or toradditional standards and should be addressed to ASTM Headquarters. Your comments 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. 395 DUP050296059 Designation: D 3130 - 90 Standard Specification for n-Propyl Acetate (96 % Grade)1 This standard is issued under the fixed designation D 3130; 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 rcapproval. 1. Scope 1.1 This specification covers n-propyl acetate (96% grade). 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for material listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D 1078 Test Method for Distillation Range of Volatile Organic Liquids2 D 1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)3 D 1296 Test Method for Odor of Volatile Solvents and Diluents2 D 1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D1364 Test Method for Water in Volatile Solvents {Fischer Reagent Titration Method)2 D1476 Test Method for Heptane Miscibility of Lacquer Solvents2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D 3545 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 1 This specification is under thejurisdiction of ASTM Committee D-! on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO1.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as D 3130 - 72. Last previous edition D 3130 - 86. 2 Annual Bock ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 05.03. 5 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 6 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Properties 3.1 n-Propyl acetate shall conform to the following re quirements: Apparent specific gravity: 20/20C 25/25C Color Pt-Co units, max Distillation, C at 760 mmHg Initial boiling point, min Dry paint, max Nonvolatile matter, mg/100 ml, max Odor Water, wt %, max8 Acidity (free acid as acetic acid), wt %, max Purity, wt %, min 0.885 to 0.890 0.880 to 0.885 15 platinum-cobalt scale 96 103 5 nonresidual 0.1 0.01 96.0 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1. Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25C. See Methods D 268 or D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 40C having a range from 72 to 126C and conforming to the requirements in Specification E 1. 5.1.4 Nonvolatile Matter--Method D 1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Methods D 1364 and D 1476. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Purity--Test Method D 3545. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 7. Keywords 7.1 ester; propyl acetate; solvent 8 This quantitative water limit ensures that the material is miscible without turbidity with 19 volumes of 99 % heptane at 20"C. 396 DUP050296060 D 3130 The American 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 resptm/bility. > This standard is subject to revision at any time by the responsible technical committee efid must be reviewed every five years andIf not revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearingt you should make your views known to the ASTM Committee oh Standards, 1916 Race St., Philadelphia, PA 19103. ;j , 397 DU P0502 96061 Designation: D 3131 - 88 Standard Specification for Isopropyl Acetate (99 % Grade)1 This standard is issued under the fixed designation D 3131; 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 isopropyl acetate (99 % grade). 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material2 D 1078 Test Method for Distillation Range of Volatile Organic Liquids2 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)3 D1296 Test Method for Odor of Volatile Solvents and Diluents2 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1476 Test Method for Heptane Miscibility of Lacquer Solvents2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D 3545 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 E 1 Specification for ASTM Thermometers5 E 300 Practice for Sampling Industrial Chemicals6 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of7 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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved March 25, 1988. Published May 1988. Originally published in D 3131 -72. Last previous edition D 3131 - 83. 2 Annual Book ofASTM Standard;;, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.03. * Annual Book ofASTM Standards, Vol 05.03. s Annual Book ofASTM Standards, Vols 05.03 and 14.03. 6 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 7 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 3. Properties 3.1 Isopropyl acetate (99 % grade) shall conform to the following requirements: Apparent specific gravity: 20/20`C 25/25`C Color, Pt-Co scale, max Distillation range, 760 mmHg Below 85"C Above 90C Nonvolatile matter, mg/100 mL, max Odor Water, weight %, max Acidity as acetic acid, weight %, max Purity, weight %, min 0.870 to 0.874 0.865 to 0.869 none none 5 nonresidual 0.2. This quantitative water limit ensures that 1 volume of the ma- terial is miscible without turbidity with 19 volumes of 99 % heptane at 20*1 0.01, equivalent to 0.093 mg of KOH per gram of sample 99.0 M Cil 'f ;|| `ill Iff ijil IS jtt '-J i 1 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 1 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the following ASTM test methods: 5.1.1 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the temperature of both specimen and water being 20 or 25C. See either the Specific Gravity section of Methods D 268 or Test Method D 4052. 5.1.2 Color--Test Method D 1209. 5.1.3 Distillation Range--Test Method D 1078, using an ASTM Solvents Distillation Thermometer 40C having a range from 72 to 126C and conforming to the requirements in Specification El. 5.1.4 Nonvolatile Matter--Test Method D 1353. 5.1.5 Odor--Test Method D 1296. 5.1.6 Water--Test Methods D 1364 and D 1476. 5.1.7 Acidity--Test Method D 1613. 5.1.8 Purity--Test Method D 3545. | ; H j j 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations or when specified shall conform to Fed. Spec. PPP-C-2020. 398 DUP050296062 D 3131 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 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 Invitedeitherforrevision ofthis standard or foradditional standards and should 6s 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. 399 DUP050296063 Designation: D 3169 - 89 Standard Specification for Refined Sunflower Oil1 This standard is issued under the fixed designation D 3169; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year dflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the iast revision br reapproval. 1. Scope 1.1 This specification covers once-refined sunflower oil, technical grade, suitable for use in protective coatings. 2. Referenced Documents 2.1 ASTM Standards: D 555 Guide for Testing Drying Oils2 D1466 Test Method for Sampling Liquid Oils and Fatty Adds Commonly Used In Paints, Varnishes, and Re lated Materials2 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)3 D1639 Test Method for Add Value of Organic Coating Materials4 D1952 Test Method for Quantitative Determination of Break in Drying Oils2 D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids2 D1960 Test Method for Loss on Heating of Drying Oils2 D1962 Test Method for Saponification Value of Drying Oils, Fatty Adds, and Polymerized Fatty Acids2 D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C 2 D1965 Test Method for Unsaponifiable Matter in Drying Oils, Fatty Adds, and Polymerized Fatty Acids2 D1967 Test Method for Color After Heating of Drying Oils2 TABLE 1 Properties of Once-Refined Sunflower Oil Property Specific gravity 25/25C Add value Saponification value Unsaponifiable matter, % Iodine value (Wqs) Loss on heating at 105C, % Color Color after heating Quantitative break, % Clarity Requirement 0.918 to 0.921 0.3 max 188 to 194 1.5 max 134 to 144 0.2 max 7 max 2 max 0.02 max clear and transparent at 25C ASTM Test Method D1963 D1639 D1962 D 1965 1959 D1960 D1544 D 1967 D1952 2090 D 2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids5 3. Properties 3.1 Sunflower oil shall be obtained solely from sunflower seed and shall be suitably processed to conform to the requirements given in Table 1. 4. Sampling 4.1 Sample in accordance with Test Method D 1466. 5. Test Methods 5.1 The properties enumerated in this specification shall be determined in accordance with the ASTM test methods listed in Table 1. The significance of the test methods is discussed in Guide D 555. 6. Keywords 6.1 drying oils; sunflower oil 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 DO'l .32 on Drying Oils. Current edition approved Oct. 27, 3989. Published December 1989. Originally published as D 3169 - 73(1988). Last previous edition D3169-73(1988). 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. * Annual Book ofASTM Standards, Vol 06.01. 5Annual Book ofASTM Standards, Vols 06.02 and 06.03. TheAmerican Society for Testing and Materials takss 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 reepproved 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 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. 400 DUP050296064 Designation: D 3257 - 88 & Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography1 This standard is issued under the fixed designation D 3257; 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 standard has been approvedfor 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. iScope .1 These test methods cover the determination of ethylzene and total eight-carbon (Q) and heavier aromatics in concentration range from 0.1 to 30 % in mineral spirits ing a distillation range from 149 to 210C (300 to 410'F) (determined by Test Method D 86. The procedures permit identification and calculation of concentrations of aro~tic components to 0.1 volume %. 1.2 It is recognized by analytical chemists that a single iumn gas chromatography analysis of an unknown sample risky. In such cases, multiple and different analytical hniques must be used for absolutely positive identifica~n, for example, several different gas chromatography "lumns, gas chromatography/mass spectrometer, or gas liromatography/infrared, etc. In these test methods the aterial is known and is clearly defined. 1.3 Oxygenated compounds, if present, may interfere and use erroneous results. Such oxygenated compounds are not prmally present in mineral spirits.. 1.4 Two test methods are covered as follows: 1'4.1 Test Method A, measurement of ethylbenzene coneht, C8 plus higher aromatics (except ethyl benzene), and otal aromatics by means of a single gas chromatographic analysis. 1.4.2 Test Method B, measurement of ethylbenzene con tent by means of a rapid gas chromatographic analysis. 1.5 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to me. 1.6 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. E 260 Practice for Packed Column Gas Chromatog raphy4 3. Summary of Test Methods 3.1 The material, with an internal standard, is introduced into a gas chromatographic column containing a strongly polar liquid phase. The polar phase has very little affinity for saturated and olefinic hydrocarbons while exhibiting a pro nounced retention of aromatics. This selectivity, which is illustrated in Fig. 1, results in the elution of all saturated and olefinic hydrocarbons in the products described above prior to the elution of toluene. Either a thermal conductivity or flame ionization detector may be used. Calibration is ob tained in Test Method A from a synthetic blend of the most important aromatic compounds. Internal standards are used in both. Test' Method A and Test Method B. A typical chromatogram is shown in Fig. 2. No t e 1--Refer to Practice E 260 for additional information on gas chromatography techniques. 4. Significance and Use 4.1 These test methods were developed to measure the types and amounts of aromatics in mineral spirits to determine compliance with air pollution regulations that restrict the aromatic content of solvents. They have been demonstrated to be workable and to produce accurate results. However, due to the sensitivity of the tests to operating variables, some laboratories having limited experi ence with gas chromatographic analyses of hydrocarbons may experience difficulty in performing the tests. TEST METHOD A--ETHYLBENZENE AND TOTAL AROMATICS CONTENTS BY MEANS OF A SINGLE GAS CHROMATOGRAPHIC ANALYSIS 2. Referenced Documents 2,1 ASTM Standards: D 86 Method for Distillation of Petroleum Products2 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals3 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 DOi.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Feb. 1, 1988. Published April 1988. Originally published as D 3257 - 73. Last previous edition D 3257 ~ 83. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03.. 3 Annual Book ofASTM Standards, Vol 15.05. 5. Apparatus 5.1 Chromatograph, any gas-liquid chromatographic in strument that has the following performance and character istics: 5.1.1 Sensitivity--The overall sensitivity must be suffi cient to detect 0.1 volume % of any aromatic compound of interest with a peak height of at least 10 % of full-scale chart deflection without loss of resolution as defined in 5.1.2, or 10 times the noise level. 5.1.2 Column--Any column and conditions may be used provided the system meets all the following criteria when the * Annual Book ofASTM Standards, Vol 14.01. 401 DUP0502 96065 D 3257 test, blend is injected into the chromatograph and the chromatogram recorded in accordance with 7.2, is analyzed as follows: 5.1.2.1 Construct tangents to the curve to intersect the baseline for the n-tridecane (C13) and toluene peaks. Mea sure the distance between the two peaks and the width of each peak as the distance along the baseline under the peak between the points of intersection (see Fig. 1). 5.1.2.2 Calculate the peak resolution,. : > R = 2Ad/(Y,+`Y2) where: . Ad == distance between Cl3 and toluene peaks, F, = width of nCu peak along the baseline, and Y2 = width of the toluene peak along the baseline. The . peak resolution, R, must be not less than 0.9, otherwise the resolution of ethylbenzene may'be lost No t e 2--The. selectivity of the column (separation of the nonaromatics from aromatics) can be increased by increasing the concentra tion of liquid phase or by increasing the temperature of the Chromato graphic column. The resolution of the aromatic compounds can be improved by increasing the length of the column or by decreasing the oven temperature or inlet pressure of the carrier gas. 5.1.2.3 fethylbenzene must be separated from paraxylene and isopropylbenzene or from paraxylene plus isopropyl benzene with the depth of the valley after ethylbenzene not FIG. 2 Typical Chromatogram of Mineral Spirits (Reduced to 40 % of original and traced) 402 DUP050296066  D 3257 | than 50 % of the ethylbenzene peak height. .1.2.4 The system must measure durene with a peak lit of at least 10 % of full scale chart deflection or at least ies the noise level. froTE 3--A combination of column materials and conditions that been found to be particularly suitable for this test method is listed in He 2. f.2 Strip Chart Recorder--A recording potentiometer ji a fiallscale deflection of 10 mV or less should be used. If %ual integration,' such as triangulation, paper cut-out or imeter, is employed the chart speed should be at least l .5 (60 in./h) in order to minimize errors in peak area lasurement. This is not necessary where a ball-and-disk or i electronic integrator is employed. j5.3 Micro Syringe--A 10-pJL micro syringe for specimen gtroduction. 5.4 Tubing--Copper, aluminum, or stainless steel. Reagents and Materials 16.1Aromatic Hydrocarbons--Toluene, ethylbenzene, pa- jgxylene, isopropylbenzene, 1,2,4-trimethylbenzene (pseudo- iimene), and 1,2,4,5-tetramethylbenzene (durene) 99.5 fol % minimum. 6.2 Carrier Gas (Note 3). 6.3 internal Standard--Cyclohexanone, 99.5 mol % min ium (see 1.6). 6.4 Liquid Phasefor Column (Note 3). 6.5 Normal Paraffin--n-Tridecane, 99.5 mol % mini- lum. 6.6 Solvent for Liquid Phase--Dichloromethane has been found satisfactory (see 1.6). 6.7 Solid Support (Note 3)--If an open tubular column is used, a solid support is not necessary. 6.8 Solventfor Test Blend--n-H.exa.rn, n-heptane, or iso- jfectane 99 mol % minimum. j|7. Calibration 7.1 Preparation of Test Blend--Prepare a test blend to fevaluate the sensitivity and resolution of the equipment and ftest procedure! To do this, pipet the exact volume of each I, hydrocarbon indicated in Table 1 into a 100-mL volumetric 1 flask. Fill to the 100-mL mark with one ofthe solvents listed 1 in 6.8 and mix by inverting several times. See 1.6. No t e 4--Durene is a solid. In preparing the-test blend, the quantity ; ofdurene required should be weighed, using as its density 0.8875 g/mL. 7.2 Select the instrument conditions and specimen size so as to give the necessary sensitivity and resolution. Inject the test blend into the column at these conditions. Change the attenuation, if necessary, so that the internal standard and TABLE 1 Normal tridecane Toluene Ethylbenzene Paraxylene Isopropylbenzene Durene (Note 4) Cyclohexanone Pseudocumene Paraffin from 8.8 Composition of Test Blend ' Volume, mL 1 2 1 2 2 0.1 2 2 87.9 TABLE 2 Typical Column and Conditions Length, m Diameter, mm: Inside Outside Liquid phase Weight % liquid Solid support: Mesh Treatment Inlet, *>C Detector. C Column. C Carrier gas Inlet pressure, KPa Row rate, mL/min Detector Recorder, mV Specimen. |iL Sample split 3.7 (12 ft) 3.2 (Vs in.) CEF* 25 Chromosorb-Ps 80-100 none 250 . 250 110 helium 550 (80 psi) 35 flame ionization 1 2 (30 to 1) A N,N-b!s (2-cyanoethyl) formamide. s A registered trademark of Manville Sales Corp., Filtration and Minerals. P.O. Box 6108, Denver, CO 80217-5108. aromatic peaks are measured with a chart deflection of not less than 25 % nor more than 95 % of full scale for attenuated peaks. Check the column performance against the requirements given in 5.1.2. 7.3 Response Factor--Assume that the aromatics in the sample have the same relative response as pseudocumene in the test blend. Using the results from the test blend, calculate the response factor as follows: r = {As/Vs)/(AJVJ where: r = relative response factor for aromatics, As = area of the internal standard peak in arbitrary units corrected for attenuation, Vs = volume %-of the internal standard in the blend, Aa. = area of the pseudocumene peak in arbitrary units corrected for attenuation, and Va = volume % of pseudocumene in the blend. 8. Procedure 8.1 Using the exact instrument conditions as were used in the Calibration, inject the test material. Inspect the chro matogram to determine that there is complete resolution between the saturated and the aromatic peaks. 8.2 Pipet exactly 1.0 mL of cyclohexanone internal standard into a 10-mL volumetric flask. Fill to the mark with the sample and mix by inverting several times. 8.3 With the exact instrumental conditions used in the calibration, inject the same volume of sample containing the internal standard. Change the attenuation, if necessary, so as to measure the area of the internal standard and aromatic peaks with not less than 25 % nor more than 95 % chart deflection on attenuated peaks. 9. Calculation 9.1 Measure the areas of all aromatic and internal standard peaks. Use of an electronic integrator is recom mended to obtain the best accuracy and precision. No t e 5--Because the Cg and heavier aromatic compounds may not be completely resolved, peak height multiplied by one half width or retention rime must not be used as a means of measuring the area. 403 DUP050296067 9.2 If a different attenuation is used for part of the chromatogram, correct to a constant attenuation basis by multiplying the area of the aromatic peaks by the ratio: Sa/Ss where: Ss - attenuation sensitivity used for the internal standard peak and Sa - attenuation sensitivity used for the aromatic peak. 9.3 Calculate the concentrations of ethylbenzene and C8 and heavier aromatics as follows: va = (Aa x r x 10)/(AS x 0.9) where: Va = volume % of the aromatic compound(s), Aa = area of the aromatic peak(s) corrected to a constant attenuation, r = relative response factor for the aromatic compounds, 10 = volume % of internal standard, As = area of the internal standard peak; and 0.9 -- factor to correct for the dilution by the internal standard. 9.4 Total Aromatics--Add the amounts of the aromatic compounds found to obtain the volume percent of total aromatics in the sample. 10. Report 10.1 Report the following information: concentrations of ethylbenzene, total aromatics, and Cg plus higher aromatics (except ethylbenzene) in volume percent to the nearest 0.1 %. 11. Precision and Bias5 11.1 The precision estimates are based on an interlaboratory study on four samples, containing approximately 6.5, 8.5, 11.8, and 16.5 % total aromatics and 0.0, 1.0, 4.0, and 0.3 % ethylbenzene. One analyst in each of six laboratories performed duplicate determinations on different days, for a total of 48 determinations of total aromatics content and 48 determinations of ethylbenzene content. The within-laboratory coefficient of variation was found to be 1.7 % relative with 23 degrees of freedom, and the between-laboratories coefficient of variation was 4.4 % relative with 5 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 obtained by the same operator on different days should be considered suspect if they differ by more than 5 % relative. 11.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 16 % relative. 11.2 Bias--Bias has not been determined for this test method. TEST METHOD B--ETHYLBENZENE CONTENT BY MEANS OF A RAPID GAS CHROMATOGRAPHIC ANALYSIS 12. Apparatus 12.1 Chromatograph--Any gas-liquid chromatographic instrument complying with the sensitivity described in 54 and equipped with a thermal conductivity detector may ; used. 12.2 Column--Any column and conditions may be usedprovided the system meets all the requirements of 14.3 and Section 17. The following column was used to establish thfel precision found in Section 17: I8-ft (5.5-m) of (6.3-mm) copper, aluminum, or stainless steel tubing packed f with 35 % by weight of N,N-bis (2-cyanoethyl) formamide 1. on 60 to 80 mesh untreated, calcined, pink diatomaceous silica.6 No t e 6--The column may be prepared in two 9-ft (2.7-m) sects and joined together, if preferred. 12.3 Strip Chart Recorder--See 5.2. ' 12.4 Micro Syringe--See 5.3. 13. Reagents and Materials 13.1 Aromatic Hydrocarbons--Benzene, toluene and eth- I ylbenzene of 99.5 mol % minimum purity (see 1.6). 13.2 Carrier Gas--Helium. 13.3 Solvent for Liquid Phase--Dichloromethane has ' been found to be satisfactory (see 1.6). ` 14. Procedure 14.1 Set ihe gas chromatograph instrument conditions as : follows: ! Detector cell temperature, "C Detector cell current, mA Injection port temperature, C Helium flow at exit, mL/min Column temperature, C 300 150 300 ' no 100 14.2 > Pipet exactly 1.0 mL of toluene internal standard into a 10-mL volumetric flask. Fill to the mark with the! mineral spirits sample, and mix thoroughly by inverting several times. See 1.6. No t e 7--Both ethyl benzene and toluene contents may be deter mined, if present, by using benzene as the internal standard. 14.3 Inject 3 pJL of sample containing the internal standard, and chromatograph under the prescribed operating' conditions. Change attenuation, if necessary, so as to mea sure the area of the internal standard with not less than 25 % nor more than 95 % chart deflection. Ethylbenzene will emerge in about 11 min. 14.4 Purge the column of high-boiling aromatics by raising the temperature to 130C. After the high-boiling components emerge, reset the column temperature to 100C. 15. Calculation 15.1 Measure the areas of the ethylbenzene and toluene internal standard peaks. See 8.1. 15.2 If different attenuations are used for the ethylben zene and internal standard peaks, correct to a constant attenuation basis, as in 9.2. 15.3 Calculate the concentration of ethylbenzene as fol lows: Ve = (Ae x 10 x 1.036)/^ 5 Supporting data ate available from ASTM Headquarters. Request RR.-D01 1015. 6 Chromosorb P produced by Manville Sales Corp. has been found satisfactor; for this purpose. 404 DUP050296068 # D 3257 , volume % of ethylbenzene, area of the ethylbenzene peak corrected to a con stant attenuation, volume % of internal standard added, relative response factor for ethylbenzene, and area of the internal standard peak. !te results may be averaged, at the 95 % confidence they differ by no more than 0.2 %, absolute. ' 8--The suggested response factor for ethylbenzene should be for the particular instrument used, in accordance with the ! described in 7.3, and with the internal standard (toluene or A used for the analysis. The response factor actually determined e used in the ethylbenzene content calculation. ' eport i5 Report the following information: concentration of enzene in volume percent to the nearest 0.1 %.. `ision and Bias The precision estimates are based on an interlaboraly in which one operator in eight different laborato,,-lyzed two samples of mineral spirits in duplicate on different days. The samples contained 1.0 and 8.0 % ethylbenzene, and were prepared by adding ethylbenzene to dearomatized mineral spirits. The results were analyzed in accordance with Practice E 180. The within-laboratory and between-laboratories standard deviations were found at dif ferent-levels of ethylbenzene content to be as follows: Within Laboratories Between Laboratories Actual ethylbenzene content, % Degrees of freedom Standard deviation 1.0 16 0.05 8.0 16 0.10 1.0 7 0.21 8.0 7 0.25 Based upon these standard deviations, the following criteria should be used for judging the acceptability of results at a 95 % confidence level. 17.2 Repeatability--Two results, each the mean of dupli cates, obtained by the same operator on different days should be considered suspect if they differ by more than 0.2 % absolute at the 1 % ethylbenzene level, or by more than 0.3 % absolute at the 8 % ethylbenzene level. 17.3 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.7 % absolute at the 1 % ethylbenzene, level, or by more than 0.9 % absolute at the 8 % ethylbenzene level. 17.4 Bias--Bias has not been determined for this test method. . The American Society for Testing and Materials takes no position respecting the velldity ofany patent rights asserted in connection with any item.mentloned 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; either reapproved orwithdrawn. 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, whlcfryou 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. 405 DUP050296069 Designation: D 3278 - 89 Standard Test Methods for Flash Point of Liquids by Setafiash Closed-Cup Apparatus1 '|| i ;J This standard is issued under the fixed designation D 3278; 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 This standard has been approvedfor use by agencies of the Department of Defense. Consul! 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 determining whether a material does or does not flash at a specified temperature or for determining the lowest finite temperature at which a material does flash when using a Setafiash Tester. The test methods are applicable to paints, enamels, lacquers, varnishes, and related products having a flash point between 32 and 230F (0 and 110C) and viscosity lower than 150 St at 77F (25C). No t e 1--Tests at higher or lower temperatures are possible. No t e 2--More viscous materials may be tested in accordance with Annex A4. No t e 3--Organic peroxides may be tested in accordance with Annex A5, which describes the applicable safety precautions. No t e 4--The U.S. Department of Labor (OSHA, Hazard Commu nications), the U.S. Department ofTransportation (RSPA), and the U.S. Environmental Protection Agency (EPA) have specified Test Methods D 3278 as one of several acceptable methods for the determination of flash point of liquids in their regulations. No t e 5--These test methods are similar to International Standards ISO 3679 and ISO 3680. 1.2 This standard should be used to measure and describe the properties of materials, products, or assemblies in re sponse to heat andflame under controlled laboratory condi tions and should not be used to describe or appraise thefire hazard orfire risk ofmaterials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a fire risk assessment which takes into account all factors pertinent to an assessment of the fire hazard ofa particular end use. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safetyproblems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Notes 7 and 12. 2. Referenced Documents 2.1 ASTM Standards: D 56 Test Method for Flash Point by Tag Closed Tester2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Belated Coatings and Materials and are the direct responsibility of Subcommittee D01.22 on Health and Safety. Current edition approved Dec. 29, 1989. Published February 1990. Originally published as D 3278 - 73. Last previous edition D 3278 - 82". 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. D 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D1015 Test Method for Freezing Points of High-Purity Hydrocarbons2 D1078 Test Method for Distillation Range of Volatile Organic Liquids3 2.2 ISO Standards:4 ISO 3679 Paints, varnishes, petroleum and related prod ucts--Determination of flash point--Rapid equilibrium method ISO 3680 Paints, varnishes, petroleum and related prod ucts^--Flash/no flash test--Rapid equilibrium method l 3. Terminology | 3.1 Definitions: 3.1.1 flash point--the lowest temperature, corrected to a f pressure of 760 mm Hg (101.3 kPa, 1013 mbar), at which j application of an ignition source causes the vapor of the j specimen to ignite under specified conditions of test. J 4. Summary of Test Methods' | 4.1 By means of a syringe, 2 mL of the sample is introduced through a leakproof entry port into the tightly j closed Setafiash Tester or directly into the cup that has been brought to the required test temperature. As a flash/no flash test, the expected flash point temperature may be a specification or other operating requirement. After1 min, a test | flame is applied inside the cup and note is taken whether or ^ not the test specimen flashes. A fresh specimen must be used if a repeat test is necessary. 4.2 For a finite flash point measurement, the temperature is sequentially increased through the anticipated range, the test flame being applied at 9F (54C) intervals until a flash is observed. A true determination is then made using a fresh specimen, starting the test at the temperature of the last interval before the flash point of the material and making tests at increasing 1F (0.5C) intervals. 5. Significance and Use 5.1 Flash point is one of the properties used to define the flammability of a liquid. It is used to classify liquids according to their flammability by governmental regulatory agencies. It may also be used to determine the presence of impurities or contaminants in a given liquid, such as the presence of residual solvents in solvent-refined drying oils. 3 Annual Book ofASTM Standards, Voi 06.03. 4 Available from American National Standards Institute, 13th Floor, 11 W. 42nd St, New York, NY 10036. 406 DUP050296070 # D 3278 fetajlash Tester,s shown in Fig. A 1,1 and described in |a i. ' Thermometers,6 7low, medium, high temperature Test to determine that the scale error does not 3.?5F (0.25C). The use of a magnifying lens assists in jfctemperature observations. jlass Syringe, 2 0.1-mL capacity at 77F (25C), to ! a' means of taking a uniform specimen. Check the by discharging water into a weighing bottle and tig. Adjust plunger ifnecessary. A disposable syringe of Precision may be used. %Hutninum Cooling Block7 (describing in Annex A2), s snugly within the test cup used for rapid cooling of aple cup. !|Barometer. Agents and Materials hfXylene,8 reference standard. | n-Butanol,9 1re0ference standard. $ Cooling Mixtures of ice and water or solid COz (dry fed acetone. ^Liquified Petroleum Gas. Heat Transfer Paste.'0 ampling j\The specimen size for each test is 2 mL. Obtain at fa 25-mL sample from the bulk source and store in a jjfr full, tightly closed, clean glass container or in other aer suitable for the type of liquid being sampled. 6: Caution--Erroneously high flash points may be obtained if lutions are not taken to avoid loss of volatile material. Do not open |e containers unnecessarily and do not transfer the specimen to the hiess the temperature ofthe specimen is at least 20F (10C) below Xpected flash point. Discard samples in leaky containers. |o t e 7: Precaution--Do not store samples in plastic bottles (poly gene, polypropylene, etc.), as volatile material may diffuse through reparation of Apparatus |.l Prior to initial use or after removal of the thermomr, insert the thermometer into its pocket (see Fig. Al.l) ph a good heat transfer paste. t2 To help in making the necessary settings during a test, ifore the initial use determine the relationship between the iperature control dial and thermometer readings at inter- not over 9F (5C) throughout the scale range of the Beater. s9.3 Place the tester in a subdued light and in a position Ip 5 Gosed-cup flash point testers and their accessories meeting the requirements Ifthe unit shown in Fig. A1.1 are available from ERDCO Engineering Corp., 721 Shuster Ave., Evanston, 1L 60202 or Stanhope-Seta Ltd., Park Close Englefield jireen, Engham, Surrey, TW20 OXD, England. | 6 Thermometers may be obtained from the suppliers of the Setaflash Tester. 7 Cooling blocks may be obtained from ERDCO Engineering Corp. " p-Xylene is available as "Flash Point Creek Fluid" from Special Products )iv., Chemical Dept., Phillips Petroleum Co., Boiger, TX 25303. 9 n-Butanol may be obtained from chemical supply companies. 10 Heat transfer paste is available from the suppliers ofthe Setaflash Tester. No. 11340 Silicone is available from Dow Corning Corp., 2030 Willard H. Dow Center, fMidland, MI 48674. G641 Heat Transfer Compound is available from General leclric Co., Products Div., 12 Corporate Woods Blvd., Albany, NY 12211. not exposed to disturbing drafts. Provide a black-coated shield, if necessary. 9.4 Read the manufacturer's operating and maintenance instructions on the care and servicing of the tester. Observe the specific suggestions regarding the operation ofthe various controls. 9.5 Check the accuracy of the tester by duplicate determi nation of the flash point of the p-xylene reference standard (Annex A3). The mean of the results should be 81 1.5F (27.2 0.8C). An additional reference standard, w-butanol (Annex A3), may be used to check the accuracy at approxi mately the temperature specified by. U.S. regulatory agencies in defining flammable liquids. The mean of duplicates should be 98 1.5F (36.7 0.8C). If not, remove the thermometer and observe whether sufficient heat transfer paste surrounds the thermometer to provide good heat transfer from the cup to the thermometer. TEST METHOD A--FLASH/NO FLASH 10. Procedure--Ambient to 230F (110C) 10.1 Inspect the inside of the test cup, lid, and shutter mechanism for cleanliness and freedom from contamina tion. Use an absorbent tissue to wipe clean, if necessary. Lock the cover lid tightly in place. 10.2 Switch the heater on, if not already at stand-by. To rapidly approach the specification flash temperature of the material under test, turn the heater dial fully clockwise (Note 8) causing the heater signal (red) light to glow. When the thermometer indicates a temperature of about 5F (3C) below the specification or target flash-point temperature, reduce the heat input to the test cup by slowly turning the heater control dial counter clockwise until the signal light goes but (Note 9). No t e 8--When a desired temperature is dialed on the controller, the elapsed time to reach this temperature may be greater than if the controller is turned "full on," but less attention is required. No t e 9--The test cup temperature is stable when the signal light slowly cycles on and off. 10.3 Determine the barometric pressure to determine the corrected specification temperature at that barometric pres sure (see 15.1). 10.4 After the test-cup temperature has stabilized at the specification or target flash point, charge the syringe with the sample being tested and insert the tip of the syringe into the filling orifice (Fig. A 1.2), taking care not to lose any material. Discharge the specimen into the test cup by completely depressing the syringe plunger, then remove the syringe. If the material has a viscosity greater than 45 SUS at 100F (38C) or equivalent of 9.5 cSt at 77T (25C ), raise the lid and discharge the contents of the syringe directly into the cup. Immediately close the lid tightly. 10.5 Set the 1-min timing device. In the meantime, open the gas control valve and light the pilot and test flames. Adjust the test flame size with the pinch valve to match the size of the (4-mm) diameter flame gage. 10.6 After 1 min has elapsed, observe the temperature. If at the specification temperature (accounting for the differ ences of the barometer reading from 760 mm), apply the test flame by slowly and uniformly opening the slide fully and closing completely over a period of approximately 2xh s 407 DUP050296071 D 3278 (Note 10), watching for a flash (Note 11) while the flame is inserted. No t e 10--When inserted, the nozzle of the ignition device should intersect the plane of the underside of the cover (see A1,1). No t e 11--The material is considered to have flashed only if a comparatively large blue flame appears and propagates itself over the surface of the liquid. Occasionally, particularly near the actual flash point temperature, application of the test flame may give rise to a halo; this effect should be ignored. 10.7 Turn offthe test and pilot flame. Clean the apparatus in preparation for the next test. 11. Procedure--32F (0C) to Ambient 11.1 If the specification or 'target flash point is at or below ambient temperature, cool the sample to 10 to 20F (5 to 10"C) below that point by some convenient means. 11.2 Cool the tester to approximately the temperature of the sample by inserting the cooling block (Pig. A2.1) filled with a cooling mixture (Notes 12 and 13) into the sample well. Dry the cup with a paper tissue to remove any collected moisture prior to adding the specimen using, a precooled syringe. No t e 12: Precaution--Be careful in handling the cooling mixture and cooling block; wear gloves and goggles. Mixtures such as dry ice and acetone can produce severe frost bite. No t e 13: Caution--Be careful when inserting the cooling block into the tester cup to prevent damage to the cup. i 1.3 Introduce the specimen as in 10.4. Allow the temper ature to rise under ambient conditions or increase the temperature of the cup by rotating the heater controller clockwise slowly until the specification .temperature adjusted for barometric pressure is reached. Determine whether the material flashes as in 10.5 and 10.6. 11.4 Turn off the test and pilot flames. Clean the appa ratus. TEST METHOD B--FINITE FLASH POINT 12. Procedure--Ambient to 230F (110C) 12.1 Preliminary or Trial Test: 12.1.1 Follow steps 10.1 to 10.5, omitting the barometric reading and using an estimated finite flash point instead of specification flash-point temperature. 12.1.2 After 1 min has elapsed, observe the temperature. Apply the test flame by slowly and uniformly opening the slide fully and closing completely over a period of 2'/2 s (Note 10), watching for a flash (Note 11) while the flame is inserted. 12.2 If a flash is observed, proceed as in 12.3. If no flash is observed, proceed as in 12.4. 12.3 Using a temperature 9F (5C) lower than the tem perature observed in 12.1.2, repeat 12.1 (Note 4). If a flash is still observed, repeat at 9F lower intervals until no flash is observed. No t e 14--Never make a repeat test on the same specimen. Always take a fresh portion for each test. 12.3.1 After establishing the approximate flash point, repeat 12.1 with a new specimen, but stabilizing the test temperature at which no flash occurred previously. Observe if a flash occurs at this temperature. If not, increase the temperature by making a small adjustment to the tempera ture controller so that an increase of 1F (O^C) occurs ; wH within 1 min. Test for a flash at each 1F interval, recording lw the temperature at which the flash actually occurs. Record the barometric pressure. Clean the tester. 4fl 12.3.1.1 Repeat 12.3.1 with a new specimen. Calculate the corrected mean temperature in accordance with 15.2.- 'fl Turn off pilot and test flames and clean the tester. | 12.4 Using a test temperature 9F (5Q higher than the fij temperature observed in 12.2, repeat 12.1 (Note 14). If no II flash is observed, repeat at 9*F higher intervals until a flash is fljl observed. .flHj 12.4.1 After establishing the approximate flash point Sj (12.4) with new specimens, make two determinations of the fjj flash point in accordance with 12.3.1 and calculate the corrected mean temperature in accordance with 15.2. fl 13. Procedure--32F (0C) to Ambient Temperature fj 13.1 Preliminary or Trial Test: 1 13.1.1 Cool the sample to 5 to 10 -F (3 to 5C) below the :v expected flash point. :] 13.1.2 Cool the tester to approximately the temperature of J the sample by inserting the cooling block filled with a cooling ' medium into the sample well. (Precaution--See Notes 12 j; and 13.) 13.1.3 Introduce the specimen using a precooled syringe [jj as in 10.4. Set the 1-min timing device. After 1 min observe :;j the temperature, then apply the test flame by slowly and J uniformly opening the slide fully and closing completely f over a period of 2'/2 s, watching for a flash (Note 11) while. I the flame is inserted. Record the temperature. 13.2 Ifa flash is observed, proceed as in 13.3. If no flash is 1 observed, proceed as in 13.4. 1 13.3 Take a new specimen and recool the sample cup to : 9F (5'C) below the previous temperature (13.1.3). After 1 1 min, check for a flash as in 13.1.3. If the material flashes, I repeat at 9F lower intervals until no flash is observed. J 13.3.1 After establishing the approximate flash point, j repeat 13.1.1 and 13.1.3 with a new specimen but stabilizing the test temperature at which no flash occurred previously. Observe if a flash occurs at this temperature. If not, increase JI J the temperature by making a small adjustment to the fj temperature controller so that an increase of 1F (0.5C) ^ occurs within 1 min. Test for a flash at each 1F interval, recording the temperature at which the flash actually occurs. Record the barometric pressure. 13.3.1.1 Repeat 13.3.1 with a new specimen. Calculate the corrected mean in accordance with 15.2. Turn off pilot and test flames and clean the tester. 13.4 Using a test temperature 9"F (5C) higher than the temperature observed in 13.1.3, repeat 13.1.3 (Note 14). If no flash is observed, repeat at 9F higher intervals until a flash is observed. 13.4.1 After establishing the approximate flash point (13.4) , make the determinations of the flash point in accordance with 13.3 and calculate the corrected mean in accordance with 15.2. 14. Clean-up of Apparatus and Preparation for Next Test 14.1 Unlock the lid assembly ofthe tester and raise to the hinge stop. Soak up liquid with an absorbent paper tissue and wipe dry. Clean the underside of the lid and filling 408 DUP050296072 # D 3278 A pipe cleaner may be of assistance in cleaning the || If the material is a viscous liquid or contains dis- solids, after soaking up most of the specimen add a lamount of a solvent suitable for the sample to the cup.' jtsoak up the solvent and wipe clean the interior surfaces S eup with an absorbent tissue paper. 15--If necessary to remove. residual high boiling solvent moisten tissue with acetone and wipe dry. g; is---If any further cleaning is necessary, remove" the lid and I assembly. Disconnect the silicone rubber hose and slide the lid ^y to the right to remove. If warm, handle carefully. I After the cup has been cleaned, its temperature may |idly increased to some stand-by value by turning the store control dial to an appropriate point 17--It is convenient to hold the test cup at some stand-by _ ature (depending on planned usage) to conserve time in bringing ||i within the test temperature range. The cup temperature may be ' r lowered by inserting the aluminum cooling block filled with an ^riate cooling mixture into the cup. & The syringe is easily cleaned by filling it several times lacetone or other compatible solvent* discharging the Mt each time, and allowing the syringe to air dry with j|unger removed. Replace the plunger, and pump several ['to displace any solvent vapor with air. $ Correction for Barometric Pressure Ip Determine the corrected specification flash point to |fed in Test Method A by the following equations: F =5 -- 0.06 (760 -- P) C = T -0.03 (760 -P) F=S-0.42 (101.3 -B) C = r-0.23(101.3-) = flash point to be observed to obtain the specification flash point at standard pressure, F ("C), jjj! = specification flash point, F (C), and || = ambient barometric pressure, mm Hg (kPa). t e 18--The barometric pressure used in this calculation must be Knbient pressure for the laboratory at the time oftest. Many aneroid feeters, such as those used at weather stations and airports, are Ibrrected to give sea-level readings. These must not be used. Jj5.2 When the barometric pressure in Test Method B |rs from 760 mm Hg, correct the flash point temperature, 1 l|y means-of the following equations: A = F + 0.06 (760 -- P) = C+0.03 (760 -5) = F+ 0.42 (101.3 -- B) = 0 + 0.23(101.3-5) here: = observed flash point, F (*C), and j?) = ambient barometric pressure, mm Hg (kPa). Report J16.1 When using the flash/no flash method, report ' ether or not the sample flashed at the required flash point and that Test Method A was used. 16.2 If an actual flash point was determined, report the mean of duplicate determinations to the nearest 1 F (0.5*0, provided the difference between the values does not exceed 2F (1C) and that Test Method B was used. 17. Precision11 and Bias 17.1 Oil the basis of an interlaboratory study of Test Method B in which one operator in each of five laboratories made two determinations on two different days on four solvents, three resins and two paints of different flash points, the within-laboratory and between-laboratory standard devi ations were found to be: Standard Deviation Materials WithinLaboratoiy BetweenLaboratory Solvents (viscosity below 45 SUS at I00F), T Resins and Paints (viscosity above 45 SUS at 100F), "F 0.98 1.89 1.55 2.41 Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 17.2 Liquids at or Below 45 SUS at 100F or Equivalent Viscosity: 17.2.1 Repeatability--Two results, each the mean of two determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 3F (1.7C). 17.2.2 Reproducibility--Two results, each the mean of two measurements, obtained by different laboratories, should be considered suspect if they differ by more than 6F (3.3"C). 17.3 Viscous Liquid Above 45 SUS at 100"F or Liquids With Dispersed Solids: 17.3.1 Repeatability--Two results, each the mean of two determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 6F (3.3"C). 17.3.2 Reproducibility--Two results, each the mean of two measurements, obtained by different laboratories should be considered suspect if they differ by more than 9T (5C). 17.4 A study to determine the precision for materials with a viscosity greater than 150 St has not been made. 17.5 The precision for liquid peroxides has not been determined, but the precision of liquid peroxides should be similar to that of other liquids. 17.6 Bias--No estimate ofthe bias of flash-point tests can be determined as no absolute values are available. In addition, the results are equipment and method dependent. 18. keywords 18.1 flash point; Setaflash Closed-Cup; organic peroxides; flash/no flash; p-xylene; n-butanol _ 11 Supporting data are available from ASTM Headquarters. Request RR:D0l1000. These data are also reported in tbs Journal ofPaint Technology, Vol 45, No. 581, p. 44. 409 DUP050296073 D3278 ANNEXES (Mandatory Information) Al. APPARATUS SPECIFICATIONS A 1.1 A typical apparatus is shown in Fig. A 1.1. Electrical heaters are fastened to tire cup in a way as to provide for efficient transfer of heat. The (ester includes a variable, heater control device with' a scaled dial and a visible signal to indicate, when energy, is or is not being applied. Energy may be supplied from a 100 to 250 V 50/60 Hz (for stationary use) or by a 12-V d-c battery service (for field use). An adjustable test flame and a pilot flame to maintain the test flame are provided. These flames may be fueled by piped gas service (fixed ideation) or by a self-contained tank of liquefied petroleum gas (7.4) (for portability). A test flame measuring 32 in. (4 mm) in diameter may be checked against a gage ring on the surface of the .tester. Never recharge the gas tank with the pilot or test flames lighted, nor in the vicinity of other naked flames. A 1-min audible signal, is a desirable accessory. The cover is fitted with an opening, slide device capable of inserting the ignition flame into the well when the slide is open. When inserted the nozzle of.the ignition device shall intersect the plane of the underside of the cover. -38.10--*rj -31.75- to s g.8 CM o ! CO .in - ARMSTRONG ARMAFLEX No. 22 -PIPE INSULATION , SIZE 6IS (1 3/8" 1.0. , 1/2" THICKNESS) F5/ 12.7Q -49.21- NOTC- -All dimensions.Are In millimetres. FIG. A1.1 Setaflash Unit 410 DUP050296074 <) D 3278 A2. COOLING BLOCK febe cooling block with dimensions as shown in Fig. A2.1 is made ofaluminum and covered with pipe insulation. A- HINGE B-LID C-PILOT JET 0,-t TEST JET E-FILLER ORIFICE . . F - GAS CONTROL SCREW G- SLIDE GUIDE H- SLIDE KNOB J- SLIDE K- LOOK CLOSURE L- SEALING 0- RING M- THERMOMETER N- SAMPLE BLOCK. ... P;.- THERMOMETER. POCKET 411 DUP0502 96075 43. SPECIFICATIONS FOR p-XYLENE AND ^BUTANOL REFERENCE STANDARDS A3.1 p-Xylene A3.1.1 Specific Gravity, 60/60`F (15.56/15.56`Q Range--0.860 minimum, 0.866 maximum. A3.1.2 Boiling Range--2"C maximum from start to dry point when tested in accordance with Test Method D 850 or Test Method D 1078. The range shall include the boiling point of pure p-xylene, which is 138.35'C. A3.1.3 Freezing Point--11.23C minimum (95 % molal purity) as determined in accordance with Test Method D 1015. A3.2 rt-Butanol A3.2.1 Specific Gravity, 20/4C Range--0.809 minimum, 0.810 maximum. A3.2.2 Boiling Range--ISC maximum from start to dry time determined in accordance with Test Method D 1078. The range shall include the boiling point of pure rc-butanol, which is 117.7'G A3.2.3 Melting Point Range--90C minimum, -89.5'C maximum. A3.2.4 Refractive Index n 20/D Range--1.3985 minimum, 1.3993 maximum. A3.2.5 Purity by Gas Chromatography--'99.5 % minimum. flf| ill Bit Hi: IIP & BKmb. Sc HI l.t jjjhurit ^Baphj fiEgerta' A4. TESTING HIGH VISCOSITY LIQUIDS A4.1 High-viscosity materials may be added to the cup by the Mowing procedure: A4.1.1 Procedure--Back load a 5 or 10-mL syringe with the sample to be tested and extrude 4 mL into the cup. Spread the specimen as evenly as possible over the bottom of the cup. A4.1.2 If the sample cannot be loaded into a syringe and extruded, use other means of adding the specimen to the cup provided a presentative 4-mL specimen can be put into the cup. A spoon of appropriate size is convenient. Push the materia] from the spoon into the cup. A4.1.3 Ifthe test specimen does not seal offthe bottom of the filling orifice, seal the orifice from the top by suitable means. A4.2 Using Test,Method A (Section 10 or 11), determine whether or not the material flashes or, using Test Method B (Section 12 or 13), determine the flash point ofthe specimen. Mgytl'oi Wmhe fflB1TM, m^ap, IBP Hp. I BK , BHf z A5, TESTING ORGANIC PEROXIDES AS, 1 Organic peroxides may be tested by Test Methods A or B with minor modifications that take into account the hazard potential of these compounds. AS. 1.1 The tester should be located behind a transparent safety shield, and fire resistant gloves should be worn. A5.1.2 The procedure in 10.1 is followed with the excep tion that the cover lid is not locked in place. Rather, a spring-wire test-tube holder is clamped to the hold-down lock on the lid to provide an extension arm about 5 in. (12.7 cm) long. A weight ofapproximately 100 g is hung from the end of the test tube holder. This arrangement adequately seals the test while allowing venting with a rapidly decomposing peroxide. A5.1.3' Follow the procedures described in Test Methods A or B (Sections 10 through 14). However, when applying the test flame, grasp the handle by means of a second test tube holder, pliers, or tongs. |tl Wm MB 1H jfl| H Wm BH mBf The American Society for Testing end Materials takes no position respectingdie 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 ol Infringement <rf such rights, are entirely theirown responsibility. This standard is suf>/ect to revision at any time by the responsible technical committee and meat be reviewed every the years and Vnotrevised, either reapproved nr withdrawn. Tour comments are invited either for revision at 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 Pace St.. PtutesSetphia', PA 19103. 412 DUP050296076 Designation: D 3329 - 89 Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography*1'2 This standard is issued under the fixed designation D 3329; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision, A number io parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. This method has been approved far use by agencies of the Department of Defense. Consult the DoD Index of Specifications and ope This test method covers the determination of the of methyl isobutyl ketone (M1BK) by gas chromatogand in addition provides a means for measuring impurities such as methyl isobutyl carbinol which are 'est. Impurities such as water and acidity are measured |ther appropriate ASTM procedures and the results are to normalize the chromatographic value. This standard may involve hazardous materials, oper and equipment. This standard does not purport to |ess all ofthe safety problems associated with its use. It is esponsibility of the user of this standard to establish ipriate safety and health practices and determine the ability ofregulatory limitations prior to,use. ferenced Documents ' ASTM Standards: |1364 'Test Method for Water in Volatile Solvents FiScher Reagent Titration Method)3 1,613'Test Method for Acidity in Volatile Solvents and hemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 |2593 Test Method for Butadiene Purity and HydroI carbon Impurities by Gas Chromatography4 1180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem|itals5 J260 Practice for Packed Column Gas Chromatography6 ary of Test Method 1 A representative specimen is introduced onto a gas" l partition column. Methyl isobutyl ketone is separated S- impurities such as acetone, 2-propanol, pentanone, iityl oxide, methylisobutyl carbinol, and several uniden"iCompounds as the components are transported through column by an inert carrier gas. The separated compo3 are measured in the effluent by a detector and recorded chromatogram. The chromatogram is interpreted by llying component attenuation and detector response fac his method is under the jurisdiction ofASTM Committee D-L on Paint and i Coatings and Materials and is the direct responsibility of Subcommittee [{.35 on Solvents, Plasticizers, and Chemical Intermediates, intent edition approved March 31, 1989. Published May 1989. Originally fished as D 3329 - 74. Last previous edition D 3329 - 84. j|UPAC approved name is 4-melhyl-2-pentanone. |Annual Book ofASTM Standards, Voi 06.03. | Annua/ Book ofASTM Standards, Vol 05.02. |Annual Book ofASTM Standards, Vol 15.05. ^Annual Book ofASTM Standards, Vol 14.01. tors to the peak areas, and the relative concentrations are determined by relating the individual peak responses to the total peak response. Water and acidity are measured in accordance with Test Methods D 1364 and D 1613 and the results are used to normalize the values obtained by gas chromatography. 4. Significance and Use 4.1 This test method provides a measurement of com monly found impurities in commercially available methyl isobutyl ketone. The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be used for specification accept ance. 5. Apparatus 5.1 Chromatograph--Any gas liquid chromatographic in strument having either a thermal conductivity or flame ionization detector provided the system has sufficient sensi tivity and stability to obtain for 0.01 % of impurity a recorder deflection of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The specimen size used in judging the sensitivity must be such that the column is not overloaded, which would result in peak broadening, loss of resolution, shifting retention times and formation of leading peaks. 5.2 Column--Any column capable of resolving methyl isobutyl ketone from the impurities that may be present. Possible impurities are hydrocarbons, acetone, 2-propanol, 2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide isomer, and methyl isobutyl carbinol. Columns that meet this requirement are described in Table 1. Other columns, including capillary columns, may be used, provided the user establishes that a column gives the required separation and the peak shapes are satisfactory for measurement so that the precision requirements of Section 12 are met. 5.3 Specimen Introduction System--Any system capable of introducing a representative specimen onto the column. Microlitre syringes have been used successfully. 5.4 Recorder--A recording potentiometer with a full-scale deflection of 5 mV or less, full-scale response time of 2 s or less, and sufficient sensitivity and stability to meet the requirements of 5.1. 6. Reagents and Materials 6.1 Carrier Gas--Carrier gas appropriate to the type of detector used. Helium or hydrogen may be employed with thermal conductivity detectors and nitrogen, helium, or argon with flame ionization detectors. The minimum purity of the carrier gas used should be 99.95 mol %. ;il I II DUP050296077 Designation: D 5008 - 89 Standard Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol By Gas Chromatography1 This standard is issued under the fixed designation D 5008; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This tesl method covers the determination of ethyl methyl pentanol content and purity value of 2-ethylhexanol. 1.2 Water and acid cannot be determined by this test method and must be determined in accordance with Test Methods D1613 and E203 and those results used 1o normalize'tthe chromatographic data. 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 1. 1.4 For hazard information and guidance, see the suppli er's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: P.1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 E 203 Test Method for Water Using Karl Fischer Reagent3 3. Summary of Test Method 3.1 A representative specimen is introduced onto a capil lary column. The 2-ethylhexanol is separated from the ethyl methyl pentanol and other impurities while the components are transported through the column by ah inert carrier gas. The separated componetits are measured in the effluent by a flame ionization detector and the areas, for the peaks are determined by a suitable integration technique. The data are interpreted by applying component detector response factors to the peak areas, and the relative concentrations are determined by relating the individual peak responses to the total peak response. Acidity and water are measured by Test Methods D 1613 and E 203, respectively, and the results are used to normalize the values obtained by gas chromatog raphy. An internal standard procedure is also included as an alternative calculation technique. With this procedure, all impurities are determined relative to the internal standard and the purity value is determined by subtracting the sum of 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0J.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved October 27,1989. Published December 1989. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 15.05. the impurities, water, and acid from 100. 4. Significance and Use 4.1 This test method is used to determine the purity value and ethyl methyl pentanol content of 2-ethylhexanol. 5. Apparatus 5.1 Chromatograph--Any gas chromatograph designed or modified for use with capillary or wide-bore capillary col umns. The gas chromatograph should be equipped with a flame ionization detector or other detector capable of oper ating with these columns and capable ofdetecting impurities at a level of 0.01 weight % with a signal-to noise ratio of at least 5:1. ; 5.2 Column--Any column capable of resolving 2- ethylhexanol from ethyl methyl pentanol and other impuri ties that may be present. The peaks should be resolved quantitatively within a practical elapsed time. Columns that meet the requirement of this test method are listed in Table 1. Other columns may be used, provided the user establishes that a column gives the required separations. 5.3 Specimen Introduction System--Any system capable of introducing a representative specimen into the gas chro matograph may be used. A 1-pL syringe has been used successfully. 5.4 Computing Integrator--Any computing integrator ca pable of accurately determining the peak areas generated during this analysis. 5.5 Analytical Balance--The internal standard technique requires an analytical balance capable of measuring 0.1 mg. 6. Reagents and Materials 6.1 Carrier Gas--Helium, purified nitrogen, or hydrogen are suitable. The carrier gas should have a minimum purity of 99.95 mol %. No t e 1: Precaution--If hydrogen is used, take special safety precau tions to ensure that the chromatographic system is free from leaks. 6.2 Detector Gases--Hydrogen and air are used for the flame ionization detector. If a make-up gas is used, helium or nitrogen are suitable. 6.3 Standards for Calibration and Identification-- Standard samples for all identifiable components present are needed for identification by retention time, and for calibra tion for quantitative measurements. In the case of the internal standard method, pure (99.0+ %) 2-ethyl-l -butanol is specified as the internal standard. Any other internal standard may be used provided it is not present in the sample and doesn't interfere with any other chromatographic peak with the column used. 514 iiSSffi DU P0502 96078 # D5008 TABLE 1. Conditions and Retention Times Case i Case it Case HI Jojumn: ''Material Length,m Inside diameter, mm Liquid phase : Film thickness, pm flection system: yhjecttoh specimen size, uL priperaiures: pColumn temperature, C (isothermal) Injection port temperature, C kjetector temperature, C pies: Icanlergas | Carrfergas flow rate, mL/min fCarrier gas velocity, cm/s pHydrogen flow rate (detector), mL/min ['Airflow rate (detector), mL/min j-Make-up gas |.Make-up flow rate (detector), mL/min -Injection split ratio fetculation technique: ppfeal retention time, min: p'ethyt-2-bufanol (internal standard) kfehyl methyl pentanol L<thylhexanol fused,silica 10 0.53 immobifzed polydimethylsiloxane* 5 direct flash vaporization 0.1 65 200 200 helium 4 30 30 300 none none normalization 5.75 . 7.76 fused siica 10 0.53 immobilized polydimethyfcsfloxane* 5 direct flash vaporization 0.1 85 200 200 helium 4 30 30 300 none none internal standard 2.24 5.75 7.76, fused silica 30 0.32 immobilized polyethylene glycol6 0.25 split 1 120 220 , 220 helium 0.6 20 30 300 helium 30 50:1 normalization 6.74 7.24 ' BSL-160, available from Alltech Assoc., 2051 Waukegan Rd.,,Deerfield, IL 60015, has been found satisfactory for this purpose. J* upekwax, available from Supelco, Irtd.. Supelco Park, Beilefonte. PA 16623, has been found satisfactory for this purpose. JfeNot applicable. If Calibration and Standardization Kl Identification--Select the conditions,, pf column, gjivunn temperature and carrier-gas flow that will give the saiy component resolution (see Table 1). Determinethe Mention time for each component by injecting small nounts of the compound either separately or in mixtures. |p7.2 Standardization--The area under each peak generBd is considered a quantitative measure of-the correJtonding compound. The relative area is proportional to jfpncentration if the detector responds equally to all the nple components. The response to different components ^generally significantly different for flame ionization deteejfcs. This difference in detector response may he corrected | use of relative response factors obtained by injecting and measuring the response of known blends: Using pure mateials, prepare a calibration mixture with each component present in the appropriate amount. If an internal standard alculation technique is used, include the internal standard this calibration mixture. If pure components are not vailable and interfering components are present, then propriate adjustments must be made in calculating the [weights of the components present 7.2.1 Chromatographic Conditions--Using a suitable nethod selected from Table 1, analyze a representative ppecimen of the calibration mixture. 7.2.2 If a computing integrator is used, follow the manu facturer's instruction manual to calculate relative response factors. If manual calculations are used, calculate relative ^response factors for each component as follows. R = (A x B)/(Cx D) Jwhere: ; R = response factor for component of interest, L A = peak area of reference component, B = weight of component of interest in calibration mixture, g>. C - peak area for component of interest in calibration mixture, and D -- weight of reference component in calibration mixture, * No t e 2--If a normalization calculation technique is used, 2ethylhexanol will be the reference component. If an internal standard calculation technique is used, the internal standard will be the reference component. 7.2.3 The calibration factor generated for ethyl methyl pentanol can be used to calculate the concentration of any unknowns present. 8. Procedure 8.1 Normalization Technique: 8.1.1 Introduce a representative specimen into the chro matograph. 8.1.2 Using the same conditions as for calibration and standardization, determine the areas for all peaks. 8.2 Internal Standard Technique: 8.2.1 Weigh 0.1 g of internal standard into a vial. Record the weight to the nearest 0.1 mg. 8.2.2 Into the same vial, weigh 20.0 g of a representative specimen. Record the weight to the nearest 0.1 mg. Close the vial tightly and mix well. 8.2.3 Introduce a representative specimen of the mixture in 8.2.2 into the gas chromatograph. 8.2.4 Using the same conditions as for calibration and standardization, determine the areas for all peaks. 9. Calculation 9.1 Normalization Technique: 9.1.1 If a computing integrator is used, follow the manu- 515 DUP050296079 # D 5008 facturer's instruction manual to compute the percent ofeach component of interest. 9.1.2 If manual calculations are made, apply the appro priate detector response factor to each peak to obtain the corrected peak response. Calculate the weight percent, W, of each component of interest as follows: W'=(/f)x(t00-G) where: E = corrected peak response for component of interest, F -- sum of corrected peak responses for all components, and G -- sum of water and add as determined by Test Methods D 1613 and E 203. 9.2 Internal Standard Technique: 9.2.1 If a computing integrator is used, follow the manu facturer's instruction manual to compute the percent of each component except the 2-ethylhexanol. 9.2.2 If manual calculations are made, apply the appro priate detector response factor to each peak to obtain the corrected peak response. Calculate the weight percent W of each component, except the 2-ethylhexanol, as follows: l00)/(Jx X) where: H = corrected peak response for component of interest, I = weight of internal standard added to sample, g, J = corrected peak response for internal standard, and K = weight of sample mixed with internal standard, g. 9.2.3 Calculate the purity value, P, in weight percent as shown below: P= 100 -L where: L = sum of water, acid, and the weight percent of all components except 2-ethylhexanol. 10. Report i 10.1 Report the following information: 10.1.1 The ethyl methyl pentanol content to the 0.001 weight % and 10.1.2 The purity value to the nearest 0.01 wei 11. Precision and Bias 11.1 In an interlaboratory study of this test m which one operator in ten laboratories tested 2-ethy with a purity value of 99.653 and which contain!: weight % of ethyl methyl pentanol, the within-la standard deviation and between-laboratory stand tion, with 9 df, respectively, were as follows: Ethyl methyl pentanol 2-EthylhcxanoI Concentration, weight Within Laboratory , Deuce : labor,to 0.001 0.004 0.01V 0043 11.2 Based upon these standard deviations, the foi criteria should be used forjudging the acceptability of at the 95 % confidence level. 11.1.1 Repeatability--Two results, each the mean1 plicates obtained by the same operator on dilTeten should be considered suspect if they differ by more ma weight % absolute for purity values or 0.001 absolute for ethyl methyl pentanol. 11.1.2 Reproducibility--Two results, each the , duplicates obtained by operators in different labo" should be Considered suspect ifthey differ by more t weight % absolute for purity values or 0.036 w absolute for ethyl methyl pentanol. 12. Keywords , 12.1 ethyl methyl pentanol content/eompositiohi chromatography; purity by gas chromatograp ethylhexanol me American Society lor Testing andMaterials takes no position respectingthe 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 ofsuch rights, are entirely their own responsibility. mis standardis subject to revision at anytime by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invitedeither 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, 7976 Race St., Philadelphia, PA 19103. Jr *4 - fir 516 ,4$ DUP050296080 Designation: D 5125 - 91 y=( % Standard Test Method for Viscosity of Paints and Related Materials by ISO Flow Cups1 This standard is issued under the fixed designation D 5125; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yew of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai. Scope .Q. 1 .This test method covers the determination of the flow j! (viscosity) of Newtonian and near-Nqwtonian paints, id related coatingsand products using ISO capillary flow ' ps- ,qTE T--If the liquid is non-Newtonian, that is shear-thinning or ttothopic, Test Method D 2196 Should be used. V V: k- i 1.2 The cup-orifice combination (ISO. cup with orifice .!meter of 3 mm; 4 mm, or 6 mm) is selected to provide an ~ux timewith the range of20 to 100 s and visebsities up to ' 0 cSf (700 mm2/s). The most commonly used cup is the ;ne with the 4-mtn orifice. ::1.3 This test method is limited to'testing materials for hich the breakpoint of the flow from the orifice of the flow Up can be determined with certainty. This point is difficult determine and reproduce for materials with flow times in cess of 100 s due to slowing-down effects. 11.4 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 alth practices and determine the applicability ofregulatory nitations prior to use.- No t e 2--The lntemational Civil Aviation Organization (ICAO) and International Maritime Organization (IMO) include in their tegula- ns a similar test (ISO 2431) to determine the viscosity of hazardous 'scous liquids. The viscosity is then used to place these liquids in a azard packaging group depending on their viscosity/flashpoint relation- ip. The U. S. Department of Transportation .permits the use of these gulations for transhipment of hazardous material within the U.S. ' *-en bound for foreign destinations; ' f; Referenced Documents 2.1 ASTM'Standards: !D 2196 Test Methods for Rheological Properties of Nonj?9 ' Newtonian Materials by Rotational Viscometer2 D 3924 Specification for Standard Environment for Con* ditioning' and Testing Paint, Varnish, Lacquer, and i Related Materials2 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 E 1 Specifications for ASTM Thermometers3 2.2 ISO Documents: 1 This test method is under the jurisdiction of ASTM Committee D-l on Miscellaneous Materials and is the direct responsibility of Subcommittee DO 1.24 on Physical Properties of Liquid Plants and Paint Materials. Current edition approved Aug. 15, 1991. Published October 1991. , 2 Annua! Bock ofASTM Standards, Vol 06.01. 3 Annual Bock ofASTM Standards, Vol 05.03 and 14.03; . ISO 2433 Paints and Varnishes: Determination of Flow Time by Use of a Plow Cup4 3. Terminology 3.1 Definitions: 3.1.1 dynamic viscosity--the ratio of the applied shear stress to shear rate. 3.1.1.1 Discussion--The SI unit for dynamic viscosity is the pascal second (Pa-s). The traditional unit is the centipoise (cP); 1 cP = I mPa-s. 3.1.2 flow time--the elapsed time from the moment when the material under test starts to flow from the: orifice of the filled cup to the moment when the flow stream of material first breaks1 close to the orifice. 3-1.3 kinematic Viscosity--the ratio of the dynamic vis cosity to the density of the liquid. 3.1.3.1 Discussion--The SI unit for kinematic viscosity is the square metre per second (m2/s). The traditional unit is the centistokes (cSt); 1 cSt = 1 mm2/s. 3.1.4 near-Newtonian liquid--a liquid in which the varia tion of viscosity with shear rate is small and the effect on viscosity of mechanical disturbances such as` stirring is negligible. 3.1.5 Newtonian liquid--a liquid in which the viscosity is independent of the shear stress or shear rate. Compare non-Newtonian liquid. 3.1.6 non-Newtonian liquid--a liquid in which the ratio of shear stress to shear rate is not constant. 4. Summary of Test Method .4.1 The ISO flow cup is filled level full with the material under test that has been conditioned at the specified mea suring temperature (see 10.2.2) and the time for the material to flow through one of the standard orifices is determined. 5. Significance and Use 5.1 This test method is useful for the determination of package and application viscosities of paints and other coatings. It is limited to Newtonian or near-Newtonian liquids. 5.2 This test method may be used similarly to ISO 2431 in conjunction with flashpoint to determine the hazard grouping of viscous liquids in international regulations. 4 Available from American National Standards Institute, 1) W. 42nd St, 13th Floor. New York, NY 10036, 517 DUP050296081 DS12S 6. Apparatus 6.1 ISO Capillary Flow Cups5--ISO cups look like Ford cups, but instead of the non-capillary hole in the bottom of t, is mandatory for referee purposes. Mix the material foor- ' oughly while at the same time avoiding, as far as possible loss of solvent by evaporation. 1 the Ford cup, the ISO cup has a 20-mm capillary and is more No t e 3--150 mL of strained material is sufficient for one tesi like a true capillary viscometer. 6.1.1 Dimensions--The dimensions of the ISO flow cup 9. Calibration and the tolerances allowed in manufacture shall be as given in Fig. 1. The most critical tolerance is the internal diameter of the jet of the cup, because the flow time is inversely proportional to the fourth power of this dimension. The jet of the cup shall be made of stainless steel or sintered carbide unless otherwise specified, and the body of the cup shall be made of a material that is corrosion resistant and is not affected by the products to be tested. 6.1.1 Construction--The dimensions not specified, such as wall thickness, shall be such that no distortion of the cup can occur in use. The external shape shown in Fig. 1 is recommended, but may be modified for convenience of use, or manufacture, provided that the protrudingjet ofthe cup is protected from accidental damage as far as possible by an external protective sleeve. Such a protective sleeve shall not be immediately adjacent to the jet, so as to prevent a capillary action when the material under test flows out 6.1.3 Finish--The interior surfaces of the cups, including the orifice, shall be smooth and free of turning marks, crevices, ledges and burrs that may cause random flow, or trap sample or cleaning material. The standard of finish required is equivalent to a maximum roughness of not more than 0.5 pm (see Note 3). 9.1 Dimensionally similar cups will give, with Newtonian liquids, such as a standard oil, similar flow times, provided that the temperature oftesting is precisely the same. The use of such liquids to calibrate cups provides a useful means of initially checking that dimensionally similar cups are within the accepted tolerances ofperformance and also for checking from time to time whether any wear or damage has taken place sufficient to bring a cup outside the accepted toler ances. 9.2 For calibration of any particular cup, use a standaul oil6, of known kinematic viscosity and draw a graph of kinematic viscosity versus temperature from the data given by the supplier for the oil. 9.3 Using the relevant procedure described in Section 10, determine the flow oftime of the oil at a known temperature within the range 68 to 80F (20 to 30C), measured to the nearest 0.1C. 9.3.1 Record this flow time, which should be in the range 30 to 100 s and preferably near the midpoint ofthis range, to an accuracy of 0.2 s. 9.4 From the prepared graph, read the kinematic viscosity at the test temperature. 9.4.1 Using the appropriate calibration graph of Figs. 2,3, No t e 3--Roughness defined as the arithmetical mean deviation R,, from the mean line of the profile. or 4, read the flow time corresponding to this kinematic viscosity. 6.2 Thermometer, accurate to 0.4F (0.2C) and graduated at 0.2"F (O.rC) intervals. Saybolt viscosity thermometer conforming to requirements for thermometer 17F and 17C (60 to 80"F) (10 to 27"C) as prescribed in Specification E 1 is required. 9.5 Ifthe two values of flow time obtained do not differ by more than 3 %, the cup may be deemed satisfactory for use. 9.6 For reference purposes, a correction factor corre sponding to the flow time deviation from that obtained using the oil may be applied. 6.3 Stand, suitable for holding the flow cup and provided with leveling screws. 6.4 Spirit Level, preferably of the circular type. 10. Procedure 10.1 Preliminary check: 6.5 Flat Glass Plate or Straight-Edge Scraper. 6.6 Stopwatch, or other suitable timing-device with scale divisions of0.5 s or finer and accurate to within 0.2 % when tested over a 60-min period. ' 6.7 Temperature-Controlled Room or Enclosure, capable of maintaining the cup and sample at a recommended, constant temperature. No t e 4--This check is earned out to show that the material is suitable for the test {that is, is Newtonian or near-Newtonian). 10.1.1 Choose a flow cup that will give a flow time of between 30 and 100 s for the material. 10.1.2 Determine the flow time by the procedure specified in 10.2, making sure that the material is well agitated before pouring into the cup. Remove the finger within 5 s of filling 7. Reagents and Materials 7.1 Certified kinematic viscosity standards.6 the flow cup. 10.1.3 Repeat the determination but this time allow the material to remain in the flow cup for 60 s before removing 8. Sampling the finger. 8.1 Sample material according to Practice D 3925. 10.1.4 If the second result differs from the first by more 8.2 Before testing, it is advisable to strain the sample than 10%, the material shall be deemed to be non- through an appropriate sieve into a clean dry container. This Newtonian and therefore unsuitable for consistency control iiH5 by flow-time measurement. i 5iSO cups available fram 1JYK.-Gatdr.cr. Inc., 1100 East-West Highway, Silver 10.2 Determination ofFlow Time: 10.2.1 Choose a flow cup that will give a flow time Spring MD 20910, Erichsen Instrument Company, 1350 Home Avenue, Akron, between 20 and 100 s, but preferably between 30 and 100 s }- OH 44310, or Paul N. Gardner Company, Inc., 316 NE 1st SL, Pompano Beach, Fthave been found suitable for this purpose. > - Standards, available from the Gmnon instrument Company, P.O. Box 16, for the test material. 10.2.2 Adjust the temperature of the strained sample and State-College, PA 16801 have been found suitable for this purpose. the flow cup, to 73.5 1.0F (23 0.5C (according to 518 J % DUP050296082 D 5125 DUP050296083 D 5125 Row time, t, sFIG. 2 Calibration Curve for 3-mm Cup Specification D 3924)) to 77 1.0'F (25 0.5"C) or to an other alternatively agreed upon temperature. No t e 5--The temperature 73.5"F <23**C) is the standard environ ment for conditioning and testing paint as specified in Specification D 3924. It also is the test temperature specified in international shipping regulations. However, 77F (25C) has been the standard temperature for measuring the viscosity of paint and other materials fortnany years and is the choice of many operators. 10.2.3 If the temperature-controlled enclosure is used, as recommended, it is advisable to condition the cup and the sample before straining, by placing them in the enclosure before use. The sample shall be considered ready for test immediately after any air bubbles entrained during the preparation and sieving procedures have dispersed. Carry out a final check that the temperature ofthe sample is within 1F (0.5C) of the agree test temperature immediately prior to filling the cup. 10.2.4 Place the flow cup on the stand, in a position free of drafts and, by using the level and adjusting the leveling screws ofthe stand, ensure that the upper rim ofthe flow cup is in a horizontal plane. 10.2.5 With the orifice closed by a finger, fill the cup with the freshly strained, bubble-free sample, pouring slowly to avoid the formation of air bubbles. If any bubbles are formed, allow them to rise to the surface and remove them. If the cup has been properly leveled, the sample will overflow 520 DU P0502 96084 0 5125 -- -W . L____ I - ____________* 0 10 20 30 40 50 60 70 80 90 100 Flow time, t, s FIG. 3 Calibration Curve tor 4-mm Cup jitenly over the rim into the gallery. Remove any meniscus &nned either by drawing the straight-edge scraper over the ||ntire rim of the cup or by sliding over the rim, a flat glass Hate with rounded edges so that no air bubbles form ^between the glass and the surface of the specimen. Then isjraw this plate horizontally across the rim ofthe cup so that, jfiihen the plate is removed, the level of the specimen coincides with the top rim of the cup. : 10.2.6 Place a suitable receiver under the flow cup so that hfc distance between the orifice of the flow cup and the ^surface of the received specimen is never less than 100 mm. ^Remove the finger from the orifice and simultaneously start II the timing device, stopping it as soon as the first break occurs in the stream of specimen close to the orifice. Record the flow time to the nearest 0.5 s. 10.2.6.1 If the test is not carried out in the temperaturecontrolled enclosure, place the thermometer in the stream of the specimen so as not to interfere with observation of the break in the flow. This is conveniently done by holding the thermometer in a suitable clamping device with the bulb so placed that it is at an angle to the direction of flow and completely immersed in the emergent stream and not less than 100 mm from the orifice. It is convenient to use the same thermometer as is used to adjust the temperature of the sample initially. Any difference in temperature from the 521 DUP050296085 1 ooo D 5125 900- 800 700 \ 600 1 g 500 1 5 j 400 2 BOO -y 200 / t 100 / / / _L v=6,90 [0 11 1 30<f< 100 ______1---- 1______ 1------ 0 10 20 30 40 50 60 70 80 90 100 Row time, f, s- FIG. 4 Calibration Curve for 6-mm Cup initially adjusted temperature shall not be greater than i.OT (0.5C). 10.2.7' Make a second determination-on another portion ofthe originally prepared sample and check, carefully that the temperature oftesting is within the prescribed limits. Record the Bow time to the nearest 0.5 s. Calculate the mean of the two determinations. Ifthe two determinations differ by more than 5 %, make a third determination. If the third determi nation add either of the previous determinations do not differ by more than 5 %, discard the other determination. Calculate the result as the mean of the two accepted determinations. If the third determination does not provide this measure of agreement, the method of test is unlikely to be suitable because of anomalous flow behavior, and consid-. eration shall be given to other methods of test. 11. Care and Checking of Flow Cups 11.1 Clean the cup immediately alter use and before the sample starts to dry, using a suitable solvent. Never use metal cleaning tools or wire. If the orifice becomes contaminated with dried deposits, soften with a suitable solvent and clean carefully, for example with a soft cloth pulled through the orifice. 11.2 Check the cups periodically for wear or damage by the calibration procedure specified in Section 9. 522 DUP050296086 D 5125 eport The test report shall include at least the following ition: .1 Type and identification of the product tested, .2 Designation (No. 3, 4, or 6) of the cup used, 3 Temperature of testing and where determined; in i, in the controlled environment, or in efflux stream, |lr.4 Flow time, and 5 Any deviation, by agreement or otherwise, from procedure described. ecision and Bias Precision--The precision of this test method has not determined by an ASTM Task Group and the following i should only be used as in guide until interlaboratory ; can be carried out. 13.1.1 Repeatability (r)--The difference between two re sults (each the mean of two accepted determination) ob tained by the same operator with the same apparatus under constant operating conditions on identical test material shall, at the 95 % confidence level, not exceed 5 % (as reported in ISO 2431). 13.1.2 Reproducibility (R)--The difference between two results (each the mean of two accepted determinations) obtained by different Operators in different laboratories or identical test material shall, at the 95 % confidence level, not exceed 10 % (as reported in ISO 2431). 13.2 Bias--The bias of. this test method will be deter mined using standard oils. However, this will only, give the bias in terms of hydrocarbon oils and will have no meaning for other materials. 14. Keywords 14.1 efflux cups; flow cups; ISO cups; viscosity The American Society tor Tasting andMaterials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of th!s.standard are expressly advised that determination at the validity of any such patent rights, and the risk of inlrlngement 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 Itnotrevised, either raapprovedor withdrawn. YourcommentsareInvited oitheTtorrevision of this standardor toradditionalstandards ana should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may affsnef. 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 Sf., Philadelphia, PA 19103. I I i. ; V. 523 DUP050296087 Designation: D 5137 - 90 Standard Specification for Hexyi Acetate1 This standard is issued under the fixed designation D 5137; the number immediately following the designation indicates the year of original adoption or, in Ihe case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (ri indicates an editorial change since the last revision or reapprovai. 1. Scope 1.1 This specification covers hexyl acetate, which is used as an active tail high boiling solvent in lacquers, automotive coatings, maintenance paints, and other related coatings. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet. 2. Referenced Documents 2.1 ASTM Standards: D268 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Materials2 D 1078 Test Method for Distillation Range Of Volatile Organic Liquids2 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)2 D1296 Test Method for Odor of Volatile Solvents and Diluents2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)2 D1476 Test Method for Heptane Miscibility of Lacquer Solvents2 D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products2 D1617 Test Method for Ester Value of Lacquer Solvents and Thinners2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 E 1 Specification for ASTM Thermometers4 E 300 Practice for Sampling Industrial Chemicals5 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, Liquid, Dry, and Paste: Packaging of6 3. Properties 3.1 Hexyl acetate shall conform to the following require ments: Acidity (five acid as acetic acid) weight %, max Apparent specific gravity 20/20T 0.02 0.872 to 0.876 1 These specifications are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Nov. 11,1990. Published December 1990.' 3 Annual Book ofASTM Standards, VoJ 06.03. 5 Annual Book ofASTM Standards, Vol 05.03. 4 Annual Book cfASTM Standards, Vols 05.03 and 14,03. 9 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 6 Standardization Documents Order Desk, Bldg. 4. Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 25/25`C Color, Pt-Co units, max Distillation range, *C Initial boiling point, min 95 % point, max Electrical Resistivity Ransburg megohms, min Ester value, weight, % min Odor Water content, weight %, max7 0.868 to 0.872 15 162 J76 20 99.0 characteristic 0.05 4. Sampling 4.1 The material shall be sampled in accordance with Practice E 300. 5. Test Methods 5.1 TEe properties enumerated in this specification shall be determined in accordance with the following ASTM methods: 5.1.1 Acidity--Test Method D 1613. 5.1.2 Apparent Specific Gravity--Determine the apparent specific gravity by any convenient method that is accurate to the third decimal place, the termination of both the spec imen and water being 20C. See Methods D 268 or Test Method D 4052. 5.1.3 Color--Method D 1209. 5.1.4 Distillation Range--Test Method D 1078 using an ASTM Solvents Distillation Thermometer 103C having a range from 148 to 202C and conforming to the require ments in Specification E 1. 5.1.5 Electrical Resistivity--An ASTM Test Method uti lizing a Ransburg Electrical Resistivity meter is under development. 5.1.6 Ester Value--Test Method D 1617. Use specimen size, reaction conditions, and ester factor as specified for methyl amyl acetate. 5.1.7 Odor--Test Method D 1296. 5.1.8 Water Content--Test Methods D 1364 and D 1476. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between the pur chaser and the supplier. 6.2 Packaging shall conform to applicable carrier rules and regulations, or when specified shall conform to Federal Spec. PPP-C-2020. 7. Keywords 7.1 ester; hexyl acetate; solvent 7 This quantitative water limit ensures that the material is miscible without turbidity with !9 volumes ofheptane at 20'C. 524 DUP050296088 D 5137 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 axpressfy advised that determination of the.validity of any such pafenf rfg/ite, 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 it not revised, either reapproved or withdrawn. Your comments are invited either forrevision 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, '1916 Race St., Philadelphia, PA 19103. PS- 525 DUP050296089 # Designation: D 5164 - 91 Standard Specification for Propylene Glycol and Dipropylene Glycol1 This standard is issued under the fixed designation D 5164; the number immediately following the designation indicates the year of original! adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers propylene glycol and dipropylene glycol for use in the preparation of surface coatings. 1.2 For specific hazard information and guidance, see the supplier's Material Safety Data Sheets. 2. Referenced Documents 2.1 ASTM Standards: D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter2 E 202 Method for Analysis of Ethylene Glycols and Propylene Glycols3 E 300 Practice for Sampling Industrial Chemicals4 2.2 U.S. Federal Specification: PPP-C-2020 Chemicals, liquid, Dry, and Paste: Packaging of5 6 7 3. Properties 3.1 Propylene glycol or dipropylene glycol shall conform to the respective properties shown in Table 1. 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 Subcommittee D0I.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved Sept. 15.1991. Published November 1991. 2 Annual Book ofASTM Standards, Vol 05.03. 3 Annual Book ofASTM Standards, Vol 15.05. 4 Annual Book ofASTM Standards, Vote 06.03 and 15.05. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. TABLE 1 Requirements for Propylene Glycol and Dipropyl Glycol Property Apparent specific gravity 20/20*0 25/25C Color, Pt-Co units, max Distillation range, 760 mmHg initial Boiling Point C min Dry point, C, max Water, wt %, max Acidity, as acetic arid, wt %, max Propylene glycol, wt %, max Dipropylene glycol, wt %, max Triprcpylene glycol, wt %, max Iron, ppm, max ____ Propylene Glycol Dipropyleiy Gy: 1.0375 to 1.0390 1.020 to 1025 1.0351 to 1.0366 1.016 to 1 OZi 15 15 185 228 190 236 0.2 0.005 NA* 1.0 NA* 0.5 0.2 ;0.01 1.0 NA* 1.0 1.0 A NA -- not applicable. 4. Sampling 4.1 The material shall be sampled in accordance Practice E 300. 5. Test Methods 5.1 The properties enumerated in this specification S be determined in accordance with Method E 202. ,T|p 5.2 The apparent specific gravity can also be determm in accordance with Test Method D 4052. 6. Packaging and Package Marking 6.1 Package size shall be agreed upon between 'he pur chaser and the supplier. 6.2 Packaging shall conform to applicable earner rule and regulations or when specified shall conform to J Spec. PPP-C-2020. 7. Keywords 'W 7.1 dipropylene glycol; propylene glycol The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with my item mentioned in this standard. Users of thle 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 eraInvited either tor revision ofthfs 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 fee/ that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 526 . DUP050296090 Designation: E 28 - 67 (Reapproved 1S82)e Standard Test Method for Softening Point by Ring-and-Bali Apparatus1 This standard is issued under the fixed designation E 28; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by the agencies ofthe Department of Defense to replace Method 4495 of Federal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. a No t e--Section 2 was added editorially and subsequent sections renumbered in June 1985. pe This test method covers the determination of the mng point of resins (including rosin) and similar mateby jngans of the ring-and-ball apparatus. err 1--For testing asphalts, tars, and pitches, see Test Method iferenced Documents ASTM Standards: |398 Test Method for Softening Point of Bitumen in .thyiene Glycol (Ring and Ballr t Specification for ASTM Thermometers3 I 'ttening Point In general, with materials of these types, softening not take place at a definite temperature. As the "nature rises, these materials gradually and impercepchange from brittle or exceedingly thick and slow~g materials to softer and less viscous liquids. For this 'n, the determination of the softening point must be jby a fixed, arbitrary, and closely defined method if the s obtained are to be comparable. `t*In this test method, the softening point is defined as nperalure at which a disk of the sample held within a pntal ring is forced downward a distance of 2.54 cm (1 nder the weight of a steel ball as the sample is heated at ribed rate in a water or glycerin bath. pparatus Ring--A brass-shouldered ring conforming to the ensions shown in Fig. 1 {a). If desired, the ring may be led by brazing or other convenient manner to a brass of about 13 B & S gage 1.5 to 2,0 mm (0.06 to 0.08 in.) .meter as shown in Fig 2 (a). For use in the powder thod ofsample preparation, the ring may be made of steel 'fninimize the possibility of its deformation during the [parting operation. This test method is underthe jurisdiction of ASTM Committee'O-l on Paint Related Coatings and Materials and is the direct responsibility of Subcom' DO] ,34 on Naval Stores. Current edition approved Sept. 8, 1967. Published November 1967. Originally sshed as E 28,- 36 T. Last previous edition E 28 - 58 T. . 2 Discontinued, see 1984 Animal Book ofASTM Standards. Vol 04.04. Annual Book ofASTM Standards, Vois 05.03 and 14.03. 4.2 Ball--A steel ball, 9.53 mm (3/s in.) in diameter, weighing between 3.45 and 3.55 g 4.3 Ball-Centering Guide--A guide for centering the ball, constructed of brass and having the general shape and dimensions illustrated in Fig. 1 (c), the use of which is optional. 4.4 Container--A glass vessel, capable of being heated, not less than 8.5 cm (3.34 in.) in diameter and not less than 12.7 cm (5 in.) in depth from the bottom of the flare. (An 800-mL low-form Griffin beaker ofheat-resistant glass meets this requirement.) 4.5 Supportfor Ring and Thermometer--Any convenient method for supporting the ring and thermometer may be used, provided it meets the following requirements: 4.5.1 Ring shall be supported in a substantially horizontal position. 4.5.2 When using the apparatus shown in Fig. I (d): The bottom of the ring shall be 2.54 cm (1.0 in.) above the horizontal plate below it; bottom surface of the horizontal plate shall be 12.7 to 19.05 mm (0.5 to 0.75 in.) above the bottom ofthe beaker; and depth of liquid in the beaker shall be not less than 10.16 cm (4.0 in.). 4.5.3 When using the apparatus shown in Fig 2 (e): the bottom of the ring shall be 2.54 cm (1.0 in.) above the bottom of the beaker, with the bottom end of the rod resting on the bottom of the beaker, and depth of liquid in the beaker shall be not less than 10.2 cm (4.0 in.) (see Fig 2 (a), (b), and (c)). 4.5.4 In both assemblies: Thermometer shall be sus pended so that the bottom of the bulb is level with the bottom of the ring and within 1.27 cm (0.5 in.) but not touching the ring. For referee work, no more than two rings shall be used. 4.6 Thermometers: 4.6.1 An ASTM Low-Softening-Point Thermometer, hav ing a range from -2 to 80C (30 to 180F), and conforming to the requirements for thermometer 15C or 15F as pre scribed in Specification E 1. 4.6.2 An ASTM High-Softening-Point Thermometer, having a range from 30 to 200"C (85 to 392F), and conforming to the requirements for Thermometer 16C or 16F as prescribed in Specification El. 4.7 Mechanical Stirrer--A two-bladed motor-driven stir rer attached to the bottom of a true vertical shaft may be used to ensure uniform heat distribution (see Fig. 2 (d) for dimensions). The direction of shaft rotation shall move the 527 DUP050296091 < E 28 .(d) Assembly ,. . , FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus Showing Two Rings liquid upward. The speed shall be within the range from 500 to 700 R/min. . ' 4.8 For the powder method of sample preparation the following additional apparatus is required; 4.8.1 Mortar and Pestle--A steel mortar and pestle with sleeve, knock-out-button, and ring support conforming to the dimensions shown in Fig. 3. 4.8.2 Hammer--A babbitt metal or a lead-impregnated rubberiiammer weighing 0.9 kg (2 lb). 4.9 Hydraulic Press--A hydraulic press capable of main taining sustained pressures up to 55 kPa (8000 psi), to be used alternatively with the hammer. 5. Preparation of Sample by Pour Method 5.1 Rosins--Select a sample representative ofthe material under test. The sample shall consist of freshly broken lumps free of oxidized surfaces. For samples received as small lumps, scrape off the surface layer of the lumps immediately before using, avoiding inclusion of finely divided material or dust. Select a quantity at least twice that necessary to fill the desired number of rings, but in no case less than 40 g, and melt it immediately in. a clean container, using an oven, hot 528 DUP050296092 No. 13 8S3 Gage Brass Wire # E28 I I JL (o) Brass Ring and Wire (b> Proper Position of Boll FIG. 2 Assembly of Apparatus Showing Stirrer and Single Shouldered Ring 6, sand, or oil bath to prevent local overheating. Take ;to avoid incorporating air bubbles in the sample, which .t not be heated above the temperature necessary to pour fthaterial readily without inclusion of air bubbles. The from the beginning of heating to the pouring of the ple shall not exceed IS min. Immediately before filling rings, preheat them to approximately the temperature at j|ch the material is to be poured. The rings, while being , should rest on an amalgamated brass plate, Pour the nple into the rings so as to leave an excess on cooling, er cooling a minimum of 30 min, cut the excess material fcieanly with-a slightly heated knife or spatula. In case the E is repeated, use a clean container and fresh sample. T- Preparation of Sample by Powder Method 6.1 Resins (Except Rosin), and Other Materials that mot Be Melted and Poured Without Altering the Soft- ling Point--Select the sample as described in Section 5 and iteak up the lumps until there are no particles larger than 175 mm (`/s in.). Mix the material thoroughly, and quarter jtfwh until a suitable quantity (approximately 50 to 75 g) is ibtained for powdering. Pulverize the quartered sample in a torcelain mortar or by other suitable means, and fractionate iy- screening through Nos. 50 and 200 sieves. Immediately se- Use the material passing the No. 50 sieve and retained on the No. 200 sieve, for preparation of the ring. Assemble the ring with the ring support, the mortar, and the knock-out-button, together with the sleeve, as shown in Fig. 3. Take care to ensure that the ring is properly centered and seated in the cut-out section of the sleeve. Pour the powdered material into the sleeve until it is about 1.27 cm (0.5 in.) above the top of the ring (approximately 3 g required). Place the pestle in the sleeve and compact the powder by rapping the pestle sharply 50 to 60 times with the leaded hammer, or by applying a pressure of 48 to 51 kPa (7000 to 7500 psi) in a suitable press, and holding this pressure for 3 to 5 min. Remove the ring from the mortar and sleeve. An excess of material shall remain above the top surface of the ring. Carefully scrape this off, until the top of the sample is level with the ring. Ifthe top and bottom surfaces ofthe sample in the ring are not smooth and level with the ring, discard, and repeat the compacting operation, using a clean ring and fresh powder. 7. Preparation of Sample by Molding Method 7.1 Resins (Except Rosin) and Other Materials that Are Heat-Sensitive and Cannot Be Melted and Poured Without Altering the Softening Point: 7.1.1 Selection ofSample--Select a sample representative of the material under test. The sample shall consist of freshly broken lumps free of oxidized surfaces. For samples received as small lumps, scrape off the surface layer of the lumps immediately before using, avoiding inclusion of finely di- 529 J DUP050296093 # E 28 Pestle (e) Shouldered Ring Ring Support (o) -Button {b) /--Mortor (cj 9v Assembled Mortar and Pestle Slide fit for Pestle 45<S. (e) Pestle -Knock-out hole for Button (c) Mortar FIG. 3 Mortar and Pestle vided material or dust, and then grind superficially in . a mortar. 7.1.2 Apparatus 7.1.2.1 Hot Plate, 3-heat, 20.32-cm (8-in.), 1000-W, with variable transformer, 7.5 A. 7.1.2.2 Aluminum or Steel Plates, 10.16 cm (4 in.) by 15.24 cm (6 in.) by 1.6 mm (`/i6 in.), 7.1.2.3 Spatula, 20.32-cm (8-in.), stiff blade. 7.1.2.4 Tongs: 7.1.3 Procedure--Turn the hot plate to low heat and allow to come to temperature. Depending on the expected softening point of the resins, use the following approximate transformer settings; Expected Softening Point 85 to 90C 125 to 130*C Transformer Setting 80 110 7.1.3.1 Place the shouldered ring, bottom down, on one end of the aluminum or steel plate, and then place this assembly on the hot plate. Place 10 to 15 g of the crushed resin on the metal plate so as to form a layer about 6.3 mm ("A in.) thick and 7.62 cm (3 in.) in diameter. The resin adjacent to the metal plate will quickly begin to soften. By means of the spatula, scrape and knead the entire mass until it is soft and plastic, using a second spatula if necessary (Note 2). Finally, gather the entire blob of resin on the spatula, remove the metal plate from the hot plate with a pair of tongs, and quickly press the resin into the the shouldered ring, applying pressure to the top of the spatula. Allow the assembly to cool somewhat; then tap the plate and spatula to ' free the ring. Trim offthe excess resin on the periphery ofthe ; ring. In order to remove excess resin from the top, grasp the ring in a pair of tongs and draw the top surface quickly and! firmly over the surface of a heated metal plate. No t e 2--Not over 5 min should be required for this operation.' Exeessive exposure to elevated temperature wiU promote changes in the. sample that result in high melting points. 8. Procedure for Materials Having Softening Points 80C (176F) or Below 8.1 Assembly of Apparatus--Fill the glass vessel, to a depth of not less than 10.16 cm (4.0 in.) and not more than, 10,78 cm (4.25 in.) with freshly boiled distilled water at 5C ' (41 F). For resins (including rosin), use water which has been cooled to not less than 45G (8rF) below the anticipated softening point, but in no case lower than 5C (41F). Locate the axis of the stirrer shaft near the back wall of the beaker, with the blades clearing the wall and with the bottom of thCv blades 1.90 cm (0.75 in.) above the top of the ring. Unless the ball-centering guide is to be used, make a slight indentation in the center of the sample by pressing the ball or a rounded 530 mmssm DUP050296094 E 28 y heated for hard materials, into the material at Suspend the ring containing the sample in the that the lower surface of the filled ring is 2.54 cm hove the upper surface of the lower horizontal plate 4), which is at least 1.27 cm (0.5 in.) and not more cm (0.75 in.) above the bottom of the glass vessel, above the bottom ofthe glass container (Fig. 2 (<?)). ball in the water but not on the test specimen, an ASTM low-softening-point thermometer so that in of its bulb is level with the bottom of the ring, 0.5 in. but not touching the ring. Maintain the perature of the water for 15 min. With suitable place the ball in the center of the upper surface of erial in the ring. Start stirring, and continue the i1i 500 to 70 0 r/min until completion of determina- feteyf--Apply heat in such a manner that the re of the water is raked 5*C (10F)/min. Avoid the using shields if necessary. `Omissible Variation in Rise of Temperature--The Oftemperature shall be uniform and shall not be over the period of the test. The maximum permisation for any minute period after the first three shall C (1F ). Reject all tests in which the rate of rise these limits. 'oftening Point--Record as the softening point the ture of the thermometer at the instant the material the lower horizontal plate (Fig. 1 (d)>, or the bottom ontainer (Fig. 2 (e)). Make no correction for the fit stem of the thermometer. dure for Materials Having Softening Points Above (I76F) Jse the same procedure as described in Section 8, ,fill the bath with glycerin (Note 3) and use an ASTM ' ftening-point thermometer. The starting temperature ^glycerin bath shall be 32C (90"F), but for resins `ng rosin) use glycerin that has been cooled to not less than 45C (81F) below the anticipated softening point, but in no case lower than 35`C (95*F). No t e 3--For materials softening around 80"C (176T) report the nature of the bath, and whether water or glycerin was used since a glycerin bath yields slightly higher results than a water bath. 10. Precautions 10.1 The stirrer motor shall be so mounted that any vibrations created by its rotation are not conveyed directly to the sample support. 10.2 The use of freshly boiled distilled water is essential, as otherwise air bubbles may form on the specimen and affect the result. Rigid adherence to the prescribed rate of heating is absolutely essential for reproducibility of results. 10.3 In Fig. 1 {b), a thin amalgamated copperplate placed on the bottom lower plate of the ring holder will prevent the material from sticking, thereby saving considerable time and trouble in cleaning. 10.4 Owing to possible danger to health if mercury is handled carelessly, the following rules should be observed at all times: 10.4.1 Store the mercury in a closed jug in a cool place, 10.4.2 Strictly avoid spilling any mercury, 10.4.3 Remove mercury vapors by working under a suitable hood with good ventilation, and 10.4.4 Keep amalgamated brass plates and other appa ratus at no higher than normal room temperature. 11. Precision 11.1Results should not differ from the mean by more than the following amounts: Softening Point Repeatability. Same Operator and Apparatus Reproducibility, Different Operators and Apparatus Below 80*C (176*F) Above 80*C (I76*F) A The precision of this test method is under continued study and values for repeatability and reproducibility will be inserted in the above table when this work has been completed. The American Society for Testing ancf Materials takes no position respecting the validity ofany patent rights assertedin connection with any Kern mentioned in this standard. Users of this standardare expressly advised that determination at the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standardIs subject to revision at anytime by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Yourcomments are invitedeither forrevision 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 feet that your comments have not received a fair bearing you should make your views known to the ASTM Committee on Standards, 1916 flace Sr., Philadelphia, PA 19103. 531 mm DUP050296095 Designation: E 852 - 82 (Reapproved 1987)*' Standard Test Methods for C4-C13 Plasticizer Grade Alcohols1 This standard is issued under the fixed designation 852; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year orlast 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. a No t e--Editorial changes were incorporated throughout in August 1987. 1. Scope 1.1 These test methods cover the chemical and physical analysis of liquid C, to Cl3 alcohols that are manufactured for further processing into plasticizers. The test methods appear in the following order Procedure '' Reagenls...................................................... .............. ................ Specific Gravity........................................................................... Acidiiy................................................. .................................. Color............................................. ............................................. Water......................................................................................... Sulfuric Acid Color..................................................................... Sec.tions 4 5to8 9 to 12 13 to 16 17 to 20 21 to 26 , NOTE l--Test Methods for carbonyl content and hydroxyl number will be added upon successful completion of interlaboratory studies. 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 891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals12 D 1193 Specification for Reagent Water3 4 * D1209 Test Method for Color ofClear Liquids (Platinum- Cobalt Scale)4 D 1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lac quer, and Related Products3 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals2 E 203 Test Method for Water Using Karl Fischer Reagent2 3. Significance and Use 3.1 These test methods may be used with specifications for C4 to C13 alcohols to determine if the quality of the alcohol is suitable for use in making plasticizers. 1 These lest methods arc under the jurisdiction of ASTM Committee E-l 5 on Industrial Chemicals and are the direct responsibility ofSubcommiltee Ei 5.53 on Alcohols and Polyalcohols. Current edition approved March 3, 1932. Published April 1982. 2 Annua/ Book ofASTM Standards, Vol 15.05. * Annua! Book ofASTM Standards, Vo! 11.01. 4 Annua/ Book ofASTM Standards, Vol 06.01. * Annual Book ofASTM Standards, Vol 06.03. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening the accuracy of the determination. 4.2 Unless otherwise indicated, references to water shall be understoodjo mean Type II or III reagent water con forming to Specification D 1193. SPECIFIC GRAVITY 5. Summary of Test Method 5.1 The specific gravity of the sample is determined at 20/20C using the hydrometer method. 6. Procedure 6.1 Determine the specific gravity of the sample at 20/ 20C using the hydrometer method described in Test Methods D 891. The determination shall be made at 20.0 o.i-c. No t e 2--For precise work the hydrometer must be calibrated at 20"C using liquids of known specific gravities at 20"C. This correction is generally less than 0.001 and may be ignored for most work. Hydrome ters are normally calibrated at 60'F or 15.56"C. 7. Report 7.1 Report the specific gravity at 20/20C to the nearest 0.0002 unit. Duplicate runs that agree within 0.0004 unit are acceptable for averaging (95 % confidence level) (see Note 3). 8. Precision and Bias 8.1 Precisian--The following criteria should be used for judging the acceptability of the results (Note 3): 8.1.1 Repeatability (Single Analyst)--The standard devia tion of results (each the average of duplicates), obtained by the same analyst on different days, has been estimated to be 0.00024 unit at 25 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 0.0007 unit. * "Reagent Chemicals. American Chemical Society Specifications." Am. Chemical Soc., Washington. DC. For suggestions on the testing of reagenls not listed by the American Chemical Society, see "Reagent Chemicals and Standards,1' by Joseph Rosin, D. Van Nostrand Co., Inc.. New York. NY, and the "United States Pharmacopeia." 532 $ DUP050296096 852 ! 8.1.2 Reproducibility (Multilaboratory)--The standard {deviation of results (each the average of duplicates), obtained |jy analysts in different laboratories, has been estimated to be jb.00066 unit at 4 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than ;Oj 0024 unit. $.1.3 Bias---The bias of this test method has not been {determined, the accuracy obtained will depend largely upon >ggthe care exercised in calibrating the hydrometer used and in maintaining the temperature of the sample at 20C. J; `No t e 3--The precision estimates1 are based on an interlaboratory Ipudy7 on one sample each Of n-butanoi, /i-hexanol, 2-ethylhexanoI, JjBE decanol. and tridecanol whose pacific gravities ranged from 0.8105 to 0.8370. A total of six laboratories cooperated in the study in which El. duplicate determinations were performed on each of two days. Practice rapf R 180 was used in developing these precision estimates. ACIDITY , Summary of Test Method , 9.1 Tee total acidity of the sample is measured by titrating Ihe sample with standard caustic solution ,to the phenol- hthalein .end point, using isopropanol as .the solvent Any idic moiety that-will titrate under these conditions.,will be eluded in the total acidity value which is expressed as ercent acetic acid. jiff. Procedure ' 10.1 Determine the total acidity of the sample using Test ethod D 1613 and isopropanol as the-solvent. |j{. Report `1, 11.1 Report the- acidity as acetic acid to the nearest 1.0001 %. Duplicate determinations that agree within 6.0014 % absolute are acceptable for averaging (95 % confi- pnee level)(see Note 4). . ... p-Precision.and Bias . 12.1 Precision--The following criteria should be used for hdging the acceptability of.results (see Note. 4): ,12.1.1. Repeatability (Single Analystb-The standard devi|tion of results (each the average of duplicates), obtained by he same analyst on different days, has been estimated to be lji3034 % absolute at 30 fff. l\vo such averages should be. psidered suspect (95 % confidence level) if they differ by core than 0.0010. % absolute. 12.1.2 Reproducibility (Multilaboratory)--The standard deviation of results (each the average of duplicates), obtained |y analysts in different laboratories, has been estimated to be 0.00146 % absolute at 5 df. Two such averages should be ponsidered suspect (95 % confidence level) if they differ by nore than 0.0053 % absolute. 12.2 Bias--The bias of this test method has not been determined. : No t e 4--The precision estimates are based on an interiaboratory study6 on one sample each of n-butanol, n-hexanol, 2-ethylhexanol, ||fecanol, and tridecanol whose acidities ranged from 0.00011 to 10.0002 % by weight as acetic acid. A total of six laboratories cooperated ` i the study in which duplicate determinations were performed on each 7 Supporting daia arc available from ASTM Headquarters. Request RR: |E!5-!031. of two days. Practice E 180 was used in developing these precision estimates. COLOR 13. Summary of Test Method 13.1 The color of the sample is visually determined by comparing the sample in a Nessler tube with a series of platinum - cobalt standards in matching Nessler tubes. 14. Procedure 14.1 Determine the color of the sample as described in Test Method D 1209. 15. Report 15.1 Report the color of the sample to the nearest 1 platinum - cobalt unit. Duplicates that agree within 3 units are acceptable for averaging (95 % confidence level) (see Note 5). 16. Precision and Bias 16.1 Precision--The following criteria should be used for judging the acceptability of results (see Note 5): 16.1.1 Repeatability (Single Analyst)--The standard devi ation of results (each the average of duplicates), obtained by the same analyst on different days, has been estimated to be 0.37 unit at 30 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 1 unit. 16.1.2 Reproducibility (Multilaboratory)--The standard deviation of results (each the average of duplicates), obtained by analysts in different laboratories, has been estimated to be 2.15 units at 5 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 8 units. 16.2 Bias--The bias, of this test method has not been determined. No t e 5--The:precision estimates are based on an.interiaboratory study7 on one sample eaph of -butanol, n-hexanol, 2-ethylhexanol, decanol, and tridecanol whose color ranged from 3.8 to 7.6 platinum cobalt units. A total of six laboratories cooperated in the study in which duplicate determinations were performed on each of two days. Practice E 180 was Used in developing these precision estimates. WATER, , 17. Summary of Test Method 17.1 The Karl Fischer titrimetric method is used to determine the water content of the sample. 18. Procedure 18.1 Determine the water content of the sample using Test Method E 203. 19. Report 19.1 Report the water content to the nearest 0.01 %. Duplicate determinations that agree within 0.02 % absolute are acceptable for averaging (95 % confidence level) (see Note 6). 533 ,,.S DUP050296097 E852 20. Precision and. Bias 20.1 The Mowing criteria should be used in judging the acceptability of results (see Note 6): 20.1.1 Repeatability (Single Analyst)--The standard devi ation of results (each the average of duplicates), obtained by the same analyst on different days, has been estimated to be 0.008 % absolute at 26 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 0.02 % absolute. 20.1.2 Reproducibility (Multilaboratory)--The standard deviation of results (each the average ofduplicates), obtained by analysts in different laboratories, has been estimated to be 0.029 % absolute at 4 df. Two such averages should be con sidered suspect if they differ by more than 0.11% absolute. 20.2 Bias--The bias of this test method has not been determined. No t e 6--The precision estimates are based on an interlaboratory study* on one sample each of n-butanol, n-hexanol, 2-etbylhexanol, decanol, Jhnd tridecanol whose water content ranged from 0.094 to 0.110% by weight. A total of six laboratories cooperated in the study in which duplicate determinations were performed on each of two days. Practice E 180 was used in developing these precision estimates. SULFURIC ACID COLOR 21. Summary of Test Method 21.1 This procedure covers-the determination of color developed in a sample when heated with concentrated sulfuric acid. It is applicable to those alcohols which are intended for conversion into plasticizer esters and are thus required to have low contents of color-developing species. 22. Reagents 22.1 Sulfuric Acid (sp gr 1.84)--Fresh, colorless concen trated sulfuric acid (H2S04). 23. Apparatus 23.1 Automatic Buret, 10-mL capacity, fitted with a TFE-fluorocarbon stopcock plug. 23.2 Lead Ring--Bend a piece of Vs-in. (10-mm) diam eter by 7.75-in. (200-mm) lead rod into a ring suitable for placing over the neck of a 250-mL Erlenmeyer flask as a weight. 23.3 Steam Bath, 98 2'C, containing enough water to cover the liquid in the sample flasks. 23.4 Because of the extreme sensitivity of this test to carbonizable materials, it is essential to clean all glassware in dichromate cleaning solution, rinse in tap water followed by methanol, and thoroughly air dry. 24. Procedure No t e 7--See 23.4. 24.1 Add 100 mL of sample to each of two clean 250-mL Erlenmeyer flasks. From an automatic buret' dropwise 8.0 mL of H2S04. Swirl the contents of each'lki constantly by hand during the addition of the acid. imperative that the swirling be constant and vigorous. 24.2 Place a lead ring around each flask and cover tffi flask with a clean, dry 100-mL beaker. Place the flasks:/' steam bath at 98 2C for a period of 60 1 min. 1 24.3 Remove the flasks from the bath and immedil place in cold tap water to cool the contents to approxima 70*C. 24.4 Determine the color of the solution as described Test Method D 1209. 25. Report -A- 25.1 Report the color of the solution to the nehresr platinum - cobalt unit. Duplicate determinations that agre within the amount shown in Table 1 are acceptable-fd' averaging (95 % confidence level) (see Note 8). 26. Precision and Bias 26.1 Precision--The following criteria should be use judging the acceptability of results (see Note 8): " 4 <" 26.1.1 Repeatability (Single Analyst)--The standard diSyi ation of results (each the average of duplicates), obtained ' the same analyst on different days, has been estimated tq! the amount shown in Table 1. Two such averages should, considered suspect (95 % confidence level) if they differ' more than the amount shown in Table 1. r, 26.1.2 Reproducibility (Multilaboratory)--The standtujd', deviation ofresults (each the average of duplicates), obtains by analysts in different laboratories, has been estimated to 1 the amount shown in Table 1. Two such averages should 1 considered suspect (95 % confidence level) if they differ' more than the amount shown in Table 1. 26.2 Bias--The bias of this test method has not yet 1 determined. No t e 8--The precision estimates are based on an interiabeiag study* on one sample each of n-butanol, re-hexanol, 2-ethylhex.tn decanol, and tridccanol whose sulfuric acid colors ranged from S&stSfr 74.1 platinum - cobalt units. A total of six laboratories cooperatedlitf the study in which duplicate determinations were performed on each o" two days. Practice E 180 was used in developing these piecisi3_ estimates. 0 to tO Pt-Co 70 Pt-Co TABLE 1 Precision for Sulfuric Acid Color Test Platinum - Cobalt Units Duplicates Repeatability Checking Limits 4 10 Degrees of Freedom Range, 95 X Confidence Level 0.6 2 4.8 17 Reproducibility DDeegcrreeeessooff Rcoannfgidej.n0e!e>* - . Freedom Level )jW 2.1 8 17.9 68 534 lit. Sills DUP050296098 # E 852 The American Society for Testing and Materials lakes ho position respecting the validity of any patent righto asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, eitherreapproved or withdrawn. Yourcomments areinvitedeither for revision ofthis standard or foradditional standards aid 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. 535 DUP050296099 AROMATIC HYDROCARBONS AND RELATED CHEMICALS DUP050296100 Last ASTIM Designation: D 362 - 84 Standard Specification for industrial Grade Toluene specification covers industrial grade toluene. 'erly under the jurisdiction of Committee D-16 on Aromatic Hydrocarbons and Related Chemicals, this specification continued in 1991. .ail 539 DUP050296101 Designation: D 835 - 90 Standard Specification for Refined Benzene-4851,2 This standard is issued under the fixed designation D 835; 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 (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers a nitration grade of benzene known as refined benzene 485. 1.2 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials utiiized in this specification. 2. Referenced Documents 2.1 ASTM Standards: D847 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons13 * D848 Text Method for Acid Wash Color of Industrial Aromatic Hydrocarbons3 D849 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons3 D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D852 Test Method for Solidification Point of Benzene3 D853 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons3 D 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 D 3437 Practice for Sampling and Handling Liquid Cyclic Products3 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 1 This specification is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and la the direct responsibility of Subcommittee D 16.0A on BTX, Cyclohexane, and Thar Derivatives. Current edition approved May 25, 1990. Published July 1990. Originally published as D 835 - 45 T. Last previous edition D 835 - 85. 3 This material was formerly known as "nitration grade benzene." 3 Annual Book qfASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 05.03. 2.2 Federal Specification: PPP-C-2020 Packaging of Chemicals, Liquid, Dry, and Paste5 2.3 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12006 3. Properties 3.1 Refined benzene 485 shall conform to the following requirements: Property ASTM Test Specification Method Acid wash color, max pass with 2 Acidity none detected Copper corrosion pass<lA or IB) Hydrogen sulfide (H2S) and sulfur dioxide (S02) none detected Appearance A Color, Pt/Co scale, max 20 Relative density, 15.56/15.56*0 0.8820 to 0.8860 or Density, 20*C, g/cro3 Distillation range including the temperature 80.1*C at 760 mm Hg pressure, max, *C Solidification point, anhydrous basis, rain, *C 0.8780 to 0.8820 1.0 4.85 D 848 D 847 D 849 D853 D 1209 D3505 or D4052 D 850 D 852 A Clear liquid free ofsediment and haze when observed at 18.3 to 25.6C (65 to 78*F). 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 5. Packaging and Labeling for U.S. Government Procure ments 5.1 United States Government procurements shall be packaged and labeled in accordance with the applicable paragraphs of Fed. Spec. PPP-C-2020. 5 Available from Standardization Documents Order Desk, Bldg. 4 Section D. 700 Robbins Avc., Philadelphia, PA 19111-5094, Attn; NPODS. 6 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402, The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, eitherreapprovedor withdrawn, yourcomments are invited either forrevision of thisstandardortoradditional standards and should be addressed to ASTM Headquarters. Your comments will receive oerefui consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair heating you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. SPWIPIBPRPR? 540 DUP050296102 Last ASTM Designation: D 836 - 84 Standard Specification for Industrial Grade Benzene Sis specification covers industrial grade benzene. Jfmerly under the jurisdiction of Committee D-16 on Aromatic Hydrocarbons and Related Chemicals, this specification Ijscontinued in 1991. 541 --;----------------- DUP050296103 # Designation: D 841 - 90 Standard Specification for Nitration Grade toluene1'2 This slandard is issued under the fixed designation D 841; the number immediately following the designation indicates the ycat of original adoption or, in the case ofrevision, the year oflost revision. A number in parentheses indicates the year pf last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovaL 1. Scope 1.1 This specification covers nitration grade toluene. 1.2 Consult OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this specification. 2.2 Federal Specification? PPP-2020 Packaging of Chemicals, Liquid, Dry, and Paste 2.3 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12006 2. Referenced Documents 2.1 ASTM Standards: D847 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons* D848 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons 5 D849 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons3 D 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D853 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons3 D 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 D2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography3 D 3437 Practice for Sampling and Handling Liquid CyclicProducts3 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 1 This specification is under the jurisdiction of ASTM Committee D-I6 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D 16.0A on BTX, Cyclohexane, and Their Derivatives. Current edition approved May 25. 1990. Published July 1990. Originally published as D 841 - 45 T. Previous edition D 841 - 85. 2 This material was formerly known as "nitration pure toluol." 5 Annual Book ofASTM Standards, Vol 06.05. 4 Annual Book ofASTM Standards, Vol 05.03. 3. Properties 3.1 Nitration grade toluene shall conform to the following requirements: Property ASTM Test Specification Method Nonaromatic hydrocarbons, max, volume % 1.5 Acid wash color, max pass with 2 Acidity none detected Copper corrosion -- pass (1A or IB) Hydrogen sulfide (H2S) and sulfur dioxide (S02) none detected Appearance Color, Pt/Co scale, max 20 Relative density, 15.56/I5.56CC 0.869 to 0.873 or Density, 20*C, g/cm* Distillation range including the temperature 110.6`C at 760 mm Hg pressure, max, C 0.865 to 0.870 1.0 D 2360 D 848 D 847 D849 D 853 D 1209 D3505 or D4052 D850 A Dear liquid free ofsediment and haze when observed at 18.3 to 25.6C (65 to 78F). 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 5. Packaging and Labeling for US. Government Procure ments 5.1 United States Government procurements shall be packaged and labeled in accordance with the applicable paragraphs of Fed. Spec. PPP-C-2020. 5 Available from Standardization Documents Order Desk, Bldg. 4 Section D. 700 Robbins Avc., Philadelphia, PA 1911 1-5094, Attn: NPODS. A Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Hem mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you fee/ 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. 542 Sit DUP050296104 Designation: D 843 - 90 Standard Specification for Nitration Grade Xylene1,2 This standard is issued under the fixed designation D 843; 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 (0 indicates an editorial change since the last revision or reapproval. pe '{phis specification covers nitration grade xylene. 'Consult OSHA regulations and supplier's Material ata Sheets for all materials used in this specification. ferenced Documents yiSTM Standards: 1 Test Method for Acidity of Benzene, Toluene, lenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons3 8 Test Method for Acid Wash Color of Industrial bmatic Hydrocarbons3 9 Test Method for Copper Corrosion of Industrial matic Hydrocarbons3 '0 Test Method of Distillation of Industrial Aromatic hydrocarbons and Related Materials3 "3 Test Method for Hydrogen Sulfide and Sulfur oxide Content (Qualitative) of Industrial Aromatic ydrocarbons3 09 Test Method for Color ofClear Liquids (Platinum` halt Scale)3 "60 Test Method for Trace Impurities in Monocyclic --matic Hydrocarbons by Gas Chromatography3 -,37 Practice for Sampling and Handling Liquid Cyclic roducts3 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meters4 2.2 Other Document: OSHA Regulations 29 CFR, paragraphs 1910.1000 and 1910.12003 3. Properties 3.1 Nitration grade xylene shall conform to the following requirements: . Property ASTM Test Specification Method Nonaromatic hydrocarbons, max, volume % 4.0 Acid wash color, max pass with 6 Acidity none detected Copper corrosion pass (1A or IB) Hydrogen sulfide (H2S) and sulfur dioxide (S02) none detected Appearance A Color, Pt/Co scale; max 20 Relative density, 15.56/15.56 *C1 * 0.865 to 0.877 or Density, 20*C, g/cm3 Distillation range at 760 mm Hg pressure. max, *C Initial distillation temperature, min. C Dry point, max, *C 0.862 to 0.872 5 137 143 D2360 D848 D847 D849 D853 D1209 D 3505 or D4052 D850 D850 D850 A Clear liquid free of sediment and haze when observed at 18.3 to25.6*C(65 to 789F). is specification j$ under the jurisdiction of ASTM Committee D-16 on ;-'c Hydrocarbons and Related Chemicals and is the direct responsibility of immittee D16.0A on BTX, Cyclohexane, and Their Derivatives, at edition approved May 25, 1990. Published July 1990. Originally 1 as D 843- 45 T. Last previous edition D 843- 80 (1985). is material was formerly known as "3* xylol." rmual Book ofASTM Standards, Vol 06.03. 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 4 Annual Book ofASTM Standards. Vol 05.03. * Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 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 suoh rights, are entirely their own responsibility. This standard is subjectto revision at any time by the responsible technical committee and must be reviewed every We years and if not revised, either reapproved or withdrawn. Yourcomments 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, ft you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 543 DUP050296105 Last ASTM Designation: D 846 - 84 Standard Specification for Ten-Degree Xylene This specification covers ten-degree xylene. Formerly under the jurisdiction of Committee D-16 on Aromatic Hydrocarbons and Related Chemicals, this specification was discontinued in 1991. A IsrO' 544 DUP050296106 Designation: D 847 - 91 Standard Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons1 This standard is issued under the fixed designation 0 847; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year ofiast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 5255 ofFederal Test Method Standard No. 141A andfor listing in the Dob Index ofSpecifications and Standards. This test method is intended for the detection of } and for the quantitative determination of acidity of ne, toluene, xylenes, solvent naphthas, and similar , ['-aromatic hydrocarbons. This standard does not purport to address all of the problems, if any. associated with its use. It is the Ability ofthe user ofthis standard to establish approfsafety and health practices and determine the applicaof regulatory limitations prior to use. For specific statements see Section 8. "erenced Documents. ASTM Standards: -193 Specification for Reagent Water2 437 Practice for Sampling and Handling Liquid Cyclic roducts3 * Other Documents: IHA Regulations, 29 CFR, Paragraphs 1910.1000 and 910.12004 erminology Definitions: ,1 acidity--Has number of milligrams of sodium hyde consumed when 100 mL of the specimen are titrated jr the conditions prescribed in this test method. ,2 acid reaction--a characteristic of materials pro ng the acid-color of the indicator used under the itions prescribed in this test method. 1.3 alkaline or basic reaction--a characteristic of the rials producing the alkali-color of the indicator used r the conditions prescribed in this test method. ununary of Test Method -:1 The acidity of aromatic hydrocarbons is detected and lined quantitatively using a sodium hydroxide titra- and a color change in a phenolphthalein indicator. This test method is under the jurisdiction of ASTM Committee D-16 on atic Hydrocarbons and Related Chemicals and is the direct responsibility of "mittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane and Their iVatives. rent edition approved Oct, 15, 1991. Published December 1991. Originally 'shed as D 847 - 45 T. Last previous edition D 847 - 87. Z3-Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Voi 06.03. 4 Available from Superintendent of Documents, U.S. Government Printing , Washington, DC 20402. 5. Significance and Use 5.1 This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in development or research work on industrial aromatic hydro carbons and related materials. This test method gives an indication of residual acidity and is a measure of the quality ofthe finished product. It is an indication of the tendency of the product to corrode equipment. 6. Apparatus 6.1 Graduate, 100-mL.5 6.2 Bottle, 500-mL glass-stoppered.5 ' 6.3 Buret, 10-mL, graduated in 0.05-mL subdivisions. 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.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 7.2 Phenolphthalein Indicator Solution--Dissolve 0.5 g of phenolphthalein in 100 mL of cp ethyl alcohol (95 %). Add 0.01 N NaOH solution cautiously until a faint pink color appears; then just remove the color with a drop or two of 0.01 N acid. 7.3 Sodium Hydroxide. Standard Solution (0.1 N). 7.4 Sodium Hydroxide, Standard Solution (0.01 N). 7.5 Sulfuric Acid, Standard (0.01 N). 7.6 Purity of Water. Distilled Water, Neutral--Boil vigor ously for 30 min, 1 to 2 L of distilled water conforming to Type III of Specification D 1193. Insert a stopper carrying a guard tube of soda lime. Rinse a 200-mL flask with this distilled water, add a 100-mL portion, and titrate in a closed system with 0.01 N NaOH solution: or heat to boiling and titrate immediately, taking care that the temperature does not fall below 80C during the titration. If more than 1 drop (0.05 mL) of 0.01 N NaOH solution is required to obtain an s Borosilicate glass or the equivalent has been found satisfactory for this purpose. 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 ihe "United States Pharmacopeia.** 545 DUP050296107 D 847 end point with phenolphthalein, adjust the pH of the water to be used by adding the calculated amount of NaOH solution. Repeat the blank titration, and readjust if necessary until the blank titration on 100 mL of the distilled water is 1 drop (0.05 mL) or less of the 0.01 N NaOH solution. The distilled water now will be neutral or very slightly add to the phenolphthalein indicator. 8. Hazards 8.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 8.2 Tests for acidity are not applicable in the presence of contaminating addic or alkaline gases, soaps, salts, or other compounds derived from the atmosphere or apparatus. The container holding the specimen, and the apparatus, water, indicator, and other materials used in the test shall be chosen so that?`-they themselves shall not appreciably affect the results. Since new corks used in specimen bottles often are bleached with oxalic acid, it is advisable to rinse them thoroughly and check them for neutrality with the indicator used in the test. Glassware shall be of add-resistant and alkali-resistant glass4 and shall be rinsed with neutral distilled water before use. The room in which the test is performed shall be chosen so as to prevent undue contamination by carbon dioxide, ammonia, or other interfering substances that may be present in the atmosphere. 8.3 The distilled water used in the test shall not alter the composition ofthe specimen nor otherwise interfere with the purpose of the work. Although inert impurities often may be neglected, care must be exercised to correct for impurities or to eliminate them entirely if they are likely to interfere. When the distilled water does not show an acid or alkaline reaction, it may be used without further adjustment to neutrality. However, if the water shows-an add or alkaline reaction, it shall be brought to a persistent pink end point before use by titration with standard 0.01 N NaOH solution (see 7.5) or standard 0.01 -V H2S04, respectively.9 9. Sampling 9.1Sampling should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regula tions. Refer to Practice D 3437 for proper sampling and handling of materials analyzed by this test method. 10. Procedure 10.1 Measure out 100 mL of the sample into the. 1 bottle. Add 100 mL of neutral distilled water (see 7~2 jj. 8.3) and 2 drops of phenolphthalein indicator saintiiSa Stopper and shake thoroughly. Without separating the ldvslr titrate the acidity, ifany, with standard 0.1 A NaOH solum: to the first persistent shade of pink, while shaking jtfS oughly. jnf 10.2 If more than 2 drops (0.10 mL) of 0.1 N XaSS solution is required to produce a persistent pink end pqj discard the results of the test. While taking precaution avoid contamination from the apparatus and atmnsi__ proceed as follows: Rinse the 100-mL graduated cylirderlu the 500-mL bottle and glass stopper with neutral disuila, water. To the bottle, add 100 mL ofthe sample and lOfffnt of neutral distilled water. Add 2 drops of phenolplu indicator solution, and shake vigorously for 10 s. Bn temperature to between 15 and 18.5"C (60 and 65T idl drop of 0.1 N NaOH solution, stopper, and shake vij. -I for 10 s. Repeat the addition of 1 drop of NaOH s stoppering, and shaking for 10 s, until a sharp pink ei 1 pomffl is secured. Repeat this procedure on a blank run wi Il H mL of the neutral distilled water. v 11. Interpretation of Results and Calculation 11.1 Unless otherwise indicated in the applicable ,| cations, the test results shall be interpreted as folldVwt?*., 11.1.1 A specimen shall be said to contain norfree ffla that is show no evidence of acidity, if 2 drops or les'slof/):} NaQH solution produces a persistent pink end point in/S test bottle. ;..*. J* 11.1.2 When more than 2 drops (0.10 mL) ijsf .OJjjjj NaOH solution is required to produce a persistent pinker point in the test bottle, the acidity shall be report a . ii tei>i's| of milligrams of NaOH required for 100 mL of specimt and shall be calculated as follows: Acidity, mg NaOH per 100 mL = 4 (A -- B) where: A =0.1 N NaOH solution required for titration sample, mL, and B =0.il N NaOH solution required for titration ofprtjj blank, mL. 12. Precision and Bias 12.1 In the case of pass/fail data no generally iiw method for determining precision is currently avails1' Ttte American Society for Testing andMaterials tokos no position respecting the validity of anypatent rights assertedin connection with any Item mentioned in this standard. Users of this standard an 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 orwithdrawn. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fed that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 79703. 546 DUP050296108 D Designation: D 848 - 81 (Reapproved 1989) Standard Test Method for Acid Wash Color of industrial Aromatic Hydrocarbons1 This standard is issued undo* the fixed designation D 848; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (r> indicates an editorial change since the last revision or reapproval. This lest method has been approved/or use by agencies ofthe Department of Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. *' Nans--Editorial changes were made throughout in November 1989. pe This test method covets the determination ofthe acid color of benzene, toluene, xylenes, refined solvent thas,-and similar industrial aromatic hydrocarbons. ' Thisstandard may involve hazardous materials, oper as,, and equipment. This standard does not purport to ress all ofthe safetyproblems associated with its use. It is tsponsibility of the.user of this standard to establish vpriaie safety and health practices and determine the Ability of regulatory Imitations prior to use. For jjc hazard statements, see Section 7 and Note 1. eferenced Documents ASTM Standards: 1193 Specification for Reagent Water2 3437 Practice for Sampling and Handling Liquid Cyclic `Products3 }2 OUter Document: ''HA Regulations. 29 CFR, paragraphs 1910.1000 and 1910.12004 erminology 1 Definition: .1.1 acid wash color--the color developed in the sepal acid when a sample is agitated with sulfuric acid under conditions prescribed in this test method. ^Significance and Use 4,1, This test method is suitable for setting specifications the materials referenced in i.l. It may also be used as an mal quality control tool and in development or research rk. `Tz The color developed in the acid layer gives an 'cation of impurities which if sulfonated would cause the .terial to be discolored. 1 This test method is under the jurisdiction of ASTM Committee D-16 on malic Hydrocarbons and Related Chemicals and is the direct responsibility of .bcommittee D16.0A on Benzene. Toluene, Xylenes, Cyclohexane, and Their rivatives. Current edition approved April 24, 1981. Published August 1981. Originally blisbed as D 848 - 45. Last previous edition D 848 - 62 (1977). ' 2Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Voi 06.03. "Available from Superintendent of Documents, U.S. Government Priming .Dice, Washington, DC 20402. 5. Apparatus 5.1 Containers for Color Standards--Clear and unblem ished, clean, French square, flint-glass, flat-bottom, glassstoppered, 1-oz capacity bottles holding 31 to 33 mL when filled to the neck or 25 mL/giass stoppered graduates.5 The bottles shall be numbered consecutively from 0 to 14. 5.2 Test Containers--Containers exactly like those de scribed in 5.1 except that each French square bottle shall be marked by etching to show when the bottle contains the volume of 7 and 28 mL, respectively. The graduate shall be marked at 28 mL only. Colored crayons and similar markers shall not be used for marking the bottles. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used provided it is first ascertained that the reagent is 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 distilled water, Type I or II as described in Specification D 1193. 6.3 Cobalt Chloride (Coa2-6H20). 6.4 Ferric Chloride (FeCl3-6H20). 6.5 Hydrochloric Acid (1+39)--Mix 25 mL of hydro chloric acid (31 weight % HC1) with 975 mL of water. 6.6 Potassium Chromate (K2Cr04). 6.7 Potassium Dichromate (K2Cr207). 6.8 Sulfuric Acid (96 0.5 weight % H2S04). 6.9 Sulfuric Acid (78 0.5 weight % H2S04). 7. Hazards 7.1 Consult current OSHA regulations and supplier's Material Safety'Data Sheets for all materials used in this test method. 7.2 When handling strong acids or acid cleaning solu- 5 Pyrex No. 2982 or Kimax No. 20039-P graduates, available from laboratory suppliers, have been found suitable for this purpose. 6 "Reagent Chemicals, American Chemical Society Specifications,*' Am. Chem. Soc., Washington. DC. For suggestions on the testing of reagents not listed by ihe American Chemical Society, see "Reagent Chemicals and Standards." by Joseph Rosin, D. Van Nostrand Co.. lac.. New York. NY, and the "United States Pharmacopeia." 547 DUP050296109 tions, proper personnel protective equipment should be worn. 8. Sampling 8.1 Sampling of materials to be tested by this test method should follow safe rules in order to adhere to all safety pre cautions as outlined in current OSHA regulations. Refer to Practice D 3437 for proper sampling and handling of aro matic hydrocarbons analyzed by this test method. 9. Cleaning of Containers 9.1 Clean the containers (Section 5) with a warm chromic acid cleaning solution, rinse with tap water followed by distilled water, and dry in an oven at 105C for 1 h. Likewise, clean all other glassware used in this test method. 10. Preparation of Reference Color Standards 10.1 Stock Solutions--Prepare the following basic reagent solutions for use in preparing the reference color standards: 10.1.1 Solution A--Dissolve 59.50 g of Co C12-6H20 in HQ (1+39) and make up to 1 L in a volumetric flask with HQ (1+39). 10.1.2 Solution B--Dissolve 45.054 g of FeCl3-6H20 in HCI (1 +39) and make up to 1 L in a volumetric flask with HCf(l + 39). 10.1.3 Solution C--Mix 3'/2 volumes of Solution A with 36'h volumes of Solution B and dilute with 90 volumes of water. 10.1.4 Solution D--Mix 3 'h volumes of Solution A with 36 \h volumes of Solution B. 10.1.5 Solution E--Prepare an aqueous solution of K2Cr04 saturated at 21C. 10.1.6 Solution F--Prepare an aqueous solution of K.2Cr267 saturated at 21"C and dilute with an equal volume of water. 10.2 Prepare reference color standard solutions having the following compositions and numbered from 0 to 14: No. 0--Distilled water. No. 1--J volume ofSolution C plus > volume of water. No. 2--5 '/2 volumes of Solution C plus 2 volumes of water. No. 3--Solution C. No. 4--L volume of Solution D plus 1 volume of water. No. 5--5>/z volumes ofSolution D plus 2 volumes of water. No. 6--Solution D. No. 7--5 volumes of Solution E plus 2 volumes of water. No. 8--Solution E. No. 9--7 volumes of Solution E plus 'h volume of Solution F. No. 10--6!/2 volumes of Solution E plus 1 volume of Solution F. No. 11--5-/2 volumes of Solution E plus 2 volumes ofSolution F. No. 12--1 volume of Solution E plus 1 volume of Solution F. No. 13--2 volumes of Solution E plus 5 volumes of Solution F. No. 14--Solution F. 10.3 Rinse the No. 0 container (5.1) and its glass stopper three times with water, fill with water, and stopper. Rinse the No. I container and its stopper three times with reference color standard solution No. 1 (Section 10.2), fill with this solution, and stopper. In this way, prepare, the set of containers of color standards from 0 through 14 having the compositions shown for the corresponding color solution standards in 10.2. When filling the French square bottles, leave Vi in. (6 mm) of vapor space below the neck of the bottle. Seal each container with paraffin to prevent loss by evaporation or seepage. 11. Procedure 11.1 Rinse a test container (5.2) twice with acid ofvtl strength specified in Table 1 for the type of sample tested (Note 1). Drain the rinsings and fill with the acid i the 7-mL mark. Add sufficient sample to bring the y volume to the 28-mL mark (Note 2). Insert the stopper " a finger over the stopper, and give vigorous shakes ' stroke of 5 to 10 in., shaking for a total of 150 cycles ovb period of 40 to 50 s, that is at a rate of 3 to 3.75 cycles/gt No t e 1--Caution: Concentrated sulfuric acid will cause seyjjgf on contact with the skin. As a precaution the test container wrapped in a towel or enclosed in a plastic bag during the s period. i No t e 2--If the room temperature is above 8ST, maintain t sample, and reference color standards at a temperature between 85F (25 and 29`C) through the test, and insulate the test contain)!# some convenient way, such as wrapping with a doth, during the slufcf period. 11.2 Allow the container to stand, protected from dip sunlight, for the period of time shown in Table l. Witi further delay, invert the coirtainer gently once or twicevf obtain a uniform color in the acid layer, and compai^C color ofthe acid layer with that ofthe standards (JG.'j). Ma ' the comparison against a white background or agSlS daylight, using transmitted light (Note 3). When rest!-" samples in Group 1 (Table 1), observe the colorof tifllf layer as well as that of the acid layer. No t e 3--Agreement of results may be improved by using i? comparator of a suitable type for observing the color of the acid lav comparison with the reference standard color solution. 11.3 Designate the color of the add layer by the njinf* of the nearest matching standard, following the nuiribfcji||p a plus or minus sign if the sample is darker oi lig respectively, than the standard. Disregard any diffetera hue and determine only whether the color ofthe acid lay" darker or lighter than the color of the reference standlarid1 which the sample most nearly corresponds. If the hut.off acid color is different from the hue of the reference icol standard, record the color number followed by (X).`- \ "No. 4 - (X)" means that the acid wash test color is sli' lighter than No. 4 color standard and that the hue pft 4 color standard is not the same as the hue of the acidI 1laj 12. Interpretation of Results tiijjj 12.1 Report Group 1 samples (Table 1) as passing the) Group 1 TABLE 1 Acid Strengths and Standing Times Sample Acid Strength, % Standing. Time^ mh J Benzene, aB ASTM grades Toluene, all ASTM grades Xylene, nitration grade Xylene, 5* Xylene, 10 Any other more highly refined products 96 Group 2 Group 3 Xylene, Industrial grade Refined solvent naphtha HMIash solvent Heavy solvent naphtha 96 78 s 548 JflHni DUP050296110 D 848 * ben the oil layer shows no change in color and when |d layer is not darker than the specified color standard, lijiness or haze in the oil layer should licit be inter- as a change in color. When testing samples ofGroups 2 or 3, disregard'the pfthe oil layer and report the sample as passing the test the acid layer is not darker than the specified color -4 don and Bias f Precision data have not been established for all types iples on which this test method is used. Limited cooperative tests were conducted in 1961, principally to establish equality with the previously used shaking proce dure. Precision estimates taken from these data are as follows: Avenge Acid Wash Color Benzene 1.4 6.1 Repeatability Degrees of Freedom 95 % Repeat' ability If 0.75 12 1.85 Xylene 4.7 12 10.2 12 0.40 1.14 Reproducibility Degrees of Freedom 95% Repro ducibility 9 2.34 10 4.47 10 1.39 10 3.52 7Jie American Society for Testing aixl 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 am expressly advised that determination ot the validity of any such patent rights, and the risk ot Infringement of aueft rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are ini/ited either for revision ofthis standard pi 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, 1918 Race St., Philadelphia, PA 19103. 549 i'fe DUP050296111 # Designation: D 849 - 88 Standard Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons1 This standard is issued under the fixed designation D 849; 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 reapproval, a superscript epsilon {<) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies ofthe Department of Defense. 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 test method determines the corrosiveness to copper of industrial aromatic hydrocarbons. No t e 1--For a similar copper strip test applicable to other petro leum products, see Method D 130 and Test Method D 183B. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address ail 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 7. 2. Referenced Documents 2.1 ASTM Standards: D130 Method for Determination of Copper Corrosion from Petroleum Products by the Copper Strip Tarnish Test2 D1838 Test Method for Copper Strip Corrosion by Liquefied Petroleum (LP) Gases3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.20004 Copper Development Association (CDA) United States of America No. HO5 British Standard (BS) 1036: 19526 2.3 Adjunct: ASTM Copper Strip Corrosion Standards (13 photolithed aluminum strips; includes Method D 130)7 3. Summary of Test Method 3.1 A polished copper strip is immersed in 200 mL of specimen in a flask with a condenser and placed in boiling 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Refated Chemicals and is the direct responsibility of Subcommittee D 16.0A on BTX Cyclohexane and Their Derivatives. Current edition approved Sept. 30, 1988. Published December 1988. Originally published as D 849 - 145 T. last previous edition D 849 - 82. 2Annual Book ofASTM Standards, Vote 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vote 05.01 and 05.05. 4 Available from Superintendent of Documents, U.S. Government Printing Office. Washington, DC 20402. 5 Available from Copper Development Association, Inc., Greenwich Office Park 2, Box 1840, Greenwich, CT 06836. 6 Available from British Standards Institute, 2 Park St., London, England WIA/2 BS. 7 Available from ASTM Headquarters. Request PCN 12-401300-00. Names of suppliers in the United Kingdom can be obtained from the Institute of Petroleum. Two master standards are held by the IP for reference. water for 30 min. At the end of this period, the copper*' is removed and compared with the ASTM Coppci Corrosion Standards. f 4. Significance and Use 4.1 This test method is suitable for setting specificatio for use as an internal quality control tool, and for development or research work on industrial aromatic h\di carbons and related materials. It also gives an indkationi the presence of certain corrosive substances witch corrode equipment, such as acidic compounds or compounds. 5. Apparatus 5.1 Flask, 250-mL, of chemically resistant glass. bottom and vial mouth. 5.2 Glass Condenser, 30-mm, with the inside diameter the condenser tube not less than 10 mm. A cork is connect the flask with the condenser. A condenser and with ground-glass joints may also be used. 5.3 Strip Polishing Vise, to hold the copper strip fii without marring the edges. For convenient vises see Mctl.o D 130. 5.4 Water Bath, of convenient design, able to i boiling water such that the contents of the flask an. merged during the test. 6. Materials 6.1 Wash Solvent--Any volatile, sulfur-free hydr: solvent may be used provided that it shows no tarnish at ., when tested at UXTC (212F) for l h. Knock-test ; wooctane (Warning--See 7.2) is a suitable solvent a should be used in case of dispute. 6.2 Polishing Materials--Silicon carbide grit paper of varying degrees of fineness including 65-pm (240-grit) papea>. or cloth; also a supply of 105-pm (150-mesh) silicon carbide ' grain and pharmaceutical grade absorbent cotton (cotto wool). 6.3 Copper Strips--Use strips 12.5 mm (Vi in.) wide, 1.5gj to 3.0 mm ('/is to >/b in.) thick, cut 75 mm (3 in.) long from 7 smooth-surfaced, hard-tempered, cold-finished copper of 99.9+ % purity. Electrical bus-bar stock is generally suitable A." (hard-temper, cold-finished type-electrolytic tough pitch (ETP) copper conforming to Copper Development Associa- < tion (CDA), United States of America No. 110, or to British ^ Standard (BS) 1036: 1952, which have proper quality). Drill / a 3.2-mm (W-in.) hole approximately 3.2 mm (Vs in.) front one end in the center of the strip. The strips may be used . 550 DUP050296112 [Jy but should be discarded when surfaces become ied on handling. Copper wire, soft, about 150 mm (6 in.) in length. ASTM Copper Strip Corrosion Standards, consisting reductions in color of typical test strips representing ing degrees of tarnish and corrosion. The reproducare encased in plastic in the form of a plaque. !ctions for care and use are given on the reverse side of plaque and in Method D 130. ards 'Consult current OSHA regulations and supplier's _ial Safety Data Sheets for all materials used in this test bd.,, /sooctane is Extremely Flammable. Harmful if in i'Vapors may cause flash fire. Keep away from heat, and open. flame. Keep container closed. Use with *te ventilation. Avoid buildup of vapors and eliminate s flf ignition, especially non-explosion-proof elec apparatus and heaters. Avoid prolonged breathing of or spray mist. Avoid prolonged or repeated skin t. paration of Strips *Surface Preparation--Remove all surface blemishes all six sides of the strip with silicon carbide grit paper of `degrees of fineness as are needed to accomplish the ed results efficiently, finish with 65-jim (240-grit) -carbide paper or cloth, removing all marks that may een made by other grades of paper used previously, diately immerse the strip in wash solvent from which it s withdrawn for final polishing or in which it may be for future use. 2--As a practical manual polishing procedure, place a sheet of Lper on a flat surface, moisten it with wash solvent, and rub the ainst the paper with a rotary motion, protecting the strip from i with the fingers with an ashless filter paper. Alternatively, the may be prepared by use of motor-driven machines using appro- dcs of dry paper or cloth. ' Pinal Polishing--Remove a strip from the wash jt Holding it in the fingers protected with ashless filter r, polish first the ends and then the sides with the flesh silicon-carbide grains picked up from a clean glass "with a pad of absorbent cotton moistened with a drop ash solvent. Wipe vigorously with fresh pads of absorcotton and subsequently handle only with stainless-steel jss; do not touch with the fingers. Clamp in a vise and the main surfaces with silicon carbide grains on absorbent cotton. Rub in the direction ofthe long axis of the strip, carrying the stroke beyond the end of the strip before reversing the direction. Clean all metal dust from the strip by rubbing vigorously with clean pads of absorbent cotton until a fresh pad remains unsoiled. When the strip is clean immediately attach the copper wire and immerse the strip in the specimen flask. No t e 3--It is important to polish the whole surface of the strip uniformly to obtain a uniformly stained strip. If the edges show wear (surface elliptical) they will likely show more corrosion than the center. The use of a vise will facilitate uniform polishing. 9. Procedure 9.1 Fasten the 6-in. (150-mm) length of soft copper wire through the hole provided near one end of the strip, taking care not to touch the strip with the fingers after polishing. Place the strip in the flask and add 200 mL of the sample. The specimen must not contain separated water. Filter through a dry filter paper, if necessary, to remove water. Connect the flask to the vertical reflux condenser by means of a properly bored cork stopper. It is absolutely necessary that a cork, not rubber, stopper be used, in order to avoid contamination of the specimen by sulfur from rubber stoppers. The copper wire may be allowed to extend into the condenser tube for convenience in removing the strip. Completely immerse the strip which should preferably lie fiat and touch the flask only at the ends of the strip. Place the flask in the gently-boiling water bath, and immerse the flask to the liquid line of the specimen within the flask. Remove the copper strip 30 min from the time the flask was immersed in the bath. Do not touch the copper strip, but remove it by the wire that has been provided. Do not allow the strip to come in contact with separated water during any part of the test, since water causes bad local staining of the copper. If it is desired to preserve the strip for future reference, dip it immediately into white shellac or lacquer. 10. Interpretation of Results 10.1 Compare the exposed strip with the ASTM Copper Strip Corrosion Standards described in 6.5. Hold the test strip and the Standard in such a manner that light reflected from them at an angle ofapproximately 45 will be observed. Report as passing strips shown in the Slight Tarnish catagory or better (1.4 or IB); all others shall be considered failures. 11. Precision and Bias 11.1 In the case of pass/fail data, no generally accepted method for determining precision and bias is currently available. The American Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such 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 reapprovedor withdrawn. Yourcomments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace St., PNIadelphla, PA 19103. 551 DUP050296113 Designation: D 850 - 91 Standard Test Method for Distillation ot Industrial Aromatic Hydrocarbons and Related Materials1 This standard is issued under the fixed designation D 850; 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 die last revision or reapproval This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor die specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the distillation of industrial aromatic hydrocarbons and related materials of relatively narrow boiling ranges from 30 to 250"C. 1.2 The values stated in SI units are to be regarded as the standard. ` 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. For specific hazard statements, see 5.6 and Section 6. 2. Referenced Documents 2.1 ASTM Standards: D86 Method for Distillation of Petroleum Products2 D 1078 Test Method for Distillation Range of Volatile Organic Liquids2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 E 1 Specification for ASTM Thermometers3 E 133 Specification for Distillation Equipment4 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12005 3. Summary of Test Method 3.1 The distillation of industrial aromatic hydrocarbons and related materials is carried out via a carefully controlled distillation wherein temperature readings are noted for the first drop of distillate and when 5,10, and each additional 10 up to 90, and 95 % of the sample has distilled over. The temperature corresponding to the dry point is also noted. 4. Significance and Use 4.1 This test method is suitable for setting specifications. 1 This tesi method is under the-jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and 1$ the direct responsibility of Subcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved Oct. 15.1991. Published December 1991. Originally published as D 850 - 45. Last previous edition D 8S0 - 90. 2 Annual Book ofASTM Standards, Vo) 06.03. 2 Annual Book ofASTM Standards, Vols 05.03 and 14.01. 4 Annual Book ofASTM Standards. Vols 05.03 and 14.02. 5 Available from Superintendent of Documents, U.S. Coverameot Printing Office, Washington, DC 20402. for use as an interna! quality control tool, and for development or research work on industrial arotnatiq carbons and related materials. 4.2 This test method gives a broad indication of purity and can also indicate.presence of excessive It will not differentiate between products of similar range. 5. Apparatus * 5.1 Flash*--A standard 200-mL side-tube, heatglass distillation flask as shown in Fig. 1, conforming following dimensions: Diameter of bulb, outside, mm Diameter of neck, inride, mm Height of flask, outside, mm Vertical distance front bottom of bulb outside to bottom of vapor-tube opening in neck, mm Length of side tube, mm Diameter ofside tube, outside, mm Angle of side tube with vertical axis of bulb and neck,' 76 t.. 21 i 179 .J 120 3 100 -3-; 7 0,5 fjj 75 3 ' The flask does not comply with Flask C of Sp E 133. 5.2 Thermometer--The ASTM Solvents Thermometer used in the test shall be as prescribed specifications for the material being tested. If no th eter is specified in the material specification, select oneii Table 1 with the smallest graduations that will ,co ' entire distillation range of the material being tested, lists several ASTM solvents distillation thermometers are suitable for testing industrial aromatic hydrocarbons.! which meet the requirements of Specification E l. 5.3 Condenser--Either of the following two condensers/: may be used: 5.3.1 The condenser specified in Method D 86. 5.3.2 As an alternative, the condenser tube may consist ot a straight glass tube 600 to 610 mm in length and 12 mm in inside diameter, of standard wall thickness (about 1.25 infill, with the exit end cut off square and ground flat. It shall be ret in a cooling trough so that at least 380 mm of the tube is in contact with the water. Clearance between the condeurei tube and any parallel side of the trough shall be not less than 19 mm. The water in the cooling trough shall be maintained at 10 to 20C. This may be done by adding ice to the water or by circulating chilied water through the trough. The trough 0 A nask suitable for use is Coming Flask No. 4680, or its equivalent. 552 DUP050296114 D 850 Zlt imn. I.D. ' FIG. 1 Distillation Flask spn* Brneter Bo. pb&c hoc p41C I*80 |02C t03C wc ASTM Thermometers tor Distillation Test of Industrial Aromatic Hydrocarbons (Name Range, C Subcfivision. C solvents dstillatlon solvents distillation solvents distillation solvents distillation solvents distillation solvents distillation . solvents dlstllation solvents distillation 46 to 102 72 to 126 98 to 152 95 to 255 123 to 177 146 to 202 17310 227 196 to 252 0.2 0.2 0.2 0.5 0.2 0.2 0.2 0.2 1 be so mounted that the condenser tube is set at an angle J75 with the vertical. KSI4 Receiver--A graduate of the cylindrical type, of uniItin diameter, with a pressed or molded base and a lipped t. The cylinder shall be graduated to contain 100 mL, and graduated portion shall be not less than 178 nor more 203 mm in length. It shall be graduated in single illilitres and each fifth mark shall be distinguished by a pnger line. It shall be numbered from the bottom up at ntervals of 10 mL. The overall height of the graduate shall Jiot be less than 248 nor more than 260 mm. The gradua tions shall not be in error by more than 1 mL at any point Ijan the scale. The bottom 1-mL graduation may be omitted. Jfrhe receiver complies with Graduate B of Specification m 133. 5.5 Support for Flask--A sheet of 3 to 6-ram hard ^.insulation board 152 mm square with a circular hole in the fc' center, supported on a circular metal shield enclosing the bunsen burner, and approximately 50 mm higher than the top of the burner. For tests of benzene and toluene, the hole ;i shall be 25 mm in diameter; for tests of materials boiling above toluene but mostly below 145C, the hole shall be 38 mm in diameter, and for higher boiling materials, it shall be 50 mm in diameter. 5.6 Heater--An electric heater or a bunsen burner, fully adjustable and capable of giving sufficient beat to distill the product at the required rate. When a bunsen burner is used. the burner shall be adjusted so as to produce an entirely blue flame. In case of dispute concerning results obtained with gas heat versus electric heat, gas heat shall be accepted as the standard. No t e 1: WARN 1NG--Superheating ofthe flask can cause erroneous results and is more likely to occur with electric heaters than with bunsen bumeis as heat sources. This problem is discussed in the section on Preparation ofApparatus in Test Method D 1078. 6. Hazards 6.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 7. Sampling 7.1 Sampling should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regula tions. Refer to Practice D 3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this test method. 7.2 The sample under test shall be transparent and free of separated water. Any separated water may ordinarily be eliminated by care in pouring the 100-mL specimen (9s 1) into the graduated cylinder. If necessary, any separated water or cloudiness may be removed by filtration, in which case the following precautions shall be taken; Use a soft paper through which the specimen filters rapidly, avoid drafts, cover the funnel with a watch glass, and filter at least 200 mL from which to take the 100 mL for distillation. Dehydration (that is, removal of dissolved water) is not permissible. Note, however, that certain materials, especially benzene, may absorb traces of water that can be significant with respect to this test. When it can be shown that failure to pass this distillation test is due to the presence of dissolved water, it shall be permissible, if mutually agreeable to the purchaser and the seller, to dry the specimen by any method agreed to by both the purchaser and the seller. 8. Assembly of Apparatus 8.1 Assemble the apparatus as shown in Fig. 2. Mount the flask on the insulation board ofappropriate dimensions, with the side tube extending through a tightly fitting cork stopper about 50 mm into the condenser tube. 8.2 Support the distillation thermometer in the neck of the flask by means of a cork stopper with the thermometer vertical and centered in the neck of the flask and in such a position that the top ofthe bulb (or top ofcontraction bulb if present) is level with the lowest point ofjuncture between the side tube and the neck of the flask (see Fig. 3). 8.3 Place the burner directly under the center of the hole in the insulation board. No t e 2--As an alternative, the apparatus specified in Method D 86, modified by the use of the flask and thermometer as specified in 8.1 and 8.2, may be used. 9. Procedure 9.1 Carefully measure a 100-mL specimen ofthe material to be tested in the 100-mL graduated cylinder at room temperature and transfer to the distillation flask, draining the cylinder at least 15 s. This is preferably done before mounting the flask in position, in order to prevent liquid 553 ;tf, life DUP050296115 # D850 from entering the side arm. Connect the flask to the condenser and apparatus, assembled as described in Section 8. Do not rinse out the graduated cylinder used to measure the sample for distillation, but place under, the lower end of the condenser tube to receive the distillate. Heat the flask slowly, especially after ebullition has begun, so as to allow the mercury column of the thermometer to become fully expanded before the first drop distills over. Regulate the rate of heating so that the ring ofcondensing vapor on the wall of the flask reaches the lower edge of the side arm in not less than 90 s, and preferably approximately 120 s, from the start ofthe rise of the vapor ring. The total time from the start of heating until the first drop falls into the receiver should be not less than 5 nor more than 10 min. Avoid major changes in heating rate. Even operation is best gained through experience with the method. When distillation starts, adjust the receiver to allow condensation to flow down its inner wall to prevent loss by spattering; then adjust the heater to continue the distillation afthe rate of 5 to 7 mL/min (abo 2 drops/s). Maintain this rate, and continue the distill: dryness. The total yield ofdistillate when testing close t benzenes, toluenes, and xylenes shall be not less than * and when testing wider boiling refined products and' oils, shall be not less than 95 %; otherwise, the test repeated. 9.2 Take the temperature reading when the first dr distillate falls into the receiving cylinder and report " initial boiling point (IBP). If necessary, take additlJ readings when 5, 10, each additional 10 up through 90S and 95 % of the specimen has just distilled over. Take a i reading when the liquid just disappears from the flask, report this reading as the dry point temperature, testing crude materials, a decomposition point, rather t dry point, may be obtained. When a decompositioapnint; reached at the end of a distillation, the temperature frequently cease to rise and begin to fall. In this case,; sss FIG.' 3 Position of Thermometer In Distillation Flask 554 DUP050296116 -D 850 ature at the decomposition point as the maximum erature observed. The decomposition point may also be pjated by the appearance of heavy fumes in the flask. |ald that occur, record the temperature at the time the i of the flask becomes substantially full of fumes. If a imposition rather than a dry point is observed, so note i recording results. |3 Observe and record the following additional data at June and place of the distillation test: ffj.l Correction for inaccuracy of the thermometer, and 3,2 Barometer reading and temperature of the barom|fThe observed barometric pressure shall be corrected by ence to standard tables and reported in terms of aetres of mercury at 0C. TABLE 3 Boiling Points of Hydrocarbons Barometric Pressure, C Benzene Ethylbenzene Pyridine Toluene m-Xylene o-Xylene p-Xylene 80.1 136.2 115.5 110.6 139.1 144.4 138.3 range of the sample does not exceed 2C, a combined correction for thermometer inaccuracy and barometric pres sure may be made on the basis of the difference between the observed 50 % boiling point and the true boiling point at 760 mm as given in Table 3. |Temperature Corrections f.l Corrections of temperature should be applied in the |;ying cases: 1.1.1 When required by the specifications, 1.1 .2 When there is any question of compliance with the Scations, and if. 1.3 When tests of the sample are to be checked against i obtained by another investigator. s1.4 When corrected temperatures are reported, nota- fShould be made of the type of corrections applied. ,2 Inaccuracy of Thermometer--This correction shall btained by calibration of the thermometer used in the and applied to the observed thermometer reading. K3 Variation from Standard Barometric Pressure--This lection shall be applied to the observed temperature after cting for inaccuracy of the thermometer and is deterl by the following equation: C=(4 + {ix (760 -- P))] x (760 -- P) (I) |re: = the correction in degrees Celsius, = constants from Table 2, = the measured barometric pressure in millimetres of If mercury corrected to 0"C. |0.4 Combined Corrections--If the overall distillation BLE 2 Constants (or Corrsctlon for Variations in Barometric Pressure (600 to 800-mm Hg) pf' Material A B H| Benzene ||k?. Toluene m . Ethylbenzene m o-Xyfene m m-Xylerto JL. p-Xylene m' Mixed xylenes Grade xylene It Solvent naphtha If! Hi-flash solvent 0.0427 0.0463 0.0490 0.0497 0.0490 0.0492 0.0493 0.0493 0.0530 0.000025 0.000027 0.000028 . 0.000029 0.000029 0.000029 0.000029 0.000029 0.000032 11. Report 11.1 Report observed temperatures to the nearest 0.1C, in.a manner conforming to the specifications of the material tested. If no definite manner of reporting is specified, report the corrected temperatures at each observed volume, and report the volume percentages of residue, recovery, and distillation loss. 11.2 In the ASTM specifications where Test Method D 850 is cited, the distillation range is defined as follows: Distillation range, C = DPT-IBP (2) where DPT is the dry point temperature and IBP is the initial boiling point. 12. Precision and Bias 12.1 The following criteria should be used forjudging the acceptability of results (95 % confidence) on distillation range: 12.1.1 Repeatability--Duplicate results by the same oper ator should be considered suspect if they differ by more than the following amounts: *C Benzene Toluene Xylene 0.16 0.23 0.26 12. i.2 Reproducibility--Results submitted by each of two laboratories should be considered suspect if the two results differ by more than the following amounts: c Benzene Toluene , Xylene 0.42 0.47 0.42 12.1.3 The bias ofthis test method has not been addressed because no standard reference materials were available. 13. Keywords 13.1 aromatic hydrocarbons; distillation 555 DUP050296117 D 850 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ofany such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years end it not revised, eiffte/reapproved or withdrawn. Your comments are invited either for r&risicn of this standard or foradditional standards and should tie addressed to ASTM Headquarters. Your comments wi8 receive careful consideration at a meeting of the responsible technical committee, which you may attend, (f you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. * J'y HE> m .Vi 556 DUP050296118 ;signation: D 852 - 87 (Reapproved 1991) Standard Test Method for Solidification Point of Benzene1 This standard is issued under the fixed designation D $52; 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. :s?< 5. Significance and Use test method covers the determination of the 'on point of benzene. : standard does not purport to address all of the blems, if any, associated with its use. It is the ,lity ofthe user ofthis standard to establish appro'ty and health practices and determine the applicafgulatory limitations prior to use. For specific nents, see Section 7. -need Documents ,'M Standards: Test Method for Freezing Point of. High-Purity rocarbons2 Test Method for Purity of Hydrocarbons from ezing Points2 5 Specification for Reagent Water3 " Practice for Sampling and Handling Liquid Cyclic "nets4 cificalion for ASTM Thermometers5 !:er Document: Regulations, 29CER, paragraphs 1910.1000 and 0.1200s 5.1 This test method may be used as a criteria for determining the purity of benzene. The closer the solidifica tion point reaches that of pure benzene, the purer the sample. 6. Apparatus 6.1 Benzene Container, a test tube 15 mm in outside diameter and 125 mm in length. 6.2 Air Jacket, a standard test tube 25 mm in outside diameter and 150 mm in length. 6.3 Ice Bath, a 1-L beaker, or similar suitable container, having an effective depth of at least 127 mm and filled with chipped or shaved ice. 6.4 Stirrer, consisting of a 1-nun wire (copper or stainless steel) or a 2-mm glass rod with one end bent into a circular form at right angles to the shaft so that it will move freely in the annular space between the thermometer stem and the wall of the smaller test tube. 6.5 Thermometer, an ASTM Benzene Freezing Point Thermometer having a range from 4.0 to 6.0C and con forming to the requirements for Thermometer 112C as prescribed in Specification E 1. 6.6 Insulation--Dry absorbent cotton or glass wool. 'tion solidification point--an empirical constant defined as perature at which the liquid phase ofa substance is in mate equilibrium with a relatively small portion of , phase. 1--Solidification point is distinguished from freezing point ` described in Method D 1015. An interpretation of mol percent in terms of freezing point is given in Test Method D 1016. ___/ of Test Method .. Solidification point is measured by noting the tnax*' temperature reached during a controlled cooling cycle ;e appearance of a solid phase. test method is under the jurisdiction of ASTM Committee D-16 on ?c Hydrocarbons and Related Chemicals and is the direct responsibility of ralttee D16.0A ou Benzene, Toluene, Xylenes, Cyclohexane, and Their Jves. ent edition approved May 29, 1987. Published July (987. Originally ed as D852 - 45. Last previous edition D 852 - 81. nnuai Book ofASTM Standards, Vote 05.01 and 06.03. ual Book cfASTM Standards, Vols 06.05 and 11.01. nnuai Book cfASTM Standards, Vol 06.03. imual Book ofASTM Standards, Vol 14.03. .variable from Superintendent of Documents, U.S. Government Printing . Washington. DC 20402. 7. Hazards 7.1 Consult the latest OSHA regulations and supplier's Material Safety Data Sheets regarding all materials used in this procedure. 8. Sampling 8.1 Sampling of materials to be tested by this test method should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations. Refer to Practice D3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this method. 9. Preparation of Apparatus 9.1 Fit the smaller test tube with a two-hole cork stopper. Through one hole insert the thermometer up to the 4.0C mark; through the other hole insert shaft of the stiner. 9.2 Place a '/s-in. (3,2-mm) layer of dry absorbent cotton or glass wool in the bottom of the larger test tube. 9.3 Insert the smaller test tube up to the lip into a cork stopper or annular ring of cork that just fits into the mouth of the larger test tube. 10. Calibration of Thermometer 10.1 Calibration of ASTM thermometer 112C is accom plished with the small scale etched on the lower portion of the thermometer. Prepare an ice bath by filling a small 557 DUP050296119 D 852 Dewar flask with crushed ice made from Type I or Type II water (as specified in Specification D1193) and add just enough chilled Type I or Type II water to make a slurry. Immerse the thermometer in the ice bath, allow 5 min for the system to reach equilibrium and read the thermometer. Solidification point values are subsequently adjusted by adding (or subtracting) the number of degrees the thermom eter is below (or above) 0.00C. 11. Procedure II. I Saturate the sample ofbenzene with water as follows: Place 7 or 8 mL of the sample in the smaller test tube, add 1 drop ofwater, and shake the tube and contents vigorously. 11.2 Insert the stopper carrying the thermometer and stirrer into the smaller test tube and adjust the thermometer so that the 4.0"C mark is just even with the top of the stopper. 11.3 Cool the smaller test tube and.contents rapidly to about 6"C ifithe ice bath, while stirring. Wipe dry the outside of the smaller test tube and insert it into the larger test tube. Place the assembled tubes in the ice bath. 11.4 Stir the benzene continuously and observe the ther mometer- reading closely. The temperature will fell to a minimum, then rise to a maximum, remain constant at this maximum for approximately 1 min, and then fall again (Note 2). The minimum temperature is due to super-cooling before solidification starts and shall not be more than 0.7C below the maximum. Record the maximum constant tem perature observed to the nearest 0.01C and designate it as "wet" (Note 3). No t e 2--If distinct minimum and maximum points are not evident, or if the temperature does not remain constant at the maximum for at least 30 s, the determination shall be repeated. No t e 3--The precision can be increased to 0.01"C by using a magnifying glass that assures a reading perpendicular to the stem of the thermometer. In such eases it may be necessary to correct for stem exposure, that under ordinary conditions this correction will be less than 0.01"C. 12. Report 12.1 Results shall be reported on the anhydrous basis. Since the determination is actually made on water-saturated benzene, the solidification point shall be corrected to the anhydrous basis by adding 0.09"C to the observed maximum temperature following the minimum. Corrections for accu racy of the thermometer shall be made. 13. Precision and Bias 13.1 Duplicate determinations on the same specimen should not differ by more than 0.02"C (Note 3). The AmericanSociety for Testing andMaterials takas no positionrespecting the validity ofanypatentrights assertedin 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 rive years and If not revised, etthef reapptoved or withdrawn. Your comments are Invited either for revision ofthis standardorforadditionalstandards 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 ehou/d make your views known to the ASTM Committee on Standards, Ibis Race St.. Philadelphia, PA 19103. DUP050296120 Designation: D 853 - 91 Standard Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons1 This standard is issued under the fixed designation D 853; 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 lest method has been approvedfor use by agencies ofthe Department ofDefense to replace Method S3I1 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. ope This test method covers the determination of the Spgen sulfide and sulfur dioxide content (qualitative) of rid aromatic hydrocarbons. 11 This standard does not purport to address all of the w. problems, if any, associated with its use. ft is the sibility ofthe user ofthis standard to establish appro ve safety and health practices and determine the applica- of regulatory limitations prior to use. For specific |d statements see Section 6. iferenced Documents p ASTM Standards: |850 Test Method for Distillation of Industrial Aromatic Jydrocarbons and Related Materials2 3437 Practice for Sampling and Handling liquid Cyclic 'roducts2 Other Documents: tSHA Regulations, 29 CFR, Paragraphs 1910.1000 and |i910.12003 luminary of Test Method |l This test method involves a qualitative color test for land S02 that utilizes filter paper containing lead acetate [ starch paper containing potassium iodate. The test is jyrmed when carrying out the Test Method D 850 ation test Significance and Use |,1 This test method is suitable for setting specifications |industrial aromatic hydrocarbons and related materials i for use as an internal quality control tool. Sf test method is under the jurisdiction of ASTM Committee D-16 on latic Hydrocarbons and Related Chemicals and is the direct responsibility of iomnuttee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their rivatives. ijtCurrenl edition approved Oct 15,1991. Published December 1991. Originally wbluhed as D 853 - 45 T. Last previous edition D 853 - 82. h*Annual Book ofASTM Standards, Vol 06.03. ^Available from Superintendent of Documents, U.S. Government Printing , Washington, DC 20402. 4.2 This test method is a qualitative one for hydrogen sulfide (H2S) and sulfur dioxide (S02). It should not be considered quantitative. It gives an indication ofthe presence of H2S or S02, or both, which may cause objectionable odors or be corrosive to certain materials of construction. 5. Reagents 5.1 Lead Acetate Solution (saturated). 5.2 Potassium Iodate Solution (100 g/L)--Dissolve 10 g of potassium iodate (KI03) in water and dilute to 100 mL. 5.3 Starch Paper--Dip strips of filter paper in starch solution and dry. 6. Hazards 6.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 7. Sampling 7.1 Sampling should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regula tions. Refer to Practice D 3437 for sampling and handling of aromatic hydrocarbons analyzed by this test method. 8. Procedure 8.1 Make a qualitative test for H2S and S02, at the time of performing the distillation test, see Test Method D 850. This is done by hanging a strip of filter paper moistened with the lead acetate solution and a strip of starch paper moistened with the potassium iodate solution on the end of the condenser1 tube. The strips are placed so that they are suspended in the upper part of the receiving cylinder so that drops ofcondensate pass between the strips without touching them. If, at the end of the test, the lead acetate paper shows discoloration, H2S is present but not S02. If the lead acetate paper shows no discoloration but the starch iodate paper develops a blue color, S02 is present but not H2S. If neither paper shows discoloration, neither H2S nor S02 is present 9. Precision and Bias 9.1 In the case of pass/fail data, no generally accepted method for determining precision and bias is currently available. 559 DUP050296121 # P 853 The American Society for Testing anti Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, anti 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 antimust be reviewed every five years anti ifnot revised, either reapprovedor withdrawn. Your comments are invited eitherforrevision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments wilf receive careful consideration at a moating of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should moke your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 560 DUP050296122 Designation: D 1015 - 89 An American National Standard Standard Test Method for Freezing Points of High-Purity Hydrocarbons1 Hus standard is issued under the fixed designation D 1015; 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. m this test method describes a procedure for the precise jsrement of the freezing points of high-purity hydrocar- fThe values stated in SI units are to be regarded as the . The values in parentheses are for information only. | This standard may involve hazardous materials, oper and equipment. This standard does not purport to all ofthe safetyproblems associated with its use. It is |sponsibility of the user of this standard to establish jtriate safety and health practices and determine the |lability of regulatory limitations prior to use. For : hazard statements, see Notes 2, 3,4, and Annex A1. ft l--For the calculation of the mola] purity of essentially pure r" iinds from measured freezing points and for procedures to be the sampling and determination of purity of certain specific |tmds, see Test Method D 1016. Iferenced Documents i^ASTM Standards: |016 Test Method for Purity of Hydrocarbons from Freezing Points2 |'265 Practice for Sampling Liquefied Petroleum (LP) pases2 4057 Practice for Manual Sampling of Petroleum and jfPetroleum Products3 nmary of Test Method The precise experimental measurement ofthe freezing It is made from interpretation of time-temperature |ing or melting curves.4 Significance and Use ||l The freezing .point measured by this test method, 1 used in conjunction with the physical constants for the carbons listed in Test Method D 1016, allows the nutation of the purity of the material under test. A vledge of the purity of these hydrocarbons is often . to help control their manufacture and to determine suitability for use as reagent chemicals c m" for conver mis itest method is under the jurisdiction of ASTM Committee D-2 on oleum ]Products end Lubricants and is the direct responsibility of Subcom- D02.04 on Hydrocarbon Analysis. irrent edition approved Oct. 27, 1989. Published December 1989. Originally as D1015 - 49 T. Last previous edition D 1015 - 84. Annual Book ofASTM Standards, Vol 05.01. 'Annual Book ofASTM Standards, Vol 05.03. For details not given here, see Glasgow, A. Jr., Rossini, F. D., and Streiff, , **Determination of the Purity of Hydrocarbons by Measurement of Freezing ins. Journal of Research, JNBAA, National Institute of Standards and inology, Vol 35, No. 6, 1945, p. 355. sion to other chemical intermediates or finished products. 5. Apparatus 5.1 Freezing-Point Apparatus,5 as shown i n Figs. 1, 2, and 3, comprising a freezing tube, a metal sheath for the freezing tube, a Dewar flask for the cooling bath, a Dewar flask for the warming bath, a stining mechanism, suitable clamps and holders for the parts, and the absorption tubes. The outer walls ofall Dewar flasks can be covered with adhesive tape to minimize danger from glass in case of breakage. No t e 2: Warning--When using liquid nitrogen as a refrigerant, provide a means to prevent condensation of oxygen in the space between the freezing tube and the metal sheath and subsequent sealing of the space by ice forming on the asbestos collar. Provide the metal sheath with suitable openings in the sides and bottom. Failure to do this may result in breakage of the freezing tube when the liquefied oxygen evaporates within the sealed space. 5.2 Resistance Bridge,6 Mueller type, reading from 0.0001 to 50 ft, in steps of 0.001 ft. 5.3 Platinum Resistance Thermometer,6 precision grade, with a resistance near 25.5 ft at 0C, calibrated by the National Institute ofStandards and Technology for the range from -190 to 500C. 5.4 Null Point Indicator, may be either a galvanometer or a microvolt ammeter. 5.4.1 Galvanometer,6 having a sensitivity of 0.1 mV/m at 1 m for highest precision or a sensitivity of 0.5 mV/m at 1 m for routine precision. 5.4.2 Microvolt Ammeterf 5.5 Lamp and Scale,6 any suitable type. 5.6 Stopwatch or Clock, preferably having graduations in minutes and hundredths of minutes. 5.7 High-Vacuum Oil Pump,6 capable of evacuating 5 A suitable apparatus is available from Reliance Glass Works. Inc., Bensenvilte, IL, Cat. No. R6876-I00. 6 Apparatus described in 5.2, S.3, 5.4 and 5.5 was manufactured by the Leeds and Northrup Co., Philadelphia, PA. under the following catalog numbers; resistance bridge. No. 8069 B: platinum resistance thermometer. No. 8163 B; galvanometer, highest precision. No. 2284 D; galvanometer, routine precision. No. 2430 A; lamp and scale. No. 2100. The galvanometer, routine precision. No. 2430-A, and the lamp and scale. No. 2100, are still available from Leeds and Northrup. The platinum resistance thermometer. No. 8163-B, is no longer available from Leeds and Northrup, but is available with the same part number from Yellows Springs Instrument Co., Yellow Springs. OH. The resistance bridge No. 8069.-B, and ihe galvanometer, highest precision. No. 2284-D, are no longer available; however, they may be obtainable from instrument exchanges or used equipment suppliers. If other available instrumentation is substituted for the original, the precision statement of Section 13 will not apply. 7 Model No. 155. manufactured by Keithley Instruments, Inc.. 28775 Aurora Rd., Cleveland, OH. or equivalent, has been found satisfactory for this purpose. 8 A suitable pump is available from Boekel Industries. Inc. Philadelphia, PA. Cat No. 91105. 561 mm- DUP050296123 D 1015 the jacket of the freezing tube to a pressure of 0.133 Pa in 10 min or less. 5.8 Seeding Apparatus, as shown in Fig. 4, for inducing crystallization. 5.9 Silica Gel Fitnnel, as shown in Fig. 5, for filtering compounds through silica gel to remove water. To be used only when specified in Test Method D 1016. 6. Materials 6.1 Carbon Dioxide Refrigerant--Solid carbon dioxide in a suitable liquid. Trichloroethylene is recommended. No t e 3: Solid Carbon Dioxide--'Warning--Extremely cold {-78.5*0- Liberates heavy gas which may cause suffocation. Contact with skin causes bums or freezing, or both. Vapors may react violently with hot magnesium or aluminum alloys. See Annex AM. Trichloroethylene--Warning--Harmful if inhaled. High concentrations may cause unconsciousness or death. Contact may cause skin irritation and dermatitis. See Annex At .2. Use refrigerant bath only widi adequate ventilation!' 6.2 Liquid Nitrogen or Liquid Air--(Warning--See Note 4.) For use as a refrigerant. If obtainable, liquid nitrogen is preferable because of its safety. 6.2.1 Use liquid nitrogen refrigerant only with adequate ventilation. If liquid air is used as a refrigerant, it is imperative that any glass vessel containing hydrocarbon or other combustible compound and immersed in liquid air be protected with a suitable metal shield. The mixing of a hydrocarbon or other combustible compound with liquid air due to the breaking of a glass container would almJbi certainly result in a violent explosion. If liquid nitrogen* used as a refrigerant, no hydrocarbon sample should evert permitted to cool below the condensation temperature v oxygen (- 183"C at 1 atm). This would not be likely to oeoS in normal operation, but might occur if the apparatus wg&jj left unattended for some time. ``. 'S3 No t e 4: Warning--Extremely cold. Liberates gas which can cai suffocation. Contact with skin causes bums or freezing, or both. Van, can react violently with hot magnesium or aluminum alloys. Sec Auri A 1.3 and A 1.4. 6.3 Silica Gel, for use in silica gel funnel.9 If the gel | been exposed to the atmosphere because of puncture loosely sealed containers, before use, dry the gel in a shall vessel at 150 to 205C for 3 h, then transfer while hoi . air-tight container. ^'*2 7. Sampling 7.1 Samplingfrom Bulk Storage: 7.1.1 Cylinder--Refer to Practice D 1265 for instruction^ on introducing samples into a cylinder from btilk siorage^Jj 7.1.2 Open Containers--Refer to Practice D 4057 4 " instructions on introducing samples into open-type! tainers from bulk storage. 9 A satisfactory gel of 28 to 200 mesh may be obtained from 1 Chemical Co., Baltimore 3, MD. Specify grade 12. Legend for Fig. 1 (see following page): A--Bracket for motor, with rubber pad. B--Motor, with reduction gears, to give 120 r/min.. C--Coupling. (See Fig. 3). D--Wheel. (See Fig. 3). E--Steel rod. (See Fig. 3). F--Bearing. (See Fig. 3}. G--Support tor bearing. (See Fig. 3). H--Support for freezing tube. i--Adjustable damp holder, J--Clamp for freezing tube. K--Stirrer. {See Fig. 3). L--Thermometer. M--Tube for inlet of dry air, wilh 12/5 spherical joint. M'--12/5 spherical joint connection to rotameter. /V--cork stopper, with holes as shown, plus a small hole for the "seed" wire: 0--Freezing tube, with silvered jacket. (See Fig. 2.) P--Stopcock on freezing tube. P'--stopcock (high vacuum) to drying tube. 9--Stopcock (high vacuum) to vacuum line. ` Q--Asbestos collar." ft--Brass cylnder, 317.5 mm <12% in.) In length and 54 mm (2V In.) in inside diameter, with bakelite coffer; when liquid nitrogen is used, the metal shield must be with suitable openings in sides and bottom (see Note 2). If liquid air is used, the metal shield should be constructed so as to keep hydrocarbon from contact liquid air (see Note 4). S--Dewar flask, lor cooling or warming bath; approximate Inside diameter, 101 mm (4 in.); approximate inside depth, 330 mm (13 in.). 7--Asbestos pad at bottom of cylinder ft. D--Wood block support. V--Table top. W--Wall. XX--Spherical joint, 18/7. V--Standard metal (copper or brass) to glass taper connections soldered. Z--Connection to vacuum pump, a--Anhydrous calcium sulfate, with Indicator, b--Anhydrous magnesium perchlorate, granular. d--Separating layer erf glass wool, e--Ascarite. /--Anhydrous calcium sulfate, g--To air. A--To source of compressed air. /--Row meter, for rates of 10 to 28 mL/min. 562 DUP050296124 jf 'f h I libration of Thermometric System and Conversion of .sistance Readings to Temperature w Calibration of Resistance Bridge--The Mueller type stance bridge should have its calibration checked at opriate intervals by measurement of a suitable external feed resistance, with intercoinparison of the resistances ue bridge. .2 Calibration of Resistance Thermometer--The plati" -resistance thermometer is provided with four calibraconstants certified by the National Institute of Standards Technology for use in converting the resistance of the rmometer into temperature according to the International iperature Scale, for use in the range from -190 to 500C, ttely, R0, C, S, and Q. If the thermometer has been ily constructed and annealed, the certified constants C, S, and /3 will not change significantly with time, but the value of R0 may change slightly. No t e 5--International Practical Temperature Scale--In 1968 a new IPTS was adopted, replacing the previous scale in use since 1948. The 1948 IPTS was based on the boiling point ofoxygen, the sulfur point, ice point, and steam point. The 1968 IPTS is based on the triple point of water, tin point, zinc point, and boiling point of oxygen. The differences in the two temperature scales T68-T4, vary. Above 100C the differences are plus; below 100`C they may be either plus or minus. If the measured freezing point is to be used for the determination of purity according to Test Method D 1016, the measured freezing point /,, and the freezing point of the pure material tf,, should be on the same temperature scale. The values oftf,, given in Test Method D 1016 are on the 1968 IPTS. Therefore, values of redetermined using thermometers calibrated on the 1948 scale should be converted to their 1968 IPTS equivalent. This conversion can be made by applying the appropriate correction from Table 1. 563 DUP050296125 0 1015 A--Hgh-vacuum stopcock, hollow plug, oblique SVfcmm bore. B--Inside opening oil freezing tube, which must have no bulge at this point. C--Slanted connection to jacket of freezing tube. j_fntemal waifs of jacket of freezing tube, sWvered. E--Spherical joint, 18/7. FIG. 2 Details of the Freezing Tube 8.3 Checking of the Ice Point--Frequent measurements (at least once every month) should be made ofthe resistance of the given platinum thermometer at the ice point, O'C, as measured on the given resistance bridge.10 This value should differ only slightly from the certified value of R0- If the difference becomes appreciable (approaching 0.001 2), the calibration of the bridge should be checked. If the bridge has not changed, the change has occurred in the thermometer, and a recalibration of it is recommended. 10 The ice point may be measured according to the procedure described by J. Busse, "Temperature, Its Measurement and Control in Science and Industry,** Section VRI, Reinbold Publishing Coip., 1941, p. 241. See also "Notes to Supplement Resistance Thermometer Certificates.** National Institute of Stand* aids and Technology, 1949. 8.4 Conversion of Resistance Readings to Temperature' When determinations are made on a number of subsiar having freezing points at different temperatures, tiinc wi| saved by making up a table giving values of the resistance,' for each unit degree of temperature in the given Values of resistance for unit degrees, for the ranges -190 to +50C and +50 to 290C, with differences b successive unit degrees tabulated for linear interpi (which is permissible), may be easily placed on a singly by 400-mm (14 by 16-in.) sheet for each range. Calcula values for the resistance, R, from unit values oftemperau, t, by means of one of the following equations: For temperatures below 0'C: R = J?o{l + 0[(1 + 0.01 ) - 10"" St - 10"3 0(t - 500)/"p For temperatures above O' C: R = t?0(l + C7[(l + 0.01 S) - lO"4 St)} where: t = given temperature, C, on the International Temper ture Scale (see Note 5), R -- resistance of the thermometer in ohms at the-,ternpc ture t, J?o- resistance of the thermometer in ohms at 0C, C, 5, and (3 = constants certified for the given thermometer by the National Institute of StancUids4a Technology. 9. General- Procedure for Determining a Freezing Curve " 9.1 Assemble the apparatus, with no refrigerant., sample yet in place, but with a stream of air, freed < dioxide and water, flowing at a rate of 10 to 20 mL/min ,f the jacket of the freezing tube with air freed of curb dioxide and water. 9.2 As required, the operator must be prepared to i crystallization in the sample as soon as possible after.'? temperature has passed below the freezing point of sample (to prevent excessive undercooling). In some c crystallization may be induced by introducing into sample at the appropriate time a small rod (ABC lr Fig/, which has been kept at an appropriate lower temporal (near O'C, -8CFC, or -180'C) (/ in Fig. 4). In other crystallization can be induced by introducing into the snm at the appropriate time crystals of the sample on the ceil end of the small rod (ABC in Fig. 4). When indue crystallization, the cold rod (with or without crystals) sho be immersed in the sample in the freezing tube for about (ifnecessary, this is repeated every 2 or 3 min). These are made by placing several millilitres of the sample in small test tube, incased in a thin metal tube, as showu Fig. 4, immersed in a refrigerant whose temperature is bel< the freezing point of the sample. A slurry or mush of hq and crystals is produced. The rod (ABC in Fig. 4), wij| crystals adhering to the helical coil C, is raised above?, liquid level in the tube E and held in position with a d stopper until required for seeding. ' ' 9.3 Fill the Dewar flask surrounding the freezitig f with the appropriate refrigerant. Temporarily reino.Vf:4 thermometer and stopper and then introduce the (usually 50 riiL of liquid in amount) through a pipe material is normally liquid, or by pouring the refrigefa liquid sample through the tapered male outlet of the i 564 Pi,.. WPS D 1015 s:, $.2 mm <Va fn.) in dameter. 5 wheel, with three holes; tapped for machine spews, spaced 12.7 mm (Vzin.). 19.05 mm in.), and 25.4 mm (1 In.) from center: normal position is 19.05 mm in.) frpm center, j rod: Hecrews. sooupSng. ifshaft. l, round. e| rod, square. |npecting pin. tsk sleeve bearing. I pipe. 12.7 mm (Vfe in.) nominal size. Sjoauplng... 9 tee. ninuni ' i^bie helical stirrer, made by winding 1.6 mm (Vie m.) diameter nlchrome wire downwards on a cylinder 14.3 mm {/i# in.) in outside diameter to form the inner helix, jdfthen-upwards over a cylinder 20.7 mm {'Vie in.) in outside diameter to form the outer helix, with the two ends silver soldered together, gpe where shaft of the double helical stirrer is joined to the stirrer shaft. Metric Equivalents 0.794 11.91 4.763 24 74.612 77.8 9.53 22.23 20.6 60.33 117.5 6.4 57.15 108 Vn 15/a? 10 Wio 2'Vie 3Vie % % IVb 2Ve 4% Vk 2% 4V< 63.5 114.3 215-91 2% 4Vz Vz FIG. 3 Details of the Stirring Assembly and Supports gtrap (E in Fig. 1 of Test Method D 1016) if the material Daily gaseous. When specified in Test Method D 1016, | the sample directly into a freezing tube {O in Fig. 1) gh silica gel to remove water. A detailed drawing of a pel used for this purpose is shown in Fig. 5. Each time a &ig or melting curve is determined after the sample is melted, it is necessary to remove the sample from the freezing tube and refilter it through silica gel into a dry freezing tube to remove water. When the sample is volatile or normally gaseous at room temperature, cool the freezing tube before introduction of the sample in order to minimize loss by evaporation. Continue the flow ofair (freed of carbon 565 mm ...v**** II DUP050296127 4CtoMdQan j D<No.Goo* t*irvr* Tf4*,DmmO.Dl f Vfin Sfirrtf) K9^eM9ie^Se*(V Fig.1 Legend). .E(Pyr* TeJ Tub*) ' FlWetot Stvetd, 5*R, G{Cork Stopper), Fig.1 Legend) .A(8okeWe Rod 3.2 tmoOO.S an /vB^Gonnon Stwr Tube) ^ (Xffichrwno Wire) Hfl-ffnt Dewor) # D 1015 5 cm. A--BakeTite rod; $ mm (Vo in.) in diameter, 317.5 mm (12V2 in.) in length. 8--German-stfver tube, seated to nichrome wire on one end and 'sweated" on bakeRtft'rod on other. C--Nkshropie wire, 1.191 mm (%4 in.) in diameter, with a heVcaJ coil on one end. 0--Stirrer, nlchrone wire 18 to 35 mm (Vie to Ve in.) in diameter, coiled on we end. f--Pyrex test tube. F--Metal shield: for precautions in use of liquid nitrogen and liquid air see R in legend to Fig. 1 and Notes 2 and 4. <3--Cork stopper, with holes as shown. W--Dewar flask, 1 pint size. /--Asbestos paddings. j--Pyrex glass tube closed on one side. K--Metal shield; for precautions in use of liquid nitrogen and liquid air see R In legend to Fig. 1 and Notes 2 and 4, FIG. 4 Apparatus for Inducing Crystallization dioxide and water) into the freezing tube in order to keep out water vapor. Start the stirrer and allow the sample to cool down to within about 15`C of the freezing point, then begin evacuation of the jacket ofthe freezing tube. 9.4 Observe the time and the resistance of the thermom eter at even intervals of0.02 to 0.05 ft (about 0.2 to 0.5"C) to determine the rate of cooling, which is continually changing as the pressure in the jacket of the freezing tube is reduced. Care must be taken to close the stopcock to the freezing tube when the desired cooling rate is obtained. In case the cooling rate is allowed to become too slow, the pressure and likewise the cooling rate may be increased by bleeding in air (freed of carbon dioxide and water) through stopcocks P' and P (Fig. 1). When a cooling rate is obtained that will give a change of 1 C in about 1 to 3 min in the range ofabout 5 to 10'C above the freezing point, close the stopcock controlling the jacket of die freezing tube. (The optimum rate of cooling will vary with the material being examined.) 9.5 When the temperature reaches a point about 5'C above the expected freezing point, record the time to 1 s (or 0.01 min) at which the resistance of the thermometer equals 0.1 or 0.05 ft. A.t the appropriate time (see 9.2) induce crystallization. The beginning of crystallization will be ac companied by a halt in the cooling of the liquid. After recovery from undercooling is substantially complete, record the resistances at intervals of about 1 min. If a galvanometer is being'used, also record the galvanometer scale at full sensitivity and with no current through the galvanometer. These observations, together with the sensitivity of the galvanometer system in terms of ohms per millimetre of A--Filter funnel, with extension as shown, pyrex glass. B--Adsorbent, silica gel. 28 to 2D0 mesh. C--Glass wool. FIG. S SUica Gel Funnel scale reading, yield a sensitivity of nearly 0.000l'C. Approx imately equal sensitivity is obtained when using a microvolt ammeter. Continue observations until the stirrer begins to labor, then .stop the stirrer. After several minutes (when a steady rate is obtained) make alternate N and R readings through the commutator at fixed intervals of about t min. Determine the difference between the two at any given time from a plot of the values against time. 10. General Procedure for Determining a Melting Curve 10.1 For determining a melting curve proceed exactly as described in Section 9 for a freezing curve, up to the point where the stirrer begins laboring. When the stirrer shows signs of laboring, make a comparison of ,V and R readings through the commutator, as in 9.5 except that the stirrer is still operating. When the laboring of the stirrer becomes quite pronounced, the freezing curve (with the stirrer still operating) is changed to a melting curve. The energy for melting is supplied in either of the two following ways: (a) the cooling bath is replaced by a warming bath and simulta neously the jacket is evacuated for an appropriate length of time (3 to 10 min). The stopcock on the freezing tube is closed; or (b) the cooling bath is left in position or replaced by a warming bath and the jacket evacuated as much as possible, leaving the stopcock to the freezing tube open to the vacuum system during the entire melting curve. In this case the thermal conductivity across thejacket is so small that the energy introduced by the stirrer provides the energy for melting. Continue the observations of time and resistance along the equilibrium portion of the melting curve as along the equilibrium portion of the freezing curve. When melting is substantially complete, as evidenced by a marked change in the rate ofchange of resistance, make observations oftime at even intervals of 0.05 ft (0.5C). The experiment is 566 I DUP050296128 # D 1015 j'--The scale of ordlnafes gives the resistance In ohms of the platinum resistance thermometer, and the.scale of abscissas gives the time in minutes. GHI represents jiiibrtum portion ot the freezing curve. Zero time Is given by the Intersection of the liquid cooling line with GHI extended. The same data are plotted in Fig. 7 with a 3 scale of temperature. FIG. 6 Time-Temperature Cooling Curve for Determining "Zero" Time in an Experiment on a Sample of Benzene BLE 1 Approximate Differences {TM-TM) in Kelvins, Between the Values of Temperature Given by the IPTS of 1968 and the IPTS of 1948 tec" 0 -10 ~20 "30 -40 -50 -60 -70 -80 -90 -100 fproo 1 -o 0.022 0.000 0.013 0.006 0.003 0.012 -0.006 ^-0.013 0.016 ' 0.024 -0.013 0.029 -0.005 0.032 0.007 0.034 0.012 0.033 0.029 0.022 R&c |S: 0 faoo poo f 300 L400 f500 600 | 700 600 I 900 hO0Q 0 0.000 0.000 .0.043 0.073 0.076 0.079 0.150 0.39 0.67 0.951.24 1 10 -0.004 0.004 0.047 0.074 0.075 0.062 0.165 0.42 0.70 0.93 1.27 20 -0.007 0.007 0.051 0.075 0.075 0.085 0.162 0.45 0.72 1.01 1.30 30 -0.009 0.012 0.054 0.076 0.075 0.069 0.200 0.47 0.75 1.04 1.33 40 -0.010 0.016 0.058 0.077 0.074 0.094 0.23 0.50 0.76 1.07 1.36 50 -0.010 0.020 0.061 0.077 0.074 0.1C0 0.25 0.53 0.81 1.10 1.39 60 -0.010 0.025 0.064 0.077 0.074 0.103 0.28 0.56 0.84 1.12 1.42 70 -0.008 0.029 0.067 0.077 0.075 0.116 0.31 0.58 0.87 1.15 1.44 80 -0.006 0.034 0.069 0.077 0.076 0.126 0.34 0.61 0.89 1.18 90 -0.003 0.038 0.071 0.076 0.077 0.137 0.36 0.64 0.92 1.21 100 0.000 0.043 0.073 0.076 0.079 0.150 0.39 0.67 0.95 1.24 |luded when the temperature has gone about 5 to 10*C lie the freezing point. pEvaluation of the Freezing Point from a Freezing Curve jj l.l To locate zero time (the time at which crystallization t have begun in the absence of undercooling), make a ainary plot of the time-resistance observations covering ijiquid cooling line and tire equilibrium portion of the ping curve. For this plot, as shown in Fig. 6, the time V is taken so that 10 mm is equivalent to 1 min and the ance scale (for a 25-ft thermometer) so that 10 mm is Ivalent to 0.02 0 (0.2C). Zero time is determined by a visual extrapolation, on this plot, of the equilibrium portion of the freezing curve back to its intersection with the liquid cooling line. ! 1.2 In order to locate accurately the resistance corre sponding to the freezing point, plot the time-resistance observations as shown in Fig. 7 with the time scale as before but with the scale of temperature magnified 10 to 200 times. The equilibrium portion of the curve, GHI, is extended back to its intersection at F with the liquid line by the simple geometrical construction shown in Fig. 8, selecting for this purpose three points (near the ends and the middle) of the equilibrium portion of the curve (Note 6). The point F gives 567 DUP050296129 # D 1015 Method: ! 1) Drew Line GH Extended tnft-3 (2J Draw Line IH Estended to (3) Draw Line JK Parallel to (4) Draw Line KG Extended to resistance thermometer, end the scale of abscisses gives the time In minutes. 6HI represents the equilibrium portion of the freezing curve: The freezing point F is determined as describedln the text end Fig. 8. These data are the same as those plotted In Hg. 6. FIG. 7 Time-Temperature Cooling Curve (or Determining the Freezing Point of a Sample of Benzene the resistance corresponding to the freezing point.11 No t e 6--The location ofthe resistance corresponding to the freezing point can be made Using algebraic expressions derived from the geometrical construction. These are as follows: */= Rt + [(J?*- R,)/(uvw - 1) where: k - t(J?a - JO/tR, - v-KZs-zp/CZ.-ZJJ, and w~[{Z,-Zj)HZs-Zf)l Zfi Zp Zh and Z, arc the times corresponding to the points F, G, H, and I, respectively, and Rf, Re Rj, and R, are the resistances in ohms corresponding to the points F, G, H, and /, respectively. It is nearly always possible to select the point H equidistant in time between G and l, so the v = 1. 11.3 The observed resistance at the point F, corrected by one halfthe difference between the N and R readings, and by a bridge zero correction, appropriate calibration corrections to the coils.of the bridge, and by an ice point correction, if necessary, is converted to temperature in degrees Celsius. 12. Evaluation of the Freezing Point froth a Melting Curve 12.1 Determine zero time from a preliminary plot (as for the freezing curve (Section 11)) of the time-resistance obser vations covering the equilibrium portion of the melting curve and the liquid warming line, as shown in Fig. 9. Zero time can usually be determined by visual extrapolation, on this plot, of the equilibrium portion of the melting curve to 11For details regarding the identification of the equilibrium portion of the curve, and the geometrical construction for determining the freezing point, see Rossini, F. D., and Taylor, W. J., "Theoretical Analysis of Time-Temperature Freezing and Melting Curves as Applied to Hydrocarbons,'' Journal ofResearch, JNBAA. National Institute ofStandards and Technology, Vol 32, No. 5,1944, p, 197. 4f Time----- v- Note--Sample.- Given 0, H, and / as any three paints on tiro t portion of the freezing curve, preferably spaced approximately ; Construction to determine FI,: Draw AC parallel to the temperature axi time (the time at which crystallization would have begun in the i undercooring).-praw AB through J parallel to the time axis. Oraw a lltii and ft Intersecting 48 at f? andAC at >. Draw a line throughHand I hi' at J. Draw a line through 4 parallel to BE, intersecting 8 at K. Draw i K end G. Intersecting AC at F. F is the described point, representhrg ti point of the given sample (see reference given in footnote 10). 3 FIG. 8 Geometrical Construction lor Determining die Fit Print its intersection with the liquid wanning line extend in temperature to its intersection with the extensions equilibrium portion of the curve. 12.2 The location of the freezing point at F ts^d exactly as in the case of the freezing curve, exetpt ihM geometrical extrapolation is made to the right as shdq Fig. 10. (See Fig. 8 and the reference in Footnote* details.) n_ 12.3 Make the conversion of resistance to tempered described in Section 1 i. 13. Precision and Bias NOTE 7--The precision of this test method was not obi accordance with RR: D02-1007.3 13.1 Results should not differ from the mean i than the following amounts: Repeatability One Rep Operator and Different C Apparatus and Apr Freezing point, C 0.005 0.0 . No t e 8--The precision data were obtained using a gaivedoi Equivalent results would be expected when using a microvolt if Deviations will be greater than those shown for very impure s compounds in which the liquid-solid equilibrium is esl gishly, and for compounds having small values of thej constant A. 13.2 Bios 568 DUP05029613Q e--The scale of ordinates gives the resistance In ohms of the platinum resistance thermometer, and the scale of abscissas gives the time m minutes, HQ represents of the equitbrium portion of the warming curve. Zero time is given by the intersection of HG extended to its Intersection with the backward extension of the liquid ing line. The same data are plotted In Rg. 10 with a magnified scale of temperature. FIG. 9 Time-Temperature Wanning Curve for Determining "Zero" Time in an Experiment on a Sample of Ethylbenzene .2.1 The procedure in this test method for measuring 'ng point has no bias because the freezing point value be defined only in terms of this test method, which is a etion of the purity of the reference materials. 14. Keywords 14.1 crystallization; freeze point; LPG; pure hydrocar bons; purity 569 DUP050296131 9 D1015 si No t e--Tits scale of ordinates gives the resistance in ohms of the platinum resistance thermometer, and the scale of abscissas gives the time In minutes, me represents 1 the equlibrlum portion of the warming curve. The freezing point F is determined as described in the text and Fig. a These data are the same as those plotted in Fig. 9. .9 FIQ. 10 Time-Temperature Wanning Curve for Determining the Freezing Point of a Sample of Ethylbenzene ANNEX (Mandatory Information) Al. PRECAUTIONARY STATEMENTS Al.l Carbon Dioxide (Solid) Use with adequate ventilation. Avoid contact with skin and eyes. Do not taste. Do not put in closed or stoppered container. Do not enter storage areas unless adequately ventilated. A1.2 Trichloroethylene Avoid prolonged or repeated breathing of vapor or spray mist. Use only with adequate ventilation. Eye irritation and dizziness are indications of overexpo sure. Do not take internally. Swallowing may cause injury, illness, or death. Avoid prolonged or repeated contact with skin. Do not get in eyes. A13 Liquid Nitrogen Use with adequate ventilation. Avoid contact with skin or eyes. Do not taste. Do not put in closed or stoppered container. Do not enter storage areas unless adequately ventilated. A1.4 Liquid Air Avoid contact with skin or eyes. Do not taste. Do not put in closed or stoppered container. 570 imi IlimiAf.-,. .'A.'Av iS DUP050296132 # D 1015 $s American Society tor Testing andMaterials takes no position respecting the validity of any patent rights asserted in connection any item mentioned in this standard. Users of this standard are expressly advised tW determination of the validity of any suoh ont rights, and the risk oi infringement of such rights, ere entirely their own responsibility. This standard is subject to revision at any time by the responsible technical comm/tree and must be reviewed every five years and revised, either reapproved or withdrawn. Yourcomments are Invited eitherfor revision of this standard or for additional standards should be addressed to ASTM Headquarters. Your comments wHi receive carefut consideration at a meeting of tha responsible urical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your 'V known to the ASTM Committee on Standards, 191$ Piece St., Philadelphia, PA 19103. 571 iilf: :/ DUP050296133 Designation: D 1016 - 89 JjfAn American Nations) Standard Test Method for Purity of Hydrocarbons from Freezing Points1 This standard is issued under the fixed designation D 10)6; 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. 1. Scope 1.1 This test method covers the sampling and determina tion of purity of essentially pure compounds for which the freezing points for zero impurity and cryoscopic constants are given.2 The compounds to which the test method is ap plicable are: , n-butane tsobutane *v n-pentane isopentane n-hexane n-heptane zt-octane 2,2,4-trimethylpentane methyleyclohexane isobutene 1,3-butadlcne isoprene(2*methyl-l,3-butadiene) benzene toluene (methylben2ene) ethylbenzene o-xylene (l2-dimcthylbenzene) w-xylene <l,3-dimethylbenzene) jvxylene (1,4-dimethylbenzene) styrene (ethenylbenzene) No t e 1: Warning--Extremely flammable liquids and liquefied gases. See Annexes A 1.5 and A 1.6. 1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only. 1.3 This standard may involve hazardous materiab, 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 Sections 1, 6, 8, and 10 through 26. No t e 2--This lest method covers systems in which the impurities form with the major component a substantially ideal or sufficiently dilute solution, and also systems which deviate from the ideal laws, provided that, in the latter case, the lowering of the freezing point as a function of the concentration is known for each most probable impurity in the given substance. 2. Referenced Document 2.1 ASTM Standard: D1015 Test Method for Freezing Points of High-Purity Hydrocarbons3 3. Summary of Test Method 3.1 After measurement of the freezing point of the actual sample, purity can be calculated from the value of 1 determined freezing point and the values give for ' freezing point for zero impurity and for the applic-3 cryoscopic constant or constants.4 3.2 For the equilibrium between an infinitesimal anjoiL ofthe crystalline phase of the major component and a liqul phase of the major component and one or more olher c 8 ponents, the thermodynamic relation between he temp lure of equilibrium and the composition of the liquid i is expressed by the equation:5 ,:}l -In N, = -ln(! - Ay A(lfa - //)[! + B{lf0 where: j Vj = mole fraction ofthe major component, - `j|l N2 = (1 - IV,) = sum of the mole fractions of all the ot;fi components, ',L if = freezing point, in degrees Celsius, of the given,$ stance (in which the mole fraction of the component is /V,), defined as the temperatutiS which an infinitesimal amount ofcrystals ofI he majs component is in thermodynamic equilibrium wit)" liquid phase (see Note 5 of Test Method D lOlf (ro = freezing point for zero impurity, in degrees Cels for the major component when pure, that is, whoiuV = 1 or ,V2 = 0, A = first or main cryoscopic constant, in mole fraction peE degree, and B - secondary cryoscopic constant, in mole fraction degree. Neglecting the higher terms not written in the brackels L, 12 can be transformed to the equation: log= 2.00000 - M/2.3026)(r/o - ^[1 + j 30/0 - tfi where: P = purity of the given substance in terms of mole percent? of the major component. 4. Significance and Use 4.1 The experimental procedures and physical consti provided by this test method, when used in conjunction w|H Test Method D 1015, allow the determination of the ofthe material under test. A knowledge ofthe purity of-tl 1 This test method is under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcom mittee D02.04 on Hydrocarbon Analysis. Current edition approved Oct. 27,1989. Published December 1989. Originally published as D J016 -- 49 T. Last previous edition D1016 - 84. 2 Numerical constants in this test method were taken from the most recently published data appearing itt "Tables ofPhysical and Thermodynamic Properties of Hydrocarbons and Related Compounds," or ASTM DS 4A, Physical Constants of Hydrocarbons C, to C,0, or both, prepared by the American Petroleum Institute, Research Project 44. ? Annual Book ofASTM Standards* Vols 05.01 and 06.03. 4 For a more complete discussion of this test method, see Glasgow, Jr., A. Streiff, A. J., and Rossini, F. D., "Determination ofthe Purity ofHydrocarbons by^j Measurement ofFreezing Points," JournalofResearch, JRNBA, National JnstHuf ! of Standards and Technology. Vol 35, No. 6, 1945, p. 355. 5 For details, see Taylor, W, J., and Rossini, F. D., "Theoretical Analysis Time-Temperature Freezing and Melting Curves as Applied to Hydrocarbons;*;' Journal ofResearch, JRNBA. Nat, Bureau Standards, Vol 32, No. 5,1944, p. 197; also Lewis, O. N., and Randall, M., "Thermodynamics and the Free Energy of;..,: Chemical Substances/' 1923, pp. 237, 238, McGraw-Hill Book Co,, New Yoric/if NY. 572 DUP050296134 D 1016 ons is often needed to help control their manufacto determine their suitability for use as reagent s or for conversion to other chemical intermediates hed products. Sampling Apparatus, as shown in Fig. 1, for with" liquefied gases (for example, 1,3-butadiene) from i storage cylinders. distilling Apparatus, as shown in Fig. 2, for removing counts ofpolymer from low-boiling compounds (for ||, 1,3-butadiene) by simple distillation at atmospheric distilling Apparatus, as shown in Fig. 3, for removing ounts of polymer from compounds with boiling room temperature (for example, isoprene) by on at atmospheric pressure. Vacuum Distilling Apparatus and Transfer Trap, as |in Fig. 4, for removing dissolved air and large |ts of polymer from a compound (for example, 1,3ne or styrene), by repeated freezing and evacuation, led by distillation of the compound in vacuum in a em. fterials Carbon Dioxide Refrigerant--Solid carbon dioxide in ble liquid. Trichloroethylene is recommended. : 3: Solid Carbon Dioxide--Warning--Extremely cold Liberates heavy gas which may cause suffocation. Contact t causes bums or freezing, or both. Vapors may react violently magnesium or aluminum alloys. See Annex Al.l. Jiylene: Warning--Harmful if inhaled. High concentrations ; unconsciousness or death. Contact may cause skin irritation i. See Annex A1.2. Use refrigerant bath onlywith adequate don! ' Liquid Nitrogen or Liquid Air--(Warning--See Note ' use as a refrigerant If obtainable, liquid nitrogen is able because of its safety. f.l Use liquid nitrogen refrigerant only with adequate ition. If liquid air is used as a refrigerant, it is ttive dial any glass vessel containing hydrocarbon or fr* combustible compound and immersed in liquid air be with a suitable metal shield. The mixing of a trbon or other combustible compound with liquid air jito the breaking of a glass container would almost iinly result in a violent explosion. If liquid nitrogen is I as a refrigerant, no hydrocarbon sample should ever be titled to cool below the condensation temperature of t (-183'C at atm). This would not he likely to occur in i operation, but might occur if the apparatus were left ftended for some time. : 4: Warning--Extremely cold. Liberates gas which can cause n. Contact with skin bums or freezing, or both. Vapors can [(violently with hot magnesium or aluminum alloys. See Annex A1.3 jjfA 1.4. h-ocedure |i'l Measure the freezing point as described in Test hod D 1015, using the modifications and constants given ctions 8 to 26 of this test method for the specific hpounds being examined. No t e 5--The estimated uncertainty in the calculated value of the purity as referred to in Sections 8 through 26 is not equivalent to the precision defined in RR D-2-1007. 8. n-Butane6 No t e 6: Warning--Extremely flammable liquefied gas under pres sure. Vapor reduces oxygen available for breathing. See Annex A 1.7. 8.1 Determine the freezing point from freezing curves, with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means ofa cold rod. 8.2 The method of obtaining the samples shall be as follows: Assemble the apparatus for obtaining the sample as shown in Fig. 1, but with no lubricant on the ground-glass joints and with the valve at the bottom of the cylinder, so that sampling is from the liquid phase. Attach to C an absorption tube containing anhydrous calcium sulfate or other suitable desiccant (except magnesium perchlorate) so that water is not introduced into the system (Note 7). Fall the flask F with the carbon dioxide refrigerant to within about 51 mm (2 in.) of the top. After about 20 or 30 min, when the system will have cooled sufficiently, remove the absorption tube and begin the collection of liquid n-butane by opening the valve K and adjusting the needle valve J so that the sample is collected at a rate of 1 to 2 mL (!iquid)/min in the condensing tube E. No t e 7--However, if some water does condense with the hydro carbon, the freezing point will not be affected significantly because ofthe extremely low solubility of water in the hydrocarbon at the freezing point of the latter. 8.3 Assemble the freezing point apparatus. Place the cooling bath in position around the freezing tube (O in Fig. 1 of Test Method D 1015). letting the temperature as read on the platinum thermometer reach about -80C when all the sample has been collected. 8.4 When 50 mL of liquid (temperature about --80"C) has been collected in the condensing tube, close the valve K (Fig. 1) and allow the liquid which has collected at 1 to warm and transfer to the condensing tube (Note 8). Replace the attaching tubes G and D on the condensing tube by caps. The liquid sample is now ready for introduction into the freezing tube (O in Fig. 1 of Test Method D 1015). No t e 8--In case the original sample contained water, there will remain at / some water that may be discarded after the hydrocarbon portion has been collected as outlined above. 8.5 When the temperature of the platinum thermometer is near --80C, remove the condensing tube (E in Fig. 1) from the Dewar flask. Wrap a cloth around the upper portion of the condensing tube (for ease of handling and for preventing the refrigerating liquid from contaminating the sample on pouring), and after removing the caps on the condensing tube, raise the stopper holding the platinum thermometer, and pour the sample through the tapered male outlet of the condensing tube into the freezing tube (O in Fig. 1 of Test 6 For further details, see Glasgow. Jr., A. R., et al. "Determination of Purity by Measurement or Freezing Points of Compounds Involved in the Production of Synthetic Rvbhcr," Analytical Chemistry, ANCHA, Vol 20,1948, p. 410. 573 DUP050296135 # D 1016 0 (Joint, I 12/30) Scale ll A--Three-way Tstopcock, borosilicate glass (similar to Coming Pyrex No. 7420). 5--Connection to vacuum for purging and for evacuating system CDEGHI. C--Capillary tube for venting, to which drying tube is also connected. D--Joint, standard taper, 12/30. borosilicate glass. E--Condensing tube, borosilicate glass. F--Dewar flask, 1-qt size, borosilicate glass (similar to American Thermos Bottle Co. No. 8645). 6--Tubing, borosilicate glass, 10 mm in outside diameter, with spherical ground-glass joints, 18/7. H--Tubing, silicate glass, 10 mm in outside diameter,- with spherical ground-glass joints, 18/7. I--Metal connection, brass spherical male joint at one end fitting to connection to needle valve at other end. J--Needle valve, brass. K--Valve on cylinder containing hydrocaibon material. L--Standard cylinder containing hydrocarbon material. M--Fitting to connect needle valve J to valve K on cylinder. FIG. 1 Apparatus for Obtaining Sample Method D 1015). Quickly replace the stopper holding the platinum thermometer and start the stirrer, with dry air flowing into the upper portion of the freezing tube through M (Fig. 1 of Test Method D 1015). 8.6 Because the material is normally gaseous at room temperature, care should be taken in disposing ofthe sample safely. 8.7 For w-butane, the freezing point for zero impurity, in air at 1 atm, is as follows: t/0 = 138.362 0.025C (3) and the cryoscopic constants are: A = 0.03085 mole fraction/C and B = 0.0048 mole fraction/C. 8.8 The cryoscopic constants given in 6.7 are applicable to samples of n-butane having a purity of about 95 mole % or better, with no one impurity present in an amount that exceeds its eutectic composition with the major component. 8.9 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: ' 574 DUP050296136 # D 1016 Dewar vessel, 1-qt capacity, borosilicate glass. I^CIamp. Distilling tubs, boroslllcate glass, 25 mm in outside diameter. Standard-taper ground-glass joint, 24/40 boroslllcate glass. -Tubing, 10 mm in outside diameter, boroslllcate glass. ||H'-f-Spherical ground-glass joints, 18/7, boroslllcate glass. j-Tubing, 8 mm In outside diameter, borosilicate glass. p-Recelver, 35 mm in outside diameter, 150 mm in length, borosilicate glass. FIG. 2 Simple Distilling Apparatus for Normally Gaseous Substances Calculated Purity, mole% Uncertainty, plus or minus, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96to97 95 to 96 0.08 0.09 0.10 0.12 0.15 0.20 Isobutene6 |No t b 9: Warning--Extremely flammable gas under pressure. Vapor duces oxygen available for breathing. See Annex A 1.7. I9. .1 Determine the freezing point from freezing curves ath the cage stirrer, with a cooling bath of liquid nitrogen liquid air), with a cooling rate of 0,3 to 0..8C/min for the Iquid near the freezing point, and with crystallization pjduced immediately below the freezing point by means of a bid rod. 9.2 Obtain the samples as follows: Assemble the apparatus j>r obtaining the sample as shown in Fig. 1, but with no pbricant on the ground-glass joints and with the valve at the ifottom of the cylinder, so that sampling is from the liquid Ihase. Attach to C an absorption tube containing anhydrous galcium sulfate or other suitable desiccant (except magnegum perchlorate) so that water is not introduced into the item (Note 7), Fill the flask F with the carbon dioxide rigerant to within about 51 mm (2 in.) of the top. After bout 20 or 30 min, when the system will have cooled fcfflciently, remove the absorption tube and begin the lollection of liquid isobutane by opening the valve K and A--Standard-taper, ground-glass joint, 24/40, borosilicate glass. B--Distilling flash, round bottom, 200-mL capacity, borosilicateglass. C--Tubing, 10 mm in outside diameter, borosilicate glass. D, O'--Spherical ground-glass joints, 18/7. borosilicate glass. E--Dewar flask, 1-qt capacity, borosilicate glass. F--Receiver, same as J In Fig. 2. FIG. 3 Simple Distilling Apparatus for Normally Liquid Substances adjusting the needle valve J so that the sample is collected at a rate of 1 to 2 mL (liquid)/min in the condensing tube E. 9.3 Assemble the freezing point apparatus. Place the cooling bath in position around the freezing tube (O in Fig. 1 of Test Method D 1015), letting the temperature as read on the platinum thermometer reach about --80C when all the sample has been collected. -- 9.4 When 50 mL of liquidjtemperature about -80C) has been collected in the condensing tube, close the valve K (Fig. 1) and allow the liquid which had collected at I to warm and transfer to the condensing tube (Note 8). Replace the attaching tubes, G and D, on the condensing tube by caps. The liquid sample is now ready for introduction into the freezing tube (O in Fig. 1 of Test Method D 1015). 9.5 When the temperature of the platinum thermometer is near -80C, remove the condensing tube (E in Fig. 1) from the Dewar flask. Wrap a cloth around the upper portion of the condensing tube (for ease of handling and for preventing the refrigerating liquid from contaminating the sample on pouring), and after removing the caps on the condensing tube, raise the stopper holding the platinum thermometer, and pour the sample through the tapered male outlet of the condensing tube into the freezing tube (O in Fig. 1 of Test Method D 1015). Quickly replace the stopper holding the platinum thermometer and start the stirrer, with dry air flowing into the upper portion of the freezing tube through M(Fig. 1 of Test Method D 1015). 575 i. ii DUP050296137 B(Tube IOmm.O.D.1 V H E(Distilling Tube) D(Veto! Shield See R, Fig. I Legend) D1016 HfPyrex Stopcock RtTo Drying Tube) K{To Vacuum Pump) L(Stopcock) L' Hhl^To Vacuum, ] p--M(24/40 $ Joint) J S-r"N{Tronsfer Trap, S0(i-Pint Dewar) A, A'--Standard-taper ground-glass joints, 14/35 borosillcate glass. B--Tubing, 27 mm in outside diameter, borosilicats glass. C, C--Clamp. D--Brass cylinder, 273 mm (10% In.) in length, 28.6 mm (1 Vo in., in inside diameter; for precautions in use of liquid nitrogen and liquid air. eee R in legend to Fig. 1 of Test Method D1015 and Notes 2 and 3 of Test Method DT015. D'--Brass cylinder, 254 mm (10 in.) in length, 47.6 mm <1% in.) in inside diameter, (see above). --Original sample. E'--DistBled sample. F, F'--Dew flask, 0.0009-m3 (1 -qt) capacity, borosillcate glass. 6 and GAbestos pad. H. H', H"--Stopcock, ground tor high vacuum, borosillcate glass. /---Spherical ground-glass joint, 18/7, borosilicate glass. J--Condensing tube, used as trap (see in Fig. 1). K--Connection to vacuum system. L, /.'--Stopcock, ground for high vacuum, borosilicate glass. M--Standard-taper ground-glass joint, 24/40 borosilicate glass. M--Receiver withdrawal, 36 mm in outside diameter, borosilicate glass. O--Dewar flask, 0.00i>5-m3 (1-pt, capacity, borosllcate glass. P--Connection to vacuum. _ ' Q--Funnel with extension, 4 mm in inside diameter, borosilicate glass. R--Connection to drying tube, borosilicate glass. FIG. 4 Apparatus for Simple Vacuum Distillation 9.6 Because of the fact that the material is normally gaseous at room temperature, care should be taken in disposing of the sample safely. ! 9.7 For isobutane, the freezing point for zero impurity, in air at 1 atm, is: 1,0 = -159.605 0.025C and the cryoscopic constants are: (4) A = 0.04234 mole fraction/C and B = 0.0057 mole fraction/C, 9.8 The cryoscopic constants given in 9.7 are applicable to samples of isobutane having a purity of about 95 mole % or better, with no one impurity present in an amount that exceeds its eutectic composition with the major component. 9.9 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole% Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 10. //-Pentane Uncertainty, plus or minus, mole % 0.10 0.11 0.12 0.14 0.16 0.20 No t e 10: Warning--Extremely flammable liquid. Harmful if in haled. Vapors may cause flash fire. See Annex A1.8. 10.1 Determine the freezing point' from freezing curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. 10.2 To obtain the sample, cool the container and //-pentane to near 0"C and transfer a sample oTabout 60 mL (liquid at the given temperature) to a graduated cylinder which has been kept refrigerated slightly below 0"C. The sample is now ready for introduction into the freezing tube which should be precooled to near --80C. 10.3 For //-pentane, the freezing point for zero impurity, in air at 1 atm, is as follows: t/0 = -129.730 0.015'C ' (5) and the cryoscopic constants are: A - 0.04906 mole fraction/'C and B = 0.0042 mole fraction/"C. 10.4 The cryoscopic constants given in 10.3 are applicable to samples of //-pentane having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 10.5 The estimated uncertainty in the calculated value/?!, the purity is as follows, in mole %: 576 DUP050296138 t D 1016 Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.07 0.08 0.09 0.10 0.12 0.14 1 Isopentane Mo t e II: Warning--Extremely flammable liquid. Harmful if inled. Vapors may cause flash fire. See Annex A 1.8. 1.1 Determine the freezing point from melting curves the double helix stirrer, with a cooling bath of liquid Sogen (or liquid air) to obtain the slurry of crystals and njd, and a warming bath of carbon dioxide refrigerant, a cooling rate of 0.3 to 0.8C/min for the liquid near the tzing point and with crystallization induced immediately tftw the freezing point, by seeding with crystals. (Crystallitibn may also be induced with a cold rod, but the recovery im iUndercooling will not be as rapid.) [J-1S.2 To obtain a sample, cool the container and isopente to near 0C and transfer a sample of about 65 mL uid at the given temperature) to a graduated cylinder ich has been kept refrigerated slightly below 0C. The iple is now ready for introduction into the freezing tube ich should be precooled to near --80C. 11.3For isopentane, the freezing point for zero impurity, air at 1 atm, is as follows: t/0 => -159.905 0.015"C (6) id the cryoscopic constants are: A = 0.04829 mole fraction/C and B -- 0.0058 mole fraction/C. j l 1.4 The cryoscopic constants given in 9.3 are applicable isamples of isopentane having a purity ofabout 95 mole % itter, with the usual impurities and with no one impurity jiresent in an amount which exceeds the composition of the Ijectic with the major component. 1.5 The estimated uncertainty in the calculated value of ie purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole 9S 0.07 0.08 . 0.09 0.10 0.12 0.14 n-Hexane i No t e 12: Warning--Extremely flammable. Harmful if inhaled. May induce nerve cell damage. Vapors may cause flash fire. See Annex ', f 12.1 Determine the freezing point from freezing curves frth the cage stirrer, with a cooling bath of liquid nitrogen ?rliquid air), with a cooling rate of 0.3 to 0.8"C/tnin for the jluid near the freezing point and with crystallization in deed immediately below the freezing point by means of a !bld rod. #12.2 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by means of i pipet or by pouring into a graduated cylinder. 12.3 For n-hexane, the freezing point for zero impurity, in air at 1 atm, is as follows: f/0 = -95.322 0.010C (7) and the cryoscopic constants are: A = 0.04956 mole fraction/C and B- 0.0039 mole fraction/'C. 12.4 The cryoscopic constants given in 12.3 are applicable to samples of n-hexane having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 12.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 13. n-Heptane Uncertainty, plus or minus, mole % 0.05 0.06 0.07 0.08 0.10 0.12 No t e 13: Warning--Flammable. Harmful if inhaled. See Annex A1.10. 13.1 Determining the freezing point from freezing curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. 13.2 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by-means of a pipet or by pouring into a graduated cylinder. 13.3 For w-heptane, the freezing point for zero impurity, in air at 1 atm, is: lf0 = -90.58.1 0.010C (8) and the cryoscopic constants are: A = 0.05065 mole fraction/'C and B = 0.0033 mole fraction/C. -- 13.4 The cryoscopic constants given in 13.3 are applicable to samples of -heptane having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 13.5 The estimated'uncertainty in the calculated value of tbe purity is as follows, in mole %: Calculated Purity, mole % Uncertainty, plus or minus,, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 0.05 0.06 0.07 0.08 0.10 0.12 14. -Octane No t e 14: Warning--Flammable. Harmful if inhaled. See Annex AMO. 14.1 Determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of carbon dioxide 577 .... X7S3K8B DUP050296139 # D 1016 refrigerant at a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. - 14.2 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by means of a pipet or by pouring into a graduated cylinder. 14.3 For n-octane the freezing,point for zero impurity, in air at 1 atm, is as follows: f/0 = -56.764 0.010'C (9) and the cryoscopic constants are: A = 0.05329 mole fraction/C and B ~ 0.003 i mole fraction/C. 14.4 The cryoscopic constants given in 14.3 are applicable to samples of -octane having a purity ofabout 95 mole. % or better, with the usual impurities and with no impurity present in an amount that exceeds the composition of its eutectic with the major component. 14.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 6.05 0.06 0.07 0.08 0.10 0.12 IS. 2,2,4-Trimethylpentane , No t e 15: Warnittg--Extremely flammable. Harmful if inhaled. Va pors may cause flash lire. See Annex Al.l 1. 15.1 For samples having a purity greater than about 99.5 mole %,. determine the freezing point from melting curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), and a wanning bath of solid carbon dioxide refrigerant, with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point and with crystallization in duced immediately below the freezing point by means of a cold rod. 15.2 For samples having a purity less than about 99.5 mole %, determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0".8'C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. 15.3 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by means of pipet or by pouring into a graduated cylinder. 15.4 For 2,2,4-trimethylpentane, the freezing point for zero impurity, in air at 1 atm, is as follows: f/0 = -107.373 0.010"C (10) and the cryoscopic constants are: A = 0.04032 mole fraction/"C and B = 0.0043 mole fraction/C. 15.5 The cryoscopic constants given in 15.4 are applicable to samples of 2,2,4-trimethylpentane having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 15.6 The estimated uncertainty in the calculated value! the purity is as follows, in mole %: Calculated Purity, mole % Uncertainty, plus or minus, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 0.05 0.06 0.07 0.08 0.10 0.12 16. Methylcyclohexane No t e 16: Warning--Flammable. Harmful if inhaled. See Art A1.10. 16.1 Determine the freezing point from melting c u p with the double helix stirrer, with a cooling bath of liqui nitrogen (or liquid air) to obtain the slurry of crystals ] liquid, and h warming bath of carbon dioxide refrigeran with a cooling rate of 0.3 to 0.8C/min for the liquid near t freezing point and with crystallization induced immediate!! below the freezing point by seeding with crystals. (Crysta zation may also be induced with a cold rod, but the recoveH from undercooling will not be as rapid.) 16.2 Obtain a sample of 60 mL (measured at roof temperature) directly from the original container by pou into a graduated cylinder. 16.3 For methylcyclohexane, the freezing point for zep impurity, in air at 1 atm, is as follows: tf0 = -126.596 0.015C '(if and the cryoscopic constants are: A -- 0.03779 mole fractiori/C and A = 0.0032 mole fraction/C. 16.4 The cryoscopic constants given in 16.3~are applicabl to samples of methylcyclohexane having a purity of about mole % or better, with the usual impurities and with no oni impurity present in an amount that exceeds the compositioi of the eutectic with the major component. 16.5 The estimated uncertainty in the calculated value the purity is as follows, in mole %: Calculated Purity, mole % Uncertainty, plus or minus, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 0.05 0.06 0.07 0.08 0.10 0.12 17. Isobutene6 No t e 17: Warning--Extremely flammable liquefied gas under presj| sure. Vapor reduces oxygen available for breathing. See Annex A 1.6. 17.1 Determine the freezing point from freezing curves.^ with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for tbfsf liquid near the freezing point, and with crystallizatio induced immediately below the freezing point by means ofa cold rod. 17.2 Obtain the samples as follows: Assemble the appa| ratus for obtaining the sample as shown in Fig. 1, but within lubricant on the ground-glass joints and with the valve bottom of the cylinder, so that sampling is. from-the ii< 578 i !ji111 u DUP050296140 # D 1016 se. Attach to C an absorption tube containing anhydrous sum sulfate or other suitable desiccant (except magne|m perchlorate) so that water is not introduced into the i. (Note 7). Fill the flask F with the carbon dioxide geraht to within about 51 mm (2 in.) of the top. After put 20 or 30 min, when the system will have cooled Idently, remove the absorption tube and begin the flection of liquid isobutene by opening the valve K and Ousting the needle valve / so that the sample is collected at ste of 1 to 2 mL (liquid)/min in the condensing tube E. 17.3 Assemble the freezing point apparatus. Place the pling bath in position around the freezing tube (O in Fig. 1 Fest Method D 1015), letting the temperature as read on ( platinum thermometer reach about --80C when all the fiple has been collected, '.4 When 50 mL of liquid (temperature about -80C) [ been collected in the condensing tube, close the valve K Y 1) and allow the liquid which has collected at I to warm ((transfer to the condensing tube (Note 8). Replace the aching tubes G and D on the condensing tube by caps. The f sample is now ready for introduction into the freezing be (O in Fig. 1 of Test Method D 1015). Ji7.5 When the temperature of the platinum thermometer fpear --80C, remove the condensing tube (E in Fig. 1) from : Dewar flask. Wrap a doth around the upper portion of condensing, tube (for ease of handling and for preventing refrigerating liquid from contaminating the. sample on puring), and after removing the caps on the condensing i?e, raise the stopper holding the platinum thermometer, I pour the sample through the tapered male outlet of the ndensing tube into the freezing tube (O in Fig. 1 of Test ethod D 1015). Quickly replace the stopper holding the gtinum thermometer and start the stirrer, with dry air Swing into the upper portion of the freezing tube through % (Fig. 1 of Test Method D 1015). 17.6 Because of the fact that the material is normally jseous at room temperature, care should be taken in posing of the sample safely. 17.7 For isobutene, the freezing point for zero impurity, f air at I atm, is as follows: l/X) = -140.337 0.020C (12) l the cryoscopic constants are: A = 0.04044 mole fraction/C and B = 0.005 mole fraction/C. , 17.8 The cryoscopic constants given in 17.7 are applicable i samples of isobutene having a purity of about 95 mole % better, with no one impurity present in an amount that xceeds its eutectic composition with the major component. i.17.9 The estimated uncertainty in the calculated value of lie purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.08 0.09 0.10 0.12 0.15 0.20 18. 1,3-Butadiene6 No t e 18: Warning--Extremely flammable liquefied gas under pres sure. May form explosive peroxides upon exposure to air. Harmful if inhaled. Irritating to eyes, skin, and mucous membranes. See Annex A1.12. 18.1 Determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point and with crystallization in duced immediately below the freezing point by means of a cold rod. 18.2 Obtain the samples as follows: Assemble the appa ratus for obtaining the sample as shown in Fig. 1, but with no lubricant on the ground-glass joints and with the valve at the bottom of the cylinder, so that sampling is from the liquid phase. Attach to C an absorption tube containing anhydrous calcium sulfate or other suitable desiccant (except magne sium perchlorate) so that water is not introduced into the system (Note 7). Fill the flask F with the carbon dioxide refrigerant to within about 51 mm (2 in.) of the top. After about 20 or 30 min, when the system will have cooled sufficiently, remove the absorption tube and begin the collection of liquid 1,3-butadiene by opening the valve K and adjusting the needle valve J so that the sample is collected at a rate of 1 to 2 mL (liquid)/min in the condensing tube E. 18.3 Assemble the freezing point apparatus. Place the cooling bath in position around the freezing tube (O in Fig. 1 of Test Method D 1015), letting the temperature as read on the platinum thermometer reach about --80C when all the sample has been collected. 18.4 When 50 mL of liquid (temperature about --80C) has been collected in the condensing tube, close the valve K (Fig. 1) and allow the liquid which has collected atV to warm and transfer to the condensing tube (Note 8). Replace the attaching tubes G and D on the condensing tube by caps. The liquid sample is now ready for introduction into the freezing tube (O in Fig. 1 of Test Method D 1015). 18.5 In some cases, it will be desirable to remove the dimer, other C8 hydrocarbons, and higher polymer from the sample of 1,3-butadiene before determining the purity: For this removal, the procedure is as follows: Assemble the apparatus shown in Fig. 2_with a small amount (10 to 100 ppm) of tertiary butyl catechol or other suitable inhibitor placed in the bottom of the distilling tube E, with no lubricant on the ground-glass joints. It is also desirable to place at the bottom of the flask a piece of carborundum or other suitable material to prevent bumping. Make a connec tion to the atmosphere through an absorption tube (as previously described in this section) at FI' so that entering air is freed of carbon dioxide and water. Place a bath containing carbon dioxide refrigerant around the distilling tube , and also around the receiver J so that the small entrance and exit tubes of J are covered with at least 5 cm of the bath. After about 20 to 30 min, when the system will have precooled sufficiently, disconnect the connection to the atmosphere at H\ remove the cap F and introduce the liquid butadiene (temperature near --80C) by pouring through a precooled funnel (such as Q in Fig. 4 which may be cooled without contamination by liquid air or liquid nitrogen) into the distilling tube. Grease the cap F and replace immediately after the introduction of the sample. Then distill the material 579 DUP050296141 <11 D 1016 by removing the bath from the distilling tube and allowing it to warm in contact with the air of the room. Distillation is complete when the distilling tube has warmed to room temperature. Disconnect the receiver with the bath around it, cap it at H and H', and transfer 50 mL (liquid at about -80C) of the liquid butadiene to the freezing tube by pouring through I in a manner similar to that described for a sample collected in the condensing tube. 18.6 When the temperature of the platinum thermometer is near -80C, remove the condensing tube (E in Fig. 1) or the receiver {J in Fig. 2) from the Dewar. Wrap a cloth . around the upper portion of the condensing tube or receiver j (for ease of handling and for preventing the refrigerating . liquid from contaminating the sample on pouring), and after removing the caps on the condensing tube or receiver, raise the stopper holding the platinum thermometer, and pour the sample through the tapered male outlet of the condensing tube or the exit tube I of the receiver into the freezing tube (O in Fig. 1 of Test Method D 1015). Quickly replace the stopper holding the platinum thermometer and start the stirrer, with dry air flowing into the upper portion of the freezing tube through M (Fig. 1 of Test Method D 1015). 18.7 Because of the fact that the material is normally gaseous at room temperature, care should be taken in disposing of the sample safely. 18.8 For 1,3-butadiene, the freezing point for zero impu rity, in air at 1 atm, is tf0 = -108.902 0.010'C (13) and the cryoscopic constants are: A - 0.03560 mole fractioh/C and B = 0.0053 mole fraction/'C. 18.9 The cryoscopic constants given in 18.8 are applicable to samples of 1,3-butadiene having a purity of about 95 mole% or better, with no one impurity present in an amount that exceeds its eutectic composition with the major component. 18.10 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.05 0.06 0.07 0.08 0.09 0.10 19. Isoprene (2-Methyl-l,3-Butadiene)6 No t e 19: Warning--Extremely flammable liquefied gas under pres sure Vapor reduces oxygen available for breathing. See Annex A 1.6. 19.1 For samples having a purity greater than about 98 mole %, determine the freezing point from melting curves, with the double helical stirrer, with a cooling bath of liquid nitrogen (or liquid air), and a wanning bath of carbon dioxide refrigerant, with the jacket of the freezing tube open to the high vacuum system during the entire melting part of the curve, with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point and with crystallization in duced immediately below the freezing point by means of a cold rod. 19.2 For samples having a purity less than about 98 mole %, determine the freezing point from freezing curves with either the aluminum cage stirrer or the double helical stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point and with crystallization induced immediately below the freezing point by means of a cold rod. 19.3 The method of obtaining the sample is as follows: When the material is in a cylinder, assemble the apparatus shown in Fig. 1, with a suitable lubricant on the ground-glass joints, and with the valve below the body of the cylinder so that the sample is obtained from the liquid phase. Evacuate. the system by connecting, through heavy-walled tubing, the opening B to a vacuum line. After evacuation, close the stopcocks to the outlets B and C, and collect the sample of isoprene (55 mL, liquid, at about -80`C) in the refrigerated condensing tube E, in which was previously placed a small amount (about 10 to 100 ppm) of tertiary butyl catechol orother suitable inhibitor. The sample as thus collected will contain the bulk of any dimer present in the original material. The sample, including substantially all of the dimer, is now ready for introduction into the freezing tube, which should be precooled to near -- 100C. When the isoprene is contained in capped bottles or sealed ampoules, cool the container and isoprene to near 0C and transfer a sample of about 65 mL (liquid at the given temperature) to a graduated cylinder which has been kept refrigerated slightly below 0C. The sample, including such amount of dimer and higher polymer as was originally present, is now ready for introduction into the freezing tube, which should be' precooled to near -- 100C. 19.4 In most cases it will be desirable to remove the dimer and higher polymer from the sample of isoprene before determining the purity. For this removal, the procedure is as follows: Assemble the apparatus shown in Fig. ~3 with no lubricant on the ground-glass joints D and D'. Place a small amount of tertiary butyl catechol or other suitable inhibitor (about 10 to 100 ppm) in the receiver Fand a larger amount (about 100 to 1000 ppm) in the distilling flask B. It is also desirable to place at the bottom of the flask B a piece of carborundum or other suitable material to prevent bumping. Place a cooling bath of water-ice around the distilling flask B and a bath containing carbon dioxide refrigerant around the receiver F. Make a connection to the atmosphere at D` through which the air is first freed of carbon dioxide and water, using a tube containing Ascarite and anhydrous calcium sulfate or other suitable desiccant. Introduce the sample (at 0C) ii\to the flask B, place the cap A in position with a suitable lubricant between the grindings, and remove the connection to the atmosphere at D'. Place a water bath (at 40 to 50Q around the flask B and distill the material into F. Stop the distillation when a small residue remains in B with the water bath at 50C. Detach the receiver F at D and cap at D and D` with the bath containing carbon dioxide refrigerant still surrounding it. Remove the sample, with the upper portion ofthe container wrapped with a cloth (for ease of handling and for preventing the refrigerating liquid from contaminating the sample on pouring), from the flask E, remove the caps and introduce the sample into the freezing tube, previously precooled to near -- 100C, by pouring; through D'. For the procedure for introducing the sample into the tube, see 18.6 on 1,3-butadiene. 580 DUP050296142 # D 1016 ;iI9.5' If the sample contains a very large amount of dimer I polymer, then the simple preceding procedure outlined not suffice because the required distilling temperature iBe-foohigh, and a more complicated procedure is used,' follows: Assemble the apparatus shown in Fig. 4, with bitonplaced in the distilling tube and receiver (plus some borundum in the distilling tube to1 prevent bumping)-as viously described in 19.4, and with all the ground joints eept that < at A lubricated. Place a cooling bath of carbon gjade'refrigerant around the distilling tube E. Permit air, of carbon dioxide and water, to enter the system 3Ugh RH" H'H in order to compensate for the'change in |ltnhe. When the sample is cooled, remove the cap A and Jreduce the sample through the funnel Q, which has been bodied with liquid air or liquid nitrogen. Then lubricate cap A and close the stopcocks H, H', and H". Place |uid air or liquid nitrogen around the condensing tube E ag. 1), which serves; as a trap, and also replace the carbon gpxidfe refrigerant around the distilling tube E (Fig. 4) with Tiiid pitrogen or liquid air. After the'isoprene has solidified, lcuh|e -the system by opening i?,and H' to the vacuum Ifein. Close the stopcocks fi and H' and remqve the bath fin E to allow the material to melt and release dissolved Crystallizes the material again and evacuate the system as Ifore. Repeat the process again, if necessary, to remove bstantially all the air. (If any hydrocarbon has been caught l the trap J; it should be distilled back into the tube E, with : stopcock H open and H` closed.) Distill the material into I' by placing carbon dioxide refrigerant around the receiver nd a water-ice bath around E (after the latter has warmed to 0C). Halt the distillation when the transfer of material |to the receiver has substantially halted, by admitting air I of water and carbon dioxide) into the system through H'H. Remove the sample from the receiving tube E lb the withdrawal receiver N. Evacuate the system LMNL, Ih L' open and L closed, through P and then close the l&pcock h'< Surround the receiver IV' by carbon dioxide gerant Remove the material by inserting the inlet tube Winter the receiver and then opening the stopcock L; This pOcedure avoids loss by evaporation. Then introduce the Iferial into the freezing tube,: previously precooled to near |0(PC, by pouring through the tapered joint at M. For the edure forintroducing the Sample into the tube, see 18.6 1,3-butadiene. P'19.6 For isDprene (2-methyl-l ,3-butadiene), the freezing Wnt fon zero'impurity, in air at 1 atm1, is: - tfQ = -145.964 O.Ctfo*C (14) |d the cryoscopic constants are: A -- 0.0330 mole fraction/C and B = 0.0030 mole fraction/"C. f 19.7 The cryoscopic constants given in 19.6 are applicable j> samples of isoprene having a purity of about 95 mole % or fetter, vritb no one impurity present in an amount that iteeeds the eutectic composition with the major component. |19.8 The estimated uncertainty in the calculated value of ie purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.08 0.10 0.12 0.15 0.20 0.25 20, Benzene No t e 20: Warning--Poison. Carcinogen. Harmful or fatal if swal lowed. Extremely flammable. Vapors may cause flash fire. Vapor harmfltl, may be absorbed through skin, See Annex A1.I3. 20.1 Determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of carbon dioxide refrigerant, with a cooling rate of 0.3 to 0:8C/min for the liquid near the freezing point and with crystallization in duced immediately below the freezing point by means of a cold rod. 20.2 Obthin a sample of 50 mL (measured at room temperature) directly from the original container by means ofa pipet or by pouring into a graduated cylinder. Then filter the sample directly into the freezing point tube (O in Fig. 1 of Test Method D 1015), through silica gel to remove water. See 9.3, and Fig. 5 of Test Method D 1015. 20.3 Fofbenzene, the freezing point for zero impurity, in air at 1 atm, is: fyo = 5.531 0.010C and the cryoscopic constants are: (15) A = 0.01523 mole fraction/'C and B -- 0;0032 mole fraction/C. 20.4 The cryoscopic constants given in 20.3 are applicable to samples ofbenzene having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 20.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.02 0.03 0.04 0.05 0.06 0.08 21. Toluene No t e 21: Warning--Flammable. Vapor harmful. See Annex A 1.14. 21.1 Determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air), with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. 21.2 A sample of 50 mL (measured at room temperature) is obtained directly from its original container by means of a pipet or by pouring into a graduated cylinder. 581 ` 'V t DUP050296143 D 1016 2L3 For toluene, the freezing point for zero impurity, in air at 1 atm, is: t/0 = -94.965 0.012'C (16) and the cryoscopic constants are: A = 0.02508 mole fraction/'C and B = 0.0019 mole fraction/'C. 21.4 The cryoscopic constants given in 21.3 are applicable to samples of toluene having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component 21.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.03 0.04 0.05 0.06 0.08 0.10 22. Ethylbenzene No t e 22: Warning--Flammable. Vapor harmful. See Annex A1.15. 22.1 Determine the freezing point from melting curves with the cage stirrer, with a cooling bath of liquid nitrogen (or liquid air) to obtain the slurry of crystals and liquid, and a wanning bath of carbon dioxide refrigerant, with a cooling rate of 0.3 to 0.8'C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by seeding with crystals. (Crystallization may also be induced with a cold rod, but the recovery from undercooling will not be as rapid.) 22.2 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by means of a pipet or by pouring into a graduated cylinder. 22.3 For ethylbenzene, the freezing point for zero impu rity, in air at 1 atm, is: tf0 = -94.949 0.015'C (17) and the cryoscopic constants are: A = 0.03471 mole fraction/'C and B = 0.0029 mole fraction/C. 22.4 The cryoscopic constants given in 22.3 are applicable to samples of ethylbenzene having a purity of about 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 22.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.05 0.06 0.08 0.10 0.12 0.14 23. o-Xylene No t e 23: Warning--Flammable. Vapor harmful. See Annex A1.16. 23.1 The freezing point is determined from freezing curves with the cage stirrer, with a cooling bath of carbon; dioxide refrigerant, with a cooling rate of 0.3 to 0.8'C/miii for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by seeding with crystals. (Crystallization may also be induced with a' cold rod, but the recovery from undercooling will not be as rapid.) 23.2 A sample of 50 mL (measured at room temperature) is obtained directly from its original container by means of a pipet or by pouring into a graduated cylinder. 23.3 For o-xylene, the freezing point for zero impurity, in air at 1 atm, is: f/0 =-25.167 0.005'C and the cryoscopic constants are: (18) A = 0.02659 mole fraction/'C and B - 0.0030 mole fraction/C. 23.4 The cryoscopic constants given in 23.3 are applicable to samples of o-xylene having a purity ofabout 95 mole % or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 23.5 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole% Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainly, plus or minus, mole % 0.02 0.03 0.04 -0.05 0.06 0,08 . 24. m-Xylene - No t e 24: Warning--Flammable. Vapor harmful. See Annex A 1.16. 24.1 Determine the freezing point from freezing curves with the cage stirrer, with a cooling bath of solid carbon dioxide refrigerant, with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by. seeding with crystals, (Crystallization may also be induced with a cold rod, but the recovery from undercooling will not be as rapid.) 24.2 Obtain a sample of 50 mL (measured at room temperature) directly from its original container by means of a pipet or by pouring into a graduated cylinder. 24.3 For m-xyle'ne, the freezing point for zero impurity, in air at 1 atm, is: tfa = -47.844 0.020'C (19) and the cryoscopic constants are: A = 0.02741 mole fraction/'C and B -- 0.0027 mole fraction/'C. 24.4 The cryoscopic constants given in 24.3 are applicable to samples of w-xylene having a purity of about 95 mole fc or better, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the major component. 24.5 The estimated uncertainty in the calculated value a the purity is as follows, in mole %: 582 DUP050296144 # D 1016 Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, mole % 0.05 0.06 0.07 0.08 0.10 0.12 5. p-Xylene | No t e 25: Warning--Flammable. Vapor harmful. See Annex AI.16. ' 25.1 Determine the freezing point from freezing curves rth the cage stirrer, with, a cooling bath pf carbon dioxide te'rcfrigerant, with a cooling rate of 0.3 to 0.8C/min for the 'squid near the freezing point, and with crystallization Sliced immediately below the freezing point, by seeding piti crystals. (Crystallization may also be induced with a bid rod, but the recovery from undercooling will not be as W-) . "2x2 Obtain a sample of 50 mL (measured at room tem perature) directly from the original container by rneans of a gipet or by pouring into a graduated cylinder. The sample is en filtered directly into the freezing point tube, (O in Fig. 1 "Test Method D 1015), through Silica gel to remove water. : 9.3 and Fig. 5 of Test Method D 1015. 25.3 For p-xylene, the freezing point for zero impurity, in Hr at I atm, is: . </o 13.258 0.012"C |nd the cryoscopic constants are: (20) A -- 0.02509 mole fraction/'C and B = 0.0028 mole fraction/C. 25.4 The cryoscopic constants given in 25.3 are applicable I samples ofp-xylene having a purity ofabout 95 mole % or letter, with the usual impurities and with no one impurity sent in an amount that exceeds the composition of its iitectic with the major component. 25.5 The estimated uncertainty in the calculated value of |he purity is as follows, in mole %: Calculated Purity, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 Uncertainty, plus or minus, moie % 0.03 0.04 0.05 0.06 0.08 0.10 f|6. Styrene (Ethenylbenzene)6 | No t e 26: Warning--Flammable. Vapor harmful. See Annex A1.15. 26.1 Determine the freezing point from freezing curves with the cage stirrer, with cooling bath of carbon dioxide refrigerant, with a cooling rate of 0.3 to 0.8C/min for the liquid near the freezing point, and with crystallization induced immediately below the freezing point by means of a cold rod. 26.2 Obtain a sample of 50 mL (measured at room temperature) directly from the original container by means of a pipet or by pouring into a graduated cylinder. 26.3 If the previous treatment Or storage condition of material was such that dimerization or polymerization may have occurred, the dimer or polymer should be removed by a 'simple vacuum distillation (Fig. 4), using the same procedure as described under isoprene (see 19.5) except that carbon dioxide refrigerant is used to refrigerate the receiver and the sample is distilled at room temperature. 26.4 For styrene, the freezing point for zero impurity, in air at 1 atm, is: //0= -30.610 0.008'C and the cryoscopic constants are: (21) A -- 0.02365 mole fraction/'C and B -- 0.0044 mole fraction/C. 26.5 The cryoscopic constants given in 26.4 are applicable to samples of styrene having a purity of not less than about 95 mole %, with the usual impurities and with no one impurity present in an amount that exceeds the composition of its eutectic with the main component. 26.6 The estimated uncertainty in the calculated value of the purity is as follows, in mole %: Calculated Purity, mole % Uncertainty, plus or minds, mole % Over 99.5 99.0 to 99.5 98 to 99 97 to 98 96 to 97 95 to 96 0.04 0.05 0.06 0.07 0.08 0.09 - 27. Precision and Bias 27.1 Precision--The precision for this test method is governed by the precision of Test Method D 1015. Test Method D 1015 must be used for the freezing point determi nations in this test method.__ 27.2 Bias--The bias for this test method is governed by the bias of Test Method D 1015. Test Method D 1015 must be used for the freezing point determinations in this test method. 28. Keywords 28.1 crystallization; freeze point; LPG; pure hydrocar bons; purity 583 :;ai DUP050296145 ANNEX (Mandatory Information) Al. PRECAUTIONARY STATEMENTS Al.l Carbon Dioxide (Solid) Use with adequate ventilation. Avoid contact with skin and eyes. Do not taste. Do not put in closed or stoppered container. Do not enter storage area unless adequately ventilated. Al .2 Trichloroethylene Avoid prolonged or repeated breathing of vapor or spray unist. Use only with adequate ventilation. Eye irritation and dizziness are indications of overexpo sure. Do not take internally. Swallowing may cause injury, illness, or death. . Avoid prolonged or repeated contact with skin. .'.Do not get in eyes. A1.3 Liquid Nitrogen Use .with adequate ventilation. Avoid contact with skin or eyes. Do not taste. Do not put in .closed or stoppered container. Do not enter storage area unless adequately ventilated. A1.4 Liquid Air Avoid contact with skin or eyes. Do not taste. Do not put in closed or stoppered container. AlJ> Extremely Flammable Liquid Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid build-up of vapors and eliminate all sources of ignition, especially nonexplosion proof electrical devices and heaters. Avoid prolonged breathing of vapor or spray mist Avoid prolonged or repeated skin contact. A1.6 Flammable Liquefied Gas Keep away from heat, sparks, and open flame and nonexplosion proof electrical devices. Use with adequate ventilation. Never drop cylinder. Make sure cylinder is supported at all times. Keep cylinder out of sun and away from heat. Always use a pressure regulator. Release regulator tension before opening cylinder. Do not transfer cylinder contents to another cylinder. Do not mix gases in cylinder. Keep cylinder valve closed when not in use. Do not inhale. Do not enter storage area unless adequately ventilated. Stand away from cylinder outlet when opening cylinder^ valve. ` I Keep cylinder from corrosive environment., { Do not use cylinder without label. >1 Do not use dented or damaged cylinder. i For technical use only. Do not inhale. A1.7 n-Butane, Isobutane 1 Keep away from heat, sparks, open flame and noh?l explosion proof electrical devices. Use with adequate ventilation. 1 , ^1 Never drop cylinder. ' ' ,' I Make sure cylinder is supported at all times. !J Keep cylinder out of sun and away from heat. dj Always use a pressure regulator. Release regulator tension before opening cylinder. I | Do not transfer cylinder contents to another cylinder. I Do not mix gases in cylinder. J Keep cylinder valve closed when not in use. Do not inhale. .j ] Do not enter storage area unless adequately ventilated, ij Stand away from cylinder outlet when opening cylinder 1 valve. | Keep cylinder from corrosive environment. Do not use cylinder without label. Do not use dented or damaged cylinder. For technical use only. A1.8 n-Pentane, Isopentane Keep.away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. -- Avoid buildup of vapors and eliminate all sources of ignition, especially nonexplosion proof electrical apparatus ! and heaters. Avoid prolonged breathing of vapor or spray mist. Avoid prolonged or repeated contact with skin. A1.9 n-Hexane Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid buildup of vapors and eliminate all sources of ignition, especially all nonexplosion proof electrical appa ratus and heaters. Avoid breathing of vapor or spray mist, use respiratory protection devices as required. Avoid skin and eye contact; use impermeable gloves and aprons as required. A1.I0 n-Heptane, n-Octane, Methylcyclohexane Keep away from heat, sparks, and open flame. 584 DUP050296146 D 1016 Keep container closed. Use with adequate ventilation. Avoid prolonged breathing of vapor or spray mist. Avoid prolonged or repeated skin contact. $1.11 2,2,4-Trimethylpentane Keep away from heat, sparks, and open flame. Keep container closed. U Use with adequate ventilation. S Avoid buildup of vapors and eliminate all sources of aition, especially nonexplosion proof electrical apparatus |d heaters. iiAvoid prolonged breathing of vapor or spray mist. | M Avoid prolonged or repeated skin contact. P' P.J.12 1,3-Butadiene % Keep away from heat, sparks, and open flame. S Avoid contact with skin and eyes. 1 Use with adequate ventilation, j Do not use air pressure to transfer. |j Never drop cylinder. f! Make sure cylinder is supported at all times. |L Keep cylinder out of sun and away from heat. L Always use a pressure regulator, p Release regulator tension before opening cylinder. || Do not transfer cylinder contents to another cylinder. It Do not mix gases in cylinder. Keep cylinder valve closed when not in use. Hi Do not inhale. jr Do not enter storage areas unless adequately ventilated, ft s Stand away from cylinder outlet when opening cylinder I' valve. .[j Keep cylinder from corrosive environment. r|* Do not use cylinder without label. '*' Do not use dented or damaged cylinders. For technical use only. Avoid breathing vapors. A1.13 Benzene Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Use fume hood whenever possible. Avoid buildup of vapors and eliminate all sources of ignition, especially nonexplosion proof electrical apparatus and heaters. Avoid prolonged breathing of vapors or spray mist. Avoid contact with skin and eyes. Do not take internally. A1.14 Toluene Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid prolonged or repeated contact with skin. A1.15 Ethylbenzene, Styrene Keep away from heat, sparks, and open flame. A primary skin irritant. Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid prolonged or repeated contact with skin. Do not take internally. ' A1.16 o-Xylene, m-Xylene, p-Xylene Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid prolonged or repeated contact with skin. 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 tilts standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, era entirely their own responsibility. ' This standard Is subject to revision atany time by the responsible technical committee end must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invitedeither forrevision ofthis standerdor 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. 585 DUP050296147 Standard Test Method for Bromine index of Aromatic Hydrocarbons by Couiometric Titration1 This standard is issued under the fixed designation D 1492; the number immediately following the designation indicates the year of original adoption or, in the case of.revisi.on, the year of last revision. A number in parentheses indirates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the amount of bromine-reactive material in aromatic hydrocar- Slt is usually applied to materials having bromine ;es below 500. No t e l--Other test methods for determining bromine-reactive ma terial are Test Methods D 1159, D 1491, and D 2710. 1,2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D891 Test Methods for Specific Gravity of Liquid Indus trial Chemicals2 D1159 Test Method for Bromine Number of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration3 D1193 Specification for Reagent Water4 * D1491 Test Method for Bromine Index of Aromatic Hydrocarbons by Potentiometric Titrations D2710 Test Method for Bromine Index of Petroleum Hydrocarbons by Electrometric Titration6 D 3437 Practice for Sampling and Handling Liquid Cyclic Products7 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals7 D 4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter8 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12009 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility Of Subcommittee D16.0E on Instrumental Analysis. Current edition approved May 29, 1987. Published July 1987. Originally published as D 1492 - 57 T. Last previous edition D 1492-78 (1984)". 2 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vol 05.01. 4 Annual Book ofASTM Standards, Vois 06.03 and 11.01. f Discontinued; see 1985 Annual Book ofASTM Standards, Vol 06.03. 6 Annual Book ofASTM Standards, Vol 05.02. 7 AnnuaI Book ofASTM Standards,Vol 06.03. ' Annual Book ofASTM Standards, Vol 05.03. 9 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 3. Definition W 3.1 bromine index--the number of milligrams ofbromini consumed by 100 g of sample under given conditions. 4. Summary of Test Method 4.1 The specimen is added to a solvent and titrated witl electrolytically generated bromine at room temperature. Thi end point is determined by a dead-stop method. The time o titration is proportional to the bromine added to the sample 5. Significance and Use 5.1 This test method is suitable for setting specification, foi use as an internal quality control tool, and for use ir development or research work on industrial aromatic hydro carbons arid related materials. This test method gives a broac indication of olefinic content. It will not differentiate be tween the types of aliphatic unsaturation. - 6. Apparatus 6.1 Amperometric-Coulometric !Apparatus, automatic, suitable for bromine index titrations with variable generatoi ; current and timer. A typical circuit diagram of suitabk : equipment is shown in Fig. 1 ,10 6.2 Syringe, 2 mL with needle and rubber cap seal. 6.3 Stirrer, magnetic. 7. Reagents 7.1 Purity of Reagent--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.11 Other grades may be used, provided it is first ascertained that thejj 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 j conforming to Type III of Specification D 1193. 7.3 Electrolyte--To make 1 L, mix 600 mL of glacial j acetic acid, 260 mL of absolute methanol, and 140 mL of ; KBr solution (119 g/L). Dissolve 2 g of Mercury II acetate ini this mixture. 1 10 Available from Refinery Supply Co., 6901 E. 12th St., Tulsa, OK 74112. ""Reagent Chemicals, American Chemical Society Specifications," Ani.jc Chem. Soc., Washington, DC. For suggestions on the testing of reagents not listed* by the American Chemical Society, see "Reagent Chemicals and Standards," b|J Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United State)|; Pharmacopeia." g; DUP050296148 # D 1492 M1LUAMETER <W^rVW'/c TIMER r-M 0^.... VA,,RIABLE_ FRO.M> ZOK-EOOKj Dl -S iI5VAC > k 200 V STIRRING MA8NET FIG. 1 Automatic Amperometric-Coulometric Titrator Circuit 7.4 Potassium Bromide Solution (119 g/L)--Dissolve 119 ; of potassium bromide (KBr) in water and dilute to 1 L. . Hazards 8.1 Consult current OSHA regulations and supplier's !aterial Safety Data Sheets for all materials utilized in this test method. Sampling 9.1 Sampling should follow safe rules in order to adhere to ill safety precautions as outlined in the latest OSHA regula tions. Refer to Practice D 3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this test aethod. llO. Procedure .10.1 Place 50 mL of electrolyte in a clean, dry titration Icell, insert the electrodes, and begin stirring. Apply the . generation current in accordance with Table 1. 10.2 Before introducing any sample and immediately jtbefore each determination, bring the coulometer to equilib rium. 10.3 Draw into the syringe the amount of sample prejjscribed in Table 1 corresponding to the estimated bromine I'index. Wipe the needle with a clean cloth, attach a rubber | cap seal to the needle, and weigh on the analytical balance. Remove the seal, add the sample to the electrolyte, and set the timer to zero. Replace the seal, reweigh the syringe, and calculate the sample weight. No t e 2--If the density or specific gravity of the sample is known (Test Methods D 891, D 3505, or D 4052 can be used), the sample can be added by means of a pipet or microburet and the weight calculated. 10.4 Begin titration of the sample. As the titration pro ceeds, keep the generation current at the selected- value. The . generation ofbromine will continue as long as it is consumed by the sample. At the end point an incremental increase in bromine concentration causes the titrator and timer to stop automatically. Forty seconds after the titrator has shut off, continue the titration. If the titrator cuts off, immediately, the end point has been reached and the titration may be considered complete. Otherwise, it may be necessary to continue the titration in steps, waiting about 40 s between steps, until the titration time increment is 4 s or less. Note the total titration time and generation current. 11. Calculation 11.1 Calculate the bromine index, B, as follows: B - Tf x 965 79.9 W where: T = titration time, s, I = generation current, mA, and W = weight of sample, g. 587 Lillis DUP050296149 D 1492 -m 12. Precision and Bias12 12.1 The following data should be used for judging the acceptability of results (95 % probability) for bromine in dexes. from 0 to 50: 12.1.1 Repeatability--The standard deviation is 0.39. Du plicate results by the same operator should be considered suspect if results differ by more than 1.15. No t e 3--Number of data used, 91; number of degrees of freedom, 61; number of cooperating laboratories, 4. 12 Precision data were generated using titrators from Central Scientitic Co., 2600 S. Kostner Ave., Chicago, IL 60623. 12.1.2 Reproducibility--The standard deviation is 1,43 The results submitted by two laboratories should be const# ered suspect if they differ by more than 4.1. No t e 4--Number of data used, 41; number of degrees of freedom. 30; number of cooperating laboratories, 4. ' TABLE 1 Sample Size and Generation Current Estimated Bromine Index Sample Weight, 9 Generation Current, mA OtoZO 20 to 200 200 to 2000 1.000 0.600 0.060 1.0 5.0 5.0 The American Society for Testing and Materials takes no position respecting the velidity ofany patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of suoh n'ghta, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either torrevision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feelthat your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1316 Race St., Philadelphia, PA 19103. 588 DUP050296150 lb Designation: D 1493 - 90 Standard Test Method for Solidification Point of Industrial Organic Chemicals1 This standard is issued under the fixed designation D 1493; 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 rcapproval. jiiSScope 1.1 This test method covers a general procedure for lining the solidification point of most organic chemi- s having appreciable heats of fusion and solidification `nts-between --20 and +150C , 1.2 This test method is applicable only to relatively pure mpounds. Values obtained for grossly impure compounds n he low because of the freezing out of one component ~g the determination. _ ;i.3 In order that the test method may be used on many teriais, a choice of certain alternatives and a selection of crattis are permitted. The report (Section 12) requires X the selected alternatives must be stated. Materials to !ch the test method is applicable in particular detail hide phenol, naphthalene, and phthalic anhydride. toTE 1--A companion test method is Test Method D 852. 1.4 This standard does not purport to address all of die etyproblems associated with its use. It is the responsibility he user ofthis standard to establish appropriate safety and Ith practices and determine the applicability ofregulatory itations prior to use. For specific hazard statements, see on 8. Referenced Documents 2.1 ASTM Standards: 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials2 `852 Test Method for Solidification Point of Benzene2 , 1015 Test Method for Freezing Point of High Purity Hydrocarbons3 1016 Test Method for Purity of Hydrocarbons from Freezing Points3 3437 Practice for Sampling and Handling Liquid Cyclic Products2 > 3438 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride2 ;D 3852 Practice for Sampling and Handling Phenol and Cresyl Add2 ;E 1 Specification for ASTM Thermometers4 :E 77 Method for Inspection and Verification of Liquid- in-GlasS Thermometers4 * * *This test method is under the jurisdiction of ASTM Committee D-J6 on aatic Hydrocarbons and Related Chemicals and is the direct responsibility of "ommittee D16.0E on Instrumental Analysis. [Current edition approved May 25, 1990. Published July 1990. Originally lished as D 1493 - 57 T. Last previous edition D 1493 - 84 {1988)**. . Annual Book ofASTM Standards, Vol 06.03. * Annual Book ofASTM Standards, Vols 05.01 and 06,03. Annual Book ofASTM Standards, Vol 14.03. 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200s 3. Terminology 3.1 Definition: 3.1.1 solidification point--an empirical constant defined as the temperature at which the liquid phase ofa substance is in approximate equilibrium with a relatively small amount of the same substance in its solid phase. 3.1.1.1 Discussion--Solidification point is distinguished from freezing point, which is described in Test Method D 1015. An interpretation of mole percent purity in terms of freezing point is given in Test Method D1016. 4. Summary of Test Method 4. i- Solidification point is measured by noting the max imum temperature reached during a controlled cooling cycle after the appearance of a solid phase in a liquid sample. 5. Significance and Use 5.1 This test method is suitable for setting specifications on compounds of the type described in Section 1. It is also suitable for use as an intense quality-control tool and fn development and research work involving these compounds. 6. Apparatus 6.1 Thermometer--An etched-stem liquid-in-glass ther mometer having a range of no more than 30C shall be used. It shall be graduated in subdivisions no greater than'0.1C. Unless otherwise specified, it shall be calibrated, for 76-mm immersion, at no fewer than three points. These shall indude the approximate solidification point of the materiaLbeing tested and two other points, respectively, about 5C above and below the soIidificati6n~point. A total immersion ther mometer can be used if it is specified for testing a particular material, as, for example, benzene. (See Test Method D 852.) The thermometer shall conform to Specification E 1. It should be so chosen that the graduation at which the solidification point is to be observed is not hidden from view when the thermometer is inserted in the sample container. Suitable thermometers are ASTM Thermometers 89C to. 96C, inclusive. Table 1 lists several of these thermometers and the materials for which, respectively, they are useful in particular in accordance with this test method. A thermom eter, for example ASTM Thermometer 17C, 18C, or 91C, is needed when the average temperature of the emergent mercury column of the solidification-point thermometer is measured. 5 Avirilable from Superintendent of Documents, U S. Government Printing Office, Washington, DC 20402. 589 gP^pjj,jj DUP050296151 : n. T/alP # D 1493 TABLE 1 ASTlVi Thermometers tor Solidification Point Range of Temperature, C Selected Standardization Temperature, C Average Temperature of Emergent Mercury Column, C 20 to 50 60 to 90 120 to 150 40 80 130 25 30 35 M Material for Test phenol naphthalene phthalic anhydride "* fSample Container--A standard heat-resistant glass tesf tube with lip shall be used. The test tube shall measure 25 mm in outside diameter and 150 mm in length. '^6.3 Stirrer{see Fig. 1)--The stirrer shall consist of a 1-ffim ieter (B&S gage 18), corrosion-resistant wire bent into a ies of three circular loops about 25 mm apart at right _ies to the shaft, the circle ofeach loop being about 20 mm ihdiameter, so that the stirrer can move freely in the annular space between the inner wall ofthe sample container and the thermometer stem when the latter is inserted in the con tainer. The shaft of the stirrer may be of any convenient length not less than 150 mm, and shall pass through an off-center hole in a two-hole cork stopper, the center hole of which holds the thermometer. The upper end of the shaft may be attached to a reciprocating device for mechanical stirring, or may be formed into a loop to facilitate lifting it for stirring by hand. 6.4 Flasks: ,6i4.1, A 200-mL, side-tube, heat-resistant glass distillation flask as described in Test Method D 850 and 6.4.2 Two narrow-neck, heat-resistant glass Erlenmeyer flasks, 400-mL capacity each. 6.5 Heaters: 6.5.1 A hot plate, and 6.5.2 An electric heater that is fully adjustable as de scribed in TeSt Method D 850, or a bunsen or similar gas burner (see Section 9.2), or both. 6.6 Insulation Board--A sheet of hard insulation board 3 to 6 mm thick and L 5 cm square, with a circular hole 50 mm in diameter in the center of it, is needed if the drying procedure given in 9.2 is used. '4mm Appro* 22mm gS msci No t e 2--Items described in 6.7, 6.8, and 6,9, are not essential for routinely testing materials that have solidification points substantially above room temperature, for example above 30C; but, for referee testing, these items shall be used always, regardless of the solidification ' points of the materials being tested. 6.7 Air Jacket--A standard heat-resistant glass tube with, lip, 38 mm in outside diameter and 200 mm in length, shall be fitted with a cork stopper bored with a hole of 25 toi 26-mm diameter and into which the sample container is to be inserted up to its lip.- 6.8 Cooling Bath--A. 2-L beaker or similar suitable con tainer having an effective depth of at least 175. mm shall be/ filled with a cooling medium, which shall be glycerin for operating at temperatures between 145 and 25C, water and ice between 25 and 0C, and alcohol and dry ice between ft. and -25C. A thermostatically controlled agitated bath may; be used optionally. (See Fig.- 2 for assembly of apparatus.) 6.9 Clamp and Ring Stand--A clamp, attached to a stand, holds the air jacket rigidly just below its lip when it is immersed in the cooling bath to a depth between 160 and 200 mm. No t e 3--Items listed in 6.10 to 6.15 inclusive, are required only for checking the accuracy of the thermometer at the solidification point of the material being tested. This check is desirable to detect changes that occur in a thermometer with time and use and to minimize errors generally.6 6.10 Thermometric Cell--A sealed glass cell made from standard-wall glass tubing, 38 mm in outside diameter, and about 140 mm in length, has a thermometer well, 120 mm deep, formed as an integral part lengthwise in it. The cell contains a relatively pure crystallizable compound of known freezing point that fills it to a level about 10 mm above the height of the 76-mm immersion mark of a partial immersion thermometer when the latter is inserted in the well down to the bottom. The well shall he made from 10-mm tubing, about 8 mm in inside diameter. (See Fig. 3.) For a total immersion thermometer,The lengths of the cell and the well shall be increased to fit. The cell shall have a calibration temperature, T,, determined with a platinum resistance thermometer and assigned to it for use as a thermometric standard. (See Section 10.) 6.11 Vacuum Flask--An open-mouthed Dewar-type of vacuum-jacketed flask is needed. Its capacity shall be nomi nally 1 pt (500-mL) in size. It shall be provided with a base to hold it upright. (See Fig. 4.) 6.12 Oven--An electrically heated oven, preferably with internal circulation of air, shall be used if the crystallizable compound described in 6.9 is solid at room temperature. The oven must be thermostatically controlled over the temperature range of 60 to 200C with tolerance of 10C at FIG. 1 Stirrer 6 hnsgonio, D. P.. Pearson, E. G,, and Saylor, C. P. Temperature--Its Measurement and Control in Silence and Indttstry, Reinhold Publishing Corp.New York, NY, Vol 3. Part 1, 1962. pp. 219-230. 590 DUP050296152 Sltrrer D 1493 s - Thermometer m - Sample Container '`Cooling Both - Air Jacket L FIG. 2 Apparatus for Determining Solidification Point |y setting in this range. Its chamber must be large enough to lid the items described in 6.10, 6.11, 6.12 and 6.13 at the pnetime. A chamber of satisfactory size shall be cubic, 500 to a side. A thermometer shall be inserted at the top fth its bulb about 125 mm below the ceiling, of the lamber. _. |6.;13 Cradle--Two pieces of fireproof, l/4-in. (6.4-mm) rd are needed to support the thermometric cell in the ||pn. The dimensions of each piece shall be about 120 mm * length, 70 mm in width, and between 6 and 12 mm in ^6.14 Safety Items--For personal protection when han ging fragile cells with contents ofa molten compound that is jjskin-irritant or that has a melting point above 60C, the gerator will need a pair of heat-resistant gloves, a long A H I4cm FIG: 4 Reference Cell in Vacuum Flask rubber apron, and a transparent visor. 6.15 Magnifying Glass--For accurately reading the tem perature indicated by the thermometer, it is advantangeous to use a magnifying glass, provided with an eyepiece and a cross-hair, and mounted on a friction-slide that fits over the thermometer stem. 7. Reagents and Materials 7.1 Cork Stoppers--Suitable corks to be used as described in 6.2, 6.3, and 6.4. 7.2 Cooling Medium--Technical grade glycerin, technical grade methanol or denatured alcohol, water, ice, and dry ice fof use with the cooling bath. 7.3 Drying Agents--A molecular sieve7 zeolite with 4A size of pores shall be used for drying liquid hydrocarbons and phenol. The zeolite may be in the form of a'powder or of cylindrical granules about 3 mm in diameter. The granules are preferred. The pore size is critical, because pores larger than 4A will absorb some hydrocarbons preferentially.' So dium hydroxide pellets can be used for drying liquid hydrocarbons and other nonacidic compounds. Anhydrous calcium sulfate granules, free of dust, can also be used. 7.4 Packing Materials--Cotton wadding, cloth wipers, and glass wool for packing around glass cells of hot, molten compounds. Thin aluminum foil, light duty wrap, will also be needed as described in 10.10. 8. Hazards 8.1 Consult the current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. '% 'l' |*38 mm-*j 9. Preparation of Sample 9.1 If a sample is either a liquid or a solid consisting of lumps, flakes, powder, etc., take the portion for drying or FIG. d Thermometric Reference Cell 7 Molecular sieve 4A obtainable from the Linde Division, Union Carbide Corp., has been found satisfactory foe this ourpost* 591 L i "T i DUP050296153 ffi D 1493 analysis, or both, as specified below, directly from its container. Guidelines for taking samples from bulk are given in Practices D 3437, D 3438, and D 3852. 9:2 If a sample is a solid mass at room temperature, melt the entire sample by heating it at about 10C above its solidification point and swirl it for homogeneity before pouring the portion, as specified below, for drying and analysis, or both. 9.3 If the sample is to be dried before being tested, place about 100 g of the material in a 400-mL Erlenmeyer flask and add about 50 g of drying agent, for example, anhydrous calcium sulfate or sodium hydroxide pellets. Liquids shall be dried at room temperature and solids on a hot plate at about 10C above their solidification point. If the sample is hygroscopic, place a very loosely fitting stopper in the flask. After 15 min, decant the sample to another flask and repeat the drying step with occasional stirring. Pour sufficient Sample into the sample container to fill it to a depth of approximately 100 mm. Then proceed as described in 10.1. 9.4 Highly hygroscopic materials, or materials like refined phenol of which the solidification point is very sensitive to moisture, shall be dried as follows: Add 15 g of 4A molecular sieve to 100 g of the molten material in a 400-mL Erlenmeyer flask; stopper the flask very loosely and place it op a hot plate at a temperature at least 10'C above the solidification point of the sample, but not hot enough to cause the sample to boil or to decompose. For example, a sample of phenol shall be heated at 60C. Heat the sample for 20 min with agitation by swirling at 5-min intervals. This method of drying is satisfactory for .phenol containing as much as 2% water, Quickly transfer the dried sample, including any entrained drying agent, to the sample con tainer to a depth of about 100 mm. TTie layer of entrained drying agent, after it has settled in the sample container, must not exceed a depth of 15 mm, If there is any doubt as to the completeness of drying, decant the molten sample from the drying agent and repeat the procedure with fresh drying agent on the same sample. After drying the sample, proceed as described in 10.1. 9.5 In an alternative method, when specified, dry the sample by heating it to its initial boiling point. Support the distillation flask on the asbestos board over the bunsen burner or the electric heater by means of the ring stand. Attach, the clamp to the lower part of the neck of the flask. Transfer about 100 g of the sample to the flask and place a solid cork stopper in the neck. Heat the flask' slowly and allow the sample to melt and then to boil gently. Any water present in the sample will condense in the neck of the flask If considerable water is present, it will distill out of the side tube of the flask and it should be collected in a receiver and then discarded. This method shall not be used for materials that have initial boiling points below 80C or above 260Cv Allow the dry condensed liquid to rise in the neck ofthe flask by further heating, for not more than 1 min, until the liquid just reaches the side tube. Remove the source of heat and the Stopper. Let the sample cool for 1 min. Then warm the neck of the flask above the side tube with a very small flame of the bunsen burner to drive off any condensed moisture. Then stopper the flask with a dry cork. Let the sample cool until it can he, poured conveniently and safely; while its temperature is still at least 10C above its solidification point, swirl it in the flask to ensure homogeneity, and pour enough of it into the sample container to reach a depth of about 100 mm. Then proceed as described in 10.1. 9.6 If the sample is not to be fired but is to be tested as received, pour it in liquid form into the sample container to a depth of about 100 mm. If it is not liquid at room temperature, heat about 100 g of it in a 400-mL Erlenmeyer flask to a temperature about 10C above its melting point and swirl it for homogeneity before pouring it into the sample container. Use this procedure in the testing of refined naphthalene. Then proceed as described in 10.1. 9.7 If the sample is a water-immiscible substance, for example a liquid hydrocarbon, mid is specified to be tested after saturation with water, proceed as described in 10.6 to introduce the sample into the sample container. Then add one drop, about 0.06 g, of water; stopper the sample container, and shake it vigorously. Then proceed as de scribed in '10.1. 10. Procedure 10.1 The cooling bath temperature shall be 5 to 10C below the expected solidification point. When the solidifica tion point of the material under test is sensitive to cooling conditions, it is desirable to keep the bath at the 5C differential. Refined naphthalene and phenol- are two such materials. For naphthalene the cooling bath shall be held at 70 to 75C, and for phenol at 30 to 35C, the higher temperature being preferable in each range. Fit the sample container lip to its lip into the cork stopper of the air-jacket. Fit the thermometer and the stirrer into the two-hole stopper of the sample- container. Adjust the partial-immersion ther mometer so that it is immersed up to its 76-mm calibration mark in the sample. The bottom of the thermometer bulbwill then be about 24 mm above the bottom of the sample container. Use this procedure exactly when naphthalene, phenol, or phthalic anhydride is being tested. 10.2 Clamp the assembly, described in 10.1 and illus trated in Fig. 2;! to the ring stand and place it so that the air jacket is immersed vertically in the cooling bath to a depth at' which at least 100 mm of length of the sample container is below the surface of the cooling medium. . 10.3 Allow the sample to cool while stirring it at the rate of about 60 strokes per minute. A mechanical reciprocating device that will simulate hand stirring is permissible. The stirrer should not touch the thermometer or the wall of the sample container. Discontinue stirring after an appreciable amount of crystals has formed but while the sample is still mainly liquid. 10.4 Observe and record the thermometer readings at regular intervals, estimating degrees to the nearest 0.01C until the temperature rises from minimum, due to super cooling, to a maximum and finally begins to drop. The true maximum temperature is the solidification point. As the temperature approaches this point on the rise, thermometer readings should be taken at 10-s intervals in order to make sure that the temperature has reached its maximum, and at least three more readings should therefore then be taken at; the maximum level, until the first drop in temperature is. , noted. This will ensure against mistaking a temporary plateau of temperature level for the true maximum tempes t ature. If there is any doubt about the trend of the readihp^f 592 DU P050296154 D 1493 fitting a graph of temperature versus time on linear graph Her will help in interpreting the data clearly. Note the jprimental maximum temperature, (See Section 11 for ` eraiure corrections to be added to te.) |grE 4--The accuracy ofthe thermometer readings can be increased ising a magnifying glass that assures a reading on a line of sight indicular to the stem of the thermometer. This should be done in ftesting of refined naphthalene and phthalic anhydride. Also, for the jrd, the average temperature, to, of the emergent mercury column |ld be taken. (See 11.1 through 11.4.) |OTE 5--If the temperature rise after initial crystallization exceeds , remelt the sample by warming it gently in the sample container jjrepeat the test. Seed with two or three small crystals of the sample i 'the temperature is 0.2 to 0.3C below the expected solidification aj.\When the sample is a liquid, these crystals may be obtained by dii'g a small quantity of the liquid in a test tube immersed directly in jcooling bath. Some compounds have more than one solidification pt due to the occurrence of metastable phases. Therefore it is lential to select, for the seeding, crystals known to be of the desired %le phase as found by a previous determinination of solidification fit. As an alternative to induce crystallization, a chilled wire may be itituted in place of small crystals ofthe sample. 40TB 6--The procedure described in 10.5 to 10.10 inclusive, is uired only for checking the accuracy of the thermometer at the dification point of the material being tested. lflO.5 When the accuracy of the thermometer is to be lecked, as indicated in Notes 3 and 6, make the check by |eans of a thermometric cell. Check immediately before |termining the solidification point of the sample. To make pe that the temperature of the emergent mercury column [ the stem of the thermometer is the same during the check pduring the determination of solidification point, carry out i operations at the same spot. 10.6 The thermometric cell contains a crystallizable com||ind. This shall be preferably a pure sample of the same npound as the sample of which the solidification point is be determined with the thermometer that is being pecked. The solidification point of the material in the cell pall be certified by a referee from the measurement made nth an accurate platinum-resistant thermometer in the well pF'the cell. Repeat the measurement under comparable bnditions with the thermometer of unknown accuracy. The Terence between the two measurements is a correction for ! test thermometer at the temperature of the solidification |pint of the test sample. (See 11.4 through 11.8.) : 10.7 Inspect the thermometer very closely, preferably with Imagnifying glass, to make sure that there are no minute Jacks in the bulb and no air bubbles in the thread or column K mercury. Ifair bubbles are noted, remove them by cooling ||e thermometer in dry ice and tapping it gently. Place the hermometer down to its immersion mark in the cooling at the .temperature at which the bath will be held for ermining the solidification point of a sample of the ipound in the thermometric cell, and hold the thermom iter there for at least 'h h. For example, Thermometer 96C Shall be conditioned thus at about 126C for use in testing |hthalic anhydride. 10.8 If the compound in the thermometric cell is solid, it nust be melted in the oven under controlled conditions at a jpemperature above its melting point by 40 to 60C. An Increment of 60"C is preferred. For example, phthalic phydride is melted at 190C, oven temperature. First, Prepare a cradle to hold the cell, by placing the two pieces of fireproof board about 20 mm apart on the oven shelf, laying them flat with their long sides parallel. Place the thermometric cell lying down lengthwise in the groove thus formed by the boards and with the nipple, where the glass was sealed in the manufacture of the cell, facing upward. Place the vacuum flask on the oven floor at the same time for conditioning. If the vacuum flask is one that is set in its base with uintaite cement, do not heat it above 120C. If the compound in the thermometric cell is normally liquid or if its solidification point is below 45C, the conditioning of the cell and the vacuum flask shall be carried out at an appropriate temperature in the cooling bath instead of the oven, in a way similar to that used for the thermometer described in 10.7. For example, a cell containing benzene shall be conditioned in cold water at 4.5 to 5.0C, and a cell containing phenol shall be conditioned in hot water at 70 to 80C. An alternative way to condition the vacuum flask is to store within it, for 'h h, a thermometric cell, for example a duplicate or a dummy, which itself has been conditioned at the appropriate temperature. 10.9 Close the oven door and leave it closed for 10 min. Then open the door and rotate the cell one complete turn in the groove ofthe cradle before reclosing the door. Repeat this turning every 2 min until the crystals in the cell have melted completely. For phthalic anhydride, repeat this turning four or five times; the crystals will be completely molten in about 20 min. This melting procedure is fairly critical in order to avoid breakage of cells containing crystals that melt at about 80"C or higher and that are fused together in a lump in the cell. Using heat-insulating gloves, take the vacuum flask out and set it on its stand. Then wrap the hot cell In cotton wadding or in several layers of cloth wipers, with both ends of the cell exposed. With due precaution against bums, grasp the bundled cell and shake it vigorously, end to end in the direction of its long axis, until a slurry or mush of fine crystals appears in it. This fairly dense mush should appear practically all at once. Its occurrence can. be promoted by directing a gentle jet of air at the top of the cell or by touching the top with a lump of dry ice. Then continue the shaking for 5.0 s longer and, with a. layer of cloth wipers or cotton wadding about the cell to provide a snug fit-in the vacuum flask, insert the cejljight side up in the conditioned vacuum flask; lay additional wadding or glass wool over it, as shown in Fig. 4, sufficiently loose to allow the thermometer later to be inserted in the well of the cell. 10.10 Insert the thermometer, which has been condi tioned in accordance with 10.7, into the well of the cell. The fit must be snug, to ensure good heat transfer through the wall of the well to the bulb of the thermometer. If the fit is loose, either wrap a turn of aluminum foil around the bulb only, or pour into the well about 0.5 mL of glycerin preheated to just slightly below the solidification point of the material in the cell, in order to improve heat transfer. Adjust the top wadding about the stem ofthe thermometer so as not to obscure the mercury thread from sight. After 5 min read the temperature to the nearest 0.0 UC, using a magnifying glass to aid in visual estimation of hundredths of a degree. Read the temperature at regular, frequent intervals and note its maximum value, the uncorrected temperature, Tu. The time to attain the maximum, and then to reveal a distinct drop in temperature, varies for differen; materials. It must be 593 :31HHU DUP050296155 01493 not less than 10 min. The intervals at which temperature readings are taken shall be every 2 min after the first reading until the sixth reading; if the maximum reading is not attained after 15 min total elapsed time, readings shall then be made at 5-min intervals. After the first 15 min, take the average temperature, T,, of the emergent stem of the thermometer with another thermometer placed alongside with its bulb at a level about half way along the length ofthe emergent mercury column. Do not hold the thermometer that is being checked, because the warmth of one's fingers can affect the value Tu as much as 0.03C. 10.11 Platinum resistance or quartz thermometers may be used to calibrate the liquid in glass thermometers used in this test method. 11. Temperature Corrections 11.1 If a thermometer other than one of those listed in Table 1 was used in this test method, calculate and report a temperature correction to be added to t^ This correction is called the emergent stem correction. In a partial immersion thermometer, this correction compensates for the difference, (4 - 4), between 4, the stem temperature at which the scale of the thermometer was standardized, and 4, the observed average temperature of the emergent column of mercury. (See Method E 77.) See Note 6 for reference to 4. For 4, see the Selected Standardization Temperature in Table 1 or see Table 2 of Specification E 1. The correction is algebraically additive. Its value is calculated by the formula Kn{ts -- 4), where K is the differential coefficient of expansion between the liquid in the thermometer and the glass of which the thermometer is made. For mercury-in-glass thermometers graduated in degrees Celsius, K = 0.00016; and n is the number of degrees Celsius between the start of the scale on a partial immersion thermometer and 4, the experimentalmaximum temperature. 11.2 In a total immersion thermometer, the emergent stem correction is Calculated differently and is needed only when the thermometer is used at partial immersion. This correction compensates for the difference, (4 -- 4), between 4, the temperature of the bulk of the thermometer, and tm the observed average temperature ofthe emergent column of mercury. One way to assign a numerical value to tb is to measure te with a thermometer of which the scale is certified to be accurate within 0.02C and to take tb - 4. Another way is to repeat the procedure without using the air jacket; then, after observing 4, let the sample remain in the apparatus for 20,min more, measure 4 again, and take the temperature of the cooling bath for the value of tb in the term (4 -- 4). 11.3 The emergent stem correction is algebraically addi tive. Its value for a mercury-in-glass thermometer graduated in degrees Celsius is calculated by the formula 0.00016 N(tb - 4), where N is the number of degrees emergent from the bath. 11.4 Report the corrected temperature as follows: /,, = 4 + 0.00016 n (4 - /,,) for a partial immersion thermometer or t = 4 + 0.00016 N (4 -- 4) for a total immersion thermometer If the thermometer scale was certified to be accurate within 0.02"C when the test was made, report t,, or t',, as the solidification point. 11.5 For referee tests, either the thermometer shall bel. stipulated to be accurate within 0.02C of scale at the level of 1 4, or the thermometer shall be checked for accuracy,' immediately prior to the measurement of 4. (See Sections! 10.6 and 10.10.) In this check the apparent scalar error is I measured. It is the difference, (Te - T,,), between thef certified calibration temperature assigned to the thermal metric cell, and the uncorrected temperature observed! with the test thermometer at the solidification point of the f reference compound in the cell. If this difference is a number between +0.02 and --0.02C, it shall be disregarded as being i indistinguishable from zero by this measurement. If the " difference is either a positive or a negative number outside of the range from +0.02 to -0.02C, inclusive, it shall be applied as an algebraically additive scalar correction. 11.6 If the thermometer was selected in accordance with Table 1 and used in accordance with 10.10, and in general whenever the emergent stem temperature is the same in the checking procedure for accuracy as in the testing procedure for solidification point, that is, whenever T0 = 4, report solidification point as follows: 4 = 4 + Kn{tx - Q + (Tc - r,,) = 4, + (rc - r,,) 11.7 If a partial immersion thermometer other than one listed in Table 1 is used, and whenever Ta = 4, report solidification point as follows; 4 = tm + (Tc - Tu) - Km{Tt, - Ta) ' where m is the number of degrees on the scale between and the start of the scale. 11.8 If a total immersion thermometer is used, report, solidification point as follows: t'gt',, + (Tc-TJ-KM{Tc-Tc) , where M is the number of degrees on the scale between T,, and the level of the surface of the molten reference com pound in the cell. 12. Report 12.1 For completeness of record and for referee tests, report the following information: 12.1.1 Whether the sample was tested dry~or watersaturated or as received^. 12.1.2 Which method of drying, if any, was used, 12.1.3 Which drying agent, if any, was used, 12.1.4 Whether the airJacket and cooling bath were used, 12.1.5 Temperature of the cooling-bath, if it was used, 12.1.6. ASTM thermometer that was used, 12.1.7 the experimental maximum temperature, as the average of at least three readings of the maximum, value, to the nearest 0.01C (see 10.4), and 12.1.8 If one of the thermometers listed in Table 1 was used and if its scale was stipulated to be accurate within 0.02C when the test was made, report 4 as the solidification point. No t e 7--See Section 11 for calculations to be made if a thermom eter other than one ofthose listed in Table 1 was used or ifa temperature correction must be added to 4. 12.2 For referee tests of refined phenol, the report shall confirm that the following requirements have been met: 12.2.1 The sample was tested dry, 1: ill 12.2.2 The drying method described in 12.1 was used, 594 siSlIIilSlsMHiW DUP050296156 D 1493 .2.3 The drying agent used was molecular sieve 4A in ular form, .2.4 The air jacket and cooling bath were used, .275 The temperature of the cooling bath was between id 35C , and .2.6 ASTM Thermometer 91C was used. The report also include the following: .2.7 The value of te, .2.8 That scale error was stipulated to be negligible if it glected, and 2.9The value oftp, if, under 12.2.8, the report does not that scale error was stipulated to be negligible. 3 For referee tests of refined naphthalene, the report i conform that the following requirements have been 3.1 The sample was tested as received, .3.2 The air jacket and cooling bath were used, '2.B.3 The temperature of the cooling bath was between and 75C , and 2.3.4 A'STM Thermometer 93C was used. The report I also include the following: 2.3.5 The value of te, 2.3.6 That scale error was stipulated to be negligible if it eglected, and 2.3.7 The value of tp, if, under 12.3.6, the report does not te that scale error was stipulated to be negligible. 2.4 For referee tests of phthalic anhydride, the report '1 confirm that the following requirements have been met: 2.4.1 The sample was tested as received, 2.4.2 The air jacket and cooling bath were used, {2.4.3 The temperature of the cooling bath was between and 126C, and 2.4.4 ASTM Thermometer 96C was used. The report 11 also include the following: .4.5 The value of l,,. 12.4.6 That scale error was stipulated to be negligible if it is neglected, and 12.4.7 The value oftp, if, under 12.4.6, the report does not state that scale error was stipulated to be negligible. 12.5 When the sample is tested water-saturated and a standard correction for the effect ofthe moisture is specified, as for benzene as described in Test Method D 852, add the correction and report the corrected solidification point. 13. Precision and Bias 13. f For the materials reported respectively in accordance with 12.2, 12.3, and 12.4, .the precision of the solidification point at the level of 95 % confidence is as follows: Refined Material Phenol Naphthalene Phthalic anhydride Repeatability, "C 0.03 0.05 0.05 - Reproducibility, "C 0.07 0.10 0.11 13.2 For a measure of precision in the checking procedure described in 10.10, the standard deviation of T,, has been found to be no greater than 0.005C in repeatability. T,, is the uncorrected temperature observed with a partial immersion thermometer at the solidificatipn point of the reference compound in a thermometric cell. 13.3 For a measure of the accuracy that is attainable in the checking procedure described in 10.10, the difference (Tc -- T'u) has been taken. Tc is the certified temperature assigned to a thermometric cell for the solidification point of the reference compound in it. T'u is a special value of Tu: in the special case in which Tu is observed with an accurate thermometer requiring no scalar correction, Tu = T'u. The following limits have been found for the value of (Tc -- T'u): Reference Compound in Thermometric Celt Phenol Naphthalene Phthalic anhydride Numerical Limits of the Value of CT. -T',,). Minimum Value, Maximum Value, deg'C deg'C -0.012 +0.020 -0.095 -0.022 -0.031 -0.112 The American Society for Testing and Material's takes no position respecting the validity ot any patent rights assertedin connection with any item mentioned in this standard. Ussrs 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. Your comments are Invited eitherfor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feet that your comments nave not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, PA 19103. 595 if? DUP050296157 A Designation: D 1555 - 91 Standard Test Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons*1 This standard is issued under the fixed designation D 1555; 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 oflast reapprovai, A superscript epsilon (t) indicates an editorial change since the last revision or reapprovai. This standard has bean 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.. No t e--Table 1 editorially corrected and the designation date was changed on July 26, 1991. 1. Scope 1.1 These tables arc for use in calculating the weight and volume of benzene, toluene, mixed xylenes, styrene, ortho xylene, meta-xylene, para-xyiene, cumene, ethylbenzene, 300 to 350F aromatic hydrocarbons, 350 to 400F aromatic hydrocarbons and cyclohexane. A method is given for calculating the volume at 60F from an observed volume at J"F. Table 1 lists the density in pounds per gallon at 60F for high purity chemicals. 1.2 A procedure for the calculation of density in pounds per gallon at 60F of materials of lower purity is provided. " No t e 1--The purchaser and the seller should agree on a reasonable policy in regard to rounding of final numbers in all computations. Rounding the final weight or volume, to not more than five significant digits is, in most cases, consistent with the experimental reliability ofthe data. No t e 2--An alternative method is Test Method D 4052. 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 consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 941 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Lipkin Bicapillary Pycnometer3 D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham Pycnometer2 D1250 Petroleum Measurement Tables2 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 2.2 Other Document: 1 This method is under the jurisdiction of ASTM Committee EM 6 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcom mittee D16.0A on BTX Cyclohexane, and Their Derivatives. Current edition approved July 26, 1991. Published September 1991. Originally published as D 1555 - 57. Last previous edition D 1555 - 90. 1 Annual Book ofASTM Standards, Vol 05.01. ' Annual Book ofASTM Standards, Vol 06.03. A Annual Botrk ofASTM Standards, Vol 05.03. TABLE 1 Relative Density and Density Data Product Benzene Cumene Cyclohexane Ethylbenzene m-Xylene o-Xylene p-Xylene Styrene Toluene Relative Density 60F/60F 0.8844t 0.8663t 0.7834 0.8718 0.8687 0.8848 0.8657 0.9110 0.8718 Density in Air at 60"F ItfH per U.S. Gallon 4f| 7-365 =3 7.214 8.522 7.259 7-234 7.367 1 1 .11 9 I 7-209 7.686 7260 M -.g 1 t Editorially corrected. TABLE 2 Application Range of Table 3 Commercial Product Benzene Toluene Mixed xylene Styrene o-Xylene m-Xylene p-Xylene Cyclohexane 300-350F Aromatic Hydrocarbons 350-400r Aromatic Hydrocarbons Cumene Ethylbenzene 95 to 100 % 95 to 100% all proportions 95 to 100% 95 toTOO % 95 to 100 % 94 to ioo % 90 to 100 % all proportions all proportions 95 to 100 % 96 to 100* m U Jj W J| 9 H m jg H M "f| M American Petroleum Institute Research Project 445 3. Significance and Use 3.1 This test method is suitable for use. in calculate weights and volumes of products outlined in Section 1. T| information gained from this method can be used determining quantities of stated aromatic hydrocarbons tanks, shipping containers, etc. 4, Basic Data 4.1 All calculations are derived from densities furaishs by the American Petroleum Institute Research Project 4 The tables are based on data for compounds of the highf purity, but can be used for materials in the range indicated Table 2. 5 "Selected Values of FYoperries of Hydrocarbons and Related Corapounc| prepared by American Petroleum Institute Research Project 44 at the Chcmij Thermodynamic Center, Department of Chemistry, Agriculture and Mechanij College Station, TX. 596 DUP050296158 0 1555 |2 The basic data and conversion factors used are given lie Appendix to the 1963 Annual Report6 of ASTM Imittee D-16. Densities listed in Table 1 are given in ASTM Data Series Publications.7 5. Tables 5.1 Table 3 contains 12 columns as follows: jjftxeecfitigs* ASTM, Vol 63, 1963. 7 "Physical Constants of Hydrocarbons C, to C,0," ASTM Data Service Publication DS4A, ASTM, 1971. jjjjjitiperature. Benzene f : X -3 rf 'I ft t K1 mlip.$: P 43 ' ' #*' IE 6 K- f m-'-'s W I; tb SI; 11 -12 El"' *3 P ;-44 U " -15 K 18 E ' 17 * ' 18 W '" i9 W 20 21 If ' 22 ' fti 23 m. *24 ft - 25 ' "la 26 iff 27 '`& K S 29 I 30 ft 31 fW1ir */':&332'3' H 85 E 36 W 37 ft 38 m <S9 i 40 " I *1 1 42 Sr 43 1 44 S 45 | 16 if 47 W 48 ft 49 1.0130 1.0124 1.0117 1.0111 1.0104 1.0098 1.0091 1.0085 1.0078 .1.0072 Toluene 1.0383 . 1.0377 1.0371 ' 1.0365 1.0359 1.0353 1.0347 1.0341 1.0336 1.0330" 1.0324 1.0318 1.0312 1.0306 1.0300 1.0294 1.0288 1.0283 1.0277 1.0271 1.Q265 1.0259 1.0253 1.0247 1.0241 1.0235 1.0230 1.0224 1.02^ 1.0212 1.0206 1.0200 1.0194 1.0188 1.0182 1.0177 1.0171 1.0165 1.0159 1.0153 1.0147 1.0141 1.0135 1.0130 1.0124 1.0118 1.0112 1.0106 1.0100 1.0094 1.0088 1.0082 1.0077 1.0071 1.0065 m-Xylene and Mixed Xylene 1.0293 1.0287 1.0282 1.0277 1.0272 1.0266 . 1.0261 1.0256 1.0251 1.0245 1.0240 1.D235 1.0230 1.0224 1.0219 1.0214 1.0208 1.0203 1.0198 1.0193' 1.0187 1.0182 1.bl77 1.0171 1.0166 1.01.61 1.0155 1.0150 1.0145 1.0139 1.0134 1.0129 1.0123 1.0118 1.0113 1.0107 1.0102 1.0097 1.0091 1.0086 1.0081 1.0075 1.0070 1.0065 1.0059 TABLE 3 Volume Corrections Volume Corrections to 60F* Styrene o-Xyleiie p-Xylene Cyclo hexane Ethyl benzene Cumene 300 to 350'F Aromatic Hydrocarbons 350 to 400F Aromatic Hydrocarbons 1.0288 1.0283 1.0278 1.0273 1.0267 1.0306 1.0300 1.0295 1.0289 1.0284 1.0297 1.0292 1.0287 1.0231 1.0276 1.0286 1.0280 1.0275 1.0270 1.0265 1.0262 1.0257 1.0252 1.02146 r.. 1.0241 1.0278 1.0273 1.0267 1.0262 1.0256 1.0270 1.0265 1.0260 1.0254 1.0249 1.0260 1.0254 1.0249 1.0244 1.0239 1.0242 1.0237 1.0231 1.0226 1.0221" 1.0236 1.0231 1.0225 1.0220 1.0215 1.0251 1.0245 1.0239 1.0234 1.0228- 1.0244 1.0238 1.0233 1.0226' 1.0222 1.0234 1.0228 1.0223 1.0218 1.0213 1.0215 1.0210 1:0204 10199 1.0194 1.0210 1.0204 1.0199 1.0194 1.0189 1.0223 1.0217 1.0212 1.0206 1.0201 1.0217 1.0211 1.0206 1.0201 1.0195 1.0208 1.0203 1.0197 1.0192 1.0187 1,0186 1.0183 1.0178 1.0172 1.0167 1.0184 1.0178 1.0173 1.0168 10163 1.0195 1.0190 1.0184 1.0179 1.0173 . 1.0190 1.0184 1.0179' -1-.0174 1.0168 1.0182 1.0177 1.0172 1.0166 1.0161 1.0162 1.0156 1.0151 *1.0145 1.0140 1.0135 1.0129 1.0124 1.0119 1.0113 1.0157 1.0152 1.0147 1.0142 10136 1.0131 1.0126 1.0121 10115 1.0110 .. 1.0167 1.0162 1.0156 1.0151 1.0145 1.0140 1.0134 1.0129 1.0123 1.0117 1.0163 1.0157 1.0152 1.0147 1.0141 1.0136 1.0130 1.0125 1.0120 1.0114 1.0156 1.0151 1.0145 1.0140 1.0135 1.0130 1.0125 1.0120 1.0114 1.0109 1.0108 1.0102 1.0097 1.0092 1.0086 1.0105 1.0100 10094 1.0089 1.0084 1.0132 1.0126 1.0119 1.0112 1.0106 1.0112 1.0106 1.0101 1.0095 1.0030 1.0109 1.0103 1.0098 1.0092 1.0087 1.0104 1.0099 1.0094 1.0088 1.0083 1.0081 1.0075 1.0070 1.0065 1.0059 1.0079 1.0074 1.0088 1.0063 1.0058 1.0099 1.0093 1.0085 1.0079 1.0073 1.0064 1.0078 1.0073 1.0067 1.0062 1.0082 1.0076 1.0071 1.0065 1.0060 1.0078 1.0073 1.0068 1.0063 1 0057 1.0266 1.0262 1.0257 1.0252 1.0248 1.0243 1.0238 1.0233 1.0228 1.0223 1.0218 1.0214 1.0209 1.0203 1.0199 1.0194 1.0189 1.0184 1.0180 t.0175 1.0170 %0165 1.0160 1.0155 1.0151 1.0146 1.0141 1,0136 1.0131 1.0126 1.0122 1.0116 1.0112 1.0107 1.0102 1.0097 1.0092 1.0087 1.0082 1.0078 - 1.0073 1.0068 1.0063 1.0058 1.0054 597 -mm Hi. DUP050296159 Temperature, Benzene 50 51 52 53 54 55 66 .57 '58 59 60 61 62 63 64 65 66 67 68 69 Vo. 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 - 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108 109 1.0065 1.0059 1.0052 1.0046 1.0039 1.0033 1.0026 1.0020 1.0013 1.0007 1.0000 0.9993 0.9987 0.9980 0.9974 0.9967 0.9961 09954 0.9947 0.9941 0.9934 0.9928 0.9921 0.9914 0.9908 0.9901 0.9894 0.9888 0.9881 0.9874 0.9863 0.9861 0.9854 0.9843 0.9841 0.9834 0.9828 0.9821 0.9814 0.9808 0.9801 0.9794 0.9787 0.9781 0.9774 0.9767 0.9761 0.9754 0.9747 0-9740 0.9734 0.9727 0.9720 0.9713 0.9706 0.9700 0.9693 0.9686 0.9679 0.9672 Toluene 1.0059 1.0053 1.0047 1.0041 1.0035 1.0029 1.0024 1.0018 1.0012 1.0006 1.0000 0.9994 0.9988 0.9982 0.9976 0.9971 0.9965 0.9959 0.9953 0.9947 0.9941 0.9935 0.9929 0.9923 0.9918 0.9912 0.9905 0.9900 0.9894 0.9888 0.9882 0.9876 0.9870 0.9865 0.9859 0.9853 0.9847 0.9841 0.9835 0.9829 0.9823 0.9818 0.9812 0.9806 0.9800 0.9794 0.9788 0.9782 0.9776 0.9770 0.9765 0.9759 0.9753 0.9747 0.9741 0.9735 0.9729 0.9723 0.9717 0.9712 m-Xylene and Mixed Xylene 1.0054 1.0048 1.0043 1.0038 1.0032 1.0027 1.0022 1.0010 1.0011 1.0005 1.0000 0.9995 0.9989 0.9984 0.9978 0.9973 0.996B 0.9962 0.9957 0.9951 0.9946 0.9940 0.9935 0.9930 0.9924 0.9919 0.9913 0.9908 0.9902 0.9897 0.9891 0.9886 0.9880 0.9875 0.9869 0.9864 0.9859 0.9853 0.9848 0.9842 0.9837 0.9831 0.9826 0.9820 0.9815 0.9809 0.9804 0.9798 0.9793 0.9787 0.9782 0.9776 0.9771 0.9765 0.9759 0.9754 0.9748 0.9743 0.9737 0.9732 TABLE 3 Continued Volume Corrections to 60F Styrene o-Xylene p-Xylene Cyclo hexane 1.0054 1.0049 1.0043 1.0038 1.0032 1.0027 1.0022 1.0016 1.0011 1.0005 1.0000 0.9995 0.9989 0.9984 0.9978 0.9973 0.9968 0.9962 0.9957 0.9951 0.9946 0.9941 0.9935 0.9930 0.9924 0.9919 0.9914 0.9908 0.9903 0.9897 0.9892 0.9886 0.9881 0.9876 0.9870 0.9865 0.9859 0.9854 0.9849 0.9843 0.9838 0.9832 0.9827 0.9821 0.9816 0.9811 0.9605 0.9800 0.9794 0.9789 0.9783 0.9778 0.9773 0.9767 0.9762 0.9756 0.9751 0.9745 0.9740 0.9734 1.0053 1.0047 1.0042 1.0037 1.0032 1.0026 1.0021 1.0016 1.0011 1.0005 1.0000 0.9995 0.9989 0.9984 0.9979 0.9974 0.9968 0.9963 0.9958 0.9953 0.9947 0.9942 0.9937 0.9932 0.9926 0.9921 0.9916 0,9911 0.9905 0.9900 0-9895 0.9889 0.9884 0.9879 0.9874 0.9868 0.9863 0.9858 0.9852 0.9847 0.9842 0.9837 0.9831 0.9826 0.9821 0.9815 0.9810 0.9805 0.9800 0.9794 0.9789 0.9784 0.9778 0.9773 0.9768 0.9762 0.9757 0.9752 0.9746 0.9741 1.0027 1.0022 1.0016 1.0011 1.0005 1.0000 0.9994 0.9989 0.9983 0.9978 0.9972 0.9967 0.9961 0.9956 0.9950 0.9945 0.9939 0.9934 0.9928 0.9923 0.9917 0.9912 0.9906 0.9901 0.9895 0.9090 0.9884 0.9878 0.9873 0,9867 0.9862 0.9856 0.9851 0.9845 0.9840 0.9834 0.9828 0.9823 0.9817 0.9812 0.9806 0.9801 0.9795 0.9789 0.9764 0.9778 0.9773 0,9767 0.9761 0.9756 0.9750 0.9745 0.9739 0.9733 0.9728 1.0066 1.0060 1.0053 1.0046 1.0040 1.0033 1.0027 1.0020 1.0013 1.0007 1.0000 0.9993 0.9987 0.9980 0.9973 0.9967 0.9960 0.9953 0.9947 0.9940 0.9934 0.9927 0.9920 0.9914 0.9907 0.9900 0.9893 0.9887 0.9880 0.9873 0.9867 0.9860 0.9853 0.9847 0.9840 0.9833 0.9827 0.9820 0.98130.9806 0.9600 0.9793 0.9786 0.9780 0.9773 0.9766 0.9759 0.9753 0.9746 0.9739 0.9733 0.9726 0.9719 0.9712 0.9706 0.9689 0.9692 0.9685 0.9679 0.9672 Ethyl benzene Cumene 1.0056 1.0050 1.0045 1.0039 1.0034 1.0028 1.0022 1.0017 1.0011 1.0006 1.0000 0.9994 0.9989 0.9983 0.9978 0.9972 0.9966 0.9961 0.9955 0.9949 0.9944 0.9938 0.9933 0.9927 0.9921 0.9916 0.9910 0.9904 0.9899 0.9893 0.9887 0.9882 0,9876 0.9870 0.9865 0.9859 0.9853 0.9848 0.9842 0.9836 0.9831 0.9825 0.9819 0.9814 0.9808 0.9802 0.9797 0.9791 0.9785 .0.9780 0.9774 0.9768 0.9763 0.9757 0.9751 0.9746 0.9740 0.9734 0.9729 0.9723 1.0054 1.0049 1.0044 1.0038 1.0033 1.0027 1.0022 1.0016 1.0011 1.0005 1.0000 0.9995 0.9989 0.9984 0.9978 0.9973 0.9967 0.9962 0.9956 0.9951 0.9945 0.9940 0.9934 0.9929 0.9923 0.9918 0.9912 0.9907 0.9902 0.9896 0.9891 0.9885 0.9880 0.9874 0.9869 0.9863 0.9858 0.9852 0.9847 0.9841 0.9836 0.9830 0.9825 0.9819 0.9813 0.9808 0.9802 0.9797 0.9791 0.9786 0.9780 0.9775 0.9769 0.9764 0.9758 0.9753 0.9747 0.9742 0.9736 0.9731 300 to 350F Aromatic Hydro carbons 1.0052 1.0047 1.0042 1.0037 1.0032 1.0026 1.0021 1.0016 1.0012 1.0006 1.0000 0.9995 0.9990 0.9984 0.9980 0.9974 0.9969 0.3964 0.9959 0.9954 0.9948 0.9943 0.9938 0.9933 0.9928 0.9922 0.9917 0.9912 0.9907 0.9902 0.9897 0.9892 0.9886 0.9881 0.9876 0.9870 0.9865 0.9860 0.9855 ' 0.9850 0.98440.9839 0.9834 0.9829 0.9824 0.9819 0.9813 0.9808 0.9803 0.9798 0.9793 0.9787 0.9782 0.9777 0.9772 0.9766 0.9762 0.9756 0.9751 0.9746 3So to 400E| Aromatit Hydro.,.'} caiboni* 1 00481.0044 1.0039 1.0034 1.0029 1.002+ 1.0019 1.0014 1-0011 1.0005 1.0000 0.9995 0.9990 0.9986 0.9980 0.9976 0.9971 0.9966 0.9961 0.9956 0.9951 0.9946 0.9941 0.9936 0.9932 0.9927 0.9922 0.9917 0.9912 0,9907 0.9902 0.9898 0.9893 0.9688 0.9883 0.9878 0.9873 0.9868 0.9863 0.9656 0.9853 0.9848 0.9844 0.9839 0.9834 0.9829 0.9824 0.9819 0.9814 0.9810 0.9805 0.9800 0.9795 0.9790 0.9785 0.9780 0.9775 0.9770 0,9766 0.9760 598 ' %v DUP050296160 # D 1555 TABLE 3 Continued Volume Corrections to 60F'1 ature, Benzene Toluene m-Xylene and Mixed' Xylene Styrene o-Xylene p-Xylene Cyclo hexane Ethyl benzene Cumene IP*10**** * 0.9666 111 0.9659 1; 112 0.9652 r 113 0.9645 f'T'14 " 0.9638 0.9706 0.9700 0.9694 0.9688 0.9682 0.9726 0.9721 0.9714 0.9710 0.9704 0.9729 0.9724 0.9718 0.9713 0.9707 0.9736 0.9731 0.9725 0.9720 0.9715 0.9722 0.9716 0.9711 0.9705 0.9700 0.9665 0.9658 0.9652 0.9645 0.9638 0.9717 0.9711 0.9706 0.9700 0.9694 It 115 if ti6 IP 117 ' 1 I18 P 119 P 120 1 I?1 if 122 sfi, 123 1' 124 0.9632 0.9625 0.9618 0.9611 0.9604 0.9597 0.9676 0.9670 0.9664 0.9659 0.9653 0.9647 0.9698 0.9693 . 0.9687 0.9682 0.9676 0.9671 0.9702 0.9696 0.9691 0.9685 0.9680 0.9675 0.9709 0.9704 0.9699 0.9693 0.9688 0.9683 019694 0.9688 0.9683 0.9677 0.9671 0.9666 0.9660 0.9655 0.9649 0.9643 0.9631 0.9625 0.9618 0.9611 0.9604 0.9597 0.9689 0.9683 0.9677 0.9672 0.9666 0.9660 , 125 '1,26 '127 i- 428 129 0.9638 0.9632 0.9626 0.9621 0.9615 u 130. ,131 132 133 134 0.9609 0.9604 0.9598 0.9592 0.9587 iJ 135 St 136 i! 137 1 138 139. , 0.9581 0.9575 0.9570 0.9564 0.9558 14<)' 141 142 143' 144 . 0,9553 0.9547 0.9541 0.9535 0.9530 145 ? 146 ' 147 148 149 0.9524 0.9518 0.9513 0.9507 0.9500 150 0.9496 on API Project 44 delta--essentially correct for all purities strove 95 5S. on API Project 44 data and non-linear regression analysis of those data using this formula RHO = EXP[--ALPHT x (TEMP - 60) x (1 - 0.8 x ALPHT x (TEMP - 60))] x.RHOT 0.9725 0.9720 0.9714 0.9708 0.9703 0.9697 0.9692 0.9686 0.9681 0.9675 0.9670 300 to 350F Aromatic Hydro carbons 0.9741 350 to 400F Aromatic Hydro carbons 0.9756 10 = the density of cyclohexane in kg/m3 at the observed temperature IT - the .coefficient of expansion of cyclohexane at 60F IMP = the observed temperature in "F, and RHOT = the density of cyclohexane in kg/m3 at 60F. 5.1.1 Column 1--Observed temperature in degrees Tahrenheit. 5.1.2 Columns 2 to 12, Inclusive--Multiplying factors for the reduction to 60F, specifically the ratio of the volume at -,60F to the volume at tF. Use of Tables 6.1 Volume Reduction to 60F--Enter the appropriate olumn pf Table 3, selecting that temperature to the nearest egree Fahrenheit at which the bulk volume was measured (temperature /), and select the corresponding volume reduc tion factor (ratio) in Columns 2 to 12. Multiply the bulk volume measurement at temperature, t, by the factor se lected from the table (see Note 1). Example I--Whal is the volume at 60F ofa tank care ofpara-xylene whose volume was measured to be 9280 U.S. gal at a mean temperature of 88.7T? Enter Table 3, Column 7, at 89.0T and note that the "volume ratio" is 0.9840. The volume at 60F is 9280 X 0.9840 = 9131.5 U.S. gal. 6.2 Converting Volume to Weight for Chemicals other 699 Ml DUP050296161 D 1555 than Mixed Xylenes Listed in Table /--Multiply the volume in gallons at 60F (5 digits) by the density in pounds per gallon at 60F (see Table 1). Extynple 2--What is the weight of para-xylene whose volume is 9280 U.S. gaiat 88.7"F? See Example 1. The weight is 9131.5 x 7.209 = 65 829 lb. 6.3 Converting Volume to Weight for Mixed Xylenes-- Correct the measured bulk volume to 60F as described in 6.1. Determine the density (all weights in vacuum) at 60T in 1 grams per millilitre as described in Section 7. Obtain the value for pounds per U.S. gallon in standard air at 60"F, by means of the following equation, and round to five digits: a = (b -A) X 8.34522 (1) where: a = pounds per U.S. gallon in standard air at 60F, b = grams per miflilitre in vacuum at 60F, and A = correction factor as given in Table 4. Multiply the corrected volume by the calculated pounds per U'S. gallon at 60"F value in order to obtain the weight in pounds in air (see Note 1). Example 3--What is the weight (in air) of the contents of a tank car of mixed xylenes having a calculated density (Section 7) of 0.87638 g/mL,(in vacuum), whose volume was measured to be 9280 U.S. gal at a mean temperature of 88.7'F? Enter Table 3 at 89F and note that the "Factor for Reducing Volume to 60"F" is 0.9808. The volume at 60"F is 9280 x 0.9808 = 9101.8 U.S. gal. From Eq I: (0.87638-0.001090) (8.34522) = 7.30449 lb per U.S. gal. The weight of mixed xylenes in the tank car is then 9101.8 x 7.30449 = 66 484 lb. 7. Density Calculation 7.1 Density determinations may be carried out by any procedure known to be reliable to four digits. Test Methods D 941, D 4052 and D 1217 are suitable and are written to give density completely in vacuum (corrected) which is required for the computation described herein. 7.2 If the methods described in Test Methods D 3505 are used, relative density in air is first converted to density in grams per millilitre in air by use of the factors given in Table 5. TABLE 4 Converting to Densities in Standard Air Density at 60F, in Vacuum, g/mL Correction Factor, A, g/mL 0.82 0.001093 0.83 0.001097 0.84 0.001095 0.85 0.001094 0.86 0.001092 0.87 0.001091 0.88 0.001090 0.89 0.001088 0.90 0.001087 TABLE 5 Factors for Converting from Relative Density in Air to Apparent Density in Air in Drams per Millilitre (Note 3) Measurement Temperature Multiply Relative Density in Air by this Number to Get Apparent Density 60/60F or 15.56/15.56*0 68/68F or 20/20'C 77/77F or 25/25"C 0.99904 at 60F 0.99823 at 68F 0.99708 at 77F No t e 3--"Relative density in air" means that all weighings were in air, and no air buoyancy correction was applied. "Apparent density" f<jr the purposes of this test is defined as the density calculated when the pycnometer volume is calibrated with water, weighed in air, and when the sample is weighed in air, and no air buoyancy correction is used for 1 either weighing, even though the density in vacuum Of water is used in I calculating the volume. "Density in air" for the purpose of this method jl is the weight per unit volume in vacuum minus the weight of a volume 1 of air equal to the difference between the volume of the sample and the volume of brass weights equivalent to the weight in vacuum of the sample. If it is desired to make a direct experimental determination of "density in air" using a pycnometer, apply the air buoyancy correction J to the water weight, calculate the true volume of the pycnometer from the weight of water in vacuum, and then fill the pycnometer with sample, weigh in air, subtract the weight of the pycnometer in air, and apply no air buoyancy correction. This sample weight in air, divided by the true volume in millilitres is the "density in air" at the experimental temperatures. Densities given in Tables D 1250 are on this basis. 7.3 Convert apparent density in grams per millilitre in air to density in vacuum by use of Table 4. 7.4 Convert density in vacuum at t degrees to density at TABLE 6 Vacuum Corrections, Apparent Density to Density in Vacuum Apparent Density, W/V Correction/ plus Apparent Density W/V Correction/ plus 0.70 0.00036 0.85 0.00018 0.71 0.00035 0.86 0.00017 0.72 0.00033 0.87 0.00016 0.73 0.00032 0.88 0.00014 0.74 0.00031 0.89 0.00013 0.75 0.00030 0.90 0.00012 0.76 0.00029 0.91 0.00011 0.77 0.0002B 0.92 0.000)0 0.78 0.0002S 0.93 0.00009 0.79 0.00025 0.94 0.09007 0.80 0.00024 0.95 0.00006 0.81 0.00023 0.96 0.00005 0.82 0.00022 0.97 '0.00004 0.83 0.00020 0.98 0.00003 0.84 0.00019 0.99 0.00001 A This table applies for all air density values between 0.0011 and 0.0013 g/mL For air densities outside this range, the vacuum correction, C, should be calculated as follows: where: c da w V W/V C = da/0.99823 x [0.99823 - (LV/V)] vacuum correction, density of air in disbalance case, g/mL, weight of sample irrpycnometer, volume of sample In pycnometer, and apparent density (Note 3). TABLE 7 Multipliers to Convert From Density in Vacuum at t Degrees to Density at 60F (15.56C) in Vacuum Product Benzene Toluene Mixed xylenes Styrene m-Xylene o-Xylene p-Xylene Cyclohexane Cumene Ethylbenzene 59"F (15C) 0.99934 0.99941 0.99946 0.99946 0.99946 0.99919 0.99945 0.99935 0.99946 0.99946 Multiplier for Temperature 68F (20C) 77F (25-0 1.00529 1.00473 1.00435 1.00434 1.00435 1.00693 1.00443 1.00528 1.00435 1.00435 1.01136 1.01011 1.00931 1.00927 1.00931 1.01573 1.00947 1.01133 1.00931 1.00931 86F (306C) 1.01753 1.01554 1.01435 1.01426 1.01435 1.02575 1.01459 1.01750 1.01435 1.01435 600 triSXteSKtwWW.!* " - JHL DUP050296162 D 1555 0F <I5.56C) using the multipliers given in Table 7 on iterpolated values. iiJixxaanrrwtjnle 4--The density in vacuum of a mixed xylenes sample was Itermmmineeddat t 25C and found to be 0.87095. The coefficient from the &|le is 1.01136. The density in vacuum at 60"F is 0.87095 x 1.01136 -- P084. l.5 Calculate pounds per U.S. gallon in air in accordance Eth 6.3. 8. Precision and Bias 8.1 Since this is a calculation method, no precision and bias statement is required. 9. Keywords 9.1 benzene; calculation; conversion; cumene; density; eth ylbenzene; fft-xylene; mixed xylene; o-xylene; p-xylene; spe cific gravity; styrene; 300 to 350F aromatic hydrocarbons; 350 to 400T aromatic hydrocarbons; toluene; volume; weight ' The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection f| with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapprovedor withdrawn. Your comments are invited either lor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 601 S3KWm -m ,, i' *'1>r|,Cs DUP050296163 Designation: D 1031 - 85 (Reapproved ,ef Standard Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method1 This standard is issued under the fixed designation D 1631; 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. el No t e--Editorial changes were made throughout in April' 1989. 1. Scope 1.1 This test method covers the determination of water in ' phenol and related materials such as cresols, xylenois, naphthalene, pyridine, and quinoline. 1.2 If ketones are present in the sample, interference from them can be avoided by employing the glycol-pyridine sample solvent specified in Test Method D 1364. 1.3 This standard may involve hazardous materials, oper ation, 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 bapplicability of regulatory limitations prior to use. For specific hazard statements, see Section 7. 2. Referenced Documents 2.1 ASTM Standards:2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method) D3437 Practice for Sampling and Handling Liquid Cyclic Products D 3852 Practice for Sampling and Handling Phenol and Cresylic Acid 2.2 Other Document:3 OSHA Regulations, 29 CFR, Paragraphs 1910.1000 and 1910.1200 3. Summary of Test Method 3.1 When solutions of iodine in methanol and of sulfur dioxide in pyridine are mixed in the presence of water, the following reaction occurs: I2 + S02 + H20 2H1 + SOs 3.1.1 Sufficient pyridine is present in the reagent to consume the hydriodic acid and sulfur trioxide: 1 This test method is under the jurisdictioo of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved March 29, 1985. Published December 1985. Origi nally published as D 163! - 59 T. Last previous edition D 1631 - 80. 1 Annua! Book ofASTM Standards, Vol 06.03. 3 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 2HI + S03 + 3C5H5N -* H S02 2CSHSN ^ + Cs H5N ^ \\ IO 3.1.2 The pyridine sulfur trioxide salt reacts with the methanol, this preventing a second mole ofwater from being consumed: S02 + CH3OH - \ o o s o 2o c h 3 / V H 3.2 When the pyridine solution contains water and the sulfur dioxide is titrated with iodine in methanol solution, the platinum electrodes remain polarized until all the water reacts. A slight excess of iodine depolarizes the electrodes, allowing current to flow through the microammeter which indicates the end point. 4. Significance and Use 4.1 This test method is particularly useful for determining small amounts of water in hygroscopic materials. However it is generally applicable to a variety of materials varying in water content from 100 ppm to solutions containing a relatively high percent of water. This test method is not applicable in the presence of mercaptans, .peroxides, or appreciable quantities of aldehydes or amines. This test method is suitable for setting specifications on materials referenced in the scope. It may also be used as an internal quality control tool and in development or research work. 5. Apparatus 5.1 The apparatus shall be assembled as shown in Fig. 1. Any suitable modification permitting equal facility and accuracy may be used. Automatic titration equipment is commercially available and may be used. 6. 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, n if 602 WASP DUP050296164 01631 6.5 When handling Karl Fischer reagent refer to Practice D 3437. 24/M I GROUND GLASS JOINTS INSULATED COPPER WIRE DRIERITE DRYING TUBE--7 TO / bur et * MERCURY ELECTRODES f j A (0) m -fit MAGNETIC STIRRER REAGENT BOTTLE FIG. 1 Titration Assembly |here such specifications are available.4 Other grades may be pjsed, provided it is first ascertained that the reagent is of lufficiently high purity to permit its use without lessening the Hfccuracy of the determination. 6.2 IodineSolution--Dissolve 150 g of iodine (I2) crystals ii 3 L of anhydrous methanol. Place the solution in the igent bottle connected to the buret as shown in Fig. 1. i 6.3 Methanol, anhydrous, containing less than 0.05 % iter. 6.4 Pyridine Solution--Place 4000 mL of refined grade idine in a 5000-mL distilling flask. Distill over and iiscard 400 mL offorecut at atmospheric pressure. Distill off 400 mL of center cut and transfer to a suitable glass bottle fitted with a two-hole stopper. Through one hole of the ipper insert a piece of glass tubing that extends almost to le bottom of the bottle; through the other hole insert a short iece ofglass tubing to serve as a vent. Through the long tube idd 400 g of refrigerant-grade sulfur dioxide (SO2) dried rough concentrated sulfuric acid (H2S04 sp gr 1.84), and ow the solution to cool. Fit the vent tube with a drying be and an aspirator bulb; connect the long tube with an dapter suitable for introducing the reagent into the titration lask. For convenience in measuring, a suitable reservoir may placed in the system. No t e 1--In place of the divided reagents described in 6.2, 6.3, and [6.4 it is permissible to employ the single solution reagent specified in Test Method D 1364 or commercial Karl Fischer reagents.I I 4 "Reagent Chemicals. American Chemical Society Specifications. "Am. Chem. IScc., Washington, DC. For suggestions on the testing of reagents not listed by the gAmerican Chemical Society, see "Reagent Chemicals and Standards," by Joseph gfeosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Ipharmacopeia." 7. Hazards 7.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. When sampling phenol and related materials follow safe rules and adhere to all safety precautions as outlined in the latest OSHA regulations. 7.2 Precautions must be taken in sampling to preclude any possibility of contamination with atmospheric moisture adhering to the walls of the pipet. 7.3 Phenol, pyridine, and related materials are extremely toxic when ingested and corrosive to the skin. Appropriate precaution must be exercised when handling them. 8. Sampling 8.1 Refer to Practice D3852 for proper sampling and handling of phenol and related materials analyzed by this test method (see 7.1 and 7.2.). 8.2 The sample size recommended, on the basis of water content expected is as follows: Expected Water Content, % Srie of Specimen, g. 0.01 to 0.03 0.03 to 03 0.3 to 0.6. 0.6 to 1.0 1.0 to 5.0 5.0 to 10.0 .10.0 to 20.0 50 25 10 5 2 1 0.5 9. Standardization of Sulfur Dioxide--Iodine Reagent 9.1 By means of pressure from the aspirator bulb, transfer sufficient pyridine solution (Warning--see 7.3) to the titration flask to cover the electrodes. If an automatic titration apparatus is used, a small amount of methanol may be added to the pyridine to improve the response of the titiator. Turn on the magnetic stirrer and turri the "zero-set" knob until a reading of 70 pA is obtained on the ammeter. Add the iodine solution dropwise from the buret until the ammeter reads a maximum value, about 130 pA. Remove the drying tube from the sidearm and quickly introduce an amount of distilled water, or water of equivalent purity, at least equal to that to be determined, weighed to the nearest 0.1 mg by means of a suitable weighing pipet. Immediately replace the drying tube. 9.2 Titrate with the iodine solution, approaching the end point dropwise until the maximum value, about 130 pA, is obtained on the ammeter. The standardization should be repeated daily. If desired, a suitable accurately weighed amount of sodium tartrate dihydrate reagent may be used in place of water as follows; Accurately weigh a small alu minum weighing dish5 containing about 0.20 to 0.22 g of powdered sodium tartrate dihydrate (Na2C4H406-2H20) to the nearest 0.1 mg. Remove the stopper from the titration flask and introduce the tartrate by inserting the spout into the opening and gently tapping so that the powder falls freely into the liquid without contacting the side walls. Do not 5 Fisher No. 2-190 or Will No. 375$ dishes have been ' '.'iii.l satisfactory for this purpose. 603 y DUP050296165 # D 1631 uP brush out the dish: accurately reweigh it and calculate the weight oftartrate used by difference. Quickly reseal the flask, turn on the stirrer, and titrate to the end point. Record the ..volume of reagent and weight of tartrate used. 9.3 Calculate the water equivalent of the sulfur dioxideiodine reagent as follows: F = 1004/5 where: F = water equivalent of the reagent, g/100 mL, A - water added, g, and B -- volume of reagent used for the titration, mL. If sodium tartrate dihydrate is used in place of water for standardizing: F= 15.66S/B where S = tartrate used, g. 10. Procedure 10.1 Repeat the procedure described in Section 9 adding, instead of water, an amount of specimen selected according to Section 8. Record all weighings to the nearest 0.1 mg. As long as an excess of pyridine remains in the titration flask, further additions of specimen and titration may be made. (Warning--See 7.3.) No t e 2--The titration flask may be removed and cleaned between specimens. Washing should be followed by an alcohol or acetone rinse and drying in a ventilated oven at 100 to 130C for several hours. The clean flask may be cooled in a desiccator or attached to the buret to cool with the openings closed with drying tubes. Ifa series of specimens is to be tested, it is preferable to continue additions ofspecimens and titration (and addition of pyridine if necessary) until the volume of liquid in the flask is too great for further titration. No t e 3--Visual observation ofthe end point may be used h i , the more precise electrometric method described if the solut'on lightcolored. During the titration the solution turns yeBaw ate addition ofthe first few millilitres ofthe reagent. This color ch not be confused with the true end point, which is brown. The Haas from yellow to brown is quite sharp and easily reproducible 11. Calculation 11.1 Calculate the amount of water in the specirncii follows: Water, weight % = CF/D where: C = sulfur dioxide-iodine reagent required for titration, the specimen, mL, and D = weight of specimen used, g. 1 12. Precision and Bias6 12.1 Precision--Duplicate results should be coa>idej$t|l suspect ifthey differ by more than the following: Range, % Repeatability (By Same Operator) Reproducibility (By Two Differcli Laboratories) 0.01 to 0.12 0.0035 0.021 12.2 Bias--Bias in this test method must be determin on an individual basis for each material being tested utili standards of known water content or the method of knd addition. 6 Data on which these precision values are based are given in the 18591 of Committee D-16, Proceedings, ASTM, Voi 59, 1959. The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If notrevised, eitherreapproved or withdrawn. Your comments are Invited eitherforrevision ofthis standard ortoradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 604 DUP050296166 Designation: D 1685 - 86 {Reapproved 1990) Standard Test Method for f:- Traces of Thiophene in Benzene by Spectrophotometry1 This standard is issued under the fixed designation D 31685; 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. t. Scope 1.1 This test method covers the determination of iophene in benzene in which the thiophene concentration between 0.1 and 250 mg/kg. Jl.2 Contaminating materials that are darkened by sulfuric id interfere and must be compensated for by a sample i determination. Neither carbon disulfide in concentra!|ns as high as 100 mg/kg nor water as high as the level of duration will interfere. | 1.3 Contaminating materials may occasionally cause the ior development in this test method to be time dependent d may also contribute to spectral interferences at 589 nm. tonsequently, test results indicating substantial thiophene, at cannot be verified by total sulfur analysis, should be cmsidered suspect. I 1.4 This standard does not purport to address all of the pfely problems associated with its use. It is the responsibility ifthe user ofthis standard to establish appropriate safety and with practices and determine the applicability ofregulatory Motions prior to use. For specific hazard statements, see ote 1, 7.1, and 8.1. > |. Referenced Documents f'2.1 ASTM Standards: P D1193 Specification for Reagent Water2 D3437 Practice for Sampling and Handling Liquid Cyclic Products3 |ML2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 Summary of Test Method 3.1 Thiophene is reacted with isatin, under prescribed inditions, to form a colored compound. The compound is itraeted into sulfuric acid, and the intensity of the color is treasured spectrophotometrically. Thiophene concentration ^obtained by correlation with knowns. i:' i |. Significance and Use 4.1 This lest method is suitable for setting specifications Sh benzene and for use as an internal quality control tool ' 1 This test method is under the jurisdiction of ASTM Committee D-16 on omatic Hydrocarbons and Related Chemicals and is the direct responsibility of |bcommittee D16.0A on Benzene, Toluene, Xylene, Cyclohexane, and Their ` rivatives. Current edition approved May 30, 1986. Published July 1986. Originally blished as D 1685 - 58 T. Last previous edition D 1685 - 81. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 08.03. M Available from Superintendent of Documents, U. S. Government Printing Sice, Washington, DC 20402. where benzene is either produced or used in a manufacturing process. It may also be used in development or research work involving benzene. 5. Apparatus 5.1 Separatory Funnels, 50, 250, 500, and 1000-mL, with glass stoppers. 5.2 Spectrophotometer--Any spectrophotometer may be used that is capable of repeatability of 0.005 absorbance units in the range from 0.1 to 1.4 absorbance and repeat ability of wavelength of 1 nm in the region from 400 to 700 nm. 5.3 Absorption Cells, 1-cm, matched, glass or silica. 5.4 Analytical Balance. 5.5 Pipets, 1, 2, 5, and 10-mL. 5.6 Graduated Cylinders, 250 and 1000-mL. 5.7 Volumetric Flasks, glass-stoppered, 50, 100, 250, and 1000-mL. ' 5.8 Filter Paper, medium filter5 and rapid hardened.6 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.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. 6.2 Purity of Waiter--Unless otherwise indicated; refer ences to water shall be understood to mean Type IV reagent water conforming to Specification D 1193. 6.3 Cadmium Chloride Solution (20 g/L)--Disstilve 20 g ofanhydrous cadmium chloride (CdCl2) or 25 g of cadmium chloride hydrate (CdCl2 2Vs HzO) in 200 mL of water and dilute to 1 L. 6.4 Sulfuric Acid (sp gr 1.84)--Concentrated H2S04. 6.5 Benzene, Thiophene-Free: 6.5.1 Wash 700 mL of benzene in a 1000-mL separatory funnel with successive 100-mL portions of concentrated sulfuric acid (H2S04) to which has been added 5 mL of isatin solution, until the H2S04 layer is light yellow or colorless. Wash the benzene with 100 mL ofwater and then twice with 100 mL ofcadmium chloride solution (CdCl2). Finally, wash 5 This method is based on the use of Whatman J. 6 This method is based on the use of Whatman 54. 7 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testings of reagents not listed by the American Chemical Society, see "Reagent Ovrnicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, N Y, and the "United States Pharmacopeia." 605 -p p: DUP050296167 # D 1685 with another 100-mL portion of water. Filter the benzene through medium filter paper into a storage bottle and tightly stopper. 6.5.2 Prepare 1400 mL of thiophene-free benzene. Mea sure the absorbance of this material by the procedure outlined in 10.2 and 11.2. The absorbance should be no greater than 0.01. 6.6 Ferric Sulfate, Sulfuric Acid Solution--Add 0.2 g of ferric sulfate (Fes(S04)3 - 9H20) together with 38 mL ofwater to a 1-L volumetric flask. Swirl to dissolve. Cautiously add about 100 mL of H2S04 and swirl. Allow time for the heat of reaction to subside and dilute to volume with H2S04. No t e 1: Caution--Protective clothing and goggles should be worn whenever H2S04 is used. ,fi,7 Isatin, Chloroform, Benzene Solution--Add 0.5 g of isfitin to 200 mL of chloroform. Heat, in a fume hood, to a temperature just below the boiling point (61C) of chloro form and maintain for 5 min with stirring. Filter into a 25Q-mL volumetric flask through hardened rapid filter paper. Wash the filter paper with two 20-mL portions of thiophene-free benzene (from 6.5) eluting the washings into the volumetric flask. Dilute to volume with thiophene-free benzene. 6.8 Thiophene.8 7. Hazards 7.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. funnel. Add 10 mL of ferric sulfate-sulfuric acid soluti^. stopper, and shake for 2 min 15 s. Allow the two phases' separate and draw off the lower H2S04 layer into a 50-nj;''l volumetric flask. Add 10 mL of H2S04 to the sepavato-v^ funnel and shake for 30 5 s. Again draw off the |owj,ai H2S04 layer into the 50-mL volumetric flask containing " first extract. Dilute to volume and mix. Repeat with eai;^ specimen. 10. Preparation of Calibration Curves 10.1 Add approximately 0.2 g of thiophene, weighed to'l the nearest 0.0002 g to a 100-mL volumetric flaskeontainin about 50 mL of thiophene-free benzene. Dilute to voluo with thiophene-free benzene and mix. This is Solution ffj Pipet 1 mL of Solution 1 into a 100-mL volumetric flasl dilute to volume with thiophene-free benzene, stopper, an mix. This is Solution 2 and will contain approximately 20f of thiophene per millilitre. 10.2 Pipet 0, 1, 2, 5, 7, and 10-mL of Solution 2 100-mL volumetric flasks and dilute to volume thiophene-free benzene. Transfer to 500-mL separatory i nels and follow the procedure in 11.2 and 11.3 for i.*concentration. Plot absorbance versus concentration in tnif' crograms per millilitre. 10.3 .Prepare Solution 3 containing approximately 40 pg; of thiophene per millilitre by pipetting 2 mL of Solution I into a 100-mL volumetric flask and diluting to volume with thiophene-free benzene. Follow the procedure in 10.2 t$ obtain the calibration curve'for 50-mL specimens. 8. Sampling 8.1 Sampling of benzene should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations. Refer to Practice D3437 for proper sampling and handling of benzene. 9. Preparation of Reagent Blanks and Sample Blank 9.1 Reagent Blende 1--To a 50-mL separatory funnel pipet 5 mL of isatin solution and 10 mL of ferric sulfatesulfuric acid solution. Stopper and shake for 2 min 15 s. The shaking is accomplished by wrist action in a rocking motion through a 180 arc roughly once each second. Allow the two phases to separate and draw off the lower H2S04 layer into a 50-mL volumetric flask. Add 10 mL of H2SO,, to die separatory funnel, stopper, and shake for 30 5 s. Again draw off the lower H2S04 layer into tlie 50-mL volumetric flask containing the first extract. Dilute to volume with H2S04 and mix. This blank is stable for 8 h and need not be repeated with each analysis during this period. 9.2 Reagent Blank 2--Into a 50-mL volumetric flask, pipet 10 mL of ferric sulfate-sulfuric acid solution and dilute to volume with H2S04. Stopper and mix. This blank is stable for 8 h and need not be repeated with each analysis during this period. 9.3 Sample Blank--Take a 100-mL portion of the CdCI2 washed and filtered benzene sample (prepared in accordance with the procedure in 11.1). Transfer to a 250-mL separatory 8 Thiophene such as Eastman Catalog No. I860 or equivalent faas been found satisfactory for this purpose. 11. Procedure 11.1 To a 500-mL separatory funnel, add 250 mL of sample and 40 mL of cadmium chloride, solution. Stopper and shake for approximately- 30 s. Allow to settle and discard tiie aqueous layer. Filter the benzene layer through medium filter paper into a 250-mL graduated , cylinder. Part of the filtered benzene is to be used for the sample blank. Proceed 1 with preparation of the sample blank as describe^ ip 9.3. From the remaining filtered benzene, transfer 100 mL to 250-mL separatory funnel. 11.2 To the separatory funnel add 5 mL of isatin solution and 10 mL of ferric sulfate-sulfuric acid solution. Stopper and shake for 2 min 15 s. Allow the phases to separate and draw off the lower H2S04 layer into a 50-mL volumetric flask..Ad4 10 mL ofH2S04 to the separatory funnel, stopper, and shake for 30 5 s. Again draw off the lower H2SQ4 layer into the 50-mL volumetric flask containing the first extract. Dilute to volume with H2S04 and mix. 11.3 Measure the absorbance ofthis material at 589 ran in a 1-cm cell versus Reagent Blank 1 (9.1) in a matched I-cm cell. Instrument conditions should be identical with those employed during calibration. 11.4 Determine the concentration of thiophene from the calibration curve (Section 10). If the absorbance is greater than 1.5, repeat the procedure using a 50-mL specimen instead of 100 mL. If the 50-mL specimen still gives absorbance above 1.5, then the specimen must be diluted with thiophene-free benzene before proceeding.' 11.5 Determine the absorbance of the sample blank (9-3) at 589 nm using Reagent Blank 2 (9.2) as reference. 606 DUP050296168 gl 1 Designation of 1 Equation of |i- Section 11 1A 1e 0 D 1685 TABLE 1 Calculation Factors Cell Solutions Solution of Sample H2S04-Fe2(S04)a; Isattn after contact with sample, (see 11.2} sample blank (see 9.3) Versus Solution of Reference reagent blank 1 (see 9.1) reagent blank 2 (see 9.2) ermine the apparent concentration of thiophene in the plple blank. Calculation !.'l Calculate the thiophene content of the sample in i per kilogram as follows: Thiophene, mg/kg = (A - B)F/d Thiophene Concentration, Range, mg/kg 100 to 250 20 to 100 2 to 20 0.4 to 2 less than 0.4 TABLE 2 Precision Limits Repeatability, Percent of Value Reproducibility. Percent of Value 11.4 12.3 13.8 14.0 less than 0.09 mg/kg 15 19 21 25 less than 0.15 mg/kg thiophene for sample determined from appropriate calibration curve (see Table 1), pg/mL, apparent thiophene determined for sample blank from appropriate calibration curve (see Table 1), pg/mL, dilution factor of sample, and density of benzene at the temperature of the sample. Precision and Bias 13.1 The data given in Table 2 should be used forjudging : acceptability of results (95 % probability). No t e 2--The precision limits given in Table 2 are based on data published as Appendix III to Report of Committee D-16, ASTM Proceedings, Am. Soc. Testing Mats., Vol 59, 1959, p. 514, 13.2 Repeatability is based on test results obtained by repetitive testing of a homogeneous sample by a single operator. Reproducibility is based on test results obtained by repetitive testing of different samples in different laboratories and different operators. 13.3 Bias--The bias of this test method has not been determined. 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 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 live years and Itnotrevised, either reapproved orwithdrawn. Your comments are invitedeitherforrevision 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 Pace St., Philadelphia, PA 19103. 1 607 rry.. Designation: D 1686 - 81 (Reapproved 1990) Standard Test Method for Color of Solid Aromatic Hydrocarbons and Related Materials in the Molten State (Platinum-Cobalt Scale)1 This standard is issued under the fixed designation D 1686; 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/ast reapprovai. A superscript epsilon (t) indicates an editorial change sinCe'the last revision or reapprovai. 1. Scope 1.1 This test method covers the visual measurement ofthe colpr of thermally stable solids melting below 150C. It is applicable only to materials in which the color-producing bodies present have light absorption characteristics quite similar to those of the standards used. 1.2 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 specific hazard statements see Sections 7, 8, and 9. 2. Referenced Documents 2s 1 ASTM Standards: D1193 Specification for Reagent Water2 D3438 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride3 D 3852 Practice for Sampling and Handling Phenol and Cresylic Acid3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Significance and Use 3.1 Color by this test method is a measure of colorproducing impurities present in the thermally stable solids. This test method is suitable for setting specifications and for use as an internal quality control tool. 4. Apparatus 4.1 Color Comparison Tubes--Matched 100-mL, tallfan Nessler tubes, provided with ground-on, optically clear, H|ss caps. Tubes should be selected so that the height of the 1'00-mL graduation mark is 300 3 mm above the bottom of the tube. The use of heat-resistant tubes is preferred for safety reasons. 4.2 Color Comparator--A color comparator constructed to permit visual comparison of light transmitted through tail-form, 100-mL Nessler tubes in the direction of their ' This test method is under the jurisdiction of ASTM Committee D-16 on Aronmie Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee DI6.0C on Oxygenated Aromatics. Current edition approved Nov. 27, 1981. Published January 1982. Originally published as D 1686 - 59 T. Last previous edition D 1686 - 61 (1977). 1'titrn,al Cook ofASTM Standards, Vols 06.03 and 11.01. iltitn Book ofASTM Standards, Vol 06.03. * Av,*ilab'.c ftxtm .Superintendent ot Documents, U.S. Government Priming Office Wi.,|llr,non> DC 20402. longitudinal axes. The comparator should be constructed si| that white light is reflected offa white plate and directed wit] equal intensity through the tubes, and should be shielded i that no light enters the tubes from the side. 4.3 Oven--An oven, preferably of the forced draft and capable of maintaining a constant temperature 1C in the range up to 150C. Alternatively, the use of an aluftiinufl heating block provided with proper temperature control orj other similar equipment is permissible, g 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall ba| used in all tests. Unless otherwise indicated, it is intend that all reagents shall conform to the specifications of 1 Committee on Analytical Reagents of the American Chem-I ical Society, where such,specifications are available.5 Other'! grades may be used, provided it is first ascertained that! 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!I ences to water shall be understood to mean Type IV reagent ! water conforming to Specification D 1193. 5.3 Cobalt Chloride (Co C12-6H20). 5.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro- j chloric add (HQ). 5.5 Potassium ChlorOplatihate (K2PtCl6). 6. Standards 6.1 Platinum-Cobalt Stock Solution--Dissolve 1.245'g of1 K2PtCl6 and 1.000 g of Co C12-6H20 in water. AM 100 mL j of HQ and dilute to 1 L with water. This solution has a color i of 500.6 7 6.2 Platinum-Cobalt Standards1--From the stock solu- j tion, prepare color standards, as given in Table 1, by diluting j the required volumes to 100 mL with water in the Nessler j tubes. If desired, these standards may be made permanent by ; sealing on the caps with a suitable colorless cement. 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, sec "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 6 The stock solution with color No. 500 may be purchased as such from chemical supply firms. Use ofthe purchased standard is satisfactory. 7 The preparation of these platinum-cobalt standards was originally described by A. Hazen, American Chemical Journal, Vol 14, p. 300 (1892), The description given in Test Method D 1686 is identical with that given in the "Standard Methods ; for the Examination of Water and Sewage," American Public Health Assn., Tenth * Edition, 1955, p. 88. A description is also given by W. W. Scott, "Standard Methods of Chemical Analysis," D. Van Nostracri Co., Inc., Fifth Ed., Vol 2. It-" 2048. 608 DUP050296170 # D 1686 TABLE 1 Platinum-Cobalt Color Standards'* I Color 1 Standard ff; No. Stock Solution, tnL Color Standard No. Stock Solution, mL s > 10 ; 15 i 20 25 30 1 35 2 40 3 50 4 60 5 70 6 100 7 8 10 12 14 20 i f Other color standards may be prepared by proportional dilution. |..l Consult OSHA regulations and supplier's Material ' Data Sheets for all materials used in this test method. 4fTE 1: Precaution--When handling molten solids in open tubes, jeqpate ventilation must be provided and proper protection should be I io prevent thermal bums. Sampling 3.1 Sampling should follow Practices D 3438 and D 3852 proper sampling and handling of solid aromatic materials tlyzed by this test method. ion? 2: Precaution--All safety precautions as outlined in the latest |HA regulations should be observed. 'Procedure jM Melt approximately 150 g of the sample and simultaiusly preheat a Nessler tube and cap in an oven mainbed at constant temperature at 10 to-20C above the Bdification point of.the sample. The sample must not be fted to more than 2QC above its solidification point 1.2 As soon as the sample is completely liquid, mix by rag with a clean dry glass rod, then quickly fill the cheated Nessler tube to the 100-mL mark with the sample cap the tube. Place the tube in the comparator and jmediately compare with the standards. ?.3 When measuring the color of solids that sublime, oe difficulty may be encountered due to condensation of solid on the cap. In such a case, the Nessler tube may be reheated in the oven after first loosening the cap, or, the color may be measured using an open Nessler tube without a cap (Precaution, see Note 3). In this latter case the caps should also be removed from the standards. No t e 2: Precaution--Adequate ventilation should be provided if open tubes are used. 9.4 In no case shall this test method be applied if the molten sample contains any visible turbidity. 10. Report 10.1 Report as the color, the number of the standard that most nearly matches the sample. In the event that the color lies midway between two standards, report the darker of the two. 10.2 If, owing to small differences in hue between the sample and the standards, an exact match cannot be obtained, but an estimate is possible, report the range over which an approximate match is obtained, and report the sample as "off hue." 10.3 If, owing to large differences in hue between the sample and the standards, no estimate is possible, report the sample as "no match." 11. Precision 11.1 Duplicate results by the same operator should be considered suspect if they differ by more than the following amounts: Platinum-Cobalt Color Repeatability Under No. 50 No. 50 to No. 100 Over No. 100 2.5 5 10 11.2 The results submitted by each of two laboratories should not be considered suspect unless they differ by more than the following amounts: Platinum-Cobalt Color Reproducibility Under No. 50 No. 50 to No. 100 Over No. 100 5 10 15 The American Society lor Testing and Materials takes no position respecting the vaTidity ofany patent rights asserted In connection with any item mentioned in thia standard. Users of thts standard are expressly advised that determination otthe validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and 'Itnotrevised, 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 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. 609 DUP050296171 .# Designation: D 2030 - 84 (Reapproved 1989)1 Standard Test Method for Water Solubility of Refined Pyridine1 This standard is issued under the fixed designation D 2030; 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. " No t e--Editorial changes were made throughout in April 1989. 1. Scope 1.1 This test method covers the determination of the solubility of refined pyridine in water. 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 Imitations prior to use. For a specific hazard statement, see Section 6. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 2.2 Other Document? OSHA Regulations, 29, CFR, paragraphs 1910.1000 and 1910.1200 3. Summary of Test Method 3.1 Specific volumes of pyridine and water are mixed, allowed to stand for 30 min at room temperature, and the clarity of the solution noted. 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0D on Organic Nitrogen Compounds. Current edition approved March 30, 1984. Published June 1984. Originally published as D 2030 - 54 T. Last previous edition D2030 - 67 (1977). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 2 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. . 4. Significance and Use 4.1 Water solubility is a qualitative detection of oj| contaminants in pyridine. 5. Reagents 5.1 Purity of Water--Unless otherwise indicated, reftjti ences to water shall be understood to mean reagent watqjf conforming to Types I to IV of Specification D 1193. 6. Hazards 6.1 Consult current OSHA regulations and supplier's! Material Safety Data Sheets for all materials used in this teg method. ; 7. Procedure 7.1 Measure 10 mL of pyridine sample in a 100-mLi mixing cylinder and dilute to 100 mL with water. Chopper,fj and mix thoroughly by shaking. Let stand for 30 Min room temperature. 7.2 Fill another cylinder with 100 mL of water compare the clarity of the specimen solution with that of the J water. ' - 8. Report 8.1 Report the appearance of the specimen solution _ "clear," "very slightly cloudy," "slightly cloudy," orlff "cloudy." ' ft j No t e--If clear the specimen "passes"; if other than clear tk| specimen "fails." 9. Precision and Bias 9.1 No statement is made about either the precision or the? bias of this test method, since the result merely states; whether there is conformance to the criteria for success; specified in the procedure. The American Society lor Testing and Materials takes no position respecting the validity ofany patent rights assertedin connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, 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, eitherreapprovedor withdrawn. Yourcomments ate invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive carelui 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 Stsndards, 1916 Race St., Philadelphia, PA 19103. 61G DUP050296172 I Designation: D 2031 - 84 (Reapproved 1989)'61 Standard Test (Method for Reducing Substances in Refined Pyridine1 This standard is issued under the fixed designation D 2031; the number immediately following the designation indicates the year of original adoption or, in the case of revision, theyearoflast 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 No t e--Editorial changes were made throughout, including the title, in April 1989. Scope .1 This test method covers the qualitative determination reducing substances in refined pyridine. 1.2 This standard may involve hazardous materials, operons, and equipment. This standard does not purport to 'ress all ofthe safety problems associated with its use. It is s responsibility of the user of this standard to establish ~ropriate safely and health practices and determine the iplicability of regulatory limitations prior to use. For egific hazard statements, see Section 6. Referenced Document 1 ASTM Standard: 1193 Specification for Reagent Water2 * \2 Other Document? pSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200. Summary of Test Method 3.1 Specified volumes of pyridine and potassium permanate are mixed, allowed to stand for 30 min at room perature, and the color of the solution noted. Significance and Use 4.1 This test method gives a qualitative means of detec1 n of reducing substances in pyridine. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be d in all tests. Unless otherwise indicated, it is intended at all reagents shall conform to the specifications of the mmittee on Analytical Reagents of the American ChemSociety, where such specifications are available.4 Other 'es may be used, provided it is first ascertained that the gent is of sufficiently high purity to permit its use without sening the accuracy of the determination. 1 This lest method is under the jurisdiction of ASTM Committee D-16 on romatic Hydrocarbons and Related Chemicals and is the direct responsibility of ^committee DI6.0D on Organic Nitrogen Compounds. Current edition approved March 30. 1984. Published June 1984. Originally Wished as D 2031 - 64 T. Last previous edition D2031 - 67(1977). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. Available from Superintendent of Documents, U.S. Government Printing ffice, Washington, DC 20402. "Reagent Chemicals, American Chemical Society Specifications," Am. ChemI Soc., Washington, DC. For suggestions on the testing of reagents not listed by American Chemical Society, see "Reagent Chemicals and Standards," by ~h Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States armacopeia. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Types I to VI of Specification D 1193. 5.3 Potassium Permanganate Solution (3.2 g/L)--Dis solve 3.2 g of potassium permanganate (KMn04) in water and dilute to 1 L in a volumetric flask. Standardization of the solution is not required. Store the permanganate solution in a brown bottle and prepare fresh every 30 days. 6. Hazards < 6.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 6.2 Clean all equipment used to store and handle the permanganate solution with concentrated hydrochloric add (HQ, sp gr 1.19) and rinse thoroughly with water. Contin uous use of such equipment without cleaning results in, a deposition of manganese dioxide (Mn02) which catalyzes reduction of the permanganate. 7. Procedure 7.1 Pipet 5 mL of pyridine sample and 0.5 mL of KMh04 solution into a 25 by I50-mm test tube. Mix thoroughly by shaking, stopper, and let stand for 30 min at room tempera ture. 7.2 Note the color of the specimen solution. If a brown color or precipitate interferes, the solution should be centri fuged or filtered through a sintered glass filter before ob serving the color of the solution. 8. Report 8.1 If the specimen solution retains any permanganate (purple-pink) color, report the specimen "passes." 8.2 If all of the permanganate color has been discharged from the specimen solution, report the specimen "fails." 9. Precision and Bias 9.1 No statement is made about either the precision or the bias of this test method, since the result merely states whether there is conformance to the criteria specified in the procedure. 611 iiitiis DUP050296173 # D 2031 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk oi infringement of such rights, are entirely their own responsibility. ' This standard is subject to revision at any time by the responslbte technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should mate your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. ! 612 DUP050296174  Designation: D 2119 - 87 Standard Test Method for Aldehydes in Styrene Monomer1 This standard is issued under the fined designation D 2119; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearof.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 This test method covers the determination of ehydes in styrene monomer.- Calculated and repotted as ildehyde. jjjl.2 This standard may involve hazardous materials, operions, and equipment. This standard does not purport to dress all ofthe safetyproblems associated with its use. It is ^responsibility of the user of this standard to establish propriate safety and health practices and determine the plicability of regulatory limitations prior to use. For cific hazard statements, see Section 7. I| Referenced Documents |U ASTM Standards: 11193 Specification for Reagent Water2 |D 3437 Practice for Sampling and Handling Liquid Cyclic Products3 12.2 Other Documents: iOSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 ' Summary of Test Method | 3.1 An alcoholic solution of hydroxylamine hydrochlo|de is added to a sample of styrene monomer. Active Idehydes present react in accordance with the following quation: RCHO + NH2OH-HCl -> RCHNOH + H20 + HC1 he hydrochloric acid, which is equivalent to the aldehyde esent in the sample, is titrated with standard sodium ydroxide solution. Ketones, if present, interfere by partially ing with the reagent. Significance and Use 4.1 This test method is suitable for determining the antity of aldehydes, both for quality control and quality surance of the product. . Apparatus 5.1 Erlenmeyer Flasks, glass-stoppered, 250-mL. Jjt 5.2 Pipets, 25-mL. 5.3 Volumetric Flasks, 100-mL. This test method is under the jurisdiction of ASTM Committee D-16 on [Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of ubcommittee D16.0H on Styrene, Ethylbenzene, Cumene, and Naphthalene. Current edition approved May 29, 1987. Published July 1987. Originally published as D 2119 - 62 T. Last previous edition D 2119-82. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U5. Government Printing ffice, Washington, DC 20402. 5.4 Bursts-, 10-mL. (Microburets are preferred.) 5.5 Thermometers, .capable of differentiating lC at am bient. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Com mittee qn 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. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type III of Specification D1193. 6.3 Hydrochloric Acid, Standard {0.05 N)--Prepare a 0.05 N solution of hydrochloric acid (HC1) by diluting 4.15 mL of concentrated HC1 (density 1.19 g/mL) to 1 L with wateri, 6.4 Hydroxylamine Hydrochloride Solution--Dissolve 20 g of hydroxylamine hydrochloride (NH2OH<HCl) in 1 L of methanol and neutralize to the red-yellow end point of thymol blue indicator. 6.5 Methanol. 6.6 Sodium Hydroxide, Standard Solution {0.05 N)--Dissolve 2.00 g of low-carbonate sodium hydroxide (NaOH) in water and dilute to 1 L. Standardize against primary standard benzoic acid. 6.7 Thymol Blue Indicator Solution--Dissolve 0,1 g of thymol sulfonphthalein, sodium salt, in water and dilute to 100 mL. 7. Hazards 7.1 Consult the latest OSHA regulations and supplier's Material Safety Data Sheets regarding all materials used in this test method. 7.2 Styrene monomer is flammable and polymerizes exothermally on contact with peroxides, mineral adds, and A1C13. 8. Sampling 8.1 Collect the sample as directed in Practice D 3437. 9. Procedure 9.1 Pipet 25.0 mL of the sample (Warning--see 7.2) into 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." 613 DUP050296175 D 2119 a 250-mL glass-stoppered Erlenmeyer flask containing 25 ml. of methanol. Record the temperature ofthe sample. Add 0.2 mL of thymol blue indicator and, if necessary, neutralize with 0.05 N NaOH solution or 0.05 N to the red-yellow end point (do not record). Add 25 mL of the neutralized hydroxylamine hydrochloride solution and allow to stand 1 h, shaking the flask occasionally. Titrate to the original red-yellow end point with 0.05 N NaOH solution, dispensed from a 10-mL buret, and record the volume used. Let stand 1 h and again titrate any acid that may have been liberated. Record the total volume of NaOH used. 9.2 Since methanol may contain aldehydes, run a blank determination on 25 mL of methanol. ill if, A -- NaOH solution required for titration of the samp mL, B = NaOH solution required for titration of the methaii blank, mL, N - normality of NaOH solution used, and C = density of styrene monomer. 11. Report 11.1 Report the aldehydes content to the nearest 0.001H 12. Precision 12.1 Repeatability--Duplicate results by the same , ator should not be considered suspect (95 % confides limit) unless they differ by more than the following: Aldehyde Content, % Repeatability, 0.004 0.0006 10. Calculations 10.1 Calculate the percentage of aldehydes benzaldehyde as follows: Aldehydes, % = [{(A - B)N x 0.106)/25C1 x 100 where: as 12.2 Reproducibility--The averages of duplicate resul submitted by each of two laboratories should not be consS ered suspect (95 % confidence limit) unless they differ f more than the following: . Aldehyde Content, % Reproducibility,-' 0.004 0.0016 , ijfl -11 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 tlielr 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 ere Invited,either torrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have hot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. mwm* 614 DUP050296176 Designation: D 2120 - 87 Standard Test Method for Inhibitor, p-fert-Butylcatechol, in Styrene Monomer1 This standard is issued under the fixed designation D 2120; 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 parenthesesindicates the year oflast reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapproval. Scope .1 .This test method covers the measurement of the bunt of residual p-tert-butylcatechol in styrene monomer "the range from 0 to 100 ppm. Any other compound ~wn to produce color when contacted with aqueous dium hydroxide solution will interfere, but may be comhsated for by including it in the preparation of the dard solutions, if its identity and concentration in the pie are known. , j o t e 1--This test method does not necessarily measure the amount /f-i'ert-butylcatechol originally added to styrene. It is known that the rinal amount gradually diminishes on storage. L2 This standard may involve hazardous materials, operifns,,and equipment. This standard does not purport to jdress all ofthe safety problems associated with its use. It is e responsibility of the user of this standard to establish propriate safety and health practices and determine the -licability of regulatory limitations prior to use. For ecific hazard statements, see Section 7. Referenced Documents 2.1 ASTM Standards: ' D1193 Specification for Reagent Water2 f D3437 Practice for Sampling and Handling Liquid Cyclic Products3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 . Summary of Test Method 3.1 The styrene monomer is extracted with aqueous dium hydroxide and the aqueous layer, containing the /m-butylcatechol as the colored quinone, is separated and e color measured. \ Significance and Use 4.1 This test method is suitable for determining the uantity of inhibitor, both for the protection against poymerization while in transit and storage, and for internal uality control. 1 This test method is under the jurisdiction of ASTM Committee D-I6 on * romatic Hydrocarbons and Related Chemicals and is the direct responsibility of ubcommittee D16.0H <m Styrene, Ethylbenzene, Cumene, and Naphthalene. Current edition approved May 29, 1987. Published July 1987. Originally ublished as D 2120 - 62 T. Last previous edition D 2120 - 82. 2 Annual Book ofASTM Standards, Vote 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U.S. Government Priming ffice, Washington, DC 20402. 5. Apparatus 5.1 Separatory Funnels, 125 mL. 5.2 Pipets, 1, 2, 5, 10, and 25 mL. 5.3 Photoelectric Colorimeter or Spectrophotometer, ca pable of absorbance measurements in the wavelength region of 485 nm. 5.4 Sample Cell--Use the cell with the maximum light path available for the instrument being used. 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Copt- mittee 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. ;, 6.2 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. 6.3 Sodium Hydroxide Solution--40 g/L. 6.4 Styrene Monomer, inhibitor-free (Warning--see 7.3). Wash styrene monomer three times with equal volumes of NaOH solution. Wash the monomer with water until the washings are neutral to litmus. No t e 2--Unhibited styrene monomer should be' kept refrigerated at 0 to 5C to prevent polymerization. 6.5 p-tert-Butylcatechol, Standard Solution (125' ppm (mg/kg))--Dissolve 0.113 g of p-tert-butylcatechol in 1000 mL of inhibitor-free styrene monomer at 20"C. (Warning-- See 7.2.) 7. Hazards 7.1 Consult the latest OSHA regulations and supplier's Material Safety Data Sheets regarding all materials used in the procedure. 7.2 Handling Precautions--p-tert-butylcatechol, particu larly when molten or in concentrated solution, is very corrosive to the skin. It is also a systemic poison when taken orally or absorbed in quantity through the skin. 7.3 Flammable Precautions--Styrene monomer is flam mable and polymerizes exothermally in the presence of peroxide, mineral acids, and aluminum chloride. 3 "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.. Nev. York, NY, and the "United States Pharmacopeia.* 615 DUP050296177 D 2120 * Sampling 8.1 Collect the sample as directed in Practice D 3437. 9.Preparation of Calibration Curve 9.1 Prepare standard solutions containing 5, 10, 15 ... 100 ppm (mg/kgj p-tert-butylcatechol (Warning--see 7.2) by adding 2, 4, 6 . . 40 mL of standard p-ferf-butylcatechol solution, respectively, to 125-mL separatory funnels and add sufficient inhibitor-free styrene monomer to make a total volume of 50 mL Add 50 mL of inhibitor-free, styrene monomer only to another 125-mL separatory funnel to serve as a blank. ' 9.2 Add 55 mL of NaOH solution to each of the (separatory funnels prepared as described in 9.1. Shake for 3 (min, allow to settle, and draw off the lower aqueous layer through a filter paper. Measure the absorbance of the clear filtrate exactly 15 min after the addition of the NaOH at a wavelength of 485 nm, using NaOH solution as a reference standard. 9.3 Prepare a calibration curve by plotting the absorbance obtained in 9.2 against the parts per million of p-tertbutylcatechol. 10. Procedure 10.1 Pipet 50 mL ofthe sample (Warning--see 7.3) in| 125-mL separatory funneLProceed as described in 9.2.1 to the calibration curve obtained in accordance with 9.3(3 note the parts per million (mg/kg) of p-terf-butylcata corresponding to the observed absorbance. 11. Report 11.1 Report the inhibitor content of the sample as : per million (mg/kg) of p-tert-butylcatechol. 12. Precision and Bias 12.1 Repeatability--Duplicate results by the sarnie qj|l ator should not be considered suspect (95 % confide! limit) unless they differ by more than the following: p-rerf-tmtylcatechol Content, mg/kg Repeatability, mg/kg 12.6 0.90 12.2 Reproducibility--The averages of duplicate restl submitted by each of two laboratories should not be co||| ered suspect (95 % confidence limit) unless they diff^f more than the following: p-fert-butylcatechol Content, mg/kg Reproducibility, mg/kg 12.6 2.46 TheAmerican Society (or Testing and Metariels 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 arty 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. Your comments ere Invited either (or revision ofthis standard or for additionafstandards 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. mil ....WiiL, 616 DUP050296178 Designation: D 2121 - 90 Standard Test Methods for Polymer Content of Styrene Monomer1 This standard is issued under the fixed designation D 2121; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon <) indicates an editorial change since the last revision or reapproval. |Scope bl These test methods cover the determination of the fine polymer content of styrene monomer. It should be , however, that dimers and trimers are not measured by test methods. |l|2 Test Method A, which is based on the use of a eltrophotometer or photometer, is intended for the quanaiive determination of the polymer content of styrene Otfomer in concentrations up to 15 mg/kg. Samples of ene monomer containing more than 15 mg/kg of styrene Klymer must be suitably diluted before measurement. U.3 Test Method B is a rapid visual procedure that is |tended for the approximate evaluation of polymer to a xijmijn concentration of 1.0 weight %. Samples ofstyrene IdhSm^r having a polymer content of 1.6 weight % or Jeater should be suitably diluted prior to measurement. 11.4 This standard does not purport to address all of the pfetyproblems associated with its use. It is the responsibility ' whoever uses this standard to consult and establish |ngwpriale safety and health practices and determine the pplicability of regulatory limitations prior to use. For ecific hazard statements, see Section 4. Referenced Documents 2.1 ASTM Standards: rD 2827 Specification for Styrene Monomer 9962 I'D3437 Practice for Sampling and Handling Cyclic jr Products2 e 2'.2 Other Document: rOSHA Regulations, 29 CFR, paragraphs 1910.1000 and 11 f910;12003 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. Hazards 4.1 Styrene monomer is flammable and polymerizes exo thermically on contact with peroxides, mineral acids and aluminum chloride. 4.2 Styrene monomer both in liquid and vapor state, when in sufficient concentrations, acts as an irritant to the eyes and respiratory tract. 4.3 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in.this test method. TEST METHOD A--DETERMINATION OF STYRENE POLYMER IN STYRENE MONOMER PHOTOMETER METHOD 5. Summary of Test Method . 5.1 This test method utilizes the fact that styrene poly mers present in the monomer are insoluble in methanol. The styrene polymer content of styrene monomer is determined by measurement of the degree of turbidity produced by the addition of dry methanol to the styrene monomer sample. 6. Significance and Use 6.1 This test method can be used for determining polymer concentrations in styrene monomer. 6.2 'This .test method will not detect dimers and trimets. 6.3 This test method can be used for plant control and for specification analysis. Purity of Reagents 3.1 Reagent grade chemicals shall be used in all tests. Inless otherwise indicated, it is intended that all reagents jjnall conform to the specifications of" the Committee on Analytical Reagents of the American Chemical Society, yhere such specifications are available.4 Other grades may be 1 These lest methods are under die jurisdiction of ASTM Committee D-l 6 bn \romaiic Hydrocarbons and Related Chemicals and are the direct responsibility of Subcommittee D16.0H on Styrene, Ethylbenzene, Isopropylbenzene. j|' Current edition approved May 25, 1990. Published July 1990. Originally published as D 2121 - 62. Last previous edition D 2121 - 84. 2 Annual Book ofASTM Standards. Vol 06.03. :i 3 Available from Superintendent of Documents, U.S. Govemnment Printing Office, Washington, DC 20402. "Reagent Chemicals, American Chemical Society Specification," American l&beimcal Society, Washington, DC. For suggestions on the testing of reagents not H$ted by the American Chemical Society, see "Reagent Chemicals and Standards," it Joseph'Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United ates Pharmacopeia." 7. Interferences 7.1 Small changes in turbidity may occur with time, it is, therefore, important that the absorbance of calibration mixtures and samples be determined after standing the same length of time. 7.2 Hexane is used for two reasons: 7.2.1 To block out any color in the styrene, and 7.2.2 To indicate dissolved water in the styrene. 8. Apparatus 8.1 Pipets, 10 and 15-mL. 8.2 Bottles or Flasks, of suitable size equipped with glass stoppers. 8.3 Spectrophotometer or Photometer Cells, with 50 to 150-mm light path. 8.4 Spectrophotometer or Photometer, capable . of absorbance measurements in wavelength region of 420 am and sensitive to 1 mg/kg of styrene polymer. 617 DUP050296179 # D2121 9. Reagents and Materials 9.1 Hexane, dry. 9.2 Methanol, dry. 9.3 Polystyrene: 9.3.1 Prepare polystyrene as follows: wash 30 iriL of styrene monomer twice with equal volumes of 1 N NaOH solution and twice with equal volumes of water. After the second water wash, filter the styrene through two layers of rapid filtering ready folded filter paper. Pour about 20 mL of this styrene monomer into a test tube and heat in an oven at 100C for 24 h to promote polymerization. At the end of this time, remove the polystyrene from the test tube by breaking the tube and discarding all glass. Grind the polymer plug to a fine powder in an agate mortar. 9.3.2 Commercially available .high-purity polystyrene pel lets can be used; however, high-molecular weight polystyrene should be specified. 9.4 Styrene Monomer, conforming to Specification D 2827. 9.5 Toluene, dry. 10. Sampling 10.1 Sampling shall conform to Practice D 3437. 11. Calibration and Standardization 11.1 Apparatus--Prepare and operate the spectrophotom eter or photometer in accordance with the manufacturer's instructions. l\.2 Reference Standards and Blanks: 11.2.1 Dissolve 0.0905. g of polystyrene in 1000 mL of toluene measured at 25G, which is equivalent to 100 mg/kg of polystyrene in styrene. 11.2.2 Make standard solutions containing 1, 3, 6,9, 12, and 15 mg/kg of styrene polymer by diluting 1, 3, 6, 9, 12, and 15 mL of the 100 mg/kg standard solution to 100 mL with toluene in a volumetric flask at 25C. 11.3 Calibration Curves and Tables: 11.3.1 Into each of a series of bottles equipped with glass stoppers pipet J5 mL of dry methanol and 10 mL of a polymer standard and mix thoroughly. Into another,series of bottles pipet 15 mL of hexane arid 10 mL of each polymer standard and mix thoroughly. Other volumes may be used, depending on the capacity of the spectrophotometer cell as long as the 3:2 proportion is maintained. 11.3.2 Allow the solutions to stand in the stoppered bottles for 15 min 1 min (Note 1): At the end of this time, pour the solutions into the spectrophotometer cells and measure the absorbance of each at a wavelength of 420 nm using the hexane/polymer standard as the blank (Note 2). No t e 1--Small changes in turbidity may occur with time. It is, therefore, important that the absorbance of calibration mixtures and samples be determined after standing the same length of time. No t e 2--The hexane is used for two reasons: (1) to blank out any color in the styrene, and (2) to indicate dissolved water in the styrene. 11.3.3 Prepare a calibration curve by plotting the absorbance against the milligrams per kilogram of polymer. 12. Procedure 12.1 Pipet 15 mL of hexane into a bottle equipped with a 12.2 Into a second bottle, pipet 15 mL of dry methanol. 12.3 Add 10 mL of styrene monomer to each bottle i mix thoroughly. 12.4 Proceed as described in 11.3.2 using the hexa styrene mixture as the blank. 13. Calculation or Interpretation of Results 13.1 Read the milligrams per kilogram of polystyre directly from the calibration curve. No t e 3--Milligrams per kilogram can be converted to weigljl percent by dividing by 10 000. * 14. Report 14.1 Report the polymer content of the sample as mil grams per kilogram of polymer. 15. Precision and Bias :>irf ||1|| 15.1 Repeatability--Duplicate results by the same oi ator should not be considered suspect unless they differ^ more than the following amount: : Range, mg/kg 0 to IS Repeatability, mg/kg 0.5 W 15.2 Reproducibility--Results submitted, by eaqh of tv^| operators using the same apparatus should not be considered, suspect unless they differ by more than the follow amount ! Range, mg/kg. 0 to 15 Reproducibility, mg/kg . 1.0 TEST METHOD B--VISUAL EVALUATION OF STYRENE POLYMER CONTENT OF STYRENE MONOMER 16. Summary of Test Method 16.1 This test method utilizes the fact that styrene poly-J mers are insoluble in methanol. The polymer , content of a| sample of styrene monomer is evaluated by visual observa-:) tion, of the degree of turbidity produced by the addition oft methanol to the sample. The order of magnitude of the polymer content of styrene monomer in the incremental steps, 0.00,1, 0.01, 0.1, and 1.0 weight % may. readily be ;i differentiated visually. For 0 % observe pure dry methanol. 17. Apparatus 17.1 Test Tube, 25 by 150-mm. il.l' Pipets, 2 and 10-mL. TABLE 1 Relationship Between Polymer Content of Styrene Monomer and Turbidity of Mixture of Two Parts by Volume Styrene Monomer and Ten Parts by Volume Dry Methanol Polymer Content of Styrene Monomer by Weight, %A Description of Turbidity of Styrene-Methanol Mixture 1.0 or greater 0.1 0.01 0.001 None milk-white opaque liquid with heavy white precipitate milk-white opaque Squid with no evidence of sedimen tation cloudiness readily visible, but mixture still transparent faint trace of cloudiness: detectable only by compari son with pure dry methanol no cloudiness discernible by comparison with pure dry methanol A It is suggested that the analyst initially perform the test using reference mixtures described In this table as a guide `.n experienced analyst Carl estimaSs the polymer content reliably without the use of reference mixtures. 618 DUP050296180 $ D 2121 17.3 Daylight Fluorescent Tube, equipped with curved [lector. 8. Reagents |!18.1 Methanol, dry. pirt.2 Polystyrene, uncolored, unfilled, unlubricated (see Ik 18.3 Toluene, dry. Procedure 19.1 Pipet 2 mL of sample of styrene monomer into a an, dry test tube, add 10 mL of dry methanol by means of a pipet, stopper the test tube with a cork covered with aluminum foil, and shake vigorously for a few seconds. 19.2 After shaking the test tube, inspect the mixture visually by looking through it toward a source of artificial daylight. Compare the observed turbidity ofthe mixture with the descriptions of turbidity given in Table 1 or against known standards. If standards are desired, they may be prepared using polystyrene and toluene. 20. Report 20.1 From Table 1 select the turbidity description that most nearly approximates that of the sample, and report the corresponding polymer content. The American Society for Testing andMaterials iakes.noposition respecting the validity of any patentrights 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-arid must.be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you 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. 619 r DUP050296181 Designation: D 2232 - 81 (Reapproved 1990) Standard Test Method for Evaporating Residue of Naphtlhalene1 This standard is issued under the fixed designation D 2232; 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. Scope 1.1 This test method covers the determination of the evaporation residue of naphthalene. 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 6.1 and Notes 2 and 3. 2. Referenced Documents 2.1 ASTM Standards: D 3438 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride12 E 145 Specification for Gravity-Convection and Forced- Ventilation Ovens3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Summary of Test Method 3.1 A weighed quantity of naphthalene is heated in a fared dish for 3 h at 105C in a forced-draft oven and the residue is weighed. 4. Significance and Use 4.1 Evaporation residue is an empirical measure of non volatile impurities in naphthalene. This test method is suitable for setting specifications and for use as an internal quality control tool. 5. Apparatus 5.1 Evaporating Dishes, porcelain, shallow form.5 5.2 Drying Oven, forced-ventilation, conforming to Spec ification E 145 Type II, Grade A or B.. 6. Hazards 6.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 7. Sampling 7.1 Refer to Practice D 3438 for proper sampling and handling of this product analyzed by this test method. No t e 1: Precaution--Sampling should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations. 8, Procedure 8.1 Place the evaporating dish in the drying oven and heat at 105 5C for at least 30 min. Remove from the oven and cool in a desiccator. Weigh the cooled dish to the nearest 0.001 g. 8.2 Transfer to the tared dish 9.5 to 10.5 g, weighed to the nearest 0.1 g, of the thoroughly mixed naphthalene spec imen. No t e 2: Precaution--Specimens for this determination should be handled in the solid state. 8.3 Place the dish and contents in the forced draft oven. Maintain at 105 5C for 180 5 min. No t e 3: Precaution--Specimens should be placed as near.the center of the oven as possible (both horizontally and vertically). The oven should not contain other volatile materials during this determination, nor should it contain objects large enough to change the flow pattern of the circulating air. The draft control on the oven should be fully open. 8.4 Remove the dish from the oven, cool in a desiccator, and weigh to the nearest 0.001 g. 9. Calculation -- 9.1 Calculate the evaporation residue content of the sample, E, as follows: E=[(B- A)/C] x 100 where: E = evaporation residue, wt %, B = weight of evaporating dish and residue, g, A = tare weight of evaporating dish, g, and C = weight of sample used, g. 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0H on Styrene. Ethylbenzene. Cumene, and Naphthalene. Current edition approved Nov. 27, 1981. Published January 1982. Originally published as D 2232 - 63 T. Last previous edition D 2232 - 67 (1977). 2 Annual Book ofASTM Standards. Vol 06.03. 3 Annual Book ofASTM Standards, Vol 14.02. * Available from Superintendent of Documents, U.S. Government Printing Office,.:WiKfeington, DC 20402. 5 Coors size Ho. 1 dishes have been found satisfactory for this purpose. 10. Precision and Bias 10.1 Precision data have been established for all types of samples. Limited cooperative tests were conducted in 1962 which provide the following data to be used for judging the acceptability of results (95 % probability). 10.1.1 Repeatability^-Duplicate results by the same oper ator should not be considered suspect unless they differ by more than the following amounts: 620 mm m-r. DUP050296182 # D 2232 Average % Evaporation Residue 0.09 0.23 0.36 Repeatability 0.01 0.02 0.02 Degree of Freedom IS 15 15 110.1.2 Reproducibility--The results submitted by each of |o laboratories should not be considered suspect unless the |o results differ by more than the following amounts: Average % Evaporation Residue Reproducibility Degrees of Freedom 0.09 0.02 0.23 0.09 0.36 0.07 4 4 4 10.1.3 Bias--Bias has not been addressed in this test method because no reference material or values were available. The American Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users ofthls '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 bo reviewed every ftve years and if notrevised, eitherreapproved or wlthdray/n. Your comments areinvited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. Ifyou 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 621 m ., DUP050296183 # Designation: D 2306 - 81 (Reapproved 1985) Standard Methods for Xylene Isomer Analysis by Gas Chromatography1 This standard is issued under the fixed, designation D 2306; the number immediately following the designation indicates die year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 Method A covers the determination of the individual Cg aromatic isomers and C9 aromatic compounds in the following xylene products: 1.1.1 Nitration grade xylene conforming to Specification D814.13.2> Industrial grade xylene conforming to Specification D 364, and 1.1.3 Ten-degree xylene conforming to Specification D 846. No t e 1--Nonaromatics may be determined using Test Method D 2360. 1.2 Method B covers the determination of toluene in the presence of significant amounts of nonaromatics in the xylene products listed in 1.1. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability ofregulatory limitations prior to use. For specific precautionary statements, see Section 5. 2. Referenced Documents 2.1 ASTM Standards: D 364 Specification for Industrial Grade Xylene2 D843 Specification for Nitration Grade Xylene3 D846 Specification for Ten-Degree Xylene3 D1319 Test Method for Hydrocarbon Types in Liquid Petroleum Products by Fluorescent Indicator Adsorp tion4 D2003 Method for Isolation of Representative Saturates Fraction from High-Olefinic Petroleum Naphthas5 D2360 Test Method for Trace rmpurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography3 D3244 Practice for Utilization of Test Data to Determine Conformance with Specifications5 D3437 Practice for Sampling and Handling Liquid Cyclic Products3 1 These methods are under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of Subcommittee DI6.0A on BTX, Cyclohexane, and Their Derivatives. Current edition approved July 31,1981. Published September 1981. Originally publitiied as D 2306 - 64. Last previous edition D 2306 - 67 (1977). 2 Discontinued, see 1981 Annual Book ofASTM Standards, Part 29. 2 Annual Book ofASTM Standards, Vol 06.03. Annual Book ofASTM Standards, Vol 05.01. iiMmttal Baok ofASTM Standards, Vol 05.02. E 260 Recommended Practice for General Gas Chroma tography Procedures6 2.2 Other Document:1 OSHA Regulations--Consult current regulations on han dling materials referenced in these methods. 3. Summary of Method 3.1 The sample is introduced into a gas-liquid partition column. The components are separated as they pass through the column with a carrier gas, and their presence in the effluent is detected and recorded as a chromatogram. Either packed or capillary columns are permitted, and either thermal conductivity or flame ionization detectors are per missible. The composition of the sample is determined from the chromatogram by comparing peak heights or areas with those obtained from a synthetic sample. No t e 2--Reference should be made to Recommended Practice E260. 4. Significance and Use 4.1 These methods are suitable for setting specifications on the materials referenced in 1.1.1 through 1. L3. These methods may also be used as an internal quality control tool and in development or research work. See Section 7 for interferences. 5. Precaution 5.1 Consult the latest OSHA regulations regarding all materials used in these procedures. 6. Sampling 6.1 Sampling of materials to be tested byThese methods should follow safe -rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations. Refer to Practice D3437 for proper sampling and handling or aromatic hydrocarbons analyzed by these methods. METHOD A 7. Interferences 7.1 Nonaromatic compounds may interfere with the de termination of toluene when certain columns are used. When the recorder chart indicates the presence of non aromatic compounds which might interfere with the mea surement of toluene, separate the nonaromatic fraction from the sample and compare the chromatographic chart on this fraction with the chart from the analysis of the aromatic 6 AnnuaI Book ofASTM Standards, Vol 14.01. 7 Available from Occupational Safety and Health Review Commission. 1825 K SL, N.W., Washington, DC 20006. 622 DUP050296184 D 2306 nple to determine the amount of interference. |No t e 3--A modification of the method and apparatus described in |t Method D 1319 may be used for the separation of nonaromatic lltions. The modification consists of adding a 5-fit section of 14-mm ling on top of the fluorescent indicator adsorption column, adding Jitional gel to nearly fill the added section and using from 10 to 100 of sample according to the volume of nonaromatics present. The paratus described in Method D 2003 may also be used. Apparatus 8.1 Chromatograph--Any gas chromatograph having eiier a thermal conductivity or hydrogen ionization detector y be used. The detector system must have sufficient ajsitivity to obtain a .deflection of at least 2 mm for 0.1 uid volume % of toluene and isopropyl benzene in the Lple being analyzed or in the synthetic blend. 8.2 Recorder--A 1 to 10-mV recorder with a full-scale iponse time of 2 s or less and a maximum noise of 0.3 % f full scale. 8.3 Column--The column must be capable of resolving ie Cg aromatic compounds as individual isomers and iparate from toluene or C9 aromatic compounds or non omatic compounds which may be present in the sample. e resolution of the column must be such that under the Iterating conditions selected the distance from the base line j the depression between two adjacent peaks must be not iore than 50 % of the height of the smaller peak. Columns lay be either packed or capillary.8 The following materials ive been used successfully as liquid substrates: | m-bis (m-phenoxy-phenoxy) benzene +2 % squalane, UCON 1540 or UCON LB-550X,9 di--propyl tetrachlorophthalate, squalane, and | 40 % 1,2,3 fs(2-cyanoethoxy) propane + 60 % oxy-to(2-ethyl benzoate) di-K-decylphthalate No t e 4--The use of other columns is permitted providing the olution obtained fulfills the requirements stated in 8.3. 8.4 Gas Chromatography System--The readout noise (evel of the operating gas chromatography system must be nfficiently low so as to affect individual C8 alkylbenzene esults by less than 0.1 % absolute. . Reagents and Materials 9.1 Pure compounds for calibration shall include toluene, thylbenzene, p-xylene, m-xylene, o-xylene and isopropyl benzene of a purity of not less than 99 %. Ifthe purity of the (calibration compounds is less than 99 %, the concentration land identification of impurities must be known so that the [Composition of the weighed blends can be adjusted for the |presence of the impurities. 9.2 Carrier Gas--Helium or hydrogen for use on thermal conductivity detector units, or nitrogen, helium, or argon for use on flame ionization detector units. 8 Capillary or open tubular columns are covered by U.S. Patient No. 2.920,478 held by the Perkin-Elmer Corp., Norwalk, CT. Such columns are available from the Perkin-Elmer Corp. 9 Registered trademarks of the Chemical Division of the Union Carbide Corp. No t e 5--When hydrogen is used, special precautions should be taken to prevent gas leakage in order to prevent possible explosion.10 9.3 Liquid Phase for column from those listed in 4.3 or other suitable material. 9.4 Solid Support for use in packed column, usually crushed firebrick or diatomaceous earth. No t e 6--Sieve sizes of 30 to 60 or 60 to 80 have been used successfully. 9.5 Liquid Charging Devices, such as micro syringes. 9.6 Column Preparation Solvents, such as dichloromethane. 10. Preparation of Apparatus 10.1 Column Preparation--In preparing packed columns, some laboratories have found that acid washing of the solid support followed by a water washing and drying in an oven improves the resolution of the column.11 The liquid sub strate is usually dissolved in a solvent, such as methylene chloride or toluene, in order to place the stationary liquid on the solid support. Liquid to solid ratios are usually about 15 to 20 g of liquid substrate to 100 g of solid. 10.2 Chromatograph--Mount the column in the chro matograph and adjust to the conditions necessary (Table 1) to give the desired separation. Allow sufficient time for the instrument to reach equilibrium as indicated by a stable recorder base line. Control the temperature in the chromato graph so that it is constant to within 0.5C without thermo stat cycling causing an uneven base line. Control the carrier gas flow at a constant rate to within 1 mL/min on a packed column or 0.2 mL/min on capillary columns. Measure % flow rate using the soap bubble technique. To do this, connect the column effluent gas to the bottom of a buret containing a small amount of liquid soap. Allow the gas to form a soap bubble flowing upward in the buret. Measure with a stopwatch the time required for a chosen bubble to flow a selected number of millilitres. 10.3 Synthetic Blends--Prepare a synthetic mixture from pure hydrocarbons containing all'of the aromatic com pounds present in the sample to be analyzed and within 5 numerical % of the concentration'of each compound pres ent. In preparing the blend, weigh each compound added on 10 Consult Pamphlet G-5, obtainable from the Compressed Gas Association, Inc., 500 Fifth Ave., New York, NY 10036. " Zlatkis, Albert, Ling, Su-Yu, and Kaufman, H. R,, "Resolution of Isometric Xylenes by Gas Liquid Chromatography." Analytical Chemistry, Vol 31, 1959, pp. 945-947. TABLE 1 Typical Concfitions for Chromatographic Separation Liquid Phase m-dfc{phenoxy-Phenoxy) Benzene UCON LB-550X Solid support, sieve size Column length, It (m) Diameter, in. (mm) Temperature, "C Carder flow, mL/mln Detector Sample size, pL Split Weight, 55 200 (61) 0.01 (0.3) 65 to 96 1 to3 flame ionization 0.6 to 1 600 to 1500+1 5 to 7 {of coating solution) 150(46) 0.01 (0.3) 60 to 70 1 to 3 flame ionization 1 to 2 600 to 1500 + 1 5 to 7 (of coating solution) 623 DUP050296185 # D2306 an analytical balance in a suitable container. The mixture should be accurate to 0.1 % of any component. 11. Procedure 11.1 Inject the desired volume of synthetic blend into the column and record the peaks on the sensitivity setting which allows the maximum peak height. Using the same sample size and instrument conditions, inject the sample into the column and record the peaks (see Note 1). 12. Calculations 12.1 Peak Height Method--Measure the peak height of each C8 aromatic component. Adjust these values to com pensate for the difference in volumes charged by multiplying each peak height of the sample by 2PJ2PS Where: =, sum of the peak heights of the standard, and SPj = sum of the peak heights of the sample, i Calculate the percentage by weight of each component as follows: Concentration, weight % = (PJP,,) * S where: P, == adjusted peak height of component in the sample, , P0 ~ observed peak height of component in the standard, and S = percentage by weight of component in the standard. 12.2 Area Measure Method--Measure the area of each C8 aromatic component and adjust these values to compensate for the difference in volumes charged by multiplying each area ofthe sample by XAJ'ZA,, where: ' 2Aa - sum of the areas of the standard, and ~LA,, = sum of the observed areas of the sample. 12.2.1 Calculate the percentage by weight of each compo nent as follows: Concentration, weight % = (AJA^) x S where: As = adjusted area of component in the sample,. Aa -- observed area of component in the standard, and S - percentage by weight of component in the standard. 12.3 formalize the results by multiplying the weight percent of each compound by (100 -- N)JT where: N -- percentage by weight of compounds other than Cg aromatics, and T = sum of the Cg aromatic compounds. 12.4 When desired, convert the analysis to a liquid volume basis by multiplying the percentage by weight ofeach aromatic compound by (specific gravity of sample)/(specific gravity of compound) using the specific gravities for the compounds shown in Table 2. TABLE 2 Specific Gravities of Aromatic Compounds Compound Sp <3r 15.50/15.S6C Toluene Ethylbenzene p-xylene m-xylene o-xylene Isopropybenzene ff-propylbenzene 0.8719 0.8717 0.8657 0.8887 0.8848 0.8663 0.8666 13. Precision 13.1 The following criteria should be used to judge the acceptability (95 % probability level) of results obtained by this method: . : 13-1.1 Repeatability--Duplicate results by the same oper ator should not be considered suspect unless they differ by mbre than the amount shown in Table 3. 13.1.2 Reproducibility^--The results submitted by each of two laboratories should not be considered suspect unless they differ by more than the amount shown in Table 3. No t e 7--The precision estimates in Table 3 are based on interiaboratory. study on six samples covering the concentration ranges indicated. One analyst in each of nine laboratories performed duplicate determina tions on the sanie day. Seven laboratories calculated results from peak heights and all nine laboratories calculated results rising area measure: meats.' Three of the samples were from petroleum and lhfee were from coal tar. Practice D 3244 was used in developing the precision estimates. METHOD B--ALTERNATIVE METHOD FOR TOLUENE IN THE PRESENCE OF NONAROMATICS 14. Summary ofMethod 14.1 The method is the same as that described in Section! 2. In addition, nonaromiatic fractions representative of the material in the sample . tQ( be analyzed are separated by Method D 2003. Gas chromatography columns to be used are evaluated using, nonaromatic fractions, and use of columns is limited to those on which 5 % of nonaromatic material result in an indication of less than 0.25. % toluene arid less than 0.5 % of any ofthe Cg compounds. 15. Apparatus - - 15.1 All of the apparatus specified in Section 8.' 15.2 Column: 15.2.1 The column must meet all of the specifications listed in 8.3. 15.2.2 No column may be used on which the ratio ofthe area of the nonaromatics to the area of toluene exceeds 0.25 or which the ratio of thearea of thd noriaromatics to the area of any of the other Cg aforriaiic compounds exceeds 0.5 as described in Section 18. Table 4 gives typical columns and conditions which have been used, .. . ! ... 16. Reagents and Materials 16.1 All reagents and materials listed in Section 9, 16.2 Normal nonane of a purity not less than 99 3 >, and 16.3 Normal decane of a purity riot less than 99 % 17. Preparation of Apparatus 17.1 Prepare the column and chromatograph according to 10.1 and 10.2. 17.2 Synthetic Blends: 17.2.1 Prepare a synthetic mixture from pure hydrocar bons containing all the aromatic compounds present in the Component Ethylbenzene Paraxyterte Metaxylene Orthoxylene C9 aromatics TABLE 3 Precision Data % Concentration Repeatability 4 to 20 9 to 30 40 to S3 5td-22 0.3 to 1 0.6 0.7 0.8 0.9 0.3 Reproducibility 1.2 1.2 2.4 1.7 0.7 624. DUP050296186 0 2306 TABLE 4 Typical Conditions for Chromatographic Separation of Nonaromatics, Toluene, and C8 Aromatics W- ___________________ |r Column Liquid Phase Meta Wgfm-Phenoxy Phenoxy) Benzene Benton-34 Di-n-Decy Phthalate ||d support, sieve size pn length, ft (m) Ketsr. in. (mm) iiperature, C program rate, deg/min pitial hold, min |hier flow ftector impie size, uL pt quid phase, wt % fsdlfler light, % 150 to 200 (46 to 61) 0.01 (0.3) 60 to 85 1 to 2 flame ionization 0.6 to 1 100 +1 to 1000 + 1 3 to 5 {% of coating solution), 10 squalane or Apiezon L 1 to 2,20 80 to 100 15 (4.6) 'A (6.4) 100 ... 60 thermal conductivity 2 5 Dlethyleno giycol succinate 8 300 (91) 0.01 (0.3} 40 to 115 15 15 i flame ionization 0.4 300 + 1 14 aple to be analyzed and within five numerical percent of tje concentration of each compound present. Include nal nonane in the synthetic blend in an amount within 3 umerical % of the concentration of the nonaromatics resent in the sample. In preparing the blend weigh each Impound added on an analytical balance in a suitable mtainer. The mixture should be accurate to 0.1 % of any jfmponent, 17.2.2 Using Method D2003, separate the nonaromatic ion from the sample or material similar to the sample to I analyzed. Prepare a blend containing 5 weight % of the |onaromatic fraction and 95 % normal decane. Label this llend A. 17.2.3 Prepare a blend containing by weight: 5 % of Ibnaromatic material, 1 % toluene, 1 % each of ethylbenene, paraxylene, metaxylene; and orthoxylene; and 90 % lormal decane. Label this Blend B. Evaluation of Column 18.1 Select the conditions to be used for the analysis of |ylene isomers. Charge Blend A into the instrument, using iifficient sensitivity and volume to obtain at least 2 mm peak height for 0.1 % toluene. Record the chromatogram so i to keep all peaks on the chart except normal decane. In a lilar manner charge Blend B, using exactly the same londitions and volume. I! 18.2 Place the chart from Blend B on Blend A so that the orresponding nonaromatic peaks are superimposed. Sketch he area of the nonaromatic portion under each aromatic ak. Measure the area of the nonaromatic portion under lach aromatic peak by a convenient method, such as eometric construction, counting of squares, weighing paper, )r use of a planimeter. 18.3 Divide the area of the nonaromatic portion under J|he aromatic peak by the area of the aromatic peak. 1 18.4 Do not use any column on which the ratio of iponaromatic to toluene areas exceeds 0.25 or the ratio of nonaromatic to any of the C8 aromatic areas exceeds 0.5. 20. Calculations 20.1 Measure the area of all peaks and adjust these values to compensate for the difference in volumes charged by multiplying each area of the sample by AJA,, where: A,, -- the sum of the areas of the standard, and A,, = the sum of the areas of the sample. Calculate the percentage by weight of each component as follows: Concentration. % weight = (AJAa) x 5 where: As = adjusted area of the component in the sample, Aa = observed area of the component in the standard, and S = the percentage by weight of component in the stand ard. 20.2 Normalize the results by multiplying the weight % of each component by 100IT where: T = the sum of the unnormalized results. 20.3 For best results on nonaromatics, Test Method D2360 should be used for the determination of these compounds. When desired the results from this analysis may be normalized to the nonaromatic by the other method by multiplying the unnormalized percent of each aromatic compound by (100 - N)/T . where: N = percentage by weight of nonaromatic compounds, and T = the sum of the aromatic compounds. 20.4 When desired, convert the analysis to a liquid volume basis by multiplying the percentage by weight ofeach aromatic compound by (specific gravity of sample)/(specific gravity of compound), using the specific gravities for the aromatic compounds shown in Table 2. For nonaromatic compounds, assume that they have the same gravity as normal nonane and use a gravity 0.7217. (19. Procedure 19.1 Inject the desired volume of the synthetic blend similar jo the sample into the column and record the peaks Ion a sensitivity setting which allows the maximum peak fjheight. Using the same sample size and instrument condijions, inject the sample into the column and record the peaks BNote 1). 21. Precision 21.1 The following criteria should be used to judge the acceptability (95 % probability level) of results obtained by this method. 21.1.1 Repeatability--Duplicate results by the same oper ator should not be considered suspect unless they differ by more than the amount shown in Table 5. 625 DUP050296187 # D 2306 TABLE 5 Precision Data--Nonaromatics, Toluene, C,,, . and C9 Aromatics Compounds Nortaromatics Toluene Ethylbenzene Paraxylene Metaxytene Orthoxylene Isopropylbenzene Other Cg aromatics X Concentration 0to2 5 to 7 0 to 0.2 3 to 5 0 to 5 IS to 25 5 to 30 40 to 65 0 to 25 0 to 0.5 0 to 0.5 Repeatability Reproducibility 0.2 0.4 0.2 2.0 0.04 0.05 0.4 1.1 OS! 0.4 0.4 1.4 0.4 0.9 0.7 1.8 0.3 0.7 0.1 0.2 0.1 0.7 21.1.2 Reproducibility--The results submitted by each oj two laboratories should not be considered suspect unless thef differ by more than the amount shown in Table 5. No t e 8--The precision estimates in Table 5 ate based on interlab ratory study on four samples covering the concentration ranges indi. cated. One analyst in each of eight laboratories performed duplical determinations on the same day. Three of the samples were- fron petroleum and one was from coal tar. Practice D3244 was used : developing the precision estimates. 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 v ' *" patent.rlghts, and the risk of infringement of such rights. are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years end ifnotrevised, either reepprovedor withdrawn. Yourcomniants are invited either.forrevision oithis,standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consjdaratioh 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. j. 626 DUP050296188 Designation: D 2323 - 84 (Reapproved 1989)61 Standard Specification for Refined Pyridine (1 Degree)1 This standard is issued under the fixed designation D 2323; 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. fl No t e--Editorial changes were made throughout in April 1989. ftScope;.' .r fl.l This specification covers refined pyridine. .. Pi .2 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in.' this pacification. , . i .. - : Referenced Documents 2.1 ,ASTM Standards:. jD 1078 Test Method for Distillation. Range of Volatile P Organic Liquids2 D1209 Test Method for Color ofGear Liquids (Platinum- f Cobalt Scale)3 ID 1631 Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method2 ID2030 Test Method for Water Solubility of Refined Pyridine2 |p 3437 Practice for Sampling and Handling "Liquid Cyclic Products2 , , , , . , D 3505 Test Method for Density or Relative Density of Pure Liquid Chemicals2 1 this specification is under the jurisdiction of ASTM Committee D-16 on matte Hydrocarbons and Related Chemicals and is the direct responsibility of ommittee D16.0D on Organic Nitrogen Compounds.' (Current edition approved March 30, 1984*. Published June 1984. Originally Ushed as D 2323 - 64 T. Last previous edition D 2323 - 68 (1977). 2 Annual Book ofASTM Standards, Vol 06.03. Annual Book ofASTM Standards, Vols 06,01 and 06.03. 2.2 Other Document:4 OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200 ; 3. Properties 3.i Refined pyridine shall conform to the following re quirements:' Appearance . Odor Specific gravity, 15.56/15.56*0 Color Total distillation range at 760 mm pressure Water Water solubility clear liquid, free of extraneous matter and sediment pyridine, characteristic 0.985 to 0.990 not darker than No. 20 on the platinum- cobalt scale not more than L0C, including the temper ature 115.3 0.1 *C not more than 0.10 weight % clear solution, no turbidity or oil film 4. Test Methods 4.1 The material shall be sampled and the properties described in this specification shall be determined in accord ance with the following ASTM standards: 4.1.1 Sampling--Practice D 3437. 4.1.2 Appearance--Visual inspection. 4.1.3 Specific Gravity--Test Method D 3505. 4.1.4 Color--Test Method D' 1209. 4.1.5 Distillation--Test' Method D 1078, using ASTM Solvents Distillation Thermometer 41C. 4.1.6 Water--Test Method D 1631. 4.1.7 Water Solubility--Test Method' D 2030. * Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. ' The American Society tor Testing end Materials takes noposition 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 ot the validity of any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and 'it not revised, either reapproved or withdrawn. Yourcomments are invited either tor revision ot this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 627 DUP050296189 Designation: D 2324 - 81 (Reapproved 1989),ei Standard Test Method for Carbon Disulfide in Benzene1 This standard is issued under the fixed designation D 2324; 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 revirion or reapproval. e 1 No t e--Editorial changes were made throughout in November 1989. 1. Scope 1.1 This test method covers the determination of carbon disulfide in benzene and other hydrocarbons. 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 (he responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For. specific hazard statements, see Section 8 and Note 1. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products3 2.2 Other Document: OSHA Regulations--29 CFR, paragraphs 1910.1000 and 1910.12004 * 3. Summary of Test Method 3.1 Under specified conditions diethylamine-cupric ace tate reagent reacts with carbon disulfide to produce the yellow-orange color of cupric diethyl-dithiocarbamate. The intensity of the color produced is measured by means of a spectrophotometer. (C2H5)2NH + CS2 --> (C2H5)2NCSSH (diethyldithiocarbamic acid) 2 (C2H5)2NCSSH + Cu (C2H302)2 - ((C2H5)2NCSS)2 Cu + 2 CH3COOH 4. Significance and Use 4.1 This test method is suitable foe setting specifications for carbon disulfide in benzene, other hydrocarbons, and gases by extraction of CS2 into an appropriate liquid hydrocarbon. It may also be used as an internal quality control tool and in development or research work. The test method is applicable to benzene that contains 0.1 to 4.0 mg/kg of carbon disulfide, or benzene that can be diiutt with carbon disulfide-free benzene to a concentration tit falls in this range. 5. Interferences 5.1 Hydrogen sulfide, sulfur dioxide, and xanthates inti fere, causing low results. Thiophene in concentrations as 1 as 100 mg/kg does not interfere. Ordinary variations of lighi temperature, and standing time do not affect the results. 6. Apparatus 6.1 Spectrophotometer5 suitable for measurements at 4 nm with a band width not greater than 35 nm. 6.2 Cells, 5-cm, chemically resistant glass. 6.3 Weighing Bulbs, either as prepared in the laboratdii or commercially supplied.6 6.4 Mohr Pipet, 5-mL equipped with suction bulb. 7. Reagents and Materials 7.1 Purity ofReagents---Reagent grade chemicals shall used in all tests. Unless otherwise indicated, it is intends, that all reagients shall confdrm to the specifications of th( Committee on Analytical Reagents of the American Cheml ical Society, where such specifications are available.7 Other? grades may be used, provided it is first ascertained that the? reagent is of sufficiently high purity to permit its use without? lessening the accuracy of the determination. 7.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water? conforming to Specification D 1193. 7.3 Benzene, carboif'disulfide-free. To a 2-L separatory funnel add 1000 mL of benzene and 200 hiL of alcoholic sodium hydroxide (NaOH) and shake well. Allow to stand 1 h, shaking at 15-min intervals. Draw off and discard the lower layer. Wash 4 times, using 300 mL of water each time, and drawing off and discarding the water (lower) layer after each washing. Filter the treated benzene through dry filter paper into a 1-L glass stoppered bottle. Check the treated benzene for the presence of carbon disulfide as described in Section 11. If carbon disulfide is present, repeat the benzene 1 This test method is under the jurisdiction of ASTM Committee D-I6 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee DI6.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved April 24, 1981. Published August 1981. Originally published as D 2324 - 64 T. Last previous edition D 2324 - 66 (1976). 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. * Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 5 The Beckman Model DU spectrophotometer, manufactured by Beckman Instruments, Inc., 2500 Harbour Blvd,, Mail Station 3ID, Fullerton, CA 92634, or equivalent instrument, has been found satisfactory for this purpose. 6 Available from Jesse Petty Glass Specialities, Box 509, Glen Ellyn, IL. 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." 628- DUP050296190 # D 2324 unification given above. Carbon disulfide-free benzene will iot undergo further diminution in absorbance at 430 trm i'hen it has been thus retreated. 7.4 Carbon Disulfide (CS2). 7.5 Cupric Acetate in Methanol--Add 1.0 0.001 g of cupric acetate monohydrate, powdered, neutral crystals to a 1000-mL glass-stoppered volumetric flask containing approxi mately 600 mL of methanol. Shake to dissolve. Dilute the contents to volume with methanol and mix thoroughly, this reagent should be prepared fresh each month, or sooner if [appreciable amounts of copper salts separate from the solution. 7.6 Diethylamine-Cupric Acetate Reagent--Using a Mohr fpet, add 2.5 mL of diethylamine to approximately 50 mL carbon disulfide-free benzene contained in a 100-mL stoppered volumetric flask. Using a graduated cylinder, 20 mL of cupric acetate solution and dilute to volume ith carbon disulfide-free benzene. Invert to mix. fttoTH 1: Precaution--In addition to other precautions, do not use the Suth for pipetting any solutions, especially where diethylamine or jjgizene are present. No t e 2--This reagent is unstable and a fresh supply must be 1 daily. Sodium Hydroxide, Alcoholic Solution (40 g/L)-- ffeigh 40 1 g of sodium hydroxide (NaOH) pellets and Insfer to a 300-mL Erlenmeyer flask containing 50 mL of later. Swirl to dissolve, cool to room temperature, and then nsfer to a 1000-mL volumetric flask. Dilute to volume th methanol (95%), and mix by shaking. Allow to stand er night. Filter the clear solution into a 1-L bottle. Hazards i8.1 Consult current OSHA regulations and supplier's MateSafety Data Sheets for all materials used in this test thod. 8.2 When handling CS2 use a fume hood free of flames, , surfaces, and sparking equipment. `.3 Wear rubber gloves when handling NaOH pellets. i Sampling . 1 Sampling of materials to be tested by this test method uld follow safe rules in order to adhere to all safety autions as outlined in cuerrent OSHA regulations. Refer Practice D3437 for proper sampling and handling of catic hydrocarbons analyzed by this test method. Calibratioaand Standardization 3.1 Prepare a calibration curve or table showing concen'on versus absorbance by making solutions in the range .0 to 4 mg/kg of carbon disulfide in carbon disulfide-free zene, and then developing the color. Read the absorb- using the method to be used in the test. The solutions be prepared by weighing the carbon disulfide in a ghing bulb, breaking it under carbon disulfide-free ben- and diluting to the proper concentrations with the e grade benzene. The dilution can be made by weighing 'more conveniently, by volume that can be reduced to weight by multiplying the volume added by the density ofthe benzene used. 11. Procedure 11.1 Filter a portion of the sample through dry filter paper to remove any water that might be present. .11.2 Pipet 30- mL of the filtered sample to a glassstoppered 50-mL volumetric flask. 11.3 Pipet 3.0 mL of the diethylamine-cupric acetate reagent into the flask (final volume = 33 mL.). 11.4 Insert the stopper and mix well. 11.5 Allow to stand 30 10 min. 11.6 Read the absorbance at 430 nm in 5-cm glass cells using the filtered sample as a reference material. r No t e 3--If the absorbance is greater than 1.0, dilute an aliquot of the material obtained in 11.1 with carbon disulfide-free benzene and repeat 11.2 through 11.6. Dilution factors must be taken into consider ation when calculating the final' results. 11.7 Obtain a reagent blank, using the procedure de scribed in 11.2 to 11.6, substituting carbon disulfide-free benzene for the sample. Subtract this value from the absorbance value of the sample obtained in 11.6. 12. Interpretation of Results 12.1 Determine the concentration by referring to the concentration versus absorbance curve or table prepared in accordance with Section 10 for each spectrophotometer. 13. Report 13.1 Report the milligrams per kilogram of carbon disulfide corresponding to the absorbance read after a factor for any sample dilution has been applied. 14. Precision and Bias 14.1 The following criteria should be used to judge the acceptability (95 % probability level) of results obtained by this test method: 14.2 Repeatability--Duplicate results by the same oper ator should not be considered suspect unless they differ by more than the following amounts at the indicated levels: CS2 Content, mg/kg Repeatability, mg/kg 0.1 to 0.8 0.8 to 4.0 0.04 " ~ 5 % of mean ' 14.3 Reproducibility--Results obtained by analysts in different laboratories should not be considered suspect unless they differ by more than the following amounts at the indicated levels: CS2 Content, mg/kg Reproducibility, mg/kg 0.1 to 0.8 0.8 to 4.0 25 % of mean plus 0.075 35 % of mean No t e 4--The above estimates of precision are based on interlaboiatory analytical studies of six samples of benzene containing 0.13, 0.54, 1.07,1.82, 6.87,19.9 mg/kg ofCS2. One analyst in each of 8 laboratories analyzed all 6 samples in duplicate on each of 2 days, and one analyst in each of 4 additional laboratories analyzed 3 samples in duplicate on each of 2 days for a total of 224 determinations. The Proposed Recommen dations for Interlaboratory Testing of Industrial Aromatic Hydrocar bons and Related Materials9 was used to determine these precision estimates. No t e 5-The precision estimates are based on data published in the 1966 Report of Committee D-16.9 stman No. 92 diethylamine, available from laboratory suppliers, has been satisfactory for this purpose. 9 Proceedings, ASTM, Vot V>, 1966. 629 si! ialJife, DUP050296191 D2324 The American Society tor Testing and Materials takes no position respecting the validity ofany patentrights asserted in connection witit 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 Itnotrevised, eitherreapproved or withdrawn. Your comments are Invited eitherfor revision ofthis standard or for 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 views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 630 DUP050296192 i Designation: D 2340 - 82 (Reapproved 1987)*1 Standard Test Method for Peroxides in Styrene Monomer1 This standard is issued under the fixed designation D 2340; 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. f' Note--Paragraphs 2.2 and 7.1 were editorially changed in May 1987 I. Scope .1.1 This test method covers the determination of the peroxide content of styrene monomer. J 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to Addressallofthe 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. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water2 D3437 Practice for Sampling and Handling Liquid Cyclic Products3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and I910.12004 . Summary of Test Method 3.1 A sample of styrene monomer is added to a solution If isopropanol and acetic acid. A saturated solution of (odium iodide in isopropanol is added and the solution refluxed. The peroxides present liberate iodine from sodium dide quantitatively. The liberated iodine is then titrated Jnth sodium thiosulfate to a colorless end point. Significance and Use J; 4.1 This test method is suitable for determining the igiiantity of peroxides in styrene monomer both for quality bntrol and quality assurance of the product. . Apparatus 5.1 Erlenmeyer l Flasks, glass-stoppered, 500-mL, uipped with 300-mm Liebig condensers having inner and luter standard taper joints. 5.2 Electric Hot Plate with totally enclosed heating unit. 5.3 Boiling Chips. This test method is under the jurisdiction of ASTM Committee D-16 on imatic Hydrocarbons and Related Chemicals and is the direct responsibility of bcommittee DI6.0H on Styrene, Cumene, Ethylbenzene, and Napthalene. Current edition approved Feb. 26, 1982. Published June 1982. Originally iublished as D 2340 - 65 T. Last previous edition D 2340 - 68 (1977). Annual Book ofASTM Standards, Vols 06.03 and 11.01. Annual Book ofASTMStandards, Vol 06.03. |;4 Available from Superintendent of Documents, U.S. Government Printing ice, Washington, DC 20402. 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.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 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. 6.3 Glacial Acetic Acid. 6.4 Isopropyl Alcohol. 6.5 Sodium iodide Isopropyl Alcohol Solution--Prepare a saturated solution of sodium iodide in isopropanol (approx imately 200 g Nal/L). 6.6 Sodium Thiosulfate, Standard Solution (0.01 N)-- Dissolve 2.5 g of sodium thiosulfate (Na^CVSHjO) and 0.1 g of sodium carbonate (Na2C03) in water and dilute to 1 L. Standardize against primary standard potassium dichromate (K2Cr207). 7. Hazards 7.1 Consult the latest OSHA regulations and supplier's Material Safety Data Sheets regarding all materials used in the procedure. 7.2 Styrene monomer is flammable and polymerizes exotherrnally on contact with peroxides,'"mineral acids,' and aluminum chloride. 7.3 Isopropyl alcohol is flammable and should be kept away from open flame and spark-producing apparatus. Use only a hot plate with totally enclosed heating unit in this analysis. 8. Sampling 8.1 Collect the sample as directed in Practice D 3437.. 9. Procedure 9.1 Add 200 mL of isopropyl alcohol into each of two 500-mL Erlenmeyer flasks containing several boiling chips. 5 "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." 631 DUP050296193 Add 10 mL of glacial acetic acid to each flask. Into one flask pipet 50 mL of the styrene monomer sample. Identify this .flask as "Sample" and the other flask as "Blank." Fit the condenser in place (Caution: see 7.2 and 7.3). Heat the contents of the flasks to boiling and pipet 50 mL of the satnratrat Nal isopropyl alcohol solution into each. 9.2 Continue boiling gently for 10 min. At the end of the boiling period, remove the flasks from the heat source. Rinse each condenser with two 10-mL portions of water, adding ithe rinsings to the respective flasks. Cool the flasks to room temperature. Titrate the liberated iodine in each flask with 0.01 N Na2S203 solution to a light yellow color and continue to titrate slowly until the yellow color just disappears. If. Calculation 10.1 Calculate the peroxide content of the samples as h|drdgen peroxide, in parts per millidn (mg/kg) as follows: ^Peroxides, mg/kg = [(A - B) X N X 1.7 X 104]/(50 X C) where: i. A ?= total millilitres of Na2S203 solution required for titration of the sample* B = total millilitres of Na^Ch, solution required'for titration of the blank, N = normality of Na2S203 solution used, and C = density of styrene monomer at temperature pipette (an approximate density of 0.9 may be used to detei mine the sample weight). 11. Report 11.1 Report the peroxide content to the nearest I mg/kgl 12. Precision 12.1 Repeatability--Duplicate results by the same oper-J ator should not be considered suspect (95 % confidence! limit) unless they differ by more than the following: Peroxide Content, mg/kg Repeatability, mg/kg 1 to 60 12.2 Reproducibility--The averages of duplicate results ^ submitted by each of two laboratories should not be consid-j ered suspect (95 % confidence limit) unless they differ by more than the following: Peroxide'Content, mg/kg Reproducibility, mg/kg 1 to 60 13 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 sublect to revision at shy time by the responsible technical committee andmust be reviewed every five years and if not revised, either reapproved orwithdrawn. Yourcomments are Invited either tor revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your, comments will receive careful conslderalion at a meeting of the responsible technical commtttea, which you may attend. It 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, 632 DUP050296194 Designation: D 2359 - 90 Standard Specification for Refined Benzene-5351 This standard is issued under the fixed designation D 2339; 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. cope S' l This specification covers a grade of benzene known as ed benzene-535. Consult current OSHA regulations and supplier's erial Safety Data Sheets for all materials used in this Scation. referenced Documents 1 ASTM Standards: 847 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons2 848 Test Method for Acid Wash Color of Industrial : Aromatic Hydrocarbons2 849 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons2 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials2 852 Test Method for Solidification Point of Benzene2 853 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons2 11209 Test Method for Color ofClear liquids (PlatinumCobalt Scale)2 D1685 Test Method for Traces of Thiophene in Benzene by Spectrophotometry2 '2324 Test Method for Carbon Disulfide in Benzene2 D2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals3 D 4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateoraetric Colorimetry3 1 This specification is under the jurisdiction of ASTM Committee EM6 on -matic Hydrocarbons and Related Chemicals and is the direct responsibility of ommittee D3 6.0A on BTX, Cyclohexane, and Their Derivatives. ! Current edition approved Oct. 26, 1990. Published December 1990. Originally Wished as D 2359 - 66 T. Last previous edition D 2359 - 85a. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 D4629 Test Method for Organically Bound Trace Ni trogen in Liquid Petroleum Hydrocarbons by Oxidative Combustion and Chemiluminescence Detection3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Properties 3.1 Refined benzene-535 shall conform to the following requirements: Property Carbon disulfide Sulfur Thiophene, max, mg/kg Nonaromatic hydrocarbons, max, weight % N-formyimorpholine as nitrogen Acid wash color, max Acidity Copper corrosion Hydrogen sulfide and sulfur dioxide (H,S, SO,) Appearance Color, max, Pt-Co scale Relative Density, 15.56/15.56 "C or Density, 2(PC, g/cm3 Distillation range including the temperature 80.1 "C at 760 mm Hg pressure, max, *C Solidification point, anhydrous basis, min, "C Specification {if needed) {if needed) 1 0.15 ASTM Test Method D 2324 D4045 D 1685 D 2360 (if needed) pass with 1 none detected pass (la or lb) none detected A 20 0.8820 to 0.8860 D4629 D 848 D 847 D 849 . D 853 D 1209 D 3505 or D 4052 0.8780 to 0.8820 1.0 " D850 5.35 D852 ....... * Clear liquid free of sediment and haze when observedat 18.3 to 25.6`C (65'fo 78F). , B Refer to Method D 850, Sample Section if drying is required. 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 5. Keywords 5.1 benzene; benzene-535 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC. 20402. 633 DUP050296195 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 ol this standard are expressly advised that determination ofthe validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapprovedor withdrawn. Your comments are Invited either forrevision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will recelve,careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race $t., Philadelphia, PA 19103.1 1. 634 DUP050296196 Designation: D 2360 - 82 (Reapproved 1987)'ei Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography1 This standard is issued under the fixed designation D 2360; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. 61 No t e--Editorial changes were made throughout in October 1987. Scope ` .1 This test method covers the determination ofthe total `aromatic hydrocarbons and trace monocyclic aromatic carbons in high-purity benzene, toluene, and mixed lenes by gas chromatography. 1.2 A small amount of benzene in toluene may not be stinguished from the non-aromatics, but the concentra- ns are determined as a composite. Small amounts of ne and/or toliiene in xylenes may not be distinguished m the non-aromatics, but the concentrations are deter- 'ned as a composite. 1.3 Non-aromatic hydrocarbons or individual trace aro- tics can be determined up to a level of 1 %. The lower `t of detection for a single non-aromatic or for a trace ,.matic is 5 mg/kg with the exception of isopropylbenzene mene) in mixed xylenes, which is 200 mg/kg. ; s.1.4 This standard may involve hazardous materials, oper- ions, and equipment. This standard does not purport to Jress all ofthe safety problems associated with its use. It is e responsibility of the user of this standard to establish propriate safety and health practices and determine the plicability of regulatory limitations prior to use. For edfic hazard statements see. Section 7 and Note 3. Referenced Documents 2.1 ASTM Standard: D3437 Practice for Sampling and Handling Liquid Cyclic Products2 2.2 Other Document: OSHA Regulations, 29 CFk, Paragraphs 1910.1000 and 1910.12003 ; Summary of Test Method ` 3.1 An internal standard, n-butylbenzene, is added to the imen which is then introduced into a gas chromato 1 This test method is under the jurisdiction of ASTM Committee D-16 on * roraatic Hydrocarbons and Related Chemicals and is the direct responsibility of bcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their erivatives. Current edition approved Oct. 29, 1982. Published January 1983. Originally Wished as D 2360 - 66 T. Last previous edition D 2360 - 79. 2 Annual Book ofASTM Standards, Vol 06.03. ^ 3 Available from Superintendent of Documents, U.S. Government Printing TfTice, Washington DC 20402. graphic column. The sample passes through the column that separates the non-aromatic and aromatic compounds. The components producing peaks on the chromatogram are detected by a flame ionization detector (FID). The peak areas are measured and the concentration of the composite non aromatics and each trace aromatic component is calculated with reference to the internal standard. 4. Significance and Use 4.1 Hydrocarbon impurities concentrations are typically required for benzene, toluene, and mixed xylenes used as chemical intermediates and solvents. This test may be used for final product inspections, process control, and research work. 4.2 This test method was primarily developed for non aromatic impurities in high-purity aromatics. As can be seen from the precision statement, this test method is not appli cable for detecting trace homologs in a high-purity aromatic product. 5. Apparatus 5.1 Chromatograph--Any instrument having a hydrogen flame ionization detector that can - be operated at -the conditions given in Table 1. The detector-recorder combina tion must have sufficient sensitivity to obtain an area, of 7 mm2/(l mg/kg) of. n-butylbenzene for a 4-pL injection volume (2000 mm2/|ig of -butylbenzene). No t ? 1--The column resolution should be such that benzene is eluted between n-C, and n-C10. The relative retention times on the specified column are: n-Q>, 0.70; benzene, 1.00; and -C10, 1.07. A column of different polarity may not separate all the nonaromatics ahead of the major aromatic or may not separate trace aromatics following it. No t e 2--In some cases it may be difficult to obtain a separated peak for cumene in mixed xylene samples. A new column will usually give adequate separation, but this separation may be lost as the colilmn ages. 5.2 Column--A 3-m length of 6.35-mm (Win.) outside diameter standard copper tubing. 5.3 Recorder, Strip Chart--A 0 to 1-mV range recording potentiometer with a response time of 1 s or less and a maximum noise level of 0.3 % of full scale. 5.4 Microsyringe, 10 and 50-p.L capacity. 5.5 Flask, volumetric, 50-mL capacity. 635 DUP050296197 # D2360 TABLE 1 Instrument Parameters jitfStector dSlumn: : Length, m Qutside diameter, mm Stationary phase, weight % Temperature: Sample inlet system 4C Detector C Column C Carrier gas Flow rate Recorder range, mV Chart speed, cm/min Sample size, piTotal analysis time, min flame ionization copper 3.0 6.35 Carbowax 1540: 25 % on Chromo sorb P, 60 to 80 mesh {Note 1) 200 200 125 helium 60 cm3/min 0 to 1 1 4 38 5.6 Dish, evaporating, 350-mL capacity. 6. Reagent and Materials 6.1 Carrier Gas, helium, 99.99 % purity. 48 6.2 Solid Support--Chromosorb P,4 60 to 80 mesh. 6.3 Liquid Phase-^Polyethylene glycol, Carbowax' 1540,5 or any other liquid phase that will satisfy the separation requirement in Note 1. 6.4 Acetone. 6.5 Methylene Chloride. 6.6 Hydrogen, 99.99 % purity 6:7 Air, compressed. 6.8 n-Butylbenzene. 6.9 Glass Wool. ' 7. Hazards 7.1 Consult current OSHA regulations and.suppliers' Ma terial Safety Data Sheets for all materials used in this test method. 8. Sampling 8.1 Guidelines for taking samples from bulk are given in Practice D 3437. 9. Preparation of Packing 9.1 Prepare packing material, Carbowax 1540 on Chromosorb P, in accordance with the following procedure: 9.1.1 Weigh 40 g ofChromosorb P solid support and pour into the evaporating dish. Dissolve 13.3 g of Carbowax 1540 in approximately 100 mL of methylene chloride (Note 3). Pour the Carbowax 1540 liquid phase-methylene chloride solution into the evaporating dish . containing the Chromosorb P solid support. Stir occasionally while allowing the solvent to evaporate without heating until the packing is thot oughly dry. No t e 3: Warning--Methylene chloride is a toxic material. Avoid inhalation. Use of a forced draft fume hood is recommended. 10. Preparation of Column 10.1 Cleaning of Column--Rinse the tubing with about 50 mL of methylene chloride followed by about 50 mL of 4 Chromosorb P is a registered trademark ofJohns-iytanville Products Corp. 5 Carbowax is a registered trademark of Union Carbide Chemical Co. acetone. Dry the tubing by passing filtered, oil-free air through it or by pulling a vacuum on it. 10.2 Packing of Column--Close one end of the tubing with a small glass wool plug and attach this end to a vacuum source. Start the vacuum and pour the packing into the open end of the tubing. Take care that the vacuum does not pull Jout the glass wool plug. While filling the column, vibrate it with an electric vibrator or tap it to settle the packing. Shut off the vacuum and when the column reaches atmospheric pressure, disconnect the vacuum source. Remove a small amount of packing from the open end of the column and insert a glass wool plug. 11. Calibration 11.1 Response Factors--A relative response factor is not required to relate the response of -butylbenzene to that of the non-aromatics since the average response for non aromatics is approximately the same as for n-butylbenzene on a flame ionization detector. However, a factor is required to relate the trace, aromatics, to the n-butyibenzene. These factors have been determined and are listed in Table 2. 12. Procedure 12.1 Preparation of Chromatograph--Install the chro matographic column and establish the operating: conditions that are listed in Table 1. Allow the chromatograph to run at the required sensitivity until a stable recorder baseline # recorded. ' 12.2 Preparation ofSample--To avoid the possibility df| non-linear response the concentration of the internal stan-; dard added should be adjusted so that it is approximately the same as the expected concentrations of impurities. An internal standard concentration ofabout 1000 mg/kg should be prepared as follows: 12.2.1 To a tared 50 mL volumetric flask carefully add, J using a micro-pipet or microsyringe, 50 pL of nbutylbenzene and weigh to the nearest 0.0001 g (0.1 mg). Fill1 to the mark with the sample to be tested, reweigh, and mix thoroughly. Care must be taken in cleaning the volumetric flasks so that no residual solvent remains to contaminate the sample. 12.3 Injection ofSample--Flush the 10-jxL syringe seyeral times with the sample mixture and inject 4 j j l L ofthe mixture through the septum into the chromatograph. Turn on the recorder and obtain the chromatogram. 13. Calculation 13.1 Interpretation of Chromatogram--Identify on the chromatogram the non-aromatic, the individual trace , aro matic, and the internal standard (n-butylbenzene) peaks by comparison to Fig. 1 or from the retention time ofstandards. TABLE 2 Component Non-aromatics Benzene Toiuena C8 Aromatics n-Butylbenzene C9 Aromatics Response Factors Relative Weight Response Factor 1.00 0.89 0.93 0.97 1.00 1.00 636 DUP050296198 I D 2360 |c range of retention times of nonaromatics, or the type of ce aromatics win depend on the specific pure aromatic ling analyzed. '13.1.1 Measure the areas under the non-aromatic, trace amatic and n-butylbenzene peaks by conventional bthods. Measurement may be accomplished by any jfethod that meets the precision requirements of Section 14. ptable methods ofmeasurement are by planimeter or by integration. 113.1.2 It may be necessary to make sure that none of the impounds in the sample interfere with the internal stan- 1 peak, g 13.2 Calculations: 113.2.1 Calculate the weight concentration of the total n-aromatics and each trace aromatic as follows: Impurity, mg/kg * -CgWrjF- _x 106 there: = total area of the non-aromatic hydrocarbon peaks or the area of a specific trace aromatic. W = weight of the n-butylbenzene internal standard added to the sample, g, F = factor to relate weight response, see Table 2, S' = weight of sample prior to adding internal standard, g, and A = peak area of the internal standard. Report to the nearest 0.01 weight units. - 13.2.2 Calculate the volume concentration of the total non-aromatics and each trace aromatic as follows: Impurity, mL/kL = CWFD SAE X 106 where: C = total area of the non-aromatic hydrocarbon peaks or the area of a specific trace aromatic, W = weight of the n-butylbenzene internal standard added to the. sample, g, F = factor to relate weight response, see Table 2, S = weight of sample prior to adding internal standard, g, A = peak area of the internal standard. If. I i; BTX Impurities Benzene: Non-aromatlcs Toluene Toluene: NA As Ag Xylene: NA Afl I' A7 Ag+ TABLE 3 Summary of Data (ASTM D16.0A.18 BTX impurities) Average Between Days Wlthin-Laboratories Degrees of Freedom Range, max Single Result Any.Laboratory Degrees of Freedom S,, + b Range, max. 447 82 536 128 35 431 81 3519 1857 6 22 65 76 18 8 46 6 19 3 160 65 6 54 5 13 6 430 6 155 185 47 1489 536 5 51 186 5 32 118 5 82 298 5 33 119 2 5 128 464 4 24 94 5 727 2646 5 1621 5900 637 DUP050296199 # D 2360 D - density of impurity (non-aromatics typically have a density of 0.68 g/cm3, and E = density of sample. Report to the nearest 0.01 volume units. 14. Report 14.1 Report the following information: 14.1.1 Total non-aromatics. 14.1.2 Each trace aromatic present in weight or volume units. 14.1.3 Purity of Sample--May be reported as 100.00 minus the impurities detected by this test method. Purity can also be obtained by a freeze point or solidification point determination. 15. Precision 15.1 The following criteria should be used to judge the ^ acceptability (95 % probability level) of results obtained by ? this test method. The criteria were derived from a round ] robin among six laboratories. The data were run on 2 days. 15.1.1 Repeatability--Results in the same laboratory- j should not be considered suspect, unless they differ by more 1 than the amount shown in Table 3. 15.1.2 Reproducibility--The results obtained by each of two laboratories should not be considered suspect, unless they differ by more than the amount shown in Table 3. 15.1.3 Bias--An interlaboratory test program is being conducted for the purpose of establishing bias values. The American Society for Testing anti Materials 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 oI the validlty of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at anytime by the responsible technical committee and must bereviewed every five years and ifnotrevised, eitherreapproved or withdrawn. Your comments are Invited eitherfor revision ofthis standard dr for additional standards and should be addressed to ASTM Headquarters. Your comments will receive carefill 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 ehould make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1? -v 638 DUP050296200 Designation: D 2403 - 91 Standard Specification for Refined Phthalic Anhydride-13081 This standard is issued under the fixed designation D 2403; 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. cope ta Sheets regarding all material used in this specification. Referenced Documents .1 ASTM Standards: 1493 Test Method for Solidification Point of Industrial Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobalt Scale)2 3438 Practice for Sampling and Handling Naphthalene, AMAa.l1e!ic. AAn_.ht__y__d1ridJe__,__a___n__dlnPLh,tlh__a_Clic. A n-1h__y__d_PripdaeM2 i/w ft W This specification is under the jurisdiction of ASTM Committee D-16 on lie Hydrocarbons and Related Chemicals and is the direct responsibility of mmittee DI6.0C on Oxygenated Aromatics. Trent edition approved Oct. 15,1991. Published December 1991. Originally 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12003 3. Properties 3.1 Phthalic anhydride shall conform to the following requirements: Property Solidification point, min, 'C Molten color, max Molten color alter heating, max Specification 130.8 30 100 Method D1493 D3366 D 3366 ,,. 4` *amPl,n8 4.1 The material shall be sampled in accordance with 5. Keywords 5.1 phthalic anhydride; solidification point; color 3Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. TheAmerican Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement 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. Yourcomments are invitedeitherfor 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 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. . . 639 DUP050296201 Designation: D 2439 - 91 Standard Specification for Refined Phenol1 This standard is issued under the fixed designation D 2439; 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 indicatesthe year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers refined phenol. 1.2 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials listed,in this specification, . 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 me. 2. Referenced Documents 2.1 ASTM Standards: D1493 Test Method for Solidification Point of Industrial Organic Chemicals2 D1631 Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method2 D1686 Test Method for Color of Solid Aromatic Hydro carbons and Related Materials in the Molten State (Platinum-Cobalt Scale)2 D3852 Practice for Sampling and Handling Phenol and Cresylic Acid2 . 2.2 Other Document: . 1 This specification is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved May 15, 1991. Published July 1991. Originally published as D 2439 - 65 T. Last previous edition D 2439 - 86. - Annua! Book ofASTM Standards, Vol 06.03. OSHA Regulations, 29 CFR, paragraphs 1910.1000 an 1910.12003 3. Properties 3.1 Refined phenol shall conform to the following.,! quirements when sampled and tested as described: Property Water content, max, weight % Solidification point, (as is), min, "C Appearance Molten color Specification 0.10 40.6 ASTM Test method D1631 D1493 A Molten liquid or crystalline solid, free of sediment and haze. * See Note 1. No t e 1--Refined phenol 'as produced is essentially colorless, pending upon both the nature and duration of subsequent handling^ may discolor. Therefore, a rigid specification for color is impractical an| for many uses it may be unnecessary. In those cases where such i specification is required, its magnitude will vary widely with t$i intended usage. The required value may be1 measured using Test Methoi D 1686. It is further recommended that the directives of Practice D 385| be strictly followed in any case where color is.important. 4. Sampling 4.1 The material shall be sampled and the propertia enumerated in this specification shall be determined in accordance with the following ASTM methods: 4;i.l'The specimens shall be placed only in a clean and dry glass container sealed with a screw cap fitted with; polyethylene liner. Rubber, cork, or coated paper closures oil liners shall not be used. ..Special care shall be taken to avoid contact with iron, dirt or moisture. Sampling shall be carried dut in accordance with Practice D 3852. 3 Available from Superintendent of Documents, U.S. Government Printing.| Office, Washington, DC 20402. The American Society for Testing and Materials takes no position respecting the validity of any patentrights asserted in connection with any tern mentioned in this standard. Users ot this standard are expressly advised that determination of the validity of any such patent rights, and the risk ot Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, 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 at 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 SL, Philadelphia, PA 19103. 640 DUP050296202 Designation: D 2827 - 881 Standard Specification for Styrene Monomer 9961* This standard is issued under the fixed designation D 2827; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A numbef in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. " No t e--Paragraphs 4.1.6 and 4.1.7 .were editorially corrected in September 1988. `ope 1 This specification covers a grade of styrene monomer Jified as "Styrene Monomer 996." 2 Consult current OSHA regulations and supplier's erial Safety Data Sheets for all materials used in this 'fication. eferenced Documents J ASTM Standards: 1016 Test Method for Purity of Hydrocarbons from freezing Points2 1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)3 2119 Test Method for Aldehydes in Styrene Monomer3 2120 Test Method for Inhibitor, p-tert-Butylcatechol, in Styrene Monomer3 ,2121 Test Methods for Polymer Content of Styrene Monomer3 340 Test Method for Peroxides in Styrene Monomer3 3437 Practice for Sampling and Handling Liquid Cyclic oducts3 2799 Test Method for Purity of Styrene by Freezing Point Method3 j3962 Test Method for Analysis of Styrene by Gas Chromatography3 590 Test Method for Colorimetric Determination of : specification is under the jurisdiction of ASTM Committee DrI6 on "'c Hydrocarbons and Related Chemicals and is the direct responsibility of mittee D16.0H on Styrene, Ethylbenzene, Cumene, and Naphthalene. -nt edition approved April 29, 1988. Published June 1988. Originally I as D 2827 - 69 T. Last previous edition D 2827 - 82. nual Book ofASTM Standards, Sate 05.01 and 06.03. uat Book ofASTM Standards, Vol 06.03. p-/ert-Butylcatechol in Styrene Monomer by Addition of Alcoholic NaOH3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Properties 3.1 Styrene monomer 996 shall conform to the following requirements when tested as described in Section 4. Purity Color Aldehydes .Peroxides, Polymer Inhibitor 99.6 % min (by weight) 10 max (Pt-Co scale) 0.02 % max as benzaldehyde J00 mg/kg max as H202 ' 10 mg/kg max 10 to 20 mg/kg (or as required) No t e 1--In the case of Styrene Monomer 996, note that weight percent purity ofthis specification is equivalent to mol percent purity as determined by Test Method D 1016. 4. Test Methods 4.1 The material shall be sampled and the properties enumerated shall be determined according to the following ASTM test methods: 4.1.1 Sampling--Practice D 3437. 4.1.2 Purity--Test Method D 3799. 4.1.3 Color--Test Method D 1209. 4.1.4 Aldehydes--Test Method D 2119. 4.1.5 Peroxides--'Test Method D 2340. 4.1.6 Polymer--Test Methods D 2121; Method A. 4.1.7 Inhibitor--Test Methods D 2120'or D 4590. ' 4.1.8 Impurities--The most common impurities can be determined by Method D 3962. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 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 of the validity of any such patent rights, and the risk of infringement of such rights; are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments 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. 641 DUP050296203 91< ) Designation: D 2870 - 86 (Reapproved 1990) Standard Test Method for Gel Time of Tar Acids1 This standard is issued under the fixed designation !) 2870; the number immediately following the designation indicates, the year of original adoption.or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers determination of the gel time of tar acids in the range from 8 to . 120 ,min. 1.2 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D2194 Test Method for Concentration of Formaldehyde : Solutions2 B3852 Practice for Sampling and Handling Phenol and Cresylic Acids2 E 1 Specification for ASTM Thermometers3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs , 1910.1000 and 1910.12004 3. Definitions 3*1 gel time--the time required for the polymerization reaction to proceed to a point where the viscous drag on a rotating spindle, partially immersed in the reaction mass, is sufficient to overcome the torsional force exerted on the spindle by a constant speed drive assembly, magnetically coupled to the spindle by a standard torsion spring. 3.2 tar acid--phenol or its homologues either individually or blended together,. 4. Summary of Test Method 4.1 Observing specific conditions, an aliquot of the wellmixed specimen is blended with powdered paraformal dehyde and triethanolamine catalyst and the gel time deter mined using an automatic gel time test meter. 5. Significance and Use 5.1 The gel time value is a measure of the reactivity of tar acids. As a quality control procedure it is one of the techniques employed to determine batch to batch unifor mity. The gel time test also serves as a means for studying thi effects of reaction variables such as composition, tempera! ture and concentration. 6. Apparatus 6.1 Automatic gel time meter and accessories5 Consisting! of (Fig. 1): 6.1.1 Constant-Temperature Bath. 6.1.2 Bath Cover Plate with center opening to accommo-J date a one-hole neoprene rubber stopper and test tube and| with condensing coil and immersion heater attached. 6.1.3 Glass Spindle, 165 by 6 mm equipped with a| magnetic coupling assembly. 6.1.4 Torsion Spring, 44.5 by 0.25-mm piano wire. 6.1.5 Lower Torsion Spring Vise with magnetic assembly.! 6.1.6 Upper Torsion Spring Vise with upper contact] assembly. 6.1.7 Lower Contact. 6.1.8 Feeler Gage, 28.067 by 2.25 mm,(1.105 by Vzi in.).] 6.1.9 Test Tube, 18 by 150 mm, borosilicate glass. 6.1.10 Variable Transformers 6.1.11 Ring Stand. 6.1.12 Thermometer--An ASTM Partial Immersion| Thermometer, having a range from 90, to 170"C and con-1 forming to the requirements for Thermometer 35C as] prescribed in Specification E 1. 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-f 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 j lessening the accuracy of the determination. 7.2 Paraformaldehyde: 7.2.1 The paraformaldehyde used for this test shall be a 3 free-flowing powder, free of lumps, passing through a 100- j mesh screen. 7.2.2 The formaldehyde content shall be 93 1 % determined by assay, according to the procedure outlined in j Test Method D 2194, with the following exceptions: 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved Oct. 31, 1986. Published December 1986. Originally published as D 2870 - 70 T. Last previous edition D2870 - 82. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 14.03. 4 Available from Superintendent of Documents, U. S. Government Printing Office, Washington, DC 20402. 5 Gel time meter available from Sunshine Scientific Instrument, Inc.,lStC| Grant Ave, Philadelphia, PA 19! 15, or its equivalent has been found satisfactory | for tiiis purpose. 6 "Reagent Chemicals, American Chemical Society Specifications,'1 Am. CheiD' | ical Soc., Washington, DC. For suggestions on the testing of reagents not lisl the American Chemical Society, see "Reagent Chemicals and Standards," bpj Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United Pharmacopeia." 642 DUP050296204 B6 0.25 C 89 to 95 3V2 to 3% 0 25 to 38 1 to 1% FIG. 1 Heating Bath Assembly for Gel Time Test : 7.2.2.1 The specimen shall be weighed on an aluminum ighing pan and quantitatively transferred to the jlenmeyer flask using 100 mL of sodium sulfite solution. 1.2.2.2 Gently swirl the flask, mechanically or manually, dissolve the sample in no more than 10 min total elapsed `e. No t e 1--A low result will be obtained if the sample is allowed to d in contact with the reagent for more than 10 min. 7.2.2.3 Titrate the sample as outlined in the Procedure tion of Test Method D 2194. 7.3 Triethanolamine, melting point 21 1C. Hazards 8.1 Consult current OSHA regulations and supplier's aterial Safety Data Sheets for all materials used in this test ethod. ' 8.2 Avoid ail contact of tar acids with the eyes and skin, ar acids act locally as corrosives to body tissue and may be Ksorbed through broken or unbroken skin. Preparation of Apparatus 9.1 Assemble the apparatus in accordance with the manturer's instructions and, using a suitable bath medium such as glycerin, adjust and control the bath temperature to 125 0.25C. 10. Sample Preparation _ . . 10.1 Samples shall be taken in accordance with Practice D 3852. 10.2 Liquid samples must be thoroughly mixed to ensure uniformity. 10.3 Solid samples must be gently heated to a temperature approximately 10C above the melting point and thoroughly mixed. 11. Procedure 11.1 During a total time interval not to exceed 10 tnin; weigh the following ingredients into a previously tared 18 by 150-mm test tube: Tar acid sample, g Paraformaldehyde, g Triethanolamine, g 7.000 0.050 2.000 0.025 1.500 0.010 11.2 Manually mix the contents of the test tube for 1.0 0.25 min, using the glass rod spindle. 11.3 Insert the test tube into the constant-temperature bath using the one-hole rubber stopper for proper alignment and immediately activ&t.she timing and drive mechanism of 643 DUP050296205 D 2870 the test meter by turning the power switch to the ON | position. 11.4 Connect the spindle to the drive assembly by means ofthe magnetic coupling and realign the test tube so that the spindle rotates in the center of the sample and the bottom of the spindle is within 6 mm (`A in.) from the bottom of the test tube. 11.5 Adjust the gap between the contacts to 2.25 mm (3/32 yin.) using the feeler gage. i 11.6 Turn the test circuit switch to the ON position. No t e 2--Once the test circuit is activated, the red pilot lamp will glow indicating that the automatic alarm has been energized. Other than ; ensuring that the bath temperature is maintained at 125 0.25C during j the remainder of the test no further attention is required. 11.7 When the gel point is reached, the timer and driv motor will stop automatically and an audible signal will bi emitted from the test meter. 11.8 Turn off both power and test switches, promptll remove the test tube from the bath, and clean the tesl spindle. 11.9 Record the gel time indicated by the test meter to thj nearest 0.1 min. 12. Report 12.1 Report the gel time value obtained in 11.9 to the nearest 0.1 min. 13. Precision and Bias 13.1 A precision and bias statement cannot be made! because these parameters are not meaningful for this test! method. The American Society for Testing ana 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 il ifnot revised, eitherreapproved or withdrawn. Your comments are invited either forrevision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, 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. 644 DUP050296206 Designation: D 2930 - 80 (Reapproved 1989)e1 Standard Test Method for Maleic Acid in Maleic Anhydride by Potentiometric Titration1 This, standard is issued under the fixed designation D 2930; 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. et NoTE-^Editorial changes were made throughout in April 1969. i Scope 1.1 This test method covers the determination of free ileic acid in refined maleic anhydride by potentiometric ation. [1.2 This test method is applicable for all concentrations of aleic acid; however, it is primarily used for concentrations flow 0.5 %. '' 83* This standard may involve hazardous materials, Oper- bns, arid equipment. This standard does not purport to fdress all ofthe safetyproblems associatedwth its use. It is ' responsibility of the user of this- standard to establish fpropriate safety and health practices arid determine the blicability of regulatory limitations prior to use. For cific hazard statements, see Section 7. i ; Referenced Documents : ASTM Standards: ` 11193 Specification for Reagent Water2 |p3438 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride3 Other Document's; l OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200.4 Summary of Test Method 13.1 This tesf method is based on a direct titration of ileic acid using a tertiary amine as the base: The titration is ried out in an anhydrous solvent system and followed !>tentiometrically by means of a pH meter. Tertiary amines > not react with anhydrides. Only one carboxylic acid group 1 titrated. ' Significance and Use 14.1 The maleic add content is usually an indication of oosure to moisture in air. Maleic anhydride reacts with ioisture to form maleic add. Apparatus 15.1 Titrimeter or pH meter, equipped with glass and jj1 This test method is under the jurisdiction of ASTM Committee D-J6 on <omatic Hydrocarbons and Related Chemicals and is the direct responsibility of ^committee Dlfi.OC on Oxygenated Aromatics. fCurrent edition approved Oct. 31, 1980. Published December 1980. Originally blished as D 2930-70. Last previous edition D 2930-70 (1975). 12 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vo) 06.03. I* Available from Superintendent of Documents, U.S. Government Printing Bee, Washington, DC 20402. calomel electrodes. The pair of electrodes shall be mounted to extend well below the liquid level. 5.2 Microburet, 5 or 10-mL size, graduated 20 divisions/mL,. 5.3 Stirrer, mechanical, that will furnish a rapid stirring action, but not such vigorous stirring that air bubbles will be drawn to the electrodes of the titrimeter or pH meter. 5.4 Beaker, 250-mL, tail-form. 5.5 Automatic Titrator can be used in place of the above apparatus. 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.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficientiy 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 IV of Specification D 1193. 6.3 Acetone, dried over Linde Type 5A molecular sieves.6 7 8 6.4 N-ethylpiperidine7 (0.05 N in acetone)--Dissolve 5.65 g.of JV-efhylpiperidine in acetone and dilute to 1 L. Prepare fresh daily. 6.5 Maleic Acids--Titrate with aqueous NaOH solution (0.5 IV) to a phenolphthalein end point to obtain assay. 7. Hazards 7.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 7.2 In addition to other precautions, handling of maleic anhydride shall be done with care. Although it is a solid at ambient temperatures, its vapor pressure is high enough to cause objectionable fumes. The fumes and dust from maleic 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." 6 Manufactured by Union Carbide Corp., Linde Div., 270 Park Ave., New York, NY 10017. 7 Methylpiperidine, Catalog No. EX828, available from Matheson Coleman & Bell, East Rutherford, NJ, has been found satisfactory for this purpose. 8 Maleic acid. Catalog No. 690, available from Fisher Scientific Co., Springfield, NJ 07081, has be*n found satisfacro' ^ this purpose. 645 '9; DUP050296207 # D 2930 anhydride are local irritants to skin and mucous membranes especially in the presence of moisture. 8. Sampling 8.1 Sample in accordance with Practice D 3438. 9. Standardization of /V-Ethylpiperidine Solution 9.1 Standardize the amine solution by titration with maleic acid. Calculate the normality E as follows: E = (G x P)(M x 11.6) where: G = maleic acid, g, M = iV-ethylpiperidine, mL, and P = purity of maleic acid as obtained in 6.5, %. No t e 1 --Only one carboxyl group titrates. The dissociation constant forthe first hydrogen is approximately 10S2. The second hydrogen is too weak to titrate. ID. Procedure 10.1 It is desirable to take enough sample so that the solution contains approximately 0.002 mole of maleic acid. If the acid content is suspected to be lower than 0.5 %, use a 10-g specimen. (Precaution--See 7.2.) 10.2 Dissolve,the specimen in 100 mL of dry acetone. 10.3 Set the beaker in place, insert the glass and calomel electrodes, start the stirrer, and commence the titration with the 0.05 N, jV-ethylpiperidine solution. Conduct the titration in the manner of the usual potentiometric titration, taking readings of pH versus millilitres of titrant. The end point may be ascertained in the conventional manner as follows: Add the titrant in 0.01-mL increments. Allow the pH to reach stability and plot the pH readings against the millilitres of titrant used. The equivalence point is then taken as the end point. 11. Calculation 11.1 Calculate the percent maleic acid A as follows: /( = (Af x IV x 0.116 x 100>/5' where: M = N-ethylpiperidine, mL, N = normality of JV-ethylpiperidine, and S - sample used, g. 12. Report 12.1 Report the percent maleic acid to the nearest 0.001 %. 13. Precision and Bias 13.1 The following criteria should be used for judging the acceptability of the results. 13.1.1 Repeatability--Toe standard deviation of single results, obtained by the same analyst on different days, has been estimated to be 6.004 % absolute at 28 df. Two such values could be considered suspect (95 % confidence level) if j they differ by more than 0.012. % absolute. 13.1.2 Reproducibility--The standard deviation of single results, obtained by analysts in different laboratories, has been estimated to be 0.015 % absolute at 16 df. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.048 % absolute. No t e 2--These precision statements were developed at maleic acid concentrations between 0 and 0.5 %. The American Society for Testing andMaterials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of Oils standardare expressly advised that determination of the validity ol any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision atany time by the responsible technical committee and must be reviewed every five years and It not revised, either reapproved or withdrawn. Your comments arc Invited either forrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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. 646 DUP050296208 Designation: D 2935 - 91 Standard Test Method for Apparent Density of Industrial Aromatic Hydrocarbons1 This standard is issued under the fixed designation D 2935: 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 lest method has been approvedfor use by agencies ofthe Department ofDefense. Consuit the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. "cope . 1 This test method covers the measurement of apparent sity in pounds in air per U.S. gallon at convenient peratures using a hydrometer, and reporting at any rifled atmospheric temperature. 1.2 This standard does not purport to address the safety blems, if any, associated with its use. It is the responsiiy of the user of this standard to consult and establish ropriate safety and health practices and determine the licability of regulatory limitations prior to use. Specific d statements are given in Section 7 and Note 3. ; Referenced Documents 1 ASTM Standards: 3437 Practice for Sampling and Handling Cyclic Products2 p I Specification for ASTM Thermometers3 rE 12 Definitions of Terms Relating to Density and Spe cific Gravity of Solids, Liquids, and Gases4 E 100 Specification for ASTM Hydrometers3 .2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12005 Terminology 3.1 Definition: 3.1.1 apparent density at 60F --the weight in air ofa unit lume of sample at 60F; in this test method, the weight is pounds, and the volume in U.S. liquid gallons. Average air this test method is assumed to have a density of 0.0012 cm3, 'No t e I--This definition is not in conflict with that given in the ' rrent version of Definitions E 12. , Summary of Test Method '4.1 A hydrometer reading is made at any convenient mperature. The difference between hydrometer reading d a tabulated value at test temperature is applied to tabular This test method is under the jurisdiction of ASTM Committee D-16 on romatic Hydrocarbons and Related Chemicals and is the direct responsibility of ubcommittee DI6.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their erivatives. Current edition approved May 15, 1991. Published July 1991. Originally Wished as D 2935 - 72. Last previous edition D 2935 - 90. * Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vols 05.03 and 14.03. 4 Annual Book ofASTM Standards, Vols 04.02 and 15.05. 1 Superintendent of Documents, U.S. Government Printing Office, ashington, DC 20402. values at any other temperature to get the apparent density at this other temperature. 4.2 The precision of this test method is such that the determination should be made in duplicate (11.1) in case of dispute or for referee purposes. In other cases single determi nations may suffice. 5. Significance and Use 5.1 This test method is intended for measurements on high-purity benzene, toluene, styrene, o~, m-, p-xylene, mixed xylenes, and cyclohexane. It can be extended for use on any material for which a precise density-temperature relationship is known. It has been tested for precision between 55 and 100'F. 5.2 This test method is not intended for use in setting specifications on industrial aromatic hydrocarbons. It may also be used as an internal quality control tool and in development or research work. 6. Apparatus 6.1 Hydrometer, ASTM pounds per gallon, having a range consistent with the density of the material being tested. The hydrometer shall conform to the requirements prescribed in Specification E 100. Table 1 shows the ranges of several hydrometers suitable for testing the industrial aromatic hydrocarbons within the scope of this method. 6.2 Thermometer, graduated in 0.1Fin the range from 54 to 101F and--conforming to the requirements for Gas Calorimeter Inlet Thermometer 50F described in Specifica tion El. 6.3 Cylinder, made of clear glass or plastic. For conven ience in pouring, the cylinder may have a lip on the rim. Use a cylinder having an inside diameter 25 mm greater than the diameter of the hydrometer and a height to provide a clearance of 25 mm between the lower end of the hydrom eter and the inside bottom of the cylinder. 6.4 Bath, for maintaining the contents of the hydrometer cylinder constant to 0.05F at any convenient temperature during the test. TABLE 1 Suitable Hydrometers for Testing Industrial Aromatic Hydrocarbons ASTM Number Normal Range, Ib/gal 294H-68T 295H-88T 296H-68T 297H68T 6.24 to 6.68 6.86 to 7.08 7.08 to 7.50 7.50 to 7.91 647 4 ..I ~m DUP050296209 # D 2935 7. Hazards 7.1 Consult the latest OSHA regulations and supplier's Material Safety Data Sheets regarding all materials used in this test method. 8. Sampling 8.1 Refer to Practice D3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this test i method. 9. Procedure 9.1 Bring the sample, cylinder, thermometer, and bath to the same temperature, preferably ambient. Pour the sample into the clean cylinder avoiding formation of air bubbles. Remove any air bubbles formed, after they have collected on the surface of the sample by touching them with a piece of clean filter paper. 9.2 Place the cylinder containing the sample in a vertical position in a location free of air currents, preferably in the water bath. Take precautions to prevent the temperature of the sample from changing appreciably during the time necessary to complete the test. Measure the temperature and leave the thermometer in the liquid. 9.3 Lower the hydrometer gently into the sample and, when it has settled, depress it about two scale divisions into the; liquid and then release; keep the rest of the stem dry, as unnecessary liquid on the stem changes the effective weight of'the instrument, and so affects the reading obtained. A slight spin imparted to the instrument on releasing will assist in bringing it to rest, floating freely away from the walls of the hydrometer cylinder. Allow sufficient time for the hydrometer to become completely stationary and for all air bubbles to come to the surface. Again measure the tempera ture of the liquid. 9.4 When the hydrometer has come to rest, floating freely, and the temperature of the sample is constant to O.PF, read tise hydrometer to the nearest Vs scale division (Note 2). The Correct reading is that point on the hydrometer scale at Whieh the surface of the liquid cuts the scale. Determine this point by placing the eye slightly below the level of the liquid t^l;sowly raising it until the surface, first seen as a distorted dspse; appears to become a straight line cutting the hydrometerscale. No t e 2--One fifth of a scale division is equal to 0.001 Ib/gal. S 3: Precaution--Avoiding breathing fumes of the sample, as aromatic hydrocarbons, particularly benzene, are toxic and pjjus when inhaled in large quantities. 915} Observe the temperature immediately before and after dbseration of the indicated density, the liquid in the cylin ler being thoroughly stirred with the thermometer, the whole mercury thread being immersed. Keep the thermom eter in the sample at all times. Should the two temperature readings differ by more than 0.1F repeat the temperature and density observations when the temperature of the sample has become more stable. 9.6 Record the mean of the thermometer reading before and after the final hydrometer reading, to the nearest O.TFas the temperature of the test. Record the hydrometer reading to nearest 0.001 lb/gal. This will require interpolation of the hydrometer subdivisions. 10. Calculation 10.1 Enter Table 2 with the temperature of the test. If the observed hydrometer reading at this temperature is greater than the table value, add the difference to the table value at 60F to get the apparent density at 60F. If the observed reading is less than the table value, subtract the difference from the table value at 60F to get apparent density at 60F. 10.2 If the temperature of the bulk ofthe material storage tank or drum is at some temperature other than 60F, the same difference observed at the test temperature may be applied to the table value at the mean bulk liquid tempera ture to obtain the. apparent density value for calculating the weight in air of the bulk material from its measured volume. 11. Report 11.1 Report the density to the nearest 0.001 lb/gal. Duplicate measurements that agree within 0.011 lb/gal are acceptable for averaging (95 % confidence level). 12. Precision 12.1 The following criteria should be used forjudging the acceptability of results: 12.1.1 Repeatability {Single Analyst)--The standard devi ation of single results obtained by the same analyst on different days has been estimated to be 0.0042 Ib/gal at 38 degrees of freedom. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.012. When duplicate determinations are made by the same analyst on each of different days, the standard deviation of results (each the average of duplicates) has been estimated to be 0.0016 Ib/gal at 38 degrees of freedom, and two such values should be considered suspect (95 % confidence level) if they differ by more than 0.0046. 12.1.2 Reproducibility {Multilaboratory)--The_standard deviation of single results obtained by analysts in different laboratories has been estimated to be 0.0091 Ib/gal at 7 degrees of freedom. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.030. When duplicate determinations are made by each laboratory, the standard deviation of results (each the av erage ofduplicates) has been estimated to be 0.0082 lb/gal at 7 degrees of freedom, and two such values should be considered suspect (95 % confidence level) if they differ by more than 0.0275. 13. Keywords 13.1 apparent density; industrial aromatic hydrocarbons; hydrometer; temperature correction 648 DUP050296210 D 2935 flflSFemoeFratur' a, ' W -5 K -4 I -3 f -2 | -1 TABLE 2 Apparent Density versus Temperature for Varying Industrial Aromatic Hydrocarbons Observed Pounds in Air per U.S. Gallon at TF4 Benzene Toluene Ethyl Benzene o-Xytene m-Xylene p-Xytene Mixed Xylenes Styrene 7.532 7.527 7.523 7.519 7.515 7.512 7.509 7.505 7501 7.497 7.612 7.608 7.604 7.600 7.596 7.478 7.474 7.471 7.467 7.463 7.478 7.474 7.471 7.467 7.463 |: o Hi i 2 | - 3 B >4 7.511 7.505 7.502 7.498 7.494 7.493 7.489 7.485 7.482 7.478 7.593 7.589 7.585 7.581 7:578 7.460 7.456 7.452 7.449 7.445 7.460 7.456 7.452 7.449 7.445 Eg & B6 if 7 8 9 Wm m 10 if 11 12 B 13 u 7.490 7.486 7.481 7.477 7.473 7.469 7.465 7.460 7.456 7.452 7.474 7.470 7.466 7.462 7.458 7.455 7.451 7.447 7.443 7.439 7.574 7.570 7.566 7.563 7.559 7.555 7.551 7.548 7.644 7.540 7/441 7.437 7.434 7:430 7.426 7.423 7.419 7.416 7.411 7.408 7.441 7.437 7.434 7.430 7.426 7.423 7.419 7.415 7.411 7.408 15 m 16 Sr 17 VK: 1198 7.448 7.444 7.440 7.435 7.431 7.435 7.431 7.427 7.424 7.420 7.536 7.533 7.529 7.525 7.521 7.404 7.400 7.397 7.393 7.389 7.404 7.400 7.397 7.393 7.389 7.765 7.761 7.757 7.753 7.749 B 20 j 21 K 22 K .23 || 24. 7.427 7.423 7.419 7.414 7.410 7.416 7.412 7.408 7.404 7.400 7.517 7.514 7.510 7.506 7.502 7,385 7.382 7.378 7.374 7.370 7.385 7.382 7.378 7:374 7.370 7.745 7.741 7.737 7.733 7.729 |. 25 1 26 1 27 1 28 29 B 30 R 31 . 32 1: 33 |. 34 1 35 B1 86 I' 37 1 38 1 39 1 40 I 41 I 42 1 43 if 44 7.460 7.455 7:450 7.446 7.441 7.406 7.402 7.398 7.394 7.389 7.385 7.381 7.377 7.373 7.368 7.364 7.360 7.356 7.352 7.348 7.343 - 7.339 7.335 7.331 7.327 7:396 7.392 7.389 7.385 7.381 7.377 7.373 7.369 7.365 7.361 7:357 7.353 7,349 7,346 7.342 7.338 7.334 7.330 7,326 7.322 7.499 7.495 7.491 7.487 7.484 7.480 7.446 7.472 7.469 7.465 7.461 7.457 7.453 7.450 7.446 7.442 7.438 7.435 7.431 7.427 7.367 7.363 7.359 7.356 7.352 7.348 7.344 7.341 7.337 7.333 7.329 7.325 7.322 7.318 7.314 7.310 7.307 7.303 7.299 7.295 7.367 7.363 7.359 7.356 7.352 7.348 7.344 7.341 7.337 7.333 7.329 7.325 7.322 7.318 7.314 7.310 7.307 7.303 7.299 7.295 7.725 7.721 7.717 7.713 7.709 7.705 7.702 7.698 7.694 7.690 -- 7.686 7.682 7.678 7.674 7.670 7.666 7.662 7.65B 7.654 7.650 1 45 1 46' 1 47 1 48 1 49 ! 50 1 61 I 52 1 53 I 54 7.436 7.431 7:427 7.422 7.417 7.413 7.408 7.403 7.399 7.394 7.322 7.318 7.314 7.310 7.306 7.302 7.279 7.293 7.289 7.285 7.318 7.314 7.310 7.306 7.302 7.298 7.294 7.291 7.287 7.283 7.423 7.420 7.416 7.412 7.408 7.404 7.401 7.397 7.393 7.389 7.291 7.288 7.284 7.280 7.276 7.273 7.269 7.265 7.261 7.257 7:291 7.288 7284 7.280 7.276 7.273 7.269 7.265 7.261 7.257 7646 7.642 7.638 7.634 7.630 7.626 7.622 7.618 7.614 7.610 Cyclohexane i - 6.605 6.601 6.596 6.592 6.588 6.584 6.580 6.576 6.572 ~ 6.568 6.564 6.559 6.555 6.551 6.547 649 DUP050296211 (P 3 s i * F 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 8B 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108 109 110 111 112 113 114 Benzene 7.389 7.384 7.380 7.375 7.370 7.365 7.361 7.356 7.351 7.346 7.342 7.337 7.332 7.327 7.323 7.313 7.313 7.308 7.304 7.299 7.294 7.289 7.284 7.280 7.275 7.270 7.265 7.260 7.255 7.251 7.246 7.241 7;236 7.231 7.226 7.222 7.217 7.212 7.207 7.202 7.197 7.192 7.187 7.183 7.178 7.173 7.168 7.163 7.158 7.153 7.148 7.143 7.138 7.134 7.129 7.124 7.119 7.114 7.109 7.104 D 2935 Toluene 7.281 7.276 7.272 7.26B 7.264 TABLE 2 Continued Observed Pounds In Air per U.S. Gallon at 1FA Ethyl Benzene 7.279 7.275 7.271 7.267 7.263 o-Xylene 7.386 7.382 7.378 7.374 7.370 m-Xylene 7.254 7.250 7.246 7.242 7.238 p-Xyieiie 7.229 7.225 7.221 7.217 7.213 Mixed Xylenes 7.254 7.250 7.246 7.242 7.328 7J260 7.258 7.251 7.247 7.243 7.259 7.255 7.251 7.247 7.243 7.367 7.363 7.359 7.355 7-352 7.234 7.231 7.227 7.223 7.219 7.209 7.205 7.201 7.198 7.194 7.234 7.231 7.227 7.223 7.219 7.239 7.235 7.230 7.226 7.222 7.239 7.235 7.231 7.227 7.223 7.348 7.344 7.340 7.336 7.333 7.215 7.212 7.208 7.204 7.200 7.190 7.186 7.182 7.178 7.174 7.215 7.212 7208 7204 7.200 7.218 7.214 7.210 7.205 7.201 7.219 7.215 7.211 7.207 7.203 7.329 7.325 7.321 7.318 7.314 7.198 7.192 7.189 7.185 7.181 7.170 7.166 7.162 7158 7.155 7.196 7.192 7.189 7.185 7.181 7.197 7.193 7.189 7.184 7.180 7.199 7.195 7.191 7.187 7.183 7.310 7.306 7.302 7.299 7.295 7.177 7.173 7.169 7.165 7.162 7.151 7.147 7.143 7.139 7.135 7.177 7.173 7.169 . 7.165 7.162 7.176 7.172 7.168 7.163 7.159 7.179 7.175 7.172 7.168 7.164 7.291 7.287 7.283 7.280 7:276 7.158 7.154 7.150 7.146 7.142 7:i3i 7.127 7.123 7.119 7.115 7.158 7.154 7.150 7:146 7.142 7.155 7.151 7.147 7.143 7.138 7.160 7.156 7.152 7.148 7.143 7.272 7.268 7.264 7.261 7.257 7.138 7.135 7.131 7.127 7:123 7.112 7.108 7104 7.100 7.096 7.138 7.136 7.t31 7.127 7.123 7.134 7.130 7.126 7.122 7.117 7-139 7.135 7.131 7.127 7.123 7.253 7.249 7.245 7.242 7.238 7.119 7.115 7.111 7.107 7.103 7.092 7.088 7.084 7.080 7.076 7.119 7.115 7.111 7.107 7.103 7.113 7.109 7.105 7.101 7.097 7.119 7.115 7.111 7.107 7.103 7.234 7.230 7.226 7.222 7.219 7.100 7.096 7.092 7.088 7.084 7.072 7.06 B 7.0647.060 7.057 7.100 7.096 7.092 7.088 7.084 7.093 7.088 7.084 7.080 7.076 * 7.099 7.095 7.091 7.087 7.083 7.215 7.211 7.207 7.203 7.200 7.080 7.076 7.072 7.068 7.064 7.053 7:049 7.045 7.041 7.037 74)80 7.076 7.072 7.068 7.064 7.071 7.067 7.063 7.059 7.055 7.079 7.075 7.071 7.067 7.063 7.198 7.192 7.188 7.184 7.180 7.061 7.057 7.053 7.049 7;045 7.033 7.029 7.025 7.021 7.017 7.061 7.057 7.053 7.049 7.045 7.050 7.046 7.042 7.038 7.034 7.069 7.055 7.051 7.047 7.043 7.177 7.173 7.169 7.165 7.161 7.041 7.037 7.033 7.029 7.025 7.013 7.009 7.005 7.001 6.997 7.041 7.037 7.033 7.029 7.025 Styrene 7.606 7.602 7.598 7.594 7.590 * Cyclohexane' 6543 6.539 6.534 6.530 6.526 '' 7.586 7.582 7.578 7.574 7.570 7.566 7.562 7.558 7.554 7.550 6.522 6.518 6.514 6.509 6.505 6.501 6.497 6.493 6.488 6.484 : m 1 ''M ..ill `11 7.546 7.542 7.538 7.534 7.530 6.480 6.476 6.471 6.467 6.463 7.528 7.522 7.518 7.514 7.510 6.459 6.454 6.450 6.446 6.442 1-i 7.506 7.502 7.498 7.494 7.490 6.437 6.433 6.429 6.425 6.420 Jj| 7.486 7.482 7.478 7.474 7.470 6.416 6.412 6.408 6.403 6.399 .-9 7.466 7.461 7.457 7.453 7.449 6.395 6.390 6.386 6.382 6.386 7.445 7.441 7.437 7.433 7.429 ~ ' 6.373 6.369 6.364 6.360 6.356 7.425 7.421 7.417 7.413 7.409 6.351 6.347 6.343 6.338 6.334 7.405 7.401 7.397 7.393 7.389 6,330 6.325 6.321 6.317 6.312 7.385 7.381 7.377 7.373 7.369 6.308 8.304 6.299 6.295 6.291 650 DUP050296212 D 2935 Itmerature, 1 *F I 115 1 116 1117 | 118 !' 119 1 120 f 121 Benzene 7.099 7.094 7.089 7.084 7.079 7.074 Toluene 7.030 7.025 7.021 7.017 7.013 7.009 TABLE 2 Continued Observed Pounds in Air per U.S. Gallon at TF* Ethyl Benzene c-Xyiene m-Xylene 'p-Xylene Mixed Xylenes 7.039 7.035 7.031 7.027 7.022 7.157 7.154 7.150 7.146 7.142 7.021 7.017 7.013 7.009 7.005 6.993 6.989 6.985 6.981 6.977 7.021 7.017 7.013 7.009 7.005 7.018 7.138 7.002 6.973 6.969 6.965 6.962 6.958 7.002 6.964 6.950 , 6.94'6 6.942 6.938 1,134 6.934 6.930 6,926 6.922 6.918. 6.914 6.910 6.906 6.902 6.898 6.894 6.890 6.886 6.882 6.878 6.874 6870 6666 6.862 6.858 ISO i These dala are not corrected for the expansion of the glass hydrometer with temperature. 6.854i Styrene 7.365 7361 7.357 7.353 7.349 7.345 Cyclohexane 6.286 6.232 6.278 6.273 6.269 6.264 TheAmerican Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the rlskot Infringement of such rights, are entirely their Own'respohslMy. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnotrevised, either reapprovedor withdrawn. Your comments are invitedeither for revision of this standard or for additional standards 1 and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1 65 L v. ... DUP050296213 Designation: D 3054 - 81 (Reapproved 1985) Standard Test Method for Purity and Benzene Content of Cyclohexane by Gas Chromatography1 This standard is issued under the fixed designation D 3054; 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 of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the benzene content and the purity of cyclohexane 995 by gas chromatography. 1.2 This test method is applicable up to 1000 mg/kg concentration of benzene and for purities of 98 % or higher of cyclohexane. 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 ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. For st, specific precautionary statement, see Section 7. 2. Referenced Documents 2.1 ASTM Standards: D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 E 260 Practice for Packed Column Gas Chromatography3 2.2 Other Document: OSHA Regulations--Consult current regulations on han dling materials referenced in this method.4 3. Summary of Method 3.1 A known amount of internal standard is added to the sample. A portion of the sample is chromatographed and the amounts of benzene and other impurities are calculated relative to the amount of internal standard added. The amount of all impurities, including benzene, is subtracted from 100.00 to establish the purity of the cyclohexane samples. The benzene content of the sample is also calcu lated separately. 4. Significance and Use 4.1 This test method is suitable for setting specifications on cyclohexane and for use as in internal quality control tool wh :re cyclohexane is either produced or used in a manufactur ng procedure. It may also be used in development or research work involving cyclohexane. ' This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0A on BTX, Cyclohexane, and Their Derivatives. Current edition approved July 31. 1981. Published September 1981. Originally published as D 3054 - 72. Last previous edition D 3054 - 77. 1 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 14.01. 4 Available from Occupational Safety and Health Review Commission, 1825 K. St., N. W,, Washington. DC 20006. 5. Apparatus 5.1 Gas Chromatograph--Any instrument with either a hydrogen flame ionization or thermal conductivity detector which in combination with the recorder is capable of i providing a minimum peak height response of 5 mm for 50 mg/kg benzene when using a maximum sample injection of 10 jiL. A proper sample injection splitter is required if capillary columns are used. 5.2 Chromatographic Column--The choice of column is based on resolution requirements. Any column may be used if it is capable of resolving all significant impurities compo nents from cyclohexane. The impurities, except for benzene, do not need to be individually resolved. Benzene and the internal standard must be individually resolved without interference from cyclohexane or any of the impurities. Potential impurities in cyclohexane-995 are listed in Table 1. The following columns or combinations of columns, and operating temperatures have been used satisfactorily by one or more laboratories: TABLE 1 __________ Impurities Known or Suggested to Be Present in Commercial Cyclohexane O4 (1)n-butane (2) isobutane . Cf (3)n-pentane. (4) isopentane (5)eydopentane Co (6) n-hexene (7) 2-methylpentane (8) 3-melhylpentane (9) methylcyclopentane (10) benzene (11) 2,2-dimethylbutane (12) 2,3-dimethylbutane C7 (13) 3,3-dlmethylpentane (14) 2,3-dimethylpentane (15) 1,1-dimethylcyctoperrtane (16) 1,t3-tiimethytcydopentane (17) 1,t2-dimethyicydopentane (18) 1.c2-dimethylcydopentane (19) 2,2-dimethylpentane (20) 2,4-dimethylpentane (21) 1,c3-dimethylcydopentane (22) ethylcyclopentane (23) methylcydohexane (24) 3-ethylpentane (25) 3-melhylhexane (26) 2-molhyihexane (27) n-heptane -- 652 jsmmb*. DUP050296214 # D 3054 .2.1 Carbowax 20M,5 25 %, on Chromosorb P6 i7n a 20-fit 0.25-in. (6-m by 6-mm) column programmed from 80 to C. .2.2 Bentone 34,1 5 %, plus 5 % H-decyl phthalate on omosorb Ws in a 20-ft by 0.25-in. (6-m by 6-mm) mn operated isothermally in the range 100 to 110C. .2.3 Capillary Column, 50 to 200-fit (15 to 62-m), coated squalane and programmed from approximately 35 to iC. .2.4 Capillary Column, 50-ft (15-m), coated with a 5-ring yphenyl ether and operated at 45'C. .3 Recorder--Kay recorder with a range of 2 mV or less, i a full-scale response of 1 s or less, and a chart speed of *o 60 in./h, (760 to 1520 mm/h). .4 Integrator--If an integrator is Used in conjunction the recorder, it should have the equivalent of at least ! counts/min. '.5 Microsyringe, capacity 50 pL, or micropipet or both, pacity 25 pL minimum. 5.6 Volumetric Flask, 100-mL capacity. Reagents and Materials 5.1 2,2-Dimethylbutane, 99.0 % minimum purity. 6.2 Alternate Internal Standard, if 2,2-dimethylbutane is t employed, 99.0 % minimum purity. 6.3 Helium. 6.4 Hydrogen and Air, if FID is employed. 6.5 Typical impurities present in commercial cyclohexane ` at least 99 % purity to be used for determining response tors where necessary, and to establish satisfactory column slution (see Table l). Precaution 7.1 Consult the latest OSHA regulations regarding all terials used in this procedure. Sampling : 8.1 Samples should be taken in accordance with Practice 3437. Procedure 9.1 Install the chromatographic column and establish ~ble instrument operation at the proper operating condins. The selected column and conditions must satisfy the olution requirements as stated in 9.2. Make reference to structions provided by the manufacturer of the chromatoaph, and to Practice E 260. * 9.2 Determine the sensitivity of the gas chromatographic 'stem by measuring the response of the addition ofapproxately 50 mg/kg benzene to "benzene-free" cyclohexane, or this test, "benzene-free" cyclohexane is cyclohexane of 9.5 weight % minimum purity containing a maximum of weight mg/kg benzene. Prepare an accurate blend of pproximately 50 mg/kg benzene in "benzene-free" cycloexane as follows: 9.2.1 Place 50 to 60 mL of "benzene-free" cyclohexane in 100-mL volumetric flask. Using a microsyringe or micropipet add exactly 5 pL of benzene to the cyclohexane, and thereafter, dilute to volume with additional cyclohexane. Based on a figure of 0.884 g/mL for the density of benzene and a figure of 0.780 g/mL for cyclohexane, 56 mg/kg of benzene will have been added. 9.2.2 Inject a proper size sample of the "benzene-free" cyclohexane base stock and the prepared benzene-cyclo hexane blend to ascertain that the sensitivity requirement of 5.1 is met. The exact size of injections depends upon the column and detector employed but should not exceed 10 pL. 9.3 Determine the chromatographic response of all major impurities relative to the intepial standard, by analyzing one or more standard blends prepared in H-nonane to contain known concentrations of the internal standard and each major impurity, in the range from 100 to 200 mg/kg. Minor impurities are considered to have a response equivalent to the internal standard. No t e--The internal standard used to determine relative response data and for the analysis of samples (see 9.5) must be a component not present in significant amounts as an impurity in the samples. 2,2Dimethylbutane was used in the cooperative work during the develop ment ofthis method and was not found, in significant quantities, in the samples tested. 9.4 Analyze each blend, using the chromatographic con ditions established in 9.1. The quantity of sample injected should be the same as used for evaluation of sensitivity requirements, 9.2. Measure the area of the individually resolved and recorded peaks and calculate the response factor F for each impurity relative to the internal standard as follows: P = (Wj/lT,) x (-42M,) where: Wj = weight of the impurity whose factor is being deter mined, W2 -- weight of internal standard used, A2 = area (or integrator reading) for the internal standard peak, and A, = area (or integrator reading) for the impurity. 9.4.1 Note that A2 and A, must be reduced to the same instrument attenuation if the instrument sensitivity was changed during the determination. 9.5 Place 50 to 60 mL of the cyclohexane sample to be analyzed into a TOO-mL volumetric flask. Accurately add, using a micropipet or microsyringe, 25 pL of internal standard to the flask and then fill the flask to the calibration mark with additional sample. Based on using 2,2-di methylbutane as the internal standard with a density of 0.649 g/mL and cyclohexane with a density of 0.780 g/mL, the concentration of the internal standard will be 0.021 weight %. Similar calculations must be made for any alter native internal standard that may be used. Mix the above, blend thoroughly, and analyze using the chromatographic conditions established in 9.2.1. 9.5.1 Measure the area of the internal standard peak and the areas of the impurities peaks including benzene. Correct all impurity peak areas by the response factors determined in accordance with 9.4. 5 Registered trademark of Union Carbide Corp. 6 Registered trademark of Johns-Manville Products Corp. 7 Registered trademark of NL Industries. 10. Calculation 10.1 Weight Percent Total Impurities: 653 DUP050296215 # D3054 Total impurities, % = (AJA2) x W _ total of the corrected areas or integrator readings for * all impurities peaks including benzene, A2 = area or integrator reading for the internal standard peak, and W = weight percent of internal standard. 10.2 Milligrams per Kilogram Benzene: Benzene, mg/kg = (Ai/A2) x W x 104 where: A3 = corrected area or integrator reading for the benzene peak. 10.3 Cyclohexane Purity (Weight Percent): Cyclohexane, % = 100.00 - percent total impurities 11. Report 11.1 Report the cyclohexane purity of the sample to the nearest 0.01 %. ,11.2 Report the amount of benzene in the sample to the nearest 1 mg/kg. 12. Precision 12.1 The following criteria should be used for acceptability of results (95 % confidence). 12.2 Cyclohexane Purity: 12.2.1 Repeatability--Duplicate results by the sam. 0j, ator should be considered suspect if they differ by more 0.01 %. ; 12.2.2 Reproducibility--The results submitted by each two laboratories should be considered suspect if they d; by more than 0.07 %. 12.3 Benzene: 12.3.1 Repeatability--Duplicate results by the same oi ator should be considered suspect ifthey differ by more the amounts shown for repeatability in Table 2. 12.3.2 Reproducibility--The results submitted by eac two laboratories should be considered suspect if they diner* by more than the amounts shown for reproducibility Table 2. TABLE 2 Precision Data for Benzene Determination Benzene Level, mg/kg 70 700 Repeatability, mg/kg 8 21 ReprodudbMty, mg/Wp" 26 139 The American Society lor Testing and Materials takas no position respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users at this standard are expressly advised that determination of the validity oi any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technics! committee and must be reviewed every live years and ifnot revised, eitherreapprovedor withdrawn. Yeur 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 feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 191S Race St., Philadelphia, PA 19103. 654 BiT' , fc, DUP050296216 Designation: D 3055 - 90 Standard Specification for Cyclohexane 9951 This standard is issued under the fixed designation D 3055; 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 (f) indicates an editorial change since the last revision or reapprovai. pe This specification covers a grade of cyclohexane Bed as "cyclohexane 995." ; Consult latest OSHA regulations and supplier's Mateifety Data Sheets on handling materials listed in this "cation. eferenced Documents ASTM Standards: ,1200 Test Method for Color of Clear Liquids (Platinum- obalt Scale)2 1353 Test Method for Nonvolatile Matter in Volatile alvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 ,1555 Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons2 '3054 Test Method for Purity and Benzene Content of Cyclohexane by Gas Chromatography2 .3437 Practice for Sampling and Handling Cyclic Products2 3505 Test Method for Density or Relative Density of Pure Liquid Chemicals2 3961 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcou- ` This specification is uniter the jurisdiction of ASTM Committee D-16 on malic Hydrocarbons and Related Chemicals and is the direct responsibility of nm'ittee D16.0A on Benzene, Toluene, Xylene, Cyclohexane, and Their 'vatives. at edition approved October 26, 1990. Published December 1990. "nally published as D 3055 - 72. Last previous edition D 3055 - 86. zAnnual Bock ofASTM Standards, Vol 06.03. lometry2 D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Properties 3.1 Cyclohexane 995 shall conform to the following requirements: Property Cyclohexane, min, weight % Benzene, max, rng/kg Nonvolatile material, max, g) 100 mL Sulfur, max, mg/kg Color, max, Pt/Co scale Specification 99.5 1000 0.001 5 10 ASTM Test Method D 3054 D 3054 D 1353 D3961 or D4045 D 1209 No t e--Although not a specification item, ifspecific gravity ofcyclo hexane 995 is to be determined. Test Methods D 3505 or D 4052 shall be employed. Ifvolume or weight ofcyclohexane 995 is to be calculated, Test Method D 1555 shall be employed. 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 5. Keyword 5.1 cyclohexane 995 -- 3 Annual Book ofASTM Standards, Vol 05.03. "Available from.Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this standsrd. Users of this standard are expressly advised that determination of the validity of any such potent rights, and the risk ot.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 IInotrevised, either reapproved or withdrawn. Yourcomments areInvited either lorrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 655 DUP050296217 Designation: D 3160 - 91 Standard Test Method for Phenol Content of Isopropylbenzene (Cumene)1 This standard is issued under the fixed designation D 3160; the number immediately following the designation indicates the year pf original adoption or, in the case of revision, the year of last revision.A number in parentheses indicates the year oflast- reapprpvai. A superscript epsilon {) indicates an editorial change since the last revision or reapprovai. * 1. Scope 1.1 This test method covers the determination of phenbl in the range from 0.25 to 50 mg/kg in refined isopropyl benzene. 5.4 Separatory Funnel, 2 L. 5.5 Volumetric Flask, 100 mL. 5.6 FipeUes, l, 2, 3, and 5mL. 5.7 Filter Paper.5 . . m;vgr 1.2 Consult current OSHA regulations and suppliers' Material Safety Data Sheets for all materials used in this test method. 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. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 , D3437 Practice for Sampling and Handling of Liquid Cyclic Products3 2.2 Other Document: . .. OSHA Regulations, 29 CFR, Paragraphs 1910.000 and 1910, 1200.4 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall lx'i used. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean Reagent water defined by Type 1 or ft of Specification D it93:' \ 6.3 Isopropylbenzene--Wash 1 L. of isdpropylbimzejHfe with "5 % aqueotis sodhlin hydroxide In`a separhtqry funnel Discard the aqueous sodium hydroxide phase arid, filter the sm isopropylbenzene through dry. filter patter.5 Store the! isopropylbenzene unddr a nitfogeiti'blanket. ThO previous steps are taken to ensure that the isopropylbenzene wifi' not contain bhenol or peroxides. " , 6.4. Solution of' 4-Arnino:AriiipyHne^'DissoY(^ 3i00 g offt amiiioiantipyrihe in distilled watch and dilute to volume in dark amber 100-mL volumetric flask. This .should be stable! 3. Summary of Test Method 3.1 The phenol content of isopropylbenzene is deter mined by the color development of phenol with 4-aininoantipyrine. The sample absorbance is compared to phenol standards at 472 nm on a spectrophotometer. fortwo^eeks. ,/ t 6.5 Ammonium Persulfate Soluhdrfc--f>iy&6\ve 2.00 g of ammonium persulfate in distilled water ahd diliite to volunu in a 100-mL Vbldihetnc flaSk. A`fresh solfftiofi should bi made up weekly. 6.6 Ammonium Hydroxide, 0.880 specific gravity. 4. Significance and Use 6.7- IsopropylAlcohol, reagent grade,, 6.8 SodiumHydroxide, 5'% weight in distilled water. 4.1 This test method is useful in determining phenol in the range from 0.25 to 50 mg/kg in commercially available isopropylbenzene. 7. Hazards ,, ,~ 4.2 Phenol will inhibit certain reactions involving isopropylbenzene. 7.1 Some materials used in this test method are toxic qr flammable, or both. . 7.2 If isopropylbenzene has been exposed to air, cumene 5. Apparatus hydVdpefoxide may be in the `sample. Exercise suitable 5.1 Balance--Any balance capable of measuring weights to the nearest 0.001 g. 5.2 Spectrophotometer--Any spectrophotometer that can measure 0 to 2 absorbance units at 472 nm with a wave length repeatability of 5 nm. 5.3 Spectrophotometer Cells, 2 cm. precautions/or handling isopropylbenzene that may contain cumene hydroperoxide. 7:3 All glassware and equipment must be clean and free of acid contamination. 7.4 isopropylbenzene peroxides will decompose violently when in contact with strong acids. 7.5 Sodium hydroxide is corrosive to the skin and eyes. iL 1 This test method is under the jurisdiction of ASTM Committee D-16 on 7.6 Phenol is corrosive and toxic. Wear rubber gloves and chemical-type safety goggles, as a minimum. Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of 7.7 Isopropyl alcohol is flammable. Keep away from Subcommittee DI6.0H on Styrene, Ethylbenzene Cumene, and Naphthalene. Current edition approved May 15, 1991. Published July 1991. ignition sources. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. -1 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents U.S. Government Printing Office, Washington, DC 20402. 5 Filter paper, IPS available from Whatman Inc., 9 Bridewell Place, Clifton. NJ 07014 or equivalent, have been found suitable for this purpose. 656 t DUP050296218 # D3160 npling Isopropylbenzene shall be sampled and handled in ice with Practice D 3437. Isopropylbenzene will form peroxides when contacted air. Sample and store isopropylbenzene in air-tight ' ere. Reparation and Calibration of Standards Accurately weigh and transfer 0.100 g of phenol to a aL tared volumetric flask and bring the total net weight 1.00 g with phenol-free isopropylbenzene as prepared in antion--See 7.6.`Mix well to dissolve. This is stock dard Solution A (1000 mg/kg by weight). ! Transfer 0, 1,2, 3, and 5 mL of Stock Solution A to a fmL volumetric flask and dilute to volume with phenol|isopropylbenzene as prepared in 6.2 to yield 0, 10, 20, nd 50-mg/kg solutions to be named Solutions B, C, D, ad F respectively. Use the following procedure for Solutions B, C, D, E, ! .1 Accurately weigh and record 3.00 g of standard Ition in a 25-mL volumetric flask and add 5 mL of led water and two drops of ammonium hydroxide. Mix 3.2 Add 0.5 mL of 4-amino-antipyrine solution folby 0.5 mL ofammonium persulfate solution. Mix well fcilet stand for 10 min. .3 Dilute to volume with isopropyl alcohol and mix Warning--See 7.7. .4 Measure the absorbance of this solution at 472 nm a 2-cm cell against a blank, using Solution B. .5 Plot a curve of absorbance versus milligram per phenol (sample size of 3.00 g). Procedure |0.l Use the procedure described in 9.3.1 to 9.3.4 using " j)-g sample instead of a standard solution. j.2 Obtain the milligram per kilogram phenol in the hple from the curve prepared in 9.3.5. t e 1--This curve assumes a sample size of 3 g. Calculation 1.1 Calculate the phenol concentration in the sample i the following equation: Cx 3 milligram per kilogram phenol = W where: C = the concentration of phenol for a 3 g sample (from the curve in 10.2), and W= the sample weight, g. 11.2 To accommodate phenol concentrations greater than 50 mg/kg, adjust the original sample size to obtain a proper absorbance reading on the curve prepared in 9.3.5. Do not further dilute the final solution as this may cause turbidity. 12. Precision and Bias 12.1 Precision--Differences between laboratories should be considered suspect if the values differ by more than the values listed in 12.1.3. Differences within the laboratory should be considered suspect if they differ by more than the values listed in 12.1.2. The round robins were conducted at 5, 10, and 20 mg/kg of phenol. Reproducibility and repeat ability may change at higher concentrations. 12.1.1 The following criteria should be used to judge the acceptability at the 95 % probability level of the results obtained by this test method. The criteria were derived from a round robin between three laboratories. The data were obtained over four days using different operators. 12.1.2 Repeatability--Results in the same laboratory should not be considered suspect unless they differ by more than the following: Level, mg/kg S 10 20 Repeatability, mg/kg 0,8., 1.1 2.6 12.1.3 Reproducibility--Results submitted by two labora tories should not be considered suspect unless they differ by more than the following: Level, mg/kg- Reproducibility, mg/kg " u 2.7 5.3 12.2 Bias--Bias of this test method caiinot be determined from the limited-amount of data. 13. Keywords 13.1 isopropylbenzene (cumene); phenol content TheAmerican Society for Testing and'Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement 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. Your comments are invited eitherforrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 10103. DUP050296219 Designation: D 3193 - 91 Standard Specification for Ethylbenzene1 This standard is issued'undeI' the fixed designation D 3193; 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 oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers ethylbenzene. 1.2 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this specification. 2. Referenced Documents 2.1 ASTM Standards: ' r' D1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale)2 D3961 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Micro- coulomctry2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 ,, D5060 Test Method for Determining Impurities in High- Purity Ethylbenzene by Gas Chromatography2 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000,and ' 1910:120a3 3. Properties 3.1 Ethylbenzene shall conform to the following requiremefnts: Property . . Purity, min, weight % Benzene, tiiax, weight % Toluenes max, weigtit'% Xylenes, max, weight Cumene, max, weight % Diethylbenzene, max, weight % Chlorides, maxVmg/kg1 Sulfur, max; mg/kg Color, max, Pt-Co Specification 99.00 0.! 0,4 0.4 0.03 0.003 $ 1 10 ASTM Test Method D 5060 " D 50fi0 D5060 D 5060 D5060. , D 5060 ' ' D 3961 D1209 , 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 1 This specification is under the jurisdiction of ASTM. Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16-OH on Styrene, Ethylbenzene Cumene, and Napthalene. Current edition approved May 15, 1991. Published July 1991. 2 Annual Book ofASTM Standards, Vol 06.03. 5. Keywords 5.1 ethylbenzene; purity '3 Available from the Superintendent-of Documents, U.S. Government Printing Office, Washington, DC 20402. , , The American Society for Testing-endMaterials takes noposition respecting the validity of anypatentrights asserted in connection ' with any item mentioned In this standard. Users of this standard are expressly advisedthat determination of the validity of any such patent rights, and the risk of Infringement ot such rights, are entirely their own responsibility. This standard subject to revision el any time.by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments ere invitedeither tor revision ofthis standardor 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, ftyou leel that your comments have not received a fair hearing you should make your views known totheASTM Committeeon Standards, 1916 Race'St:, Philadelphia, PA 19103. DU P0502 96220 (Designation: D 3264 - 86 Standard Specification for industrial Grade Aniline1 Tbis standard is issued under the fixed designation D 3264; 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. iris specification covers industrial grade aniline. ' i^VThe properties included, in this specification are those Jfe characterize the above material. If additions are deemed jfc, these will'be added when their inclusion becomes desirable inecessary methods become available. Iff.:- ' enced Documents MkSTM Standards: - Test Method for Distillation Range of Volatile feknicLiquids2 5 209 Test Method for Color of Clear Liquids (Plati- n-Cobalt Scale)2 , 1^93 Test Method for Solidification Point of Industrial Organic Chemicals2 |i)36 Practice for Sampling and Handling Aniline2 l'05 Test Method for Density or Relative Density of ... : Liquid Chemicals2 589 Test Method for Nitrobenzene in Aniline2 Specification for ASTM Thermometers3 33 Test Method for Water Using Karl Fischer Reagent4 his specification is under the jurisdiction of ASTM Committee D-16 on Stic Hydrocarbons and Related Chemicals and is the direct responsibility of Ipimittee D16.0D on Organic Nitrogen Compounds, jffrent edition approved May 30, 1986. Published July 1986. Originally f as D 3264 - 73 T. Last previous edition D 3264 - 76 (1980). nual Book,ofASTM Standards, Vol 06.03. iqhual Book ofASTM Standards, Vol 14.03. 'Annual Book ofASTM'Standards, Vol 15.05. TABLE 1 Physical Requirements for industrial Grade Aniline Appearance Specific gravity. 20/4"C Color! Total distillation range at 760 mm Hg pressure 95% (2.0 to 97.0 mL) Solidification point Water Nitrobenzene dear, colorless to light yellow liquid, free of extraneous matter and sediment. Aniline is light sensitive and will darken on exposure to light and air 1.020 to 1.024 not darker than No. 100 on the platinum- cobalt scale not more than 1.0C, including the tempera ture of 184.2C not more than 0.5'C not lower than --G.20nC (anhydrous basis) not more than 0.05 weight % not more than 0.0002 weight % 3. Properties 3.1 Industrial grade aniline shall conform to the require ments in Table 1. 4.Test Methods 4.1 The material shall be sampled and the properties described in this specification shall be determined, in accord ance with the following ASTM practice and test methods: 4.1.1 Sampling--Practice D 3436. 4.1.2 Appearance--Visual Inspection. 4.1.3 Specific Gravity--Test Method D 3505. 4.1.4 Color--Test Method D 1209. 4.1.5 Distillation--Test Method D 1078 using ASTM- Solvents Distillation Thermometer 103C having a range from 148 to 202C and conforming to Specification El. 4.1.6 Solidification Point--Test Method D 1493. 4.1.7 Water--Test Method E 203. ' 4.1.8 Nitrobenzene--Test Method D 4589. The American Society for Testing end Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of (his standard are expressly advised that determination of the validity of any such patent rights, apd 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 notrevised, eitherreapprovedor withdrawn. Yourcomments are invitedeither for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 659 DUP0502 96221 Designation: D 3366 - 90 Standard Test Method for Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobait Scale)1 & This standard is issued under the fixed designation D 3366; 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 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 visual measurement of the color of maleic and phthalic anhydride melt before and after prolonged heating under specified conditions of time and temperature. Color values are expressed in terms of platinum-cobalt standards. 1.2 This standard does not purport to address all of the safety problems associated with its use. It is die responsibility of the user of this standard to consult and establish appro-, priate safety and health practices and determine the applica bility of regulatory limitations prior to use. For specific precautionary statements see 7.2. 2, Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D 3438 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, arid Phthalic Anhydride3 2.2 Other Document: OSHA Regulations, 29.CFR, paragraphs 1910.1000 and 1910.12004 * 3. Summary of Test Method 3.1 A freshly melted specimen is filled to mark into a Nessler tube arid compared with Platinum-Cobalt color standards. 3.2 After heating for 2 h at a prescribed temperature, the specimen is again compared to the color standards. 4. Significance and Use 4.1 The color of maleic anhydride and phthalic anhydride can be an indication of the purity of these materials. High colors normally indicate contamination. Nessler tubess having a total length of about 300 mm. Thg? height of the 50-mL gradation mark shall be within 200 tti? 250 mm above the exterior bottom of the tube. In a given sg$ the graduation marks shall not vary by more than 3 nw$ti The use of heat resistant glass is required. 5.2 Color Comparator, constructed to permit visual corrb parison of light transmitted through the 50-mL Nessler tui in the direction of their longitudinal axes. (The com] should be constructed so that white light is reflected ol white plate and directed with equal intensity through ,1 tubes, and should be shielded so that no light enters the tubls from the side.) . No t e 1--For convenience of operation, an electrically heated; insu- > lated comparator tube may be used to prevent the solidification or maleic or phthalic anhydride. 5.3 Electric Healing Block6--An electrically heated'alV minum block, such as shown in Fig. 1, having the following1 operating characteristics: Maleic anhydride temperature regulation, "C Heating time for sample from 60 to 140"C, minutes "" Phthalic anhydride temperature regulation, "C .' Heating time for sample from 150 to 250C, minutes Temperature gradient, sample well to thermometer well, "C max 140 2 25 3' 250 2 25 5 2 The operating characteristics of the heating block used ate*! critical. 6. Reagents 6. i Purity ofReagents--Reagent grade chemicals shall beta used in all tests. Unless otherwise indicated'it is"intended thaf-j all the reagents should conform to the specifications of Committee "on Analytical Reagents of the American Cheml ical Society, where such specifications are available.7 Othei 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 reference! to water shall be understood to mean reagent water con- 5. Apparatus 5.1 Color Comparison Tubes--Matched sets of 50-mL 1 Tbis test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. CuiTent edition approved October 26* 1990. Published December 1990. Originally published as D 3366 - 74. Last previous edition D 3366 - 85. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annua} Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, D.C. 20402. 5 Kimble No. 4S31SA-50 or H5315B-50 Nessler tubes have been found;! satisfactory for this test; available from Fisher Scientific, VWR Scientific and other j laboratory supply houses (Fisher Scientific, Corporate Headquarters, ill Forbes j Avenue, Pittsburgh, PA 15219; VWR Scientific, Marketing Department, P.O. Boa I 13645, Philadelphia, PA 19101). | 6 A commercial unit designed in accordance with specifications given in this I method may be obtained from Petrolab Corporation, 874 Albany-Shaker Road, jj Latham, New York 12110, Cat. No. 3366. It is identified as "Heater, Color Tubes, PA, ASTM." 7 "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 "Reagents Chemicals and Stan- ] dards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the i "United States Pharmacopeia." 660 DUPd50296222 # 0 3366 Os . THERMOMETER WELL 5/6-IH* DIAMETER* 3-IN. DEEP atOMINOM BLOCK 6-IN. DIAMETER* U-IM. LONG "HEATED BY HAND OS CARTRIDGE BEATER .6H0LES FOR 50-ML NESSLER TUBES I 1/16-IN. DIAMETER* 9 1/4-IN. DEEP -STAIRLESS STEEL ENCLOSURE WITH FIBERGLASS INSULATION TABLE 1 Platinum--Cobalt Color Standards^ Color Standard No. Stock Solution mL Color Standard No. Stock Solution mL 5 0.5 35 3.5 10 1.0 40 4.0 15 1.5 50 5.0 20 2.0 60 6.0 25 2.5 70 7.0 30 3.0 100 10.0 A Other color standards may bs prepared by proportional dilution in steps of 20 as Mows: No. 120, No. 140, No. 160, ate. fo @ CONTROLS FOEPOWERy , TEHFERATURE AND RATE FIG. 1 Heat Stability Block rag to Specification O' 1193, Type II. *Cobalt Chloride (CoCl2 6H20). Hydrochloric Acid (sp gr 1.19)--Concentrated hydro|e acid (HQ). Potassium Chloroplatinate (K2PtCl6). zards Consult current OSHA regulations and supplier's Irial Safety Data Sheets for materials used in this test |bd. Precaution--Handle maleic anhydride and phthalic |dride with care. Both materials are solid at ambient peratures but when heated to the molten state they cause gctionable fumes. The fumes and dust from these matefare local irritants to the skin and mucous membranes, fjeially in the presence of moisture. Material Safety Data should be obtained from the manufacturers and |ulted for proper handling procedures. npling R Sample in accordance with Practice D 3438. Standards jjl Platinum-Cobalt Stock Solution3,--Dissolve 1.245 g of rtCl6 and 1.000 g of CoCl2 6H20 in water. Add 100 mL lCl and dilute to 1 L with water. This solution is defined lor standard No. 500. f.2 Platinum Cobalt Standards9--From the stock solu- prepare color standards by diluting the required voi les as given in Table 1, to 50 mL with water in the Nessler "The stock solution with color No. 500 may be purchased as such from piuical supply firms. Use of the purchased standards is satisfactory. 5 The preparation of these platinum-cobalt standards was originally described riazen, A. American Chemical Society Journal, Vol. 14, 1892, p. 300. The 'ription given in this test method and in ASTM Test Method D 1209, Test for far of Clear Liquids (Platinum-Cobalt Scale), which appears in the Annual Book TM Standards, Vol 06.03, is identical with that given in the Standard j|Wj for the Examination of Water and Sewage, American Public Health ociation, Tenth Edition, 1955, p. 88. A description is also given by W. W. Scott ^Standard Methods of Chemical Analysis, D. Van Nostrand Co., inc,, Sixth Ition, Vol. 2, Part B, p. 2424. tubes. When not in use, protect these standards from contamination and evaporation by the use of suitable caps on the tubes. 10. Procedure 10.1 Melt an approximately 75-g sample (Note 2) and simultaneously preheat a> Nessler tube in an oven, electric heating block, or other similar equipment held at a temper ature of 60C for maleic anhydride and 15CTC for phthalic anhydride. 10.2 As soon as the sample is completely liquid, mix by stirring with a clean, dry, glass rod; then quickly fill the preheated Nessler tube to the 50-mL mark with the sample and place in the comparator; immediately compare with the standards and record as the color of the sample in the molten state. 10.3 Place the filled Nessler tube in the heating block which has been regulated at the appropriate temperature; For maleic anhydride For phthalic anhydride 140 2'C 250 2"C Use a small ring of glass wool around the top of the hole to support in a vertical position and to seal off the dead air space between the tube and the heating block. Allow the tube to remain in the block for 2 h (which includes 90 min at the test temperature). Protect tubes adequately from contamina tion during the test period. No t e 2--Place a small quantity of glass wool in the bottom of each hole to ensure against breakage of Nessler tubes ancHhenmometers. * 10.4 Remove 'the tube, place in the comparator, and immediately compare with the standard. Record as the color after heating in the molten state. 10.5 In no case apply this test method if the molten sample contains any visible turbidity. II. Report 11.1 Report the following information: 11.1.1 Report (!) color in the molten state, and (2) color in the molten state after heating. 11.1.2 Report as the color, the number of the standard that most nearly matches the sample. In the event that the color lies midway between two standards, report the darker of the two. 11.1.3 If, owing to differences in hue between the sample and the standard, a definite match cannot be attained, report the range over which an apparent match is obtained, and report the sample as "off hue". 11.1.4 If, owing to large differences in hue between the 661 DUP050296223 # D 3366 sample and the standards, no estimate is possible, report the sample as "no match." 12. Precision 12.1 Repeatability--Duplicate results by the same oper ator should be considered suspect if they differ by more than the following amounts; Platinum Cobalt Color Repeatability Maleic Anhydride Molten color Color after heating Phthalic Anhydride 10 to 20 20 to 40 5 10 Molten Color Color after heating 15 to 40 40 to 70 S 10 12.2 Reproducibility--Duplicate results by each of laboratories should be considered suspect if they differ more than the following amounts: ' Maleic Anhydride Molten color Color after heating Phthalic Anhydride Molten color Color after heating Platinum Cobalt Color 10 to 20 20 to 40 15 to 40 40 to 70 Reproduribli 0.6 P< a 25 A P4 = average platinum-cobalt color. 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 me expressly advised that determination of the validity ofany such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard Is subiect to revision at any time by the responsible technical committee and mustbe reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 Race St., Philadelphia, PA 19103. DU P0502 96224 Designation: D 3436 - 91 Standard Practice for Sampling and Handling Aniline1 This standard is issued under the fixed designation D 3436; 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. us practice covers procedures for sampling and ; aniline. ay person sampling or handling aniline should have ` first aid instructions and equipment available for use vent of personal contact or exposure. This standard does not purport to address all of the problems, if any, associated with its use. It is the ' ibility ofthe user ofthis standard to establish approafety and health practices and determine the appjicaf regulatory limitations prior to use. For specific "Statements, see Sections 3, 4, 5, 6, and 7. ferenced Documents ASTM Standard: "0 Practice for Sampling Industrial Chemicals2 Other Documents: "A Regulations, 29 CFR, paragraphs 1910.1000 and 910.12003 FT Regulations, 49 CFR, Subchapters B and C; Parts 1-1793 cription of Product ? Typical Properties and Characteristics (See Table I): Stability--Aniline is a stable material under normal tions. It does not decompose at its boiling point or . exposed to high environmental temperatures for long Although the vapor given off at elevated temperais flammable, aniline can be handled with little danger Should aniline ignite, it may be successfully extin- ed with water, applied in the form of a fog or spray (see Solubility--Aniline is miscible with alcohol, ether, ne, and most organic solvents. It is only slightly soluble ter. Classification and Regulations: 4.1 Aniline is classified by the Department of Transpor ts a Poisonous Liquid, Class B (Regulation 173.347) a Class 6 Poison by the United Nations. As such, it be packaged in DOT specification containers when ped by rail, water, or highway, and all of the DOT practice is under the jurisdiction of ASTM Committee D-16 on tic. Hydrocarbons and Related Chemicals and is the direct responsibility of mitteeD16.0J on Sampling and Handling Aromatic and Cyclic Hydrocar- rrent edition approved Oct. 15, 1991. Published December 1991. Originally ' ed as D 3436 - 75. Last previous edition D 3436 - 86. nual Book ofASTM Standards, Vols 06.03 and 15.05. vailabie from Superindendent of Documents, Government Printing Office, `ngton, DC 20402. TABLE 1 Typical Properties and Characteristics of Aniline Chemical names Common names Empirical formula Physical form Color Light sensitivity Boiling point Specific gravity Solidification point, anhydrous basis, min Explosive limit lower Flash point Closed cup Open cup anltne, aminobenzene, benzenamlne, phenylamine aniline, aniline oil c 6h 5n h 2 oJy liquid at normal temperature colorless to light yellow (dear) tends to become amber brown In color upon exposure to air and light 184:2C (364F) at 760 mm Hg 1.022 at 20/4C -6.2*0 <21 F) 1.3 volume % in air . 70.0C (158E) 75.6C (168F) Regulations regarding loading-handling and labeling must be followed. 3.4.2 Department of Transportation (DOT) Regulations regarding the shipping of this chemical are specified in 49CFR. Regulations include the handling of aniline packages and return of empty containers. All containers should carry an identifying label or stencil and must bear' the DOT POISON label. Aniline is ordinarily transported in tank cars, tank trucks, or metal drums. 3.5 Toxicity--Although aniline is highly toxic, it may be handled safely if proper precautions are observed. The odor of aniline can usually be detected without difficulty in concentrations as low as 0.5 ppm in the atmosphere. Avoid contact with skin. Maintain adequate ventilation. 4. Hazards 4.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials utilized in this practice. 4.2 Health: 4.2.1 Aniline is highly toxic and may enter the body easily and rapidly by absorption through the intact skin, by ingestion, or by inhalation of the vapor. The most common incidences of accidental poisoning are due to spillage of the liquid on the skin or clothing resulting in direct skin contact or the prolonged inhalation of vapor because of inadequate ventilation. 4.2.2 Aniline causes the oxygen-carrying pigment in'the blood, hemoglobin, to change to a form known as methemoglobin; thus the ability of the blood to transport oxygen to tissues is reduced in aniline poisoning. The systemic effects of poisoning varies with the intensity of the exposure. Cyanosis, the most common symptom of aniline poisoning, is characterized by a bluish tinge which results from the inadequate oxygenation of tissues. Discoloration is most noticeable on the cheeks, lips, ears, fingernail beds, or 663 DUP050296225 # D 3436 oral membranes. When the liquid has penetrated the skin, the area of contact will sometimes appear cyanotic. Poi soning may also give rise to headaches, palpitation, dizziness, nausea, difficult breathing, convulsions, and psychic disturb ances. Some authorities claim the effects of aniline poisoning are increased by the consumption of alcohol. Aniline is likewise a mild irritant to the eyes and could cause corneal damage. If a splash occurs, wash the eyes with profuse amounts of water for a minimum duration of 15 min. In all cases, contact a physician as soon as possible. 4.2.3 The threshold for aniline-skin is 2 ppm (10 mg/m3 of air) as defined by the American Conference of Govern mental and Industrial Hygienists. The most potential contri bution to the overall exposure to aniline is by the cutaneous route, either by airborne, or more particularly, by direct contact with the skin. Therefore, the threshold limit value for aniline-skin is 2 ppm to suggest appropriate measures for the prevention of cutaneous absorption so that the threshold limit is not invalidated. With respect to airborne exposure, the threshold limit value of aniline is 2 ppm (10 mg/m3 in air) for an 8-h working exposure. 4.3 Fire: 4.3.1 Aniline has a flash point well above room tempera ture. Consequently, ignition in air is difficult and the rate of flame propagation is slow. Use methods for controlling Class B fires. Fires involving aniline can be extinguished with carbon dioxide, dry chemical, and water fog. If water is used on an aniline fire in which the liquid temperature is near or above the boiling temperature of water, there will be a boil-over as a result of rapid, steam formation and spattering of the aniline. This increases the toxic hazard. Therefore, in fighting large fires use fog, foam, or spray in preference to a solid stream of water. 4.3.2 Always avoid skin contact or inhaling of vapors while combating a fire. Fire fighters must be equipped with standard firemans' clothing plus respiratory protection. 4.4 Persons handling aniline must use proper protective equipment. However, protective equipment is not an ade quate substitute for safe working conditions, proper ventila tion, and good work practices. Personal protective equip ment only protects the worker wearing it and other unprotected people in the work area may still be exposed to danger. Education of the worker in the proper use of protective equipment is essential. 5. Unloading of Tank Cars*or Tank Trucks 5.1 Always keep in mind that the main hazards are exposure to liquid aniline and toxic fumes. Personal protec tive equipment is not an adequate substitute for safe working conditions and intelligent conduct on the part of employees working with aniline. Furthermore, the correct usage of personal protective equipment requires the education of the worker in the proper employment of the materials available to him. 5.2 Level and secure any tank car or tank truck against movement during unloading. In the case of tank cars, use derails. Set the truck brakes and block the wheels. 5.3 Prior to unloading, read and observe all caution markings on both sides of the transport and the dome. Equip each transport with a safety valve and an approved rupture disk, in accordance with DOT specifications. 5.4 Sample the contents of the tank car or tank tiu through the open dome or manhole. The person taking ! sample must wear the proper protective equipment (e Section 6). 5.5 The preferred method for unloading tank trucks is hy> pump and not air pressure. Unloading oftank cars throught dip leg inserted in the dome is preferred to bottom loading. Do not use air pressure for unloading of tank cars.;^ Use of a pump is recommended. 5.6 Inspect lines prior to unloading to ensure that the 11 connections and valve settings are correct and that there artf no loose or broken connections. If a spill, leak, or overflow occurs during the unloading, stop the pump or air sunJf promptly, shut off valves and clean up the spill before otf! actions are taken. Avoid the dumping of large quantities,! aniline on the ground. Flush all spills promptly with water, 5.7 When loading is completed, and lines have be drained, close all valves tightly. Remove or reverse D(J| DANGEROUS placards. 6. Sampling of Tank Cars or Tank,Trucks No t e--FFoor full deefteails concerning the proper sampling procedures consult Praactice E 300. 6.1 Aniline is extremely hygroscopic and great care musf be taken to obtain a suitable sample and to protect it during the determination of its solidification or boiling points, or both. Since aniline also slowly darkens due to slight oxida tion to aif and light, take the samples in brown (amber) glass bottles. 6.2 Since aniline is homogeneous, only limited sampling1 is usually required. Samples may be taken,through an opcu-:jj manhole or dome by means ofa clean, dry, 1 -pt amber boi held in a clean, dry sheath ofstainless steel or nickel attach to a long rod or light-weight chain of the same material (i Fig. 2 ofPractice E 300). Avoid copper ifthe material is to bfj used for the manufacture of copper-free dyes or rubber,,, chemicals. Iron, in some instances, causes undesired contam ination and should be treated in a similar manner. 6.3 Fit the sample bottle with a glass stopper to which i| attached a light, metal chain. Lower the bottle to an.approx| imate middle of the tank and pull tfie stopper,out with |j sharp jerk ofthe chain. Then raise it at such a rate that it is* essentially foil when it emerges from the liquid. Stopper the,, bottle before making any attempt to rinse the material from the outside. 6.4 Emphasis should be placed on cleanliness and dry ness. Both the sample bottle and its holder must be clean and dry. Transfer the sample to another bottle for storage.'A suitable bottle for storing the sample is one commonly;, known as a "Boston Round." The storage sample bottle must ( be made of amber glass, with a screw cap closure fitted with | a polyethylene liner. \ 7. Handling and Sampling of Drums 7.1Aniline is usually shipped in 55-gal steel drums. The sj following types are normally utilized: steel drums not over 55 gal in capacity and with welded seams and reinforced- i chimes; where their capacity is over 25-gal (DOT-5,5A, 5B), | single-trip steel drums with welded body seams (DOT-17C); I as well as 5-gal type and the DOT-17E classification. Do not use paraffin- or plastic-lined drums. Mild steel or cast iron 664 DUP050296226 D 3436 scommended if discoloration is to be kept at a precautions are taken, drums may be used ge. Store them under a shed-type roof to protect Dm the direct sun. Handle containers carefully to damage, and examine shipments carefully for [ drums. Drums are not pressure containers and must ded by using a self-priming, hand or motor-driven |or by gravity flow. It is necessary that the operator wear goggles and other ve equipment and use a bung or plug wrench when the body plug from a drum. Place the drum stand to one side and turn your face away during eration. After the plug starts to loosen, give it not an one full turn. If internal pressure exists, allow it to i the atmosphere. Then the operator can loosen the tier and remove it. : drums are emptied by gravity, insert a valve or i the end bung and support and block the container at movement. ;It is recommended that a stainless steel sampling tube be utilized for sampling drums. Avoid copper tubing, partic ularly if the material is to be used for the manufacture of copper-free dyes or rubber chemicals. The tube should be designed so that it will be within 6 in. of the bottom (a detailed description of the drum sampling tube is given in Practice E 300). Insert the open tube through the bung of the upright drum and lower it to the bottom. With the thumb over the upper opening, withdraw the tube (thief) quickly and transfer the contents into a bottle. Wear clean rubber or PVC gloves during this operation. Avoid handling any part of the tube that has been immersed in the liquid. Do not permit the hands to come in direct contact with any part of the sample. 7.6 As an alternative sampling procedure, transfer the sample directly from the sampling tube into a side-arm vacuum flask by means of siphoning with a double-valve aspirator bulb. Before collecting the sample, thoroughly flush the device with the material being sampled. Then transfer the material from the vacuum flask to the amber-colored sample bottle. 8. Keywords 8.1 aniline; handling; sampling The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision atany time by the responsible technical committee 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 lor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee. which you may attend. If you feel that your comments have not received a fair hearing you should make yourviews known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296227 Designation: D 3437 - 89 Standard Practice for Sampling and Handling Liquid Cyclic Products1 2 This standard is issued under the fixed designation' D 3437; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice covers procedures for sampling and handling several liquid cyclic products. These specifically cover liquids at ambient temperature and include benzene, toluene; xylenes, cyclohexane, styrene, pyridine, ethylben zene, and isopropylbenzene. 1.2 Any person sampling and handling these products should have specific first aid instructions and equipment available for use in the event of personal contact or exposure. 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. Fot specific hazard statements, see Sections 5 and 6, 2. Referenced Documents 2.1 ASTM Standard: E 300 Practice for Sampling Industrial Chemicals^ 2.2 American National Standards Institute Standard: Z 288.1 Flammable and Combustible Liquids Code3 2.3 API Document? RP-500A Classification of Locations for Electrical Instal lations in Petroleum Refineries4 2.4 Other Documents: OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.2000s U.S. DOT Regulations, 49 CFR Transportation, Subchap ters B and C, Parts 171-1795 3. Significance and Use 3.1 This practice is issued to provide information useful in establishing sampling and handling procedures. It is expected that this information will only be utilized in conjunction with an existing health and safety program. The information provided herein cannot be used as a substitute for expert lThis practice is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0J on Sampling and Handling Aromatic and Cyclic Hydrocar bons. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 3437 - 78. Last previous edition D 3437 - 83. 2 Annual Book ofASTM Standards, Vols 06.03 and 15.05, 3 Available from American National Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036. 4 Available from American Petroleum Institute, 1220 L Sl NW, Washington, DC 20005. 3 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. TABLE 1 Physical Properties Product Boiling Point, *C Benzene Cyclohexane Ethylbenzene Isopropylbenzene Pyridine Styrene Tqluene Xylene (mixed) 80 80 136 152 115 145 1.10 137 to 144 - Specific Gravity, ?! 15.5/15.5*0 tff; 0.88 0.78 .j 0.87 \ ^ 0.87 0.90 0.91 0.87 0.87 safety and medical advice, but rather as a supplement to such advice. 4. Description of Products (See Table 1) 4.1 These liquids are marketed in different grades of purity so the physical,properties will vary somewhat. 4.2 Benzene, toluene, xylene, cyclohexane, styrene, pyridine, and ethylbenzene are classified by the Department of Transportation as flammable liquids, and containers must bear flammable liquid labels. Trucks and tank cars must have flammable liquid placards. Isopropylbenzene is classi fied as a combustible liquid; trucks and tank cars must have combustible placards. 4.2.1 These products are ordinarily transported in steel drums, tank cars, tank trucks, barges and ships. 4.2.2 While these products are dangerous when handled improperly, their unloading need not be hazardous providing the hazards are recognized and handling' instructions are rigidly observed. ~- ' 5. Hazards 5.1 Health--Consult current regulations and supplier's Material Safety Data Sheets for all materials used in this practice. 5.2 Fire: 5.2.1 All of these liquids introduce a potential fire hazard where they are stored, handled, or used. 5.2.2 Vapors of all of these materials can form explosive mixtures with air. 5.2.3 Foam, carbon dioxide, dry chemical, or water fog can be used in fighting fires of these products. Special alcohol-type foam is required to extinguish effectively a fire involving pyridine. 6. Safety Precautions 6.1 Unloading operations must be conducted by carefully instructed employees. 6.2 Be sure that the storage tank is safely vented before connecting the unloading line. 666 DUP050296228 D 3437 ABLE 2 OSHA Exposure Limits in the Atmosphere Reference--Code of Federal Regulations 29 Part 1910.1000 Product Ceiling Values, PPm 8-h Weighted Average, ppm ane zene ibenzene (cumene) 1 300 100 SO, 5 200 100 300 200 100 'limits are under constant revision and latest published regulations should be consulted.) 'Take extreme care to prevent spills and leaks. In case 'al is spilled, wash contaminated areas thoroughly with quantities of water and collect the liquid in the plant cal waste system.' Because of the flammability of vapors, do not permit or open flames in the vicinity of bargfes, ships, tank 5jtank trucks, drums, or storage tanks. All electrical ment and wiring shall be of a type specified by and be installed in accordance with the National Electrical after determining whether or not the operation is M out in a classified or unclassified area for electrical llations. Electrically bond tank cars, tank trucks, and Ls by an approved method! Smoking is absolutely !bited. re 1--Sec API-RP500 and ANSI Z 288.1, Chapters VI and VIII, etric installations. 5 t>o not permit workmen to enter an empty storage 1, barge, ship, tank car, or tank truck until it has been oughly washed out with warm water, followed by a ough steaming, and the tank atmosphere analyzed for en as well as flammables. Entry should not be made out respiratory protection if the vapor space is not in pliance with OSHA TWA values. SUPERVISOR'S APVAL FOR ENTRY IS REQUIRED IN EVERY CASE. nloading and Sampling of Tank Cars .1 Unloading: ,1.1 Because of the flammable properties of these mates, the unloading of tank cars-containing chemicals is a ardous operation. Carefully read and follow all shipper's actions and all caution markings on both sides of the k and dome. .1.2 Before removing the manhole cover or outlet valve ;, relieve the tank car of all internal pressure by venting tank. This can be accomplished by raising file safety ye, or opening the vent on the dome at short intervals. If ting to relieve pressure will cause a dangerous amount of -r to escape, defer venting and unloading until the ssure is reduced by allowing the car to stand overnight or erwise cooling the contents. .1.3 Use bonding facilities for protection against static -ks during the unloading of tank cars through open es. This shall consist of a bond wire permanently ctrically connected to the unloading pipe or some part of structure in electrical contact with the unloading pipe. Provide the free end of such wire with a clamp or equivalent device for convenient attachment to some metallic part of the tank car. Such bonding connection shall be made fast to the tank car before dome covers are raised and shall remain in place until unloading is complete and all dome covers closed and secure. This bond wire is not required when the unloading pipe is all metal and the unloading pipe is electrically bonded to the rail tracks. No t e 2--See ANSI Z288.1, Chapter VI. 7.1.4 Tank cars can be unloaded through the dome connection or through the bottom outlet. Never use air pressure for this purpose. Use of a pump or nitrogen pressure are the recommended methods. If the car does not have an eduction pipe, insert one and remove the contents by pumping. If it is necessary to leave the car unattended after unloading has been started, disconnect all unloading connec tions. First close all valves tightly and apply the closures to all other openings securely. 7.2 Sampling: 7.2.1 Sample,s may be taken through the manway opening by means of a clean, dry, 1-qt (l-L) bottle held in a clean, dry sheath of nickel or stainless steel attached to a long rod or lightweight chain of the same material. Fit the bottle with a glass stopper to which is attached a light metal chain. Lower the bottle to near the bottom of the tank and pull out the stopper with a sharp jerk of the chain. Raise it at such a rate that it is about three fourths full when it emerges from the liquid. Stopper the bottle before attempting to rinse the material from the outside. Label the sample bottle according to OSHA Regulations. 7.2.2 Emphasis should be placed on cleanliness and dryness. Both the sample bottle and its holder must be CLEAN AND DRY. Transfer the sample to another bottle for storage. A suitable bottle for storing the sample is one known as a "Boston Round." The closure should be a screw cap with poly-seal or an aluminum foil liner. 7.2.3 If new bottles are used, first rinse them thoroughly with acetone or methanol and then dry in a hot-air oven. Hold in a desiccator while cooling to ambient temperature. Protect them from dirt or moisture by"enclosure in'a polyethylene bag.-Rinse used bottles very thoroughly with water, detergents, and solvents and then treat as new bottles. No t e 3--Brown bottles are recommended for sampling and storing photo-sensitive products. 7.3 Return Precautions: 7.3.1 As soon as the tank car is completely unloaded, close all valves tightly, remove the unloading connections, and make all other closures tight, except the heater coil and steam connections. Observe DOT regulations concerning return placarding. 8. Unloading and Sampling of Tank Trucks 8.1 Unloading: 8.1.1 Because of the flammable properties of these mate rials, the unloading of tank trucks containing them is a hazardous operation. Follow the shipper's instructions and all caution markings. 8.1.2 Stop the engine before unloading a truck, and do not start it again during the entire unloading operation unless it is necessary to operate the pump by power take-off. ipnww!....... . DUP050296229 D 3437 Set truck brakes and block the wheels. 8.1.3 Before making any connection or contact between the tank truck and the unloading line or other unloading equipment, electrically bond the tank truck in a manner similar to that for tank cars as described in 7.1.3. 8.1.4 Tank trucks can be either top or bottom unloaded in the same manner as for tank cars as described in 7.1.4. 8.1.5 Air pressure is not permissible for unloading tank trucks of these materials. Nitrogen pressure is permissible for this purpose. 8.2 Sampling; 8.2.1 Sample a tank truck in the same way as tank cars, with the same rigid adherence to the precautions against moisture and color degradation. 9. Unloading and Sampling of Drums 9.1 Unloading: 9.1.1 When a carload or truckload of drums is received, open the truck doors or the doors on both sides of the car, as the case may be, to allow thorough ventilation of the vehicle before entering it Examine each shipment for leaking drums. Remove all potential sources of ignition from the area. 9.1.2 Before drums are opened, they should be properly supported. Products should not be dispensed from drums into metal containers unless the nozzle or fill pipe is in electrical contact with the container. This can be accom plished by maintaining metallic contact during filling, by a bond wire between them, or by other conductive paths having an electrical resistance not greater than 106 Q. Bonding is not required where a container is filled through a closed system, or is made of glass or other nonconductij material. 9.1.3 It is necessary that the operator wear goggles and u a bung or plug wrench when removing the body plug from a drum of one of these materials. Place the drum upright stand to one side, and turn the face away during^the'* operation. After the plug starts to loosen, give it not mors than one full turn. If internal pressure exists, allow if to \ escape to the atmosphere. Then loosen the plug further and remove it. _ 9.1.4 The preferable safe method for emptying drums is by hand pump. If an electrical pump is used, it shall be installed in accordance with the National Electrical Code and shall be suitable for the electrical classification of the area in which it is located. If these drums are emptied by gravity, the faucets must be self-closing. The use of pressure for emptying drums is not recommended. 9.2 Sampling: 9.2.1 The use of a stainless steel sampling tube is recom mended for drum sampling. The tube should be designed so that it will be within about 1 in. {25 mm) of the bottom and have a suitable capacity.. (A detailed description of drum sampling tube is given in Practice E 300.) Insert the open 4 tube through the top bung of an upright drum and lower it to tij the bottom. With the thumb over the upper opening, withdraw the tube quickly and transfer the contents into a bottle. 9.2.2 Clean and dry the bottles in the same manner as the tank car sampling bottles. 10. Unloading and Sampling Barges and Ships 10.1 Sample and handle barges and ships in a manner similar to top unloading of tank cars and tank trucks (see 7.1.4). TheAmerican Society for Testing amtMaterials 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 infringsment 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, eitherreepprovedor withdrawn. Your comments are invitedeither forrevision 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 fair hearing you should make your views known to the ASTM Committee an Standards, 191$ Race St., Philadelphia, PA .19103. 668 DUP050296230 Designation: D 3438 - 89 Standard Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride*1 This standard is issued under the fixed designation D 3438; 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. m phis practice covers procedures for sampling and Dg naphthalene, maleic anhydride, and phthalic anhy|in various solid forms, and as liquids at elevated atures from the viewpoints of quality assurance and Any person sampling or handling these products I have specific first aid instructions and equipment hte for use in the event ofpersonal contact or exposure. This standard may involve hazardous materials, oper and equipment. This standard does not purport to 'ss all ofthe safety problems associated with its use. It is Responsibility of the user of this standard to establish opriate safety, and health practices and determine the [icability ofregulatory limitations prior to use. eferenced Documents If ASTM Standard: - 1300 Practice for Sampling Industrial Chemicals2 Other Dnrumpnt? SHA Regulations, 29 CFR, Paragraph 1910.1000 and 1910.12003 IS. DOT Regulations, 49CFR Transportation, Subchap ters B and C, Parts 171-1793 Significance and Use 1?1 This practice is issued to provide information useful in Wishing sampling and handling procedures. It is expected this information will only be utilized in conjunction i an existing health and safety program. The information |vided cannot be used as a substitute for expert safety and dical advice, but rather as a supplement to such advice. fDescription of Products (See Table 1) 4.1 Phthalic anhydride is hot classified as hazardous by fe Department of Transportation and is therefore hot iject to DOT regulations governing the transportation of rdous articles. Maleic anhydride and napthalene are ssified as hazardous by the Department of Transportation ad are subject to DOT regulations. Maleic anhydride has `This practice is under the jurisdiction of ASTM Committee D-16 on omatic Hydrocarbons and Related Chemicals and is the direct responsibility of ommittee D16DJ on Sampling and Handling Aromatic and Cyclic Hydrocar- |Current edition approved Nov. 24, 1989. Published January 1990. Originally jblished as D 3438 - 75. Last previous edition D 3438 - 83. p 2 Annual Book ofASTM Standards, Vols 06.03 and 15.05. i * Available from Superintendent of Documents, Government Printing Office, Washington, DC 20402. TABLE 1 Typical Physical Properties Product Melting Point, C Boiling Point, 6C Forms Naphthalene Maleic anhydride Phthalic anhydride 80 53 130 218 (sublimes) 200 (sublimes) 264 (sublimes) flakes, balls, liquid, rods, tablets rods, briquettes, liquid flakes, liquid the classification ORM-A-2215 RQ, and naphthalene has the classification ORM-UN-I334 RQ. 4.1.1 These products are normally transported in several types of containers, including cartons, barrels, bags, cans, metal and fiber drums, tank trucks, tank cars, and barges. 4.2 While these products are dangerous when handled improperly, particularly at elevated temperatures, their un loading need not be hazardous provided the hazards are recognized and handling instructions are rigidly observed. 5. Hazards 5.1 Health--Consult current OSHA regulations and sup plier's Material Safety Data Sheets for all materials used in this practice. 5.1.1 Aside from the risk of bums in handling these products when molten, and a possibility of dermatitis from impurities, particularly in crude grades, industrial use does. not present a significant health hazard. However, ordinary handling precautions must be observed to protect personnel from contact with molten material or excessive exposure `to~ dusts or high concentrations of vapor. 5.1.2 Precautions must be observed to protect personnel from excessive inhalation of vapors and dust. No t e 1--For permissible exposure limits see OSHA Regulations, paragraph 1910.1000. 5.2 Fire: 5.2.1 These products in both the solid and liquid forms are combustible, and introduce a potential fire hazard where they are stored, handled, or used. 5.2.2 Naphthalene, maleic and phthalic anhydride vapors or dust can form explosive mixtures with air. 5.2.3 When molten naphthalene, at temperatures above 11 (PC, comes into contact with water, foaming or possible explosion may result. 5.2.4 Dry chemicals, carbon dioxide, and foam can all be used in fighting fires involving these materials. 5.2.5 Maleic anhydride decomposes violently in the pres ence of amines or alkali metals, especially at elevated temperatures. Avoid contaminating maleic acid with these metals. 669 DUP050296231 # D 3438 6. Protective Equipment 6.1 Persons handling molten naphthalene, maleic, and phthalic anhydrides require eye, face, respiratory, body, skin, and hand protection. 6.2 Personal protective equipment is not an adequate substitute for good safe working conditions, proper ventila tion, and intelligent conduct. Correct usage of protective equipment requires education in its proper use. 7. Safety Precautions 7.1 Unloading operations of molten liquids should be performed only by carefully instructed personnel. 7.2 Exercise care to prevent spills and leaks. If they do occur, only properly protected personnel should remain in the contaminated area. 7.3 Allow spilled material to cool and solidify. If the spill is large, rope the area off. 7.4 Because of fire and explosion hazards, do not permit open flames in the vicinity of tank carriers, other shipping containers, or storage tanks. Provide all electrical fixtures with vapor-proof globes and explosion-proof safety devices. Ground tank carriers and metal drums by an approved method. Prohibit smoking. 8. Unloading Tank Cars or Tank Trucks 8.1 Before unloading the tank car, observe all safety precautions. Always, follow shipper's instructions for un loading, and read and observe all caution markings on both sides of the tank or dome. In general, the safety precautions and procedures recommended are also applicable to tank trucks and barges. 8.2 Always keep in mind that these materials are hot enough when molten to cause severe bums. 8.3 Because these materials are solids at temperatures below 50C, it is necessary to apply steam to the heater coils of the car to melt the material and get it hot enough for unloading. 8.4 Opening of the tank car dome cover, connection of steam or heater coils, attachment of delivery lines and pumps should all be done by accepted safety procedures. 8.5 Avoid steam pressures and temperatures that will raise the temperature to a point where expansion will cause an overflow at the top of the dome. It is recommended that the contents be heated with steam coils and held at the temper atures listed below until completely molten. Heating the contents more than 5C above these temperatures is dan gerous, because of the likelihood of boil-over. Product Recommended Maximum Temperature, "C (T) Naphthalene Maleic anhydride Phthalic anhydride 90 094) 70(158) 140 (284) 8.6 With the tank car dome cover still open and the contents of the car completely liquefied, the product is ready to be sampled and unloaded.9 9. Sampling Tank Cars 9.1 Use brown 1-qt (1-L) bottles made of heat-resistant glass with screw caps to collect samples of molten maleic anhydride and phthalic anhydride. Use metal 1-qt cans with screw caps for sampling molten naphthalene. No t e 2--Caps must have aluminum foil liners. 9.2 Install the can or glass bottle in a suitable weighted''* sampling harness, constructed in such a way that the top of the container is held in an upright position, when the apparatus is lowered into the car. 9.3 Obtain the sample through the open dome. Lower the can or bottle in the weighted harness quickly to the bottom of the compartment, and raise it slowly at such a rate so that it is about three fourths full as it emerges from the liquid. 9.3.1 Remove the sample apparatus carefully, taking care not to strike it sharply against the tank car. As soon as the sampling container is removed from the harness, cap and wipe it off with a rag before the material solidifies on the' threads. 9.3.2 Attach an identification tag to the sample container: 9.3.3 It should be emphasized that cleanliness and the absence of moisture are absolutely essential to ensure that a truly representative sample is obtained from the tank cai The practices recommended for Practice E 300 should be observed. 10. Sampling Metal Drams and Cans of Naphthalene 10.1 Before heating the container of naphthalene, pro' ide a vent and protect the material from contamination. Melt the naphthalene under dry heat. If it is necessary to use a: water bath for melting, protect the naphthalene from any moisture contamination. 10.2 To ensure a representative sample, mix the contenis of the container thoroughly by a suitable means. 10.3 Sample the naphthalene as soon as possible after it t melted and mixed. Collect the sample in tinned cans! ' Sampling may be done either by dipping out portions or by-| means of a heated pipet 11. Sampling Solid Naphthalene. (Chips, Flakes, Balls) 11.1 Bulk Quantities: 11.1.1 Take a representative sample, preferably from a falling naphthalene stream, using a straight-path sampler. Adjust sampler feed rate, slot width, cutter speed, and frequency to collect V2 lb of sample per 10 000 lb (4540 kg) of naphthalene. 11.1.2 Melt the entire naphthalene sample and mix thor oughly before analyzing. 11.2 Bags: 11.2.1 Using a small thief 8 to 12 in. (203 to 305 mm) remove about V2 lb of sample from 1 bag out of every 40 bags (4000 lb) (1814 kg) of naphthalene. Take the sample from the filling ear or, if necessary, by opening one comer of the bag. Place each sample in a plastic bag or brown glass jar labeled with proper identification. 11.2.2 Make a composite blend from the individual samples. Melt the blend and mix thoroughly before ana lyzing. 11.3 Drums (200 to 240 lb (91 to 109 kg)): 11.3.1 Insert a thief into the center of the drum to the hallway point and remove about 200 g of naphthalene. Sample 1 drum out of every 20 drums (4000 to 5000 lb (1814 to 2268 kg)). Place each sample in a plastic bag or glass jar labeled with proper identification. 670 ! / DUP050296232 D 3438 .2 Make a composite blend from the individual Melt the blend and mix thoroughly before ana- pling Solid Phthalic Anhydride and Maleic Anhy- For the purpose of this sampling procedure, a sample defined as 2000 lb (907 kg) consisting of forty 50-lb leg) bags, for phthalic anhydride and maleic anhydride. S are usually shipped on a pallet. It is recommended that 10 % of the shipment be with a maximum of five sample units comprising a site sample. A maximum of five sample units may be composited lalysis with a minimum of 200 g taken from each unit. Sample containers shall be brown glass bottles, fitted uminum foil-lined caps. Before use, clean and dry the in a clean air convection-type oven. 12.5 Nickel, high-density polyethylene, polypropylene, or stainless steel-type scoops are recommended for taking samples of product from the bags selected for sampling. 12.6 Place samples taken for interlaboratory testing or shipment in a polyethylene bag (hat is subsequently sealed and placed in a brown bottle containing a desiccant. If a sample exchange between purchaser and seller is indicated, duplicate samples must be taken and packaged as recom mended. 12.7 Extreme care and good judgment are necessary to ensure that the samples truly represent the product. Since the maleic and phthalic anhydride is packaged in multiwall moisture-resistant paper bags, take care in obtaining the sample. 12.8 Remove approximately 75-g portions from each of the bags selected from a sample unit and place in a wide-mouth brown bottle with a polyethylene-lined cap. Seal the opened bags with a suitable tape. 12.9 Label die bottle and bags properly for future identi fication in the testing laboratory. The AmericanSociety 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 ate expressly advised that determination of the validity of any auch 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 Invitedeithertor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you leal that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.' DUP050296233 i Designation: D 3439 - 89 Standard Test Methods for Assay of Alkaline Cresylate Solutions From Petroleum Sources1 This standard is issued under the fixed designation D 3439; 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 the assay of cresylic acid in alkaline cresylate solutions. These test methods apply specif ically to materials of petroleum origin and may not be fully applicable to materials from other sources, such as cqal tars. 1.2 The procedures appear in the following sections: Sections Crude Cresylic Acid-Cylinder Method --................................ : Water Content of Crude Cresylic Acid....................................... Cresylic Acid Distillate (to 230"C) Content of Crude Cresylic Add....................................................................................... Sulfur Compounds in Cresylic Acid Distillate........................ .. Neutral Oil in Cresylic Acid Distillate .'............ ............................ ` 8 9 10 11 12 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 ahd determine the applicability of regulatory imitations prior to use. For a specific hazard statement, see Section 7 and Note 1. 2. Referenced Documents 2.1 ASTM Standards: D 95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation2,3 D850 Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials3 D 1193 Specification for Reagent Water4 D 1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)2 D 3852 Practice for Sampling and Handling Phenol and Cresylic Acid3 E 1 Specification for ASTM Thermometers5 6 2.2 Other Documentsf OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200. 3. Terminology 3.1 Description of Term Specific to This Standard, * These test methods are under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals, and are the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved April 28, 1989. Published June 1989. Originally published as D 3439-75 T. Last previous edition D 3439-78 (I983)el. 2 Annua/ Book ofASTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vols 14.03 and 05.03. 6 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 3.1.1 cresylic acid--any mixture of phenol alkyl-substituted, monohydric phenols, and litnited nolic constituents where normal boiling points are 23 less. 4. Summary of Test Methods < 4.1 The assay of cresylic acid is obtained by deducting (fy sum of the amounts of- individual impurities from amount of crude cresylic acid in the sataple. 1 4.2 The impurities normally present in crude cresylic aiS include water, neutral oil, sulfiir compounds, and residue. 5. Significance and Use 5.1 Alkaline cresylate solutions are produced as a hy; product of petroleum refining. This standard is used bj? producers and consumers to determine the cresylic aci> content of these solutions as a matter of commerce. 6. Purity of Reagents 6.1 Purity ofReagents--Reagent grade chemicals shnll I used in all tests. Unless otherwise indicated, it is intende that all reagents shall conform to the specifications of 1 Committee on Analytical Reagents of the American Chen^fg ical Society, where such specifications are available.7 Oth^* grades may be used provided it is first ascertained that 1 reagent is of sufficiently high purity to permit its use withouCj 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 j conforming to Type III of Specification D 1193. 7. Hazards 7.1 Consult current OSHA regulations and supplier's^ Material Safety Data Sheets for all materials used in this test-} method. 8. Crude Cresylic Acid, Cylinder Method 8.1 Summary of Test Method--This test method is used for determining the amount of crude cresylic acid in a; sample and for the recovery of adequate sample quantity for subsequent impurity analyses. A measured sample quantity is neutralized with sulfuric acid solution and allowed to cool and settle. The organic phase is then separated and the quantity of crude cresylic acid is measured. 8.2 Apparatus: 7 "Reagent Chemicals, American Chemical Society Specifical ... 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." DUP050296234 D 3439 1 Beakers, 2000 and 3000-mL capacity, with approsiphon tube. 2 Graduated Cylinders, calibrated "to contain" 500 000-mL graduated sections. .3 pH Meter, with glass electrode and calomel referClectrode. "4 Separatory Funnel, 500-mL capacity. ' Reagents: ,1 Sodium Hydroxide Solution, (NaOH) 20 weight %. ,2 Sulfuric Acid (H2S04), 50 weight %. Procedure: `1 Accurately measure an appropriate volume of repre've spedmen (at 60F) (15.6C) to ultimately recover 400 mL of organic phase. Normally, a lOQO-mL en is adequate. Transfer the specimen to a 2000 or ` mL beaker and, using an appropriate mixer, neutralize iilly with H2S04. TE 1: Precaution--Use extreme care; protect the face with a safety or goggles. tt 2--It has been found that large errors will result from ,uate mixing in the neutralization step. A high-shear, propeller jr has been found to be most reliable for completing neutralization it 2 to 3 min after the addition of H2S04. If a magnetic mixer is , a 3-in. stirring bar running at maximum (coupled) speed will pally complete the neutralization within 10 to 15 min after addition, plete neutralization can be verified by allowing the mixed phases to withdrawing a 1-mL specimen of organic phase mixing die men with 1 to 2 mL of distilled'water in a small test tube, shaking rously, and measuring pH with pH-indicator paper. Neutralization nplete when the results ofthis test are substantially neutral (pH 6 to 4.2If necessary, adjust the pH of the mixture to 6.5 to with NaOH solution. Allow it to cool and stratify, sfer quantitatively the organic phase to a large aratory funnel and allow it to settle at least 6 h (Note 3). !t: collects, drain the aqueous phase from the bottom ionally. TE 3--When a stabilized emulsion is formed or when solid rial is present in the neutralized mixture, it is required that the acid be vacuum filtered prior to measurement of percent wet : acid. This is readily accomplished by transferring the crude acid to `separatory funnel through a Buchner funnel, under vacuum, using -ratory funnel as the filtrate receiver. The use ofan appropriately glass fiber filter disk8 as the filtration medium is recommended, ^ugh conventional filter paper can be used. Quantitative transfer is ed by washing the filter with a small portion of the aqueous phase ' Iting from neutralization. It is convenient to remove most of the cus phase by means of a siphon tube prior to filtration in order to imize the volume to be filtered. . .4.3 After the aqueous phase has been completely scav1 from the separatory funnel, transfer the organic phase . a graduated cylinder of appropriate size. Accurately easure the volume of organic phase at 60F (15.6C) and ort the volume ratio oforganic phase to original specimen volume percent of crude cresylic acid (cylinder method), "tain the organic phase for Impurity testing. Water Content of Crude Cresylic Acid 9.1 Determine the water content of the crude cresylic acid the procedure outlined in Test Method D95. The 8 A Whatman GF/A filter disk available from Whatman, Inc., 9 Bridewell ce, Clifton, NJ 07014, or equivalent, has been found suitable for this purpose. determination is performed on a representative specimen of the organic phase from the crude cresylic acid determination by the cylinder method (Section 8). The water content of the crude cresylic acid phase is normally in the range from 3 to 12 volume %. Consequently, with a sample trap of 10-mL capacity, a specimen size of 50 to 100 mL is normally adequate. No t e 4--In many repetitive applications of this test method on similar samples, it may be found that the water content of the crude cresylic acid will show little variation from sample to sample. It may be permissible in these instances to use a standardized, agreed-upon value for the water content. 10. Cresylic Acid Distillate Content of Crude Cresylic Acid 10.1 Summary of Test Method--A representative spec imen of the crude cresylic acid is subjected to distillation at atmospheric pressure. The distillation is terminated at a specified vapor temperature and the portion of the specimen distilling over is reported as distillate. 10.2 Apparatus--The distillation thermometer to be used is ASTM Thermometer 111C which covers the range from 170 to 250C with 0.2C graduations as prescribed in Specification E 1. 10.3 Procedure--Perform the distillation in accordance with the procedure outlined in Test Method D 850 with appropriate modifications: 10.3.1 Record the temperature of the 100-mL specimen to be distilled so that the distillate can be adjusted to the same temperature for volume measurement 10.3.2 Terminate the distillation when the vapor temper ature reaches 230C corrected for barometric pressure or upon reaching dryness, whichever occurs first. The correc tion factor shall be 0.60C reduction in thermometer reading for each 10 mm Hg below 760 mm observed atmospheric pressure. The distillation rate is 4 to 5 mL of distillate over per minute. Cut off heat to the distillation flask when the vapor temperature is 230C (corrected for barometric pres-- sure) and immediately direct a stream ofair on to the neck of the distillation flask at the juncture of the sidearm and the neck. .. 10.3.3 Accurately measure the volume ofthe distillate at the same temperature as the 100-mL original specimen and report the volume ratio of the distillate to the original crude cresylic acid charged as volume percent of cresylic acid distillate. Retain the distillate for impurity analyses for neutral oil and sulfur. 11. Sulfur Compounds in Cresylic Acid Distillate 11.1 Determine the sulfur content of the cresylic acid distillate on a representative specimen of the resuspended distillate (Note 5) by the procedure outlined in Test Method D 1552 or an equivalent method. Multiply the sulfur con tent, expressed as weight percent, by an appropr ite factor to convert it to an equivalent volume percent of ulfur com pounds in the cresylic acid distillate. In the absence of an experimentally determined factor, use a value of 4.0 (or some other value agreed to by the purchaser and the seller). A procedure for experimentally determining the appropriate sulfur factor on a specific lot of cresylate stock is given in the Appendix XL 673 DUP0502 96235 #) D 3439 Wa No t e 5--At times it is practical to preheat the distillate and resuspend the entire mixture prior to obtaining representative specimens for sulfur and neutral oil analyses. 12. Neutral Oil in Cresylic Acid Distillate 12.1 Summary of Test Method--This test method is used to determine the neutral oil content of the cresylic acid distillate. For purposes of this test, neutral oil is defined as the organic phase resulting from mixing the specimen with an excess of NaOH solution in accordance with 12.4, with appropriate corrections made for the sulfur contained in this organic phase. 12.2 Apparatus: 12.2.1 Centrifuge Bottles,9 50-mL with 1,6-mL graduated neck. 12.2.2 Centrifuge Bottles,10 50-mL, with 5-mL graduated neck. 12.2.3 Centrifuge, capable of accommodating and whirling the centrifuge bottles at a speed which can be controlled to give a relative centrifugal force of between 500 and 800 at the bottom of the bottles. A speed of 1500 r/min and diameter of swing of 20 in. will satisfy this condition according to the following equation: R -- 265 -Jffd where: R -- revolutions per minute, / =,relative centrifugal force, and d = diameter of swing measured between bottoms of oppo site bottles when in rotating position, in. . 12.3 Reagent---Sodium hydroxide solution, (NaOH) 20 weight %. 12.4 Procedure: 12.4.1 Measure by means of a pipet an appropriate representative specimen of the resuspended cresylic acid distillate into a centrifuge bottle (Note 6). A specimen size of 10 mL is normally, appropriate. Add approximately 35 mL of NaOH solution in aliquots and mix thoroughly. Fill the centrifuge bottle to a level near the top of the graduated portion, using additional NaOH solution. No t e 6--The sulfonation bottle is used when the distillate has a high neutral oil content. 12.4.2 Place the bottle and contents in the centrifuge and spin at 1500 r/min for 15 min. Remove and read the volume of organic phase to the nearest division (Note 7). Report the ratio of organic phase volume to original sample volume as volume percent of neutral oil. 9 Kimble 1000C Milk Test Bottle, Babcock 6M-in. overall height, 18 g, graduated to 8 % in 0.1 % subdivisions, available from Fisher Scientific, Corporate Headquarters. 711 Forbes Ave,, Pittsburgh, PA 15219, or an equivalent, has been found satisfactory for this purpose. Kimble 2085-50 Cream Test Bottle, Babcock 6V:'-in. overall height, gradu ated to 50 % in 0.5 % subdivisions, available from Fisher Scientific, or an equivalent, has been found satisfactory for this purpose. No t e 7--In instances where emulsions are formed, jt is-M warm the contents of the centrifuge bottle with hot water ocdi bath for 3 to 5 min prior to. centrifugation. In the event that"1TM phase is present in the zone between the aqueous and after centrifugation, the neutral oil is read as the volume of'i phase, excluding the emulsion layer. : || 12.4.3 Since the above organic phase may include significant quantities of sulfur compoulf have been already accounted for in Section accurate to perform a correction and express'if content on a sulfur compound-free basis. This plished by determining the sulfur content of a sp the neutral oil, multiplying the sulfur content by i priate factor (normally a value of 4.0), and deerTM neutral oil content by this allowance for sulfur comp N (corrected) = [JV (uncorrected)] [1 - (weight fraction sulfur in neutral oiljj 13. Calculation 13.1 Calculate the volume percent cresylic acid ' A, of the crude cresylic acid mixture or alkaline cri solution as folIows (Note 8): tv s .+ An r i 4 = [q 1.00 "D 100 J [looj where: ' -vs C = crude cresylic abid content; as determined by cyjj| method, volume % W = water content of crude cresylic acid, volume %,". D = distillate content (to 230C), volume %, S = Sulfur compounds in cresylic acid distillate, vclun and, N -- neutral oil content in cresylic aciii distillate, vohj No t e 8--The volume basis to- be used is a- standard 60*F volume basis on both the specimen and the cresylic acid. If,aj| performed on a specimen at some other temperature, then the-s priate specific gravity, corrections are made to adjust results toi (15.6*0) volume basis. 14. Precision and Bias . 14.1 Precision data have not been fully established controlled conditions. From cooperative tests conducts date, the following criteria should be used for judging! acceptability of results: 14.2 Repeatability---The standard deviation of n (each the average of duplicates) obtained by the same anpl on different days, has been estimated to be 0.44 volume " 26 df. Two such values should be considered suspect (9! confidence level) if they differ by more than 1.3 volume 14.3 Reproducibility--The standard deviation of fesi (each the average of duplicates) obtained by analysts different laboratories, has been estimated to be L05' volume % at 80F (26.7C). Two such values should be' considered suspect (95 % confidence level) if they differ by more than 3.5. -y 674 DUP050296236 APPENDIX (Nonmandatory Information) XI. DETERMINING THE APPROPRIATE "SULFUR FACTOR" Explanatory Remarks '1.1.1 In analyzing cresylate solutions of petroleum orthe most prominent impiirity consists of sulfur comds. The predominate form ofthese sulfur compounds is omatic thiophenols. The homolog distribution of the oris substituted thiols is normally a consistent distribun ratio, fixed by thermodynamic equilibrium relation- 1.1.2 "Sulfur Factor" is the numerical value used to vert sulfur content in weight percent to volume percent compounds. It has been found,- from analysis of yiate streams of diverse origin, that the appropriate iir factors" are remarkably consistent within the range of u6s 3.7 to 4.1. .2 Summary of Test Method [X 1.2.1 The procedure used for determining the appro ve "sulfur factor" for a given stock is based upon, the fact t the aromatic thiols are easily oxidized to their corre- ding disulfides. This oxidation is readily affected by air n the thiols are present as their corresponding base salts an alkaline solution. .3 Procedure XI .3.1 Take up an appropriate specimen of criide cresylic 'd (normally 75 to 100 mL) into 300 mL of 20 % NaOH , ution. Then denude the alkaline cresylate solution of any tral oil by extraction with petroleum ether (3 to 100-mL rtions) and strip out the remaining petroleum ether with a nitrogen stream. . XI.3.2 Place the solution in a large, high-speed blender provided with a gentle air purge and with a provision for maintaining a temperature of 130 10F (54.4 5.5C). Turn on the blender, air, and temperature control. Monitor the thiol concentration by periodic specimen withdrawal and electrometric titration with 0.0050 N silver nitrate solution. The solvent used is 4 % ammoniacal caustic and file electrodes silver-silver sulfide and glass as reference. When the thiol concentration has diminished to less than 1/100th of its initial value, cease the oxidation and transfer the blender contents to a suitable separatory funnel. X 1.3.3 After the contents of the separatory funnel are allowed to settle, recover the organic disulfide phase. It is sometimes necessary to introduce 10.to 20 mL of diethyl ether to effect a clean separation, in which case the ether must be evaporated on a steam bath with a vacuum. XI.3.4 Determine the density of the recovered (and solvent-free) disulfide phase at 60F (15.6C) in a micro pycnometer. X 1.3.5 Determine the sulfur content (in weight percent) of the recovered disulfide phase by a suitable combustion method. X1.4 Calculation XI .4,1 From the sulfur content of the disulfide phase, the average molecular weight of the mixture of thiols from which the disulfides were formed may be readily calculated. XI.4.2 'With appropriate specific gravity corrections al lowing for the fact that the sulfur compounds are present in the thiol state (that is, using specific gravities corresponding to the appropriate thiols), calculate the "sulfur factor." The American Society for Testing and'Materiais (sites no position respecting the validity of any patent rights asserted in connectionwith any Item mentioned in this standard. Users of this standard are expressly advised thatdetermination of the validity of any such patent rights, and the nsk of infringement of such rights, are entlrelynhelrov/n responsibility. This standard Is sub]ect to revision at any time by theiespShsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. tPOr cekrhBnts'ara InitteSdeittier tor revision ofthis Stamfordor.for additionalstandards and should be addressee to ASTM Headquarters. You? comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you teel 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. DUP050296237 Designation: D 3504 - 91 Standard Specification for Maleic Anhydride1 This standard is issued under the fixed designation D 3504; 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 specification covers maleic anhydride. 1.2 Consult, current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this specification. D3438 Practice for Sampling and Handling Naph Maleic Anhydride, and Phthalic Anhydride2 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.10(j 1910.12003 2. Referenced Documents 2.1 ASTM Standards: D1493 Test Method for Solidification Point of Industrial Organic Chemicals2 D3366 Test Method for Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobalt Scale)2 3. Properties 3.1 Maleic anhydride shall conform to the folio requirements: ^ Property Solidification point, min, C Molten color, max Molten color after heating, max ASTM| Methg D14| D 33 D33M 4. Sampling 4,1 This material shall be sampled in accordance Practice D 3438. 1 This specification is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved Oct. 15,1991. Published December 1991. Originally published as D 3504 - 76. Last previous edition D 3504 - 87. 2 Annual Book ofASTM Standards, Vol 06.03. 5. Keywords 5.1 color; maleic anhydride; solidification point 3 Available from Superintendent of Documents, U.S. Government 1 Office, Washington, DC 20402. The American Society for Testing and Materials takes ho position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard ere expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committeeand must be reviewed every five years and ifnot 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. 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. 676 DUP050296238 Designation: D 3505 - 91 Standard Test Method for Density or Relative Density of Pure Liquid Chemicals1 This standard is issued under the fixed designation D 3505; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the.DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. scope This test method describes a simplified procedure for leasurement of density or relative density ofpure liquid icals for which accurate temperature expansion fiincare known. It is restricted to liquids having Vapor res not exceeding 600 mm Hg (0.8 atm) at the ibration temperature, and having viscosities not exg 15 cSt at 20C (60F). . Means are provided for reporting results in the folig units: insity g/cm3 at 20C :nsity g/ml at 20C ielative density 20C/4C dative density 60T/60T (15.56C/15.56C) Ipmmercial density, lb (in air)/U.S. gal at 60F Jommercial density, lb (in air)/U.K. gal at 60F. E I--This test method is based on the old definition of 1 L -- dm3 (1 ml = 1.000028 cm3). In 1964 the General Conference eights and Measures withdrew this definition of the litre and Ired that the word "litre" was a special name for the cubic thus making 1 mL = 1 cm3 exactly. 2--An alternative method for determining relative density of liquid chemicals is Test Method D 4052. 3 This standard does not purport to address the safety Jems, if any, associated with its use. It is the responsi- of whoever uses this standard to consult and establish opriate safety and health practices and determine the 'icability of regulatory limitations prior to use. Specific d statements are given in 7.1. Referenced Documents |1 ASTM Standards: 1193 Specification for Reagent.Water2 * 1555 Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons3 > 3437 Practice for Sampling and Handling Liquid Cyclic Products3 >4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter4 1 Specification of ASTM Thermometers5 H;This test method is under the jurisdiction of ASTM Committee D-I6 on natic Hydrocarbons and Related Chemicals and Is the direct responsibility of |pmmhtee D16.0E on Instrumental Analysis, urrent edition approved May 15, 1991. Published July 1991. Originally jished as D 3505 - 76. Last previous edition D 3505 - 84". Wfinnual Book ofASTM Standards, Vols 06.03 and 11.01. ^Annual Book ofASTM Standards, Vol 06.03. ^Annual Book ofASTM Standards, Vol 05.03. ^Annual Book ofASTM Standards, Vols 05.03 and 14.03. E 12 Definitions of Terms Relating to Density and Spe cific Gravity of Solids, Liquids, and Gases6 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12007 3. Terminology 3.1 Definitions: 3.1.1 density--the mass of material per unit volume at a given temperature called the "reference temperature." Weight corrected to a standard acceleration of gravity and corrected for the buoyant effect of air is used to measure mass. This method specifies the use of a beam balance to determine weight so that no correction for variation in acceleration of gravity is necessary. When a torsion or spring balance is used, such correction must be applied. 3.1.2 relative density--the ratio of the density of the material at reference temperature "t" to the density of pure water, in consistent units, at reference temperature t2. It is common practice to use reference temperature ^ equal to t2. 3.1.2.1 Since the mass of water at 4"C is very close to 1 g/mL or 1 g/cm3, it is common practice to set the reference temperature t2 for water at 4C. When this is done and the density of the material is given in grams per millilitre, or grams per cubic centimetre, the value of density is very nearly identical to the value for relative density. Thus, density at 20C in g/cm3 or g/mL, is nearly identical with relative density 20C/4C. -- 3.1.3 commercial.^density--weight per unit volume without correcting for the buoyant effect of air and is limited in this document to pounds (in air) per U.S. gallon at 60F, or pounds in air per U.K. gallon at 60F. This is the density most commonly used in commercial transactions in the petroleum and coal chemicals industry in the United States and Canada. 3.2 The definitions included in Definitions E 12 are applicable to this test method. 4. Summary of Test Method No t e .3--See Appendix for details on the method and derivation of formulas. 4.1 For materials listed in Table 1 the sample is drawn into a weighed and calibrated bicapillary pycnometer. The filler pycnometer is allowed to come to equilibrium at any 6 Annual Book ofASTM Standards, Vols 04.02 and 15.05. 7 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 677 DUP050296239 # D 3505 TABLE 1, PART I 20 C Reference Temperature Multiplier, F20, for use in Computing Density, 12.1 CHOOSE A MULTIPLIER f o r t h e ma t e r ia l b e in g me a s u r e o PYCNOMETER EQUILIBRATED. TEMP MIXED DEGC BENZENE TOLUENE XYLENES 0XYLENE M- xyl ene Px y l e n e STYKENE CYCLO HEXANE 10.0 10.2 10 4 10.6 10*8 0.98822 0.98845 0.98868 0.96691 0.96914 0.98941 0.98962 0.93983 0.99003 0.99024 0.9902a 0.99047 0.99066 0.99085 0.99104 0.99052 0.99070 0.99089 0.99107 0.99126 0.99028 0.99047 0.99066 0.99085 0.99104 0.99011 0.99030 0.99049 0.99069 0.99088 0.99029 0.99048 0.99066 0.99085 0.99104 0.98912 0.98933 0.96953 0.98973 0.96993 11.0 11.2 11.4 11.6 11.8 0.9893T 0.96960 0.98982 0.99005 0.99028 0.99045 0.99066 0.99086 0.99107 0.99128 0.99123 0.99142 0.99161 0.99179 0.99198 0.99144 0.99163 0.99181 0.99200 0.99218 0.99123 0.99142 0.99161 0.99179 0.99198 0.99107 0.99126 0.991*6 0.99165 0*99184 0.99123 0.99142 0.99161 0.99180 0.99199 0.99013 0.99034 0.99054 0.99075 0.99095 12.0 12.2 12.4 12.6 12.8 0.99051 0.99074 0.99097 0.99120 0.99144 0.99143 0.991o9 0.99190 0,99211 0.99231 0.99217 0.99236 0.99255 0.99274 0.99293 0.99237 0.99255 0.99274 0.99292 0.99311 0,99217 0.99236 0.99253 0.99274 0.99293 0.99204 0.99223 0.99242 0.99262 0.99281 0.99218 0.99237 0.99256 0.99275 0.99294 0.99116 0.99136 0.99157 0.99178 0.99199 13.0 13.2 13.4 13.6 13.8 0.99167 0.99190 0.99213 0.99236 0.99259 0.99252 0.99312 0.99273 0.99331 0.99294 "0.99350 0.99315 0.99369 0.99335 0.99389 0.99329 0.99348 0,99367 0.99385 0.99404 0.99312 0.99331 0.99350 0.99369 0.99389 0.99300 0.99320 0.99339 ' 0.99358 0.99376 0.99313. 0.99332 0.99351 0.99370 0.99390 0.99220 0.99240 0.99261 0.99232 0,99303 14.0 14.2 14.4' 14.6 14.6 0.99282 0,99305 0.99329 0.99352 0.99375 0.99356 0.99408 0.99422 0.99408 0.99397 6.99409 0.99377 0.99427 0.99441 0.99427 0.99417 0.99428 0.99398 0.99446 0.99460 0.99446 0.99436 0.99447 0*99419 0.99465 0.99478 0.99465 0.99456 0.99466 0.99440 0.99484 _0.9949_7__0.99484___0r99475_ _0.9948S_ 0.99325 0.99346 0.95JN7 0.99363 0.994i0 15.0 15.2 15.4 IS.6 15.8 0 * 99398 0.99421 0.99445 0.99466 0.99491 0.99461 0.99461 0.99502 0.99523 0.99544 0.99503 0.99522 0.99541 0.99561 0.99580 0.99516 0.99534 0.99553 0.99572 0.99590 0.99503 0.99522 0.99541 0.99561 0.99580 0.99495 0.99514 0*99534 0.99553 0.99573 0.99504 0.99523 0.99542 0.99562 0.99581 0.99431 0.99452 0.99474 0.99496 0.99517 16.0 16.2 16.4 16.6 16.8 0.99515 0.99538 0.99561 0.99585 0.99608 0.99565 0.99586 0.99607 0.99628 0.99649 0.99599 0.99618 0.99637 0.99657 0.99676 0.99609 0.99628 0.99646 0.99665 0.99684 0.99599 0.99618 0.99637 0.99657 0.99676 0.99592 0.99612 0.99631 0.99651 0.99670 0.99600 0.99619 0.99638 0.99658 0.99677 0.99539 0.99561 0.99582 0.99604 0.99626 17.0 17.2 17.4 17.6 17.8 0.99632 0.99655 "0`. 99679" 0.99702 0.9972,6 0.99670 0.99691 O'. 99712 0.99733 0.99754 0.99695 0.99714 0799734 0.99753 0.99772 0.99703 0.99721 0.99740 0.99759 0.99778 0.99695 0.99714 0.99734 0.99753 0.99772 0.99690 0.99710 0.99729 0.99749 0.99768 0.99696 0.99715 0.99734 0.99754 0.99773 0199648 0.99670 0.99692 0.99715 0.99737 18.0 18.2 18.4 18.6 18.8 0.99749 0.99773 0.99796 0.99820 0.99843 0.99775 0.99796 0.99817 0.99838 0.99859 0.99791 0.99811 0.99830 0.99849 0.99669 0.99797' 0.99815 07 99834 0.99853 0.99672 0.99791 0.99011 0.99830 0.99849 0.99869 0.99788 0.99808 0.99827 0.99847 0.99867 0.99792 0.99811 0.99831 0.99850 0.99869 0.99769 0,99761 0*99804 0*99626 0*99849 19.0 19.2 19.4 19.6 19.6 0.99867 0.99890 0.99914 0.99938 0.99961 0.99860 0.99901 0.99S22 0*99943 0.99964 0.99888 0.99907 0.99927 0.99946 0.99966 0.99891 0.49910 0.99926 0*99947 0,99966 0.99888 0.99907 0.99927 0.99946 0.99966 0.99886 0.99906 0.49926 0.99946 0.99965 0.99886 0.99903 0.99927 0.99946 0.99966 0.9n 871 0.9989* 0.99317 0.99939 0.99962 20.0 0.99985 0.99985 0.99985 0.99965 0.99985 0.99985 0.99985 0.99965 DUP050296240 9 D 3505 TABLE 1, PART I Continued CHOOSE A MULTIPLIER FOR THE MATERIAL BEING MEASURED CORRESPONDING TO THE BATH TEMPERATURE AT WHICH THE p y c n o me t e r e q u il ib r a t e d . TEMP MIXED DEGC eENZENE TOLUENE XYLENES 0XYLENE MXYLENE PXYLENE s t y r e n e CYCLOHEXANE 20,0 20.2 20.A 20.6 20*6 0.99985 1.00009 1.00032 1.00056 1.00080 0.99985 1 .00006 1.00027 1.00048 1.00069 0.99985 1.00004 1.00024 1.00043 1.00063 0.99985 1,00004 1.00023 1.00042 1.00061 0.99985 1.00004 1.00024 1.0G043 1.00063 0.99985 1.00005 1.00025 1.00044 1.00064 0.99985 1.00004 1.00024 1.00043 1.00062 0.99985 l.OOOCA 1.00031 1.00054 1.00077 ' 21.0 21.2 21.4 21.6 21.8 1.00104 1.00128 1.00151 1.00175 1.00199 1.00091 1.00112 1.00133 1.00154 1.00175 1.00082 1.00102 1.00121 l.OOUl 1.00160 1.00080 1.00099 1.00118 1.00137 1.00156 1.00082 i 0.0102 1.00121 1.00141 1.00160 1 *00084 1 .00104 1.00124 1.00143 1.00163 1.00082 1.00101 1.00121 1.00140 1.00159 1.00100 1.00124 1.00147 1.00170 1.00194 22.0 22.2 22.A 22.6 22.8 1.00223 1.00247 1.00271 1.00295 1.00319 1.00196 1.00218 1*00239 1.00260 1.00281 1.00180 1.00199 i.00219 1.00238 1.00258 1.00175 1.00194 1.00213 1.00232 1.0 0251 1.00180 1.00199 1.00219 1.00238 1.00258 1.00183 1.00203 1.00223 1.00243 1.00263 1.00179 1.00198 1.00216 2.00237 1.00257 1.00217 1.00241 i0 0264 1.00268 1.0(1312 23.0 23.2 23.A 23.6 23.8 1.00342 1.00366 1.00390 1.00414 1.00438 1 .003,02 1.00324 1 .00345 1.00366 1.00387 1.00278 1.00297 1.00317 1.00336 1.00356 1.00270 1.00289 1.00308 1.00327 1.00346 1.00278 1.00297 1.00317 1.00336 1.00356 1*002.83 1.00303 1.00322 1.00342 1.00362 1.00276 1.00296 1.00315 1.00335 1.00354 1*00336 1.00360 1.00383 1.00*06 1. 00*32 2A.0 2A.2 2A , A 24*6 24.8 1.00462 1.00487 1.00511 1.00535 1.00559 1 004oV 1.00430 1.00451 1.00473 1.00494 1.00376 1.00395 1.00*15 1.00435 1.00454 1.00365 1.00384 1.00403 1.00422 1.00442 1.00376 1.00395 1.00415 1.00435 1.00454 1.00382 1.00402 1.0042? 1.00442 1.00462 1.00374 1.00393 1.00413 1.00432 1.00452 1.00456 1.00450 1.00604 1.00529 100553 25.0 25.2 25.4 25.6 25.8 1 *.00383 1.00607 1.00631 1.00656 1.00680 1.00615 1.00537 1.00b58 1.00579 1.00601 1.0047a 1.00461 1.00474 1.00482 1 .0Q471 1.00494 1.00480 1.00494 1.00502 1.00491 1.00514 ~1.00459"TTOFSTa -T. 50522" ~r.oo5ii 1.00533 1.00518 1.00533 1.00542 1.00530 1.00553 1.00537 1.00553 1.00563 1.00550 1.00677 1.00602 1.00627 1.00651 1.00676 26.0 1.00704 1.00622 26.2 1.00728 1.00b43 26.4 T.OUTssr" 1.00665 26.6 1.00777 1.0 0686' 26.8 1.00801 1.00707. 1.00573 1.00557 1.00573 1.00583 1.00593 1.00576 L.00593 1.00603 1.00512 ~l'.ODW~mn56T2~ T.006'23 1.00632 1.00614 1.00632 1.00643 1.00652 1.00634 1.00652 1.00663 1.00569 1.00589 T77T06U9 1.00626 1.00648 1.00701 1,00726 1 0075i l,0077o 1.00601----- 27.0 27.2 27.4 27.6 27.8 1.00825 1.00850 1.W874 1.00899 1.00923' 1.00729 1.00750 i .tnrnr 1 .00793 1.00815 1.00672 1.00692 1.00711 1.00731 T.00751 1.00653 1.00672 1.09691 1.00711 1.00730 1.00672 1.00692 1.00711 1.00731 1.00751 1.0(1683 1.00703 1.00724 1.00744 1.00764 1.00667 1.00667 1.00707 1.00726 1.00746 1.00826 1.00851 1 00878 1.00902 1.00927 ~` 28.0 28.2 1874 28.6 28.8 1.00947 1.00972 7.00996 1.01021 1.01045 1.00836 1.00858 '1.0 08T9 1.00901 1.00922 1.00771 1.00791 1.00811 1.00831 1.00851 1.00749 1.00769 T. 00788 1.00807 1.00827 1.00771 1.00791 1.00811 1.00831 1.00851 1.0.0784 1.00804 1.00825 1.00845 1.00865 1.00766 1.00766 1.00805 1.00825 1.00845 1.00953 1.00976 1.0102 V 1.01055 29.6 29.2 IV. 4" 29.6 29.8 1.01070 1.00944 1.01094 1.0Q9t>5 1.01119 " i .00967 1.0)143 1*01006 1.01168 1.1/1030 1.00871 1.00646 1.00891 1.00866 i.ob9lV "TVO'OBbS 1.00931 1.00904 1.00951 1.00924 1.00871 1.00891 r.ooQir 1.00931 1.00951 1.00885 1.00906 V.0 092b " 1.00946 1.00966 1.00864 1.00864 1.0096a 1.00924 1.009*4 woio*: l.Olli7 1.0 1 l .5 7 1.0115-KOjJ*5 30.0 1.01192 1.01051 1.00971 1.00943 1.00971 1.00987 1.00963 1.01211 679 DUP050296241 TEMP MIXED OESC BENZENE TOLUENE XYLENES 0- MXVLENE `XYLENE h ^- xyl ene st yr ene CYCLO^**HEX4NE 10.0 10.3 10.4 10.6 10.8 0.99341 0.99364 0.99387 0.99410 0.99433 0.99405 0.994*6 0.99446 0.99467 0.99488 0.99454 0,99473 0.99492 0.99511 0.99530 0 ,99467 0.99485 0.99504 0,99523 0.99541 0 099454 0.99473 0.99492 0.99511 0.99530 0.99444 0 .`99464 0.994*3 0,99602 0199522 0.99454 0.99473 0.99492 0.99511 0.99530 0.96403 0.99*?4 0,99444 0,99464 0.99435 11.0 11.3 11.4 11.6 11.8 0.99456 0.99479 0.99502 0.99525 0.99546 0.99509 0.99530 0.99550 0.99571 0.99592 0,99549 0.99568 0.99587 0.99606 0.99625 Q..99S60 0.99S78 0.99597 0.99615 0.99634 0.99549 0.99568 0.99587 0.99606 0.99625 0.99541 0.99560 0.99580 0.99599 0.996 T9 0,99549 0.99568 0.99587 0.99606 0.99625 0.99505 0.99525 0.99546 0.99557 0.99567 12.0 12.2 12.4 12.6 12.8 0.99571 0.99594 0.99617 0.996*0 0.99664 0.99613 0.99634 0.99655 0.99675 0.99696 0.99644 0.99663 0.-99682 0.99701 0.99721 0.99653 0.99671 0.99690 0.99708 0.99727 0.99644 0.99663 0.99682 0.99701 0.99721 0.99638 0.99657 0.99677 0.9969b 0.99716 0 ,*39644 0..99663 0.99662 0.99.701 0.99721 0.99606 C.99o29 0.99649 0.99670 0.99691 13.0 13.2 13.4 13.6 _____ 13.8_ 0.99687 0.99710 0.99733 0.99756 0.99760 0.99717 0.99740 0.99738 0.99759 0.99759 6,*997*78 0.99760 0.99797 0 .2980.1 _ _0_.9981b_ 0.99746 0.99764 6.99783 0.99802 0.99820 0.99740 0.99759 0.99778 0.99797 0,99816 0.99735 0,99755 0.99774 0.99794 0.99813 0.99740 0.99759 0.99778 U.99797 0.9981b 0,99712 0.9**733 0,9 c 7't 4 0,9977b 0.9079': 14.0 14.2 14.4 14*6 __ .3.4,0 0.99803 0.99826 0.99350 0.99873 0,99896 0.99822 0.99843 0,99563 0.998b * 0_._9990S 0.99835 0.8985* 0.98fc7* 0.99B93 0.99912 0.99839 0.99858 0.99876 0.99895 0.99914 0.99335 0.99854 0.99874 0.99893 0.99912 0.998.33 0.99852 0.99872 0.99891 0.99911 0.99635 0.99855 0.99874 0.99893 0.99912 0.9*618 0.9c39 0.9*832 0.99V :.-3 15.0 15.2 154 15.6 15.8 0 *99920 0,99943 0.99966 0.99990 1.00013 0.99926 0.99947 0.99968 0.99909 1.00010 0.99931 0.99933 0.99950 0.99951 0.99970 ~0T999TO~ 0.99989 0.99989 1,00008 1.00006 0.99931 0.99950 0.99970 0.99989 1.00008 0.99930 0.99950 0.99969 0.99989 1.00009 0.99931 0.99950 0.999*70" 0.99989 1.00008 0.99925 0.99946 0.99968 0.99989 1.00011 16.0 16.2 16 4 16,6 16.6 1.00037 1.00060 1.60084 1,00107 1.00131 1.00031 1,00027. 1.00026 1.00052 1.. 00047 1.00045 1.00073 --1700066 ~TT0 0 064 i.00094 1.00065 1.00083 1.00115 1.00105 1.00102 1.00027 1,00047 1.00066 1.00085 1.00105 1.00028 1.00048 1.00.067 1.00087 1.00107 1.00027: 1.00047 1.00066 1.00085 1.00105 1.00033 1.00055 1.00077 1.00099 2.00221 [` 17.0 1.00154 1.00136 1.00124 1.00120 1.00124. _1.00126 1.00124 1.00143 {: 17.2 1.0017a 1.00158 1.00143 1.00139 1.00143 1.00146 1.00143 1.00165 17*4 1.00201 1,00179 1.00163 1.00158 1.00183 1.00166 1,00162 1.00187 17.6 1*00225 1.00200 1.00162 1.C0177 1.00162 1.00286 1.00182 1.00210 17.8 1.00249 1.0022.1 1.00201 1.0019b 1.00201 2.00205 1.00201 1.00232 18.0 18.2 18.4 18.6 18.8 1.00272 1.00296 1.00319 1.00343 1.00367 1.00242 1.00263 1.00284 1.00305 1.00326 1.00221 1.00240 1.00259 1.00279 1.00298 1.00215 1.00234 J.00252 1.00271 1.00290 1.00221 1.00240 1.00259 1.00279 1.00298 1.00225 1.00245 1.00264 1.00284 1.00304 1.08220 1.00240 1.00259 1.00278 1.00298 1.00254 1.00277 1.00299 1.00322 1.00344 19,0 1 .00391 1.00346 1.00318 1.00309 1.00318 1.00324 1.00317 1.00367 19.2 1.00414 1.00369 1.00337 1.00328 1.00337 1.00344 1.00337 1.00390 19.4 1 .00430 1.00390 1.00357" 1.0 034 7 1.00357 1.00363 *"i".*0*0356 1 . 0 0 * i 3 i 96 1.00462 1.06411 1.00376 1.00366 1.00376 2.00383 X.00375 1.00435 j 19.8 1.00486 1.00432 1.00396 1.00385 1.00396 1.00403 i.003ys 1.00453 i 20,0 1 ,0 0809 1.00453 1.00415 1,00404 1.00415 1.00423 1.00414 1.004 til 680 I DUP050296242 # D 3505 TABLE 1, PART II Continued CHOOSE A MULTIPLIER FOR THE MATERIAL BEING MEASURED COKRESPONDIN6 TO THE BATH TEMPERATURE A T WHICH THE PYCNOMETER EQUILIBRATED. - TEMP MIXED DE6C BENZENE TOLUENE x y l e n e s 0- xyl ene MXYLENE Px y l e n e STYPENE CYCLOHEXANE 20.0 20.2 20.4 20.6 20.8 1.00509 1.00533 1.00557 1.00581 1.00605 1*00453 1.00474 )00496 1.00517 1.1)0538 1.00415 1.00435 1*00454 1.00474 1.00493 1.00404 1.00423 l .00442 1.00461 1.00480 1.00415 1.00435 .1.00454 1.00474 1.00493 1*00423 1.00443 1.00463 1.00482 1.00502 1.004U 1.00434 1*00453 1.00472 1.00492 1.004ft) 1.0QSU4 ). 00527 )*0055) 1.00574 21.0 21.2 21.4 21.6 21.8 1.00629 1.00653 X . 00677 1.00701 1.00725 1.00559 1.00581 1*00602 1.00623 1*00644 1.00513 1.00532 1.00552 1.00572 1.00591 1.00499 1.00518 1.00537 1.00556 1.00575 1.00513 1.00532 1.00552 1.00572 1.00591 1.00522 1.00542 1.00562 1.00582 1.00602 1.00511 1.00531 1.00550 1.00570 1.00589 1.00597 1.00621 1* 00644 1.00891 22.0 22.2 22.4 22.6 22.8 1.00749 1.00773 1.00797 1 .00821 1.00845 1.00666 1.00687 1*00708 1.00730 1.00751 1.00611 1.00630 1.00650 1.00670 1.00689 1.00594 1.00613 1.00632 1.00652 1.00671 1.00611 1.00630 1.00650 1.00670 1.00689 1.00622 1.00642 1.00662 1*00682 1.00702 1.00609 1.00628 1.00648 1.00667 1.00687 1.00715 1.00738 1.00762 1.00786 1.00810 23.0 23.2 23.4 23.6 23.8 1.00869 1.00893 1.00917.. 1.00941 1.00965 1.00772 1.00794 1.00815 1.00636 1.00658 1.00709 1.00729 1.00748 1.00768 1.00788 1.00690 1.00709 i6 0728 1.00747 1.00767 1.00709 1.00729 1.0-0748 1.00768, 1.00788 1.00722 1.00742 1.00762 1.00782 1.00802 1*00707 1.00726 1.00746 1.00765 1.00785 1.008)4 1.0085ft 1.00906 1.00930 24.0 24.2 24.4 24.6 24.8 25.0 25.2 25.4 25.6 25.8 1.00990 1.01014 1.01038 1.01062 1.01066 1.01111 1.01135 1.01159 1.01184 1.01206 1.00879 1.00900 1.,00922 1,00943 1.Q096S 1.00986 T. 01007 1 .01029 1 .01050 1.01072 l.00808 1.00627 1.00847 1.00867 1.00867 1.0090b 1*00926 1.00946 1.00966 1*00966 1.0078b 1.00805 U00824 1.00843 1.00863 1.00808 1.00827 . 1*0 034-7 1.00867 1 .00887 1.00882 1.00901 1.oov.gr 1.00940 1.00959 1.00906 1*00926 1*00946 1.00966 1.00986 1.00822 1.00842 1 0 0 ft b2 1.00882 1.00902 1.00805 1.00624 1.00844 1*00863 1.00683 1.00922 1*00943 1.00963 1 .00983 1.01003 1.00903 1.00922 T700942 1.00962 1.00981 1.00954 1.00979 1.01013 1.0102b 1.01052 1.01077 1.02101 1.0 )T26 1.0!151 1.0117o ^ 26.0 26.2 56.4 26.6 26.8 1.01232 1.01257 TTi/1281 1.01305 1.01330 1.01093 1.01115 1 .01X86 ' 1*01158 1.01179 1.01906 1.00978 1.01025 1.00997 1.0X045" imion 1*01065 1.01036 1.01-085 1.01055 1.01006 1.01025 1.01045 1.01065 1*01085 ,1.01023 1.01043 1.01064 1.01084 1.01104 1.01002 1.01201 1.01021 1.02226 irorarr" ).0125i 1.01060 1.01276 1*01050 1.01301 27.0 27.2 27.4 27.6 27.8 1.01354 1.01379 TTTTUirS 1*01438 1.01452 1.0120i 1.01222 1.0T244 1*01265 1.01287 1.01105 1.01125 1.01145 1.01165 1.01185 i.01075 1.01094 1.01113 1.01133 1.01162 1.01105 1.01125 .01145 1.01165 1.01185 1.01124 1.01144 1.01165 1.01185 1.01205 1.01099 1.01 llV 1.01139 1.01159 1.01)78 1.01326 1.01352 1.01377 1.014J2 1.01426 28. 0 28.2 ----------- -2814- 2S.6 28.8 1.01477* 1*01306 1.01205 1.01172 1.01501 1.01330 1.01225 1.01191 1.01526" "rrsrcs 2--h o t t a s -T.01210 1.01551 1.01373 1*01265 1 .01230 101575 1.013V5 1.01285 1.01249 1.01205 1.01225 1.01225 1.01246 1.0T24T- 1.01266 1.01265 1.01286 1.01285 1.01307 1.01196 1.01218 1.01236 1.01258 1.01278 1.01454 1*01479 1.6 Be- 5 1.01531 1.01657 29.0. 1.01600 1.01416 1.01305 1.01269 1.01305 1.01327 1.01297 1.015*3 29.2 1.01624 1.01438 1.01325 1.01288 1.01325 1.01347 1.01317 1.01609 - ~29";v 1 *05649 Io0i'4o0 1.01345 1.01308 l*til34 T.bTTSS 1701537 i0 3 29.6 1.0)674 1*01461 1.013b5 1.01327 1.01365 L .01388 1.01357 l.Oltfel 29.8 1.01699 1.01503 1.01385 1.01347 1.01385 1.01408 1.01377 1 .01637 30.0 1.01723 1.01524 1.01405 1.0)366 1.01405 1*02429 1.01397 1.0171- 681 DUP050296243 D 3505 convenient temperature between 10 and 30C (50 and 86F). The equilibrium temperature is measured to the nearest 0.02C. The weight is determined using a beam balance. The density, relative density, or commercial density at the desired reference temperature is then calculated from the sample weight, a calibration factor proportional to an equal volume of water, and a multiplier which corrects for the buoyancy of air and the change in volume of the pycnometer and the sam ple due to deviation from the chosen reference temperature. 4.2 For liquids not listed in Table 1, the sample is equilibrated at the desired reference temperature, usually 20C or 60T (15.56C), the density, relative density, or commercial density is then calculated from the sample weight, a calibration factor proportional to ah equal volume of water and a term which corrects for the buoyancy of air. In the case of volatile liquids such as pentane, the time between reading of volume at the equilibrium temperature and weighing must not be prolonged, otherwise weight loss through evaporation may result in errors.8 m m 5. Significance and Use 5.1 This test method is suitable for setting specification, for use as an internal quality control tool, and for use in development or research work on industrial aromatic hydro carbons and related materials. In addition to the pure liquid chemicals for which expansion functions are known, it may also be used for liquids for which temperature expansion data are not available, or for impure liquid chemicals if certain limitations are observed. Information derived from this test can be used to describe the relationship between weight and volume. 6. Apparatus 6.1 Pycnometer, 9 to 10-mL capacity, conforming to the dimensions given in Fig. 1, constructed of borosilicate glass, and having a total weight not exceeding 30 g. 6.2 Bath, having a depth of at least 300 mm, capable of being maintained constant to +0.02C at any convenient temperature between 10C (50F) and 30"C (86F). Provide a support for the pycnometer (see Fig. 2) constructed of any suitable noncorrosive metal. . , No t e 4--If the laboratory air temperature does not vary more than 0.02"C during temperature equilibration a special bath is not needed. 6.3 Bath Thermometer, An ASTM Precision Thermom eter, having a range from -"8 to +32C and conforming to the requirements for Thermometer 63C as prescribed in Specification El. 7. Hazards 7.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials utilized in this test method. 8. Sampling 8.1 Refer to Practice D 3437, for proper sampling and a For a more complete discussion on the use of this design pycnometer, see Lipken, Davidson, Harvey and Kurtz, Industrial Engineering Chemistry, Analyt ical Edition; Vol 16, 1944, p. 55. No t e--The graduation lines shall extend around the entire circumference of the i| pycnometer at the integral numbers 0,1, 2 cm, etc., half way around at the hnif'! divisions 0.5,1.5, etc., and shorter lines for the intermediate subdivisions. FIG. 1 Pycnometer f.; handling of aromatic hydrocarbons analyzed by this test' method. 9. Preparation of Apparatus 9.1- Acid Cleaning; for use when the pycnometer is to b&"!j calibrated or when liquid fails to drain cleanly from the ofthe pycnometer or its capillary. Thoroughly clean with 1 a chromic acid solution;and rinse well with reagent water conforming to Type III of Specification D1193. Other suitable cleaning procedures may be used. Dry at 105 to I10C for at least 1 h, preferably with a slow current of filtered air passing through the. pycnometer. 9.2 Solvent Cleaning, for use between determinations.!! Rinse with toluene and then with anhydrous acetone, drying with a filtered stream of dry air., ~-- 10. Calibration of Apparatus 10.1 Using the procedure described in Section 11, deter mine the weight of freshly boiled reagent water conforming to Type III of Specification D 1193 held by the pycnometer with the water level at each of three different scale points on the graduated arms. Two of these water levels must be at opposite ends of the scale. Make all weighings on the same day, using the same balance and weights. 10.2 Calculate the volume, VT p, at each scale point tested by means of the following equation; carry all calculations in 6 non-zero digits and round to 4 decimal places: Pycnometer capacity, VTp, mL -- A x (,Ww/d,"1) + B(T - l) where: A = air buoyancy coefficient, a constant for the temper ature range involved = 1.001064 VT p = volume of pycnometer at reference temperature, T Ww = weight of water in air, contained in the pycnometer, g 682- DUP050296244 D 3505 arms ofthe pycnometer against the corresponding calculated volume, VT p. Ifa straight line cannot be drawn through the three points, discard the data and determine three additional points so that a straight calibration line can be drawn such that no data point lies more than 0.0002-mL units from the line. If neither set of data meets the condition, the diameters of the graduated capillary arms are not sufficiently uniform, and the pycnometer should be discarded. 10.4 From the curve obtained, prepare a table of apparent volume, VA, (sum of scale readings of both arms), as apparent volume against corresponding calculated volumes, VT p, in increments of 0.0001 mL. Label this table with the reference temperature to which it applies. 'E---Ail dimensions are in inches! . . '' FIG. 2 Pycnometer Holder = density of water at r (see Table 2) = test temperature, C = reference temperature, 20C or 15.56C , and = volumetric coefficient of expansion df-9.5 mL of a borosilicate glass pycnometer, 9.262/6 X 10~s mL/ c. 10.3 Prepare a calibration curve by plotting apparent lume, VA, that is, the sum of the scale readings on the two 11. Procedure 11.1 Weigh the clean, dry pycnometer to 0.1 mg and record the weight 11.2 With the sample at approximately the test tempera ture, fill the pycnometer by holding it in an upright position and placing the hooked tip in the sample; the liquid will then be drawn over the bend in the capillary by surface tension. Allow the pycnometer to fill by siphoning (about 1 min) and break the siphon when the liquid'level in the bulb arm of the pycnometer reaches the lowest graduation mark. 11.3 Thoroughly dry. the wet tip. Wipe the body of the pycnometer with a chemically clean, lint-free cloth slightly damp with water (Note 4) and weigh the filled pycnometer to the nearest 0.1 mg. No t e 5--In atmospheres below 60 % relative humidity, drying the pycnometer by rubbing with a dry cotton cloth will induce static charges equivalent to a loss of about 1 mg or more in the weight of the pycnometer. This charge may not be completely dissipated in less than `/2 h, aiid can be detected by touching the pycnometer to the wire hook in the balance and then drawing it away slowly. If the.'pycnometer exhibits an attraction for the wire hook, it may be considered to have a static charge. --- 11.4 Place the pycnometer in the holder in a constanttemperature bath held at any convenient temperature 10 and 30C within 0.02C; for materials not listed fist Table 1, hold the bath exactly at the desired reference temperature, usually 15.56C or 20C. When the liquid level has reached temper ature equilibrium (usually in about 10 min) and while still in * TABLE 2 Density of Water*, g/ml <,c 0.0 0.1 0.2 0.3 0.4 0.5 0.56 0.6 0.7 0.8 0.9 15 0.999 13 11 10 08 r07 05 04 04 02 00 *99 16 0.998 97 96 94 92 91 89 87 66 84 82 17 80 79 77 75 73 72 70 68 66 . 64 18 62 61 59 '57 ' 56 53" 51 49 47 45 19 43 42 40 38 36 34 32 30 27 25 20 23 21 19 17 15 13 11 09 07 04 21 02 00 *98 *96 93 *91 *89 *87 *85 *82 22 0.997 80 78 75 73 71 69 66 64 62 59 23 57 54 52 50 47 45 42 40 38 35 24 33 30 28 25 23 20 18 15 13 10 25 08 05 02 00 *97 *95 *92 *89 *87 *84 26 0.9&6 81 79 76 73 71 68 65 63 60 57 27 54 '52 49 46 43 41 38 35 32 29 28 26 24 21 18 15 12 09 06 03 00 29 0.995 .98 95 92 89. 86 83 80 77 74 72 30 68 65 62 59 56 53 50 46 . 43 40 A Abstracted from Tilton and Taylor, U.S. National Bureau of Standards Research Paper 971, NBS Journal ofResearch Vol 18,1917, p. 213. This paper is a statistical alysis of the data of Chappuis, Travaux Et Memoirea du Bureau International de Poid ef Mesurea, Vol 13,1907, p. D39. 683 DU P0502 96245 D 3505 X the bath, read the scale to the nearest 0.2 small division at the liquid level in each arm. 12. Calculation 12.1 Table 1 Materials--Compute the density or relative density, or both, by means of the following equations: Density, g/mL at 60F = w* XF6o + 0.00121 Density, g/mL at 20C = Ws --~i X F20 + 0.00X21 *20 Density, g/cm3 at 20C = \~~z F20 + 0.0012l| 0.99997 Relative density 60/60T \~ x F60 + 0.0012l] 1.00096 Vfs\ I where: Ws = observed weight of sample, corrected for variation of weights, g, W20p, V60 p = calculated volume, VT p, ofsample at 20C or 60T, millilitres, obtained from the pycnometer calibration table (Note 5), ^20> ^60 = constants taken from' Table 1. Corre sponding to the test temperature, fC No t e 6--For frequently examined products it should prove conven ient to combine Table 1 with the calibration table described in 10.2. 12.2 General Method--Compute the density or relative density, or both, by means of.the following equations: w* Density, g/mL at 20C = -+ C V20 Density, g/cm3 at 20"C = |pr-- + cj 0:99997 Relative density 60/60F = [ y--~ + c] 1.00096 1 Fso J where: W* = observed weight of sample, corrected for vari ation of weights, g, Veop = calculated volume, VTP, of sample at 20C or 60F obtained from the pycnometer calibra tion table, and C = air buoyancy correction factor from Table 3. 12.3 Pounds per Gallon--Compute the commercial den- TABLE 3 Air Buoyancy Correction (Section 1 w/v c W/V C W/V 0.70 0.00036 0.80 0.00024 - o.9o;; 0.71 0.00035 0.81 0.00023 0.91 0.72 0.00033 0.82 0.00022 0.92 0.73 0.00032 0.83 0.00020 0.93 0.74 0.00031 0,64 0.00019 0.94 0.75 0.00030 0.85 0.00018 0.95 0.76 0.00029 0.86 0.00017 0.96 0.77 0.00028 0.87 0.00016 0.97 0.78 0.00026 0.88 0.00014 0.98 0.79 0.00025 0.89 0.00013 0.99 sity, pounds (in air) per U.S. gallon and U.K. gaH follows: 12.3.1 From Pycnometer Data: lb/U.S. gal (in air) at 60F = Ws/V60l` xfMx 8.346 lb/U.K. gal (in air) at 60"F = Ws/V60p 10:0* 12.3.2 Convertedfrom d6Q, gfmL: lb/U.S. gal (in air) at 60*F = g/mL x 8.3464 - 0.0100 lb/U.K. gal (in air) at 60"C = g/mL x 10.0236 - 0.0121 13. Precision and Bias9 13.1 The following data should be used for judging; acceptability of results (95 % probability) for the mate Table I: 13.1.1 Repeatability--Duplicate results by the same ator should not be considered suspect unless they differ more than the following, amounts: 0.0002 g/mL 13.1.2 Reproducibility--The results submitted by laboratory should not be considered suspect unless it < from that of another laboratory by more than the foil, amounts: 0.0003 g/mL 14. Keywords 14.1 correction for temperature expansion; density; 1 liquid chemicals; relative density f Source of precision data: The Coal Tar Research Association, Oxford K Gomcrsal, Checkbeaton, Yorks, U.K.., Standardization of Tar Products, T Committee, Document No. 0763, Serial No. GPI-67. APPENDED (Nonmandatory Information) XI. METHOD AND FORMULA DETAILS X1.1 Introduction X1.1.1 The manipulative simplicity of this test method is possible, for the materials listed in Table 1, because accurate temperature-density functions have been developed by com puter curve fitting for these materials. Moreover, it is known for the purity range of the commercially produced materials of Table 1, that they parallel the temperature-density func tion of the pure materials. Refer to Method D 1555. Also, the temperature coefficient of expansion of borosilicate laboratory glassware is constant and accurately known. Thus, it is possible, within certain limits, to weigh a calibrated, temperature equilibrated pycnometer containing a substance of known temperature density function and then calculate the density at any other temperature, taking into 684 DUP050296246 P^ene ||uene pied xylenes Bfylene r&Xylene . IXylena fp-ene fycbhexane 0.8997261 0.6B5 420 0 0.880 9667 0.896902 5 0.880956 7 0.878103 7 0.923 892 7 0.794423 5 ft D 3505 TABLE X1.1 -1.021 458 -9.230 00 -8.3i0 26 -8.335 07 -8.310 26 -8.457 83 -8.802 93 -7.226 22 Values for do, a, 8, and 7. E-03 E-04 E-04 E-04 E-04 E-04 E-04 E-04 -7,1726 --4.154 8 -5.180 -4.1548 -3.310 6 -1.2904 -3.89482 E-07 E-Q7 E-08 E-07 E-07 E-07 E-06 -4.155 6 E-09 -1.73557 E-08 |unt the change in volume of both the substance and the tometer. Basic Data |l.2.1 The temperature-density functions of the several iucts of Table 1, except for styrene, are based on data sloped by API Research Project 44, but contain one more ant figure than the values published in "Selected Valfbf Hydrocarbons and Related Compounds" by American |oleum Institute Research Project 44. Data for styrene : obtained from Dow Chemical Co. 11.2.2 The respective temperature-density functions of fjmateiials of Table 1 are based on computer curve fitting he data to a power series equation of the form: r= do + ext + fit2 + yt3 + ... density of substance at temperature, t = density of substance at 0C = temperature, "C a, f), y, .. .-power coefficent10 series tl.2.3 The values of d0, a, /?, and y for the products of j>le 1 of this test method are tabulated in Table XI. 1. [1.2.4 The value of D at the two most commonly used jsrence temperatures, 60F (15.56C) and 20C, are given fowl Substance zene e xylenes, iylene [ylene rlene le tohexane Ofo-c 0.879 010 1 0.866 960 0 0.880 178 4 0.864 170 0 0.86t 055 6 0.906 235 2 0.778 274 3 Dlo-r 0.883 658 6 0.871 058 1 0.883 904 9 0.867 925 3 0.864 863 2 0;910 164 1 0.782 171 1 C1.2.5 To enable the user of this test method to extend it materials not listed in Table 1 for which temperature ity data are available, derivations of the formulas used provided in Sections XI.3 and*X1.4. .3 Density Definition |X1.3.1 Density is defined as follows: d t` = ms/v t s (i) ftere: rs = density of a substance, g/mL at reference tempera ture T, = mass of substance, and = volume of substance, mL, at "reference" tempera ture T. [ 10 For a complete description of the development of these coefficients refer to tumual Report of Committee D-16," Proceedings, American Society for Testing fed Materials, Voi 63, 1963. X1.3.2 Mass is determined by correcting the weight W* of a certain volume of the substance contained in a pycnometer, for the buoyancy of air and variation in local acceleration of gravity. When a beam balance is used no correction is necessary for acceleration of gravity. XI.3.3 The volume, VTS, of the substance at the chosen reference temperature, T, is obtained by making two correc tions to the apparent volume observed in the pycnometer. X1.3.3.1 The first correction is to obtain the true volume of the pycnometer, V:p, at the test temperature, tC. The volume of the pycnometer, VT p, is known by calibration at the reference temperature, T. Its volume at the test temper ature, Vtp, is calculated from a knowledge of the cubical coefficient of expansion of the glass and the measured deviation of the test temperature from the reference temper ature. The volume of the substance, V,s, and the volume of the pycnometer are identical at the test temperature. XI.3.3.2 The second correction is to correct the true sample volume at the test temperature, V,s, to the volume it would occupy at the reference temperature, V,s. X1.4 Pycnometer Calibration, Section 10 of this Test Method Xl.4.1 The pycnometer volume at the reference temper ature is calculated from the mass and density of water contained in the pycnometer at the calibration temperature, t, C, using the equation: -- AWw Vip = `^~r+B(T-t) (2)-- where: VTP = pycnometer volume at the reference temperature, mL, Ww =. weight of water in the pycnometer using a beam balance and calibrated brass weights, d,w = density of pure water, g/mL, at the calibration test temperature, t = calibration test temperature, "C, T = reference temperature, C, A = constant for correcting the observed weight ofwater to mass, and B = cubical coefficient of expansion of 9.5-mL pycnometer of borosilicate glass, mL/mL C. No t e X1,1 --The first terms of Eq 2 gives the true volume ofwater at the calibration temperature; that is, the true volume of the pycnometer at the calibration test temperature, t. The second term corrects this volume to the volume of the pycnometer at the reference temperature; in other words, the volume that the pycnometer would contain if it were at the reference tempera ture with the liquid level at the same two marks. Xl.4.2 Constant A, Correcting Ww to Mass, Mw\ 685 JPHNHWPR DU P0502 96247 D 3505 W* {l V + --d,a". - ^dj = AW <3) where: Mw -- mass of the water in the pycnometer, g, Ww -- weight of the water in the pycnometer, g, 2da -- average density of air, g/mL (=0.00121) within the calibration temperature range db = average density of brass weights within the calibra tion temperature range, g/ml (=8.100), and d,w = defined above. No t e XI.2--For the buoyancy correction it is adequate to use the average density of water11 within the test temperature range, as follows: t d," 10 15 20 25 30 35 Mean 0.999 700 I 0.999 128 6 0.998 233 6 0.997 075 1 0.995 678 3 0.994 035 6 0.997 308 55 No t e X1.3--At t = 15.56-C, d,TM = 0.999 042 3 , (, . 0,001 21 0.001 21\ ^ = '1 + 00.999773300885555 ' 8.1 / ~ 1.001 064 (4) Xl.4.3 Constant B, volume expansion factor for 9.5-mL pycnometer, mL/C B = 9.5 C = 9.5 x 3 x C' x 1.000028 C = volumetrical temperature coefficient of expansion of borosilicate glass = 9.7 50273 x 10~6 mL/mL-C C'- linear coefficient of expansion of borosilicate glass = 3.25 x 10-c cm/cm C No t e X1.4--Two manufacturers of low expansion borosilicate glass list their coefficients as 3.2 and 3.3 x 10~6, respectively. * B = 9.5 x 1.000028 X 3 x 3.25 x 10~6 = 9.262759 X 10~5 mL/"C therefore: V" = 1.001064 x Ww- + 0.00009263 (T-t) d,' when T = 20C; d,w = 0.9982336 (5) when T = 60F; d,w = 0.9990423 Vfoc = W" x 1.002835 + 0.00009262 (20 - t) (6) Vg0.c = Ww x 1.002024 + 0.00009262 (15.56 - t) (7) XI.4.3.1 Error introduced by using average single value for the pycnometer rather than true pycnometer volume. Average deviation 0.5 mL Maximum expansion factor error for a 20C range B (error) = 0.5 X 0.00000975 x 20 = 0.0000975 mL XI.4.4 Development of Factor F and the constant 0.00121 (Section 12 and Table 1) of the test method. ws Dts, g/mL V7P xFr+ 0.00121 (see 12.1) X 1.4.5 The factor F contains the following corrections: J1 Waterdensity obtained from: Tilton & Taylor, National Bureau ofStandards Research Paper RP971, Journal ofResearch of the NIST, Vol 18, February \ 937. It corrects the pycnometer volume, VT ", as read, fron pycnometer calibration table, (Va versus VT", 103)-' actual sample volume at the test temperature, V/. XI.4.6 Corrects the actual sample volume V ' volume it would occupy at the reference temperatur XI.4.7 Converts the observed sample weight (m mass. No t e XI.5--If a torsion or spring balance is used, a inirectiou! local acceleration of gravity must also be applied to the obsep <_d >. ' weight. Xl.4.7.1 y,`~ Vt p (lm u + CT) v,"= V,s= V' + V'C{t~t') VT" = V' + V'C(T- t') where V' = volume of the pycnometer at t' = 0C; and C = defined above. V* = K'(l + Ct) VT" = V (1 + CT) V.s 1 + Ct XI.4.7.2 VjP 1 +CT ,= V'{^)+V`~V- XI.4.7.3 M- -w*(i 1 - 121 ooom\ \ dts 8.1- ) 3 * To solve Eq 10 it is necessary to know the density ofthd substance, d,s, at the test temperature. Instead ofthis value, is adequate for the buoyancy correction to use an apprg mate density calculated from the observed weight IVs ai the corrected sample volume Vts, thus: Ms-Ws(i4_ 0-00121 Q-002n \ + WsjVts '8:1 } XI.4.8 Combining Eqs 1, 8, 9, and 11 to arrive al equation for factor F: Ms yy-y-($} simplified M* -- Ws (l + --------- --\ l W/Vf dj M* = Ws ^1 ~jj + daVj combining Eqs 1, 11, and 9: 686 DUP050296248 D 3505 idDj+ d,,Vf Vf -- n s--WLl* _ (L\ (hf. + d dr_ Dt ~ v,s V db)d? dd* taring for V/ from Eq. 8. d-/ " df +4 "itm + d 2d31s a d,s The last tenn varies between 0.001196 and 0.001232 for the (12) temperature range, 10 to 30C, of the test and can be rounded to 0.00121. Also, dr _d0 + aT + PT2 + yT3..... /(o'. (13) d* do + at + (It2 + ft3.... from Eq 1 of the basic data. Thus, Eq 16 reduces to: t>T=^FT + 0.M\2\ (14) where: dn + <xT+ &T2 4- yT3V(I\ +CCT7 \( d\ d0 + st + pfi + yt3 \l+oA 4/ F20 values given in Table I Part I, are the solution to the preceding equation when T = 20C and t is any 0.2'C value from 10 to 30C. F60 values given in Table 1, Part II, are the solutions to the above equation when T is 15.56C (60F) and t is any 0.2 value from 10 to 30C. 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 for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296249 Designation: D 3626 - 85 (Reapproved 1990)' Standard Test Method for Tar Acid Composition by Gas>Liquid Chromatography1 This standard is issued under the fixed designation D 3626; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 'i No t e--Unit of measurement information added editorially in September 1990. 1. Scope 1.1 This test method covers the quantitative determina tion of phenol and certain homologues of phenol in tar acid mixtures by gas-liquid chromatography. 1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for informa tion only. 1.3 This standard does not purport lo address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health, practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Sections 7 and 9. 2. Referenced Documents 2.1 ASTM Standard: D 3852 Practice for Sampling and Handling Pheiiol and Cresylic Acid2 E 260 Practice for Packed Column Gas Chromatography3 4 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200* thermal conductivity detector. 5.2 Recorder, with a full-scale response time of 1 s of.is 5.3 Attenuator--A multistep attenuator for the detS, output signal may be used to maintain peaks within the of the recorder. The attenuator must be accurate to absolute over the total scanning range. ` 5.4 Packed Column, A packed column made of 6 4-- (0.25-in.) outside diameter, 0.89-mm (0.035-in.) wall t1ii3 ness, stainless steel tubing at least 2.44 m (8 ft) long. It sl|| be packed as described in 9.1. 6. Reagents and Materials 6.1 Solid Support, acid-washed, silanized, diatomacetj earth of 60 to 80 mesh. 6.2 Stationary Phase, trimethyl pelargonate as the tionary phase.5 Acetone is a suitable solvent, for trimp, pelargonate. 7. Hazard 7.1 Consult current OSHA regulations and supplie Material Safety Data Sheets for all materials used in thistKSjji method. 3. Summary of Method 3.1 The sample composition is determined by standard gas chromatographic technique using trimethyl pelargonate as the stationary phase. Percent composition is determined by calculating the ratio of the individual peak areas to the total area of all peaks. No response factors or internal standards are used. 4. Significance and Use 4.1 This test method is suitable for the general quantita tive analysis of commercial tar acid mixtures. It may be used as a tool for quality control and specification purposes by producers and users. 5. Apparatus 5.1 Chromatograph--A gas chromatograph having a 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D I6.0C on Oxygenated Aromatics. Current edition approved March 29, 1985. Published December 1985. Origi nally published as D 3626 - Tt. Last previous edition D 3626 - 80. 2 Annual Book ofStandards, Vol 06.03. 2 Annua! Book of Standards, Vol 14.01. 4 Available from Superintendent of Documents, U S. Government Printing Office, Washington, DC 20402. 8. Sampling 8.1 Samples shall be taken in accordance with PractieiM D 3852. 9. Procedure 9.1 Column Preparation--The column packing should prepared in the ratio of 1 + 4 parts by weight (20 % loacungj stationary phase to solid support. Dissolve the statioi phase in sufficient acetone so that the solution will cover solid support completely in a flat, shallow glass or porceli vessel. Place in the oven at 105C and dry to constant wei) with occasional stirring. Warning--Acetone is flammabl and mixtures of its vapors with air are explosive. Use well-vented, explosion proofoven and avoid contact withthe| flame or sparks. Add the free-flowing packing thus obtained' to the column with the aid of a small funnel, using efficienbf vibration to achieve the densest packing reasonably possible. Insert glass wool plugs in each end of the column to retain the packing. Finally, bend the column to the appropriate 5 Trimethyl pelargonate suitable for use is commercially available under the designation or Celanese Ester No. 9 from certain chromatography supply houses such as; Chromatography Associates, New Castle, DE 19720; Chemical Research Services, Inc., Addison, IL 60101; and Applied Science Labs, State College. PA 16801. 688 DUP050296250 Order of Elution--The order of elution and compo; groupings is as follows: 3.1 phenol. 3.2 0-cresol. 3.3 2,6-xylenol. 3.4 m- and p-cresol. 3.5 o-ethylphenol. (.3,6 2,4- and 2,5-xylenoL 1.7 2,4,6-trimethylphenol. |,3.8 2,3- and 3,5-xylenol; m- and p-ethylphenol; oropylphenol; 2,3,6-trimethylphenol. 3.9 3,4-xylenol. 13.10 Cg and Cw phenols (may contain multiple peaks). See Fig. 1 for a typical chromatogram showing satisory resolution. Determine the retention times of isomers (listed in the example chromatogram (Fig. 1) experimen- "Calculation .1 Calculate the percent composition for each compo: grouping as follows: where: W = area percent of sample component, A = area of component peak, and P = total area of all peaks. 11. Report 11.1 Report the following information: 11.1.1 Percent composition for each component grouping as follows: 11.1.1.1 Area percent of sample component, 11.1.1.2 Area of component peak, and 11.1.1.3 Total area of all peaks. 12. Precision and Bias 12.1 Precision--The following criteria shall be used for judging the acceptability of results: 12.1.1 Repeatability (Single Analyst)--The standard devi ation of results (each the average of duplicates) obtained by the same analyst on different days has been estimated to be 0.13 % absolute. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.38 % absolute. 12.1.2 Reproducibility (Multilaboratory)--The standard deviation of results (each the average of duplicates) obtained by analysts in different laboratories has been estimated to be 0.69 % absolute (at nine, degrees of freedom). Two such values should be considered suspect (95 % confidence level) if they differ by more than 2.21 % absolute. 12.2 Bias--The bias ofthis method cannot be determined because no referee method is available to determine the true value. .phenol ' ortho-cresol i 2,6-xylenol ! meta- and para-cresol ortho-ethylphenol ` 2,4- and 2,5-xylenol | 2,4,6-trimethylphenol 1,2,3- and 3,5-xylenol; meta- and para-ethylphenol; orthoisopropylphenol; 2,3,6-trimethylphenol r 3,4-xylenol ; C,, and Cn0 phenols (may contain multiple peaks) FIG. 1 Typical Chromatogram .... ....... DUP050296251 D 3626 APPENDIX (Nonmandatory Information) XI. INFORMATION PROCEDURE FOR SEPARATION OF INDIVIDUAL COMPONENTS AND ISOMERS Xl.l Test Method D3626 has been a valuable1 tool acceptable for the general quantitative analysis of commer cial tar acid mixtures. For those occasions where a more discreet separation of the individual components or isomers may be required, the following procedure is offered for information purposes. XI.2 Summary of Method--The sample composition is determined by capillary gas chromatography. The weight percent composition is calculated from the ratio of the., individual peak areas to the total area of all peaks using appropriate response factors determined for each component by means of a standard sample. XI.3 Apparatus: ' ` XI.3.1 Chromatograph--A gas chromatograph compat ible with capillary columns, equipped with constant-temper ature column oven, aii inlet splitter, high-temperature flame ionization detector, and an electrometer capable of Plea suring 10 to 11 A or less. X1.3,2 Recorder--A .1-mV range strip chart recorder with full-scale response time of 1 s or less. X 1.3.3 Peak Integrator--Disk chart integrator or elec tronic digital integrator to measure the peak areas. XI.3.4 Capillary Column--A capillary column prepared from Type 316, 321, or 374 stainless steel tubing with 1.56-mm (0.0625-in.) outside diameter and 0.25-mm (0.01- in.) to 0.50-mm (0.02-in.) inner diameter with a length of 30.5 mm (100 ft ) to 61 mm (200 ft) should be used. It should be prepared as described in XI.5. XI.3.5 Syringe, capable of 0.3 to 0.5-jrL delivery. XI.4 Reagents and Materials: XI.4.1 Purity of Reagents-- Reagent grade chemicals shall be used in all cases. 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. X 1.4.2 Acetone. Xl.4.3 Dichloromethane. XI.4.4 Methanol. X 1.4.5 Orthophosphoric Acid. X 1.4.6 Standards for Calibration--Standard samples of known composition representative of samples to be ana lyzed. 6 "Reagent Chemicals, American Chemical Society Specifications," Aon. 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." XI A.7 Stationary Partitioning Phase--Di-isodecylphthai.-- late, chromatographic grade. *' X1.5 Column Preparation: X 1.5.1 It is imperative that the inner surface of the capillary be perfectly dean before coating with substrate, to insure a uniformly wettable surface. Current cleaning proce dure for new tubing is to wash sequentially with methdnqlmH dichloromethane, and acetone. Caution--Acetone1 and meth^'.-:- anol are flammable and certain mixtures of vapors with air ^ are explosive. Use in a well-vented, explosion-proofareaand' avoid contact with flame or spark, To do" this, attach a 20-mL reservoir made from a length of 12.7-mm ('/a-in.J'j stainless steel pipe to one end of the capillary tubing (using m pipe to tube fittings). Fill the reservoir with the solvent (Sixer W to remove any particulate matter) and connect the other end of the reservoir to a high-pressure nitrogen or helijim source. m About.414 to 552 kPa_(60 to 80 psig) is sufficient to force the' m solvent through the capillary. XI.5.2 Inspection of the last washings will m indicate M whether the column is clean. If there is any evidence of contamination, repeat the entire washing process. A particu., Italy dirty column may require niuch higher pressure for the ;,f initial flushing steps. .` w X1.5.3 Many substrates have been investigated for resolu tion of cresylic acid homologs, however, the most practical to date is di-isodecylphthalate. Place a solution of 9.5 % weight di-isodecylphthalate and 0.5 % weight orthophosphoric acid in filtered acetone in the reservoir attached to the nitrogen Cylinder and force through the column at a positive pressure. Force 3 to 5 mL of solution through the column. Determine pressure to be used by connecting the empty capillary tube to the reservoir and, adjusting gas pressure, -by means of a regulator, until bubbles exit the open- end at a rate of about one in 5 s. (Put the end into a small beaker of liquid so bubbles can be observed.) Stop gas flow by means of a shut-off valve but, do not change the regulator setting. Put the coating solution into the reservoir and force subsequently through the column at the pre-set pressure. XI.5.4 The two main factors that determine coating thickness are concentrations of solution and rate of coating. Control them as closely as possible. XI .5.5 After coating, allow to purge for several hours at ambient temperature, preferably overnight. Before using. put into an oven, establish carrier flow and bake at 120'Cfor 3 h. Then decrease to an operating temperature rangefrom x 100 to 110C. It is desirable to program the oven to 120C at a slow rate during conditioning. X1.5;6 This conditioning or weathering process removes the last traces of volatile solvent from the column coating, and it seems to fix the substrate film so it does not bleed out of the column during use. Any bleeding of substrate results in a "noisy" signal, tailing after component elution, and a generally irregular baseline. X1.6 Operating Conditions: DUP050296252 D 3626 20 2 30 FIG. X1.1 Capillary Chromatogram showing satisfactory resolution. The retention times of isomers not listed in the example chromatogram (Fig. XI. 1) must be determined experimentally. XI.8 Calculation Method: XI.8.1 A response factor must be obtained for each component This is done by injecting a standard sample of known composition using identical conditions as for the unknown sample. Obtain the apparent percentage of each component as follows: ,, A x 100 where: P -- apparent percent of standard component, A = area of component peak, and T - total area of all peaks. '-- X 1.8.2 Calculate"the response factor for each component by dividing the actual, known percentage by the apparent percentage of that component in the standard sample as follows: where: R = response factor component, C = actual percentage of component, and Pi = apparent percentage of component in standard sample. XI.8.3 Determine the weight percent of each component in the sample by calculating the corrected area of each component peak and dividing by the sum ofall the corrected peak areas as follows: A. = A, X R where: WWPP DUP050296253 A, = Corrected area of sample component, and A2 = area of sample component A, Peak x 100 # D 3626 where: W = weight percent component, and T, = total corrected area of all peaks. The American Society for Testing andMaterials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement 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 it not revised, either reapproved or withdrawn. Yourcomments are Invited eitherfor 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, 1916 Race St., Philadelphia, PA 19103. 692 k' DUP050296254 Designation: D 3627 -91 Standard Test Method for Color of Cresylic Acids ("C" Series Stendards)1 This standard is issued under the fixed designation D 3627; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapprovai. ope . This test method covers the determination ofthe color esylic acids. The material under test is compared to color standards that are expressed in terms of the pries color standards.2 This standard does not purport to address all of the problems, if any, associated with its use. It is the Insibility of the user of this standard to establish appro ve safety and health practices and determine the applicaI of regulatory limitations prior to use. For specific ' l statements, see Section 6. Referenced Documents |i ASTM Standards: 11193 Specification for Reagent Water3 33852 Practice for Sampling and Handling Phenol and |,Cresylic Acid4 Other Document: 'SHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200s Significance and Use 111 Color is an important characteristic in certain tar acid 1 applications. This test method may be used for quality atrol and specification purposes by producers and users. Apparatus If. 1 BottlesIsfor Color Standards andfor Testing, clear and gblemished, clean, French square, flint glass, flat-bottom, i-stoppered, 30-mL (1-oz) capacity bottles holding 31 to |mL when filled to the neck. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be ted in all tests. Unless otherwise indicated, it is intended at all reagents shall conform to the specifications of the bmmittee on Analytical Reagents of the American Chem 'This test method is under the jurisdiction of ASTM Committee D-16 on iromauc Hydrocarbons and Related Chemicals and is the direct responsibility of " ommittee D16.0C on Oxygenated Aromatics. ; Current edition approved May 15, 1991. Published July 1991. Originally jfiblished as D 3627 - 77. Last previous edition D 3627 - 82 (1986)ei. ;2 T6hese color standards have traditionally been known as the Barrett Color-"C" s (Barrett Division of Allied Chemical Corp.) and have been in general use : at least 1957. 3 Annual Book ofASTM Standards, VolsO6.03and 11.01. 4 Annual Book ofASTM Standards, Vol 06.03. ! Available from Superintendent of Documents. U.S. Government Printing ffice, Washington, DC 20402. 6 Pyrex No. 2982 or Kimax No. 2039-P graduates have been found to be uitable substitutes. ical Society, where such specifications are available.7 Other grades may be used provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Specification D 1193, Type IV minimum. 5.3 Ferric Chloride (FeCl3 6H20). 5.4 Cobalt Chloride (CoCl2 - 6H20). 5.5 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 6. Hazards 6.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials utilized in this test method. 7. Cleaning of Bottles 7.1 All glassware should be thoroughly cleaned, rinsed with distilled water, and dried either at room tenperature or in an oven at 1.05C for 1 h before use. 8. Preparation of Reference Color Standards 8.1 Use the following basic stock solutions for preparing the reference color standards: 8.1.1 Solution A--Add 75 mL of concentrated HC1 6 distilled water in a 3000-mL volumetric flask, dilute to the mark with water and mix thoroughly. 8.1.2 Solution B--Dissolve 1000 g of_FeCl3 6H20 in exactly 600 mL of Solution A. Filter the resulting solution if any turbidity persists. 8.1.3 Solution C--Dissolve 100 g of CoCl2-6H20 in exactly 100 mL of Solution A. Filter the resulting solution if any turbidity persists. 8.2 Prepare the reference color standard solutions as shown in Table 1 using a 100-mL buret to dispense volumes up to 250 mL and using a 250-mL pipet for the remaining volumes. Mix each solution thoroughly and immediately transfer to separate color-standard bottles and stopper tightly. Identify each bottle with its appropriate designation. 8.3 Keep these standards tightly stoppered at all times to prevent evaporation. Coat the entire top of each bottle With sealing wax. Prepare a fresh set of standards at least once a year. 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." 693 DUP050296255 i D 3627 Standard Number C-Va C-V* C-Ve C-Va C-% C-1 C-1V4 C-1 Vs C-2 C-2Vi C-3 C-3'A C-4 C-S 06 07 C-8 C-9 C-10 Solution A. mL 18 12 6 250 250 250 250 250 250 30 30 ' 30 20 .. TABLE 1 Reference Color Standard Solutions Solution B. mL Solution C, mL Distilled Water, mL 1.0 2.0 2.8 4.0 5.6 8.0 12,0 16.0 20.0 40.0 80.0 130.0 250.0 250.0 1.0 1.5 1.9 2.5 3.2 4.0 4.0 4.0 5.5 10.0 15.0 10.0 20.0 20.0 220 220 170 180 200 100 55 Series/mL 18 12 of C-/, * 18 of C-ys jfy 12 of C-Vj+,9 12 of C-1 j 12 of C-1+ iff 12 Of C-1V, *3 9. Sampling 9.1 Samples should be taken in accordance with Practice D 3852. 10. Procedure 10.1 If the sample is solid, melt the entire sample using an appropriate container suspended in a water bath maintained at a suitable temperature. 10.2 Carefully fill a clean test bottle with sample and compare its color intensity to the color reference standards by holding the bottles against a white background using transmitted light, 11. Report 'J 11.1 Report the color of the sample as the "C" cole which it most nearly corresponds in color intensity. 12. Precision and Bias 12.1 A precision and bias statement cannot be because these parameters are not meaningful for th method. 13. Keywords 13.1 color; cresylic acids; phenol The American Society for Testing and Materials takes no position respecting the validity olany patent rights asserted in connection with any item mentioned in this standard. Users 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, eitherreapprovedor withdrawn. Yourcomments are invited either forrevisionofthis 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 hearing you should-make your views known to the ASTM Committee on Standards, 1916 Race SL, Philadelphia, PA 19103. 694 DUP050296256 Designation: D 3760 - 79 (Reapproved 1984) Standard Method for Analysis of Isopropylbenzene (Cumene) by Gas Chromatography1 This standard is issued under the fixed designation D 3760; the number immediately following the designation indicates die year of original adoption or, in the case of revision, tbe year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. scope jtl This method covers the determination of the purity of propylbenzene (cumene) by gas chromatography and in iition provides a means for measuring certain impurities |h as nonaromatics, tert-butyl benzene, and ethylbenzene Such are of interest. .2 This standard may involve hazardous materials, operbns, and equipment. This standard does not purport to mress all ofthe safety problems associated with its use. It is H responsibility ofwhoever uses this standard to consult and Iablish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. cific precautionary statements are given in Section 5. Referenced Document P 2.1 ASTM Standard: *E 260 Practice for Packed Column Gas Chromatography2 Summary of Method ! 3.1 A known amount of internal standard is added to the aple. A portion of the sample is chromatographed, and pneentratjons of the various impurities are calculated rela ve to the known amount of internal standard that is added, he total amount of all impurities is subtracted from 100 % |p calculate the assay of isopropylbenzene. Significance and Use 4.1 This method is useful in determining the purity of isopropylbenzene with normal impurities present including sopropylbenzenes. If extremely high boiling or unusual apurities are present in the isopropylbenzene, this method ffvould not necessarily detect them and the purity calculation vould be erroneous. 4.2 Prior to utilizing this gas*chromatograph procedure |br isopropylbenzene, a hydroperoxide determination should be made. TTiis result should be used in the evaluation of the chromatogram, as cumene hydroperoxide, if present, will yield decomposition products that will elute in the chroImatogram thereby giving incorrect results. |S. Precaution 5.1 All materials used in this procedure are highly toxic land flammable. Consult the latest OSHA regulation re- 1 This method Is under the jurisdiction ofASTM Committee D-16on Aromatic 1 Hydrocarbons and Related Chemicals and is die direct responsibility of Subeomfmittee D 16.0H on Styrene, Ethylbenzene, Isopropylbenzene. Current edition approved Feb. 23, 1979, Published May 1979. 2 Annual Book ofASTM Standards, Vol 14.01. garding all materials used in this procedure. 5.2 If isopropylbenzene has been exposed to air, cumene hydroperoxide may be in the sample. Exercise suitable precautions for handling isopropylbenzene which may con tain cumene hydroperoxide. 6. Apparatus 6.1 Chromatograph--Any suitable chromatograph equipped with a flame ionization detector in combinatioii with a recorder dr other data acquisition device may be used provided that the system has adequate sensitivity and sta bility to measure impurities in concentrations of 0.005 %. The sample size used in judging the sensitivity must be such that the column is not overloaded. If a capillary column is used, the chromatograph must be equipped with a proper sample injection splitter. 6.2 Chromatographic Column--The choice of column is based on resolution requirements. Any column may be used that is capable of resolving all significant impurities from isopropylbenzene and from the internal standard. A sample chromatogram is shown in Fig. 1. Any column that gives equivalent resolution will be acceptable. -The following columns have been used successfully: 6.2.1 Support Coated Open Tubular Column, 50 ft (15.2 m) in length, 0.020 in. (0.51 mm) in inside diameter with liquid phase of 5-ring polyphenyl ether plus Apiezon L.3 6.2.2 Capillary, 200 ft (61 m) in length, 0,010 in. (0.25 mm) in inside diameter, coated with meta-bis (m-phenoxy phenoxyl) benzene. 6.2.3 Bentone 344, 5 % plus diisodecyl phthalate, 5 % on Chromasorb W, 80- to 100 mesh, 14 ft (4.3 m) in length. Vs in. (3.2 mm) in outside diameter. 7. Reagents and Materials 7.1 n-Butylbenzene, high-purity (best grade obtainable). 7.2 Carrier Gas--Helium, chromatographic grade. 7.3 CompressedAir--Breathing air (oil-free). 7.4 Isopropylbenzene, high-purity. 7.5 Hydrogen, high-purity. 7.6 Specific Impurity, high-purity (for example, tertbutylbenzene). 8. Procedure 8.1 Install the chromatographic column and establish stable instrument operation at the proper operating condi- 3 This column is available from the Perkin-Elmer Cbrp, Norwalk, Conn., Part MBMA 009-0363. 4 Registered trademark of NL Industries. 695 DUP050296257 D 3760 TABLE 1 Operating Conditions for isopropylbenzene Analysis Column temperature, C Injection block temperature, C Detector temperature, C Carrier gas flow rate, cmP/min Air flow rate, cm3/min Hydrogen flow rate, cm3/min Make-up gas flow rate, cm3/min Sample split ratio Sample size (to injection block), pi 115 190 250 3-4 250 25 20 20:1 2 tions. The column that was used to generate the chromato gram shown in Fig. 1 is that described in 6.2.1. Operating conditions that were employed are summarized in Table 1. If another column is used it will likely require different operating conditions. Refer to instructions provided by the manufacturer of the chromatograph and to Practice E 260. 8.2 Into a 100-cm3 volumetric flask, pipet exactly 1.0 cm3 of n-butylbenzene. Dilute to volume with the isopropyl benzene sample to be analyzed and shake to mix. Inject an appropriately sized sample to achieve the sensitivity stated in, 6.1 and illustrated in Fig. 1. Determine the area under each impurity peak and die n-butylbenzene peak. 8.3 Identify the impurity components by comparing re tention times with those determined for specific components from the analysis of calibration blends. 9. Calculations 9.1 Calculate the concentration of each unn nearest 0.0001 % as follows: . *. Impurity concentration, weight % = --Impurity area.-. -butylbenzere3gj, 9.2 Calculate the isopropylbenzene purity ^ Isopropylbenzene concentration, weight % = iQQ(j impurity concentrated 10. Report 10.1 Report the purity of isopropylbenzene to 0.01 %. .{ 10.2 Report the concentration of impurities of int the nearest 0.01 %. 11. Precision and Bias 11.1 Repeatability-Single Analyst--Tits standard* tion of purity results (each the average of dup obtained by the same analyst on different days p-DUsoprop. Component 1. Nonaromatics 2. Ethyfcenzene 3. p-Xylene 4. m-Xylene 5. o-Xylsne 6. Isopropylbenzene 7. n-Propylbenzene 8. tert-Butylbenzene 9. sec-Butylbenzene Concentration Weight* 0.0110 0.0020 0.0016 0.0023 0.0009 99.72 (by difference) 0.0253 0.0261 0.0034 Component 10. -Methyl styrene 11. Unidentified 12. Unidentified 13. Unidentified 14. Unidentified 15. n-Butylbenzene 16. m-Diisopropylbenzene 17. p-Oiisopropylbenzene FIG. 1 Chromatogram of Isopropylbenzene 696 Concentration Weight * 0.0084 0.0021 0.0008 0.0015 internal standard 0.0969 (0.1 added) 0.1006 (0.1 added) DUP050296258 # D 3760 d to be 0.0016 % absolute at 5 degrees of freedom, h averages should be considered suspect. {95 % ce level) if they differ by more than 0.0058 % These data were obtained on samples having an level of 0.0833 % absolute. Reproducibility-Multilaboratory--The standard deof purity results (each the average of duplicates) obtained by analysts in different laboratories has been estimated to be 0.009 % absolute at 4 degrees of freedom. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 0.0357% absolute. 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 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. Yourcomments are Invited eitherforrevision ofthis standardorfor 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 net received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 697 DUP050296259 4 Designation: D 3797 - 88 Standard Test Method for Analysis of o-Xyiene by Gas Chromatography1 This standard is issued under the fixed designation D 3797; the number immediately following the designation indicates, the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of known impurities in, and the purity of, o-xylene by gas chromatog raphy. 1.2 This standard may .involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D3437 Practice for Sampling and Handling Liquid Cyclic Products12 E 260 Practice for Packed Column Gas Chromatography3 E 355 Practice for Gas Chromatography Terms and Relationships3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Summary of Test Method 3.1 A known amount of internal standard is added to the sample. A portion ofthe sample is chromatographed and the amounts of impurities are calculated relative to the amount of internal standard added. The amount of all impurities is subtracted from 100.0 to calculate the o-xylene purity. Results are reported in weight percent. 4. Significance and Use 4.1 This test method is suitable for setting specifications on o-xylene and for use as an internal quality control tool where o-xylene is used in a manufacturing process. It may be 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved April 29, 1988. Published June 1988. Originally published as D 3797 - 79. Last previous edition D 3797 - 82s'. 2 Annual Book ofASTM Standards, Voi 06.03. 3 Annual Book ofASTM Standards, Vo! 14.01. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. used in development or research work involving o-xyk is generally applied to impurities of nonaromatics, utf ethylbenzene, p- and m-xylene, and C9 aromatics in o-wl of 90 % purity or higher. 4.2 Purity is commonly reported by subtracting the mined expected impurities from 100.0. Absolute cannot be determined if unknown impurities are presen' 5. Interferences 5.1 Nonaromatic compounds in the xylene boiling may interfere with one or more of the internal stanj listed in 7.5 when certain columns are used. Known im ties of commercial o-xylene should be checked for adei separation in the column selected. 6. Apparatus 6.1 Chromatograph--Any gas chromatograph equi; with either a thermal conductivity or hydrogen flame iol tion detector consistent with the type column used, detection system must be sufficiently sensitive to prodifi minimum response equivalent to 100 pV per 0.01 components of interest on a recorder or electronic integral 6.2 Chromatograph Column--The choice of columns based on resolution requirements. Any column may be if it is capable of resolving all significant impurity com) nents from o-xylene and the added internal stam Column may be either packed or capillary. A proper samplej^j injection splitter is required if capillary columns are usecUi; Listed in Table 2 are columns or combinations of columav-C and operating conditions that have been used satisfactorily' by one or more laboratories. 6.3 Recorder--Any recorder with 2mV gr less full-scale, response of- 1-s, and satisfactory, providing a chart speed of 30 the recorder-detector to 60 system in./h will reis^-'';:4, peat to 0.01 weight %. 6.4 Integrator--If any integrator is used in conjunction with the detector, it should provide repeatable response to 0.01 weight %. 6.5 Microsyringe, 10-pL. 6.6 Volumetric Flask, 100-mL capacity. 6.7 Volumetric Pipet, 1-mL. 7. Reagents 7.1 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- *( if DU P050296260 D 3797 ciety, where such specifications are available.5 Other may be used, provided it is first ascertained that the It is of sufficiently high purity to permit its use without jng the accuracy of the determination. Carrier Gas--Chromatographic grade helium or hyfor use on thermal conductivity detector units, or :n, helium, or argon for use on flame ionization ir units is recommended. Pure compounds for calibration shall include le (Note 1), toluene, ethylbenzene, p-xylene, ene, o-xylene, isopropylbenzene, isooctane (Note 2), lie (Note 2), n-undecane (Note 2), of a purity not less 9 %. If the purity of the calibration compounds is less 9 %, the concentration and identification ofimpurities known so that the composition of the final weighed can be adjusted for presence of the impurities. e 1--n-nonane represents the nonaromatic in a sample. ;e 2--Any of these compounds may be used as' an internal provided it elutes free of Contamination. Solid Support or Liquid Phase, or Both--See Table 2 list of acceptable items. T ! rds Consult current OSHA regulations and supplier's rial Safety Data Sheets for all materials used in this test hod. Sampling ' Sampling of xylene should follow safe rules jn order to : to all safety precautions as outlined in current OSHA atioris. Refer to Practice D 3437 for proper sampling iihandlmg of aromatic hydrocarbons analyzed by this test hod. i Preparation of Apparatus j)!l Column Preparation--The method used to prepare afnns is not critical provided that the finished column Iduces the desired separation. Partitioning liquids, supt, and loading levels used successfully in cooperative \vork p listed in Table 2. 1.2 Mount the column in thechromatograph and adjust conditions as necessary (Table 2) to give the desired ation. Allow sufficient time for the equipment to reach librium as-indicated by a stabje recorder baseline. Calibration 11.1 Prepare a synthetic mixture from pure hydrocarbons gth all of the aromatic compounds present in the sample to analyzed containing approximately 94.0 weight % Sylene and the expected significant impurities at their Ipected concentration. Suggested composition is given bw in weight percent. Pure grade or better o-xylene must used in preparing the calibration mixture. The pure Saterial itself must be analyzed and corrections made in the Imposition of the calibration blend as required. 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. c. Washington, DC. For suggestions on the testing of reagents not listed by the nerican Chemical Society, see "Reagent Chemicals and Standards," by Joseph isin, D. Van Nostrand Co., Inc., New York, NY, and the "United States tarmacopeia." oxyleoe toluene p-xylene m-xylene ethylbenzene . isopropyl benzene TMionaoe (0.876)'* (0.862) (0.857) . (0.860) (0.863) (0.857) (0.714) 94 % 1% J% i% .1 %. 1% l% in parentheses are density in grams per millilitre at 25'C. 11.2 Determine the response of each component except o-xylene relative to the internal standard. (Suggested internal standard isooctane, -oetane, K-undecane.) Dilute 1 mL of internal standard to 100 mL with the above synthetic mixture (use d = 0.874 g/mL for synthetic mixture), inject the resulting solution to the chromatograph and determine the response factor for each impurity relative to the internal standard. Measure the area of each peak except o-xylene (n-nonane represents the nonaromatics in a sample). (^>J C, where: A/ = peak area of impurity fin calibration blend, As = peak area of internal standard in calibration blbnd, AB,i = peak area of impurity i in o-xylene base stock, Aj},s = peak area ofinternal standard in o-xylene base stock, Cs = concentration of internal standard, wt %, c, = concentration of impurity in calibration blend, wt %. 11.3 Calculate response factors to the nearest 6.001. 12. Procedure 12.1 Pipet 1.0 mL of internal standard into a 100-mL volumetric flask and dilute to the mark with the sample to be analyzed. Mix well. 12.2 Charge an appropriate amount to the chromato graph. 12.3 Measure the area of all peaks except the o-xylenepeak. A typical chromatogram is shown in Fig, 1. 13. Calculation 13.1 Calculate the amounts of individual-impurities as required and. the total concentration of all impurities.' Sum the area of all nonaromatic peaks. Calculate the o-xylene by difference. c m (4,)(CV) 1 (Asxm C, = 2C,. o-xylene = 100.0 - C, ->f where: , C, -- tqtal concentration of all impurities in weight percent. 14. Report 14.1 Report individual impurities to the nearest 0.01 %. 14.2 Report total impurities to the nearest 0.1 %, and 14.3 Report o-xylene content to nearest 0.1 %. 14.4 For concentrations of impurities less than 0.005 %, report as <0.01 %. 15. Precision and Bias 15.1 The following criteria should be used to judge the 699 DUP050296261 D 3797 i 26 24 MINUTES FIG.' 1 o-Xylene Analysis acceptability (95 % probability level) of results obtained by this test method. The criteria were derived from a round robin between 8 laboratories. The data were run on 2 days using different operators. 15.2 Repeatability--Results in the same laboratory should not be considered suspect unless they differ by more than the amount shown in Table 1. 15.3 Reproducibility--The results submitted by each of two laboratories should not be considered suspect unless they differ by more than the amount shown in Table 1. 15.4 Bias--No bias statement can be made for this test method at this time; however Subcommittee D16.0A is interested in conducting an interlaboratory test program to TABLE 1 Component o-Xylene Ethylbenzene m-Xylene p-Xylene Isopropyl benzene Repeatability and Reproducibility ---------------- as. Concentration weights Repeatability Reproducibilityi 90 to 99 1 to 2 4 2 3 1 0.6 0.15 0.063 0.21 0.060 0.081 0.010 0.040 . 0.49 "H 0.18 1 0.36 ;'|1 0.36 0.46 $ 0.46 0.3S determine the bias. Interested parties should contact the Staff Manager for Committee D-16, ASTM Headquarters. DUP050296262 # D 3797 TABLE 2 0-Xylene Instrumental Conditions if A B C D E F No. 1 No.2; ling mild phase P pcentration, weight % |liJ support fihslze ipment p#>. ft (m) lie diameter, m. (mm) per fmL/min InaKeup, mL/min I'mL/mln |mL/mln g-'inL/mln lerature, C: Sector alumn ogress rate stainless steel BBTCP* -- -- -- -- 200(61.0) 0.01 (0.25) FID 2 40 40 -- 400 175 200 80 --- ' stainless steel DBTCP8/ Apiezon L 4.0/1.5 -- -- -- . 250 (76.2) 0.02(0.51) FID 5 -- 20 250 stainless steel DNPTCPD -- -- -- -- 200(61.0) 0.02 (0.51) FID -- . --40 160 500 230 250 95 . --- 250 200 50 -- stainless steel Carbowax 1540 -- -- -- -- 300(91.4) 0.01 (0.25) FID 1.5 30 30 -- . 300 250 250 90 1/1for; mge, mV eed, in./min Jte: i!ume, *iL jit emai standard ution -- Otol 0.25 0.3 . 100:1 isooctane 1 +100 -- Otol 0.5 0.2 2:1 n-octane -- . Otol 0.5 0.6 40:1 /sooctana 1 +100 Otol 0.5 1.0 100:1 n+jndecane 1+99 g'Butylbanzyl tetrachlorophthalate, 10 % solution In methylene chloride used to coat capilary. Dlbutyl tetrachlorophthalate. 'Diluted with 94.5 % methylene chloride for coating capilary. ^Dkt-propyl tetrachlorophthalate. J[Bentone-34/OS-124 (polyphenyl ether. 5-ringe). If 1,2,3-trIs(2-cyanoelhoxy)propane. stainless steel B-34/OS124f 5/5 Chromosorb W 80-100 acid washed 10 (3.1) Ve (3.2) -- 40 35 400 stainless steel TCEPf 20 Chromosorb P 80-100 add washed 18 (5.5) Ve (3.2) stainless steel Carbowax 1540 __ _ _ __ 300/91.4) 0.01 (0.25) FID 2.6 . --- 32 __ 300 20 170 120 230 120 -- -- 4<,C/min 25 __' 140 Oto 1 0.5 Otol 0.5 0.2 0 MIBK 1+100 0.5 370:1 n-decane 1 + 100 The American Society for Testing and Materials takes noposition respecting the validity of any patent rights assertedin connection with any Item mentioned in this standard. Users of this standard ere 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 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, tf 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. 701 DUP050296263 * Designation: D 3798 - 89 m Standard Test Method for Analysis of p-Xylene by Gas Chromatography1 This standard is issued under the fixed designation D 3798; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (t) indicates an editorial change since the last revision or reapprovai 1. Scope 1.1 This test method covers the determination of known impurities in, and the purity of p-xylene by gas chromatog raphy (GC). It is generally meant for the analysis ofp-xylene of 99 % or greater purity. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 D4588 Guide for the Analysis ofp-Xylene2 E 260 Practice for Packed Column Gas Chromatography3 E 355 Practice for Gas Chromatography Terms and Relationships3 E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method4 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.I2005 3. Summary of Test Method 3.1 A known amount of an internal standard is added to a sample of p-xylene. The prepared sample is mixed and analyzed by a gas chromatograph equipped with a flame ionization detector (FID). The peak area of each impurity and the internal standard is measured. The amount of each impurity is calculated from the ratio of the peak area of the internal standard versus the peak area of the impurity. Purity by GC (the p-xylene content) is calculated by subtracting the sum of the impurities found from 100.00. Results are reported in weight percent. 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee Dld.OA on Benzene, Toluene, Xylenes, Cyclohexane and Their Derivatives. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 3798 - 79. Last previous edition D 3798 - 83I. 2 Annual Book ofASTM Standards, Vol 06.03. 3 AnnualBook ofASTM Standards, Vol 14.01. 4 Annual Book ofASTM Standards, Vols 06.03 and 14.02. s Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 4. Significance and Use 4.1 This test method is suitable for setting specificatio on p-xylene and for use as an internal quality control too" where p-xylene is produced or is used in a manufacturiq process. It may also be used in development or research i involving p-xylene. It is generally applied to determimi^' those commonly occurring impurities such as nonaromatFq,. hydrocarbons, benzene, toluene, ethylbenzene, w-xylen" o-xylene, and cumene (isopropylbenzene). 4.2 Purity is commonly reported by subtracting the det4|j[ mined expected impurities from 100.00. However, a gas:-^ chromatographic analysis cannot determine absolute pu if unknown components are contained within the mate-' being examined. Absolute purity of p-xylene can be dejjf mined by measuring the freezing point depression. Refer to',, Guide D 4588 for determining other chemical and physical properties of p-xylene. 5. Interferences f 5.1 The Internal standard chosen must be sufficiently^ resolved from any impurity and the p-xylene peak. 6. Apparatus 6.1 Gas Chromatograph--Any chromatograph having flame ionization detector that can be operated at th conditions given in Table 1. The system should have suf ficient sensitivity to obtain a minimum peak height response! for a 0.001 weight % impurity twice the height of the signal) background noise. 6.2 Columns--Both capillary and packed columns haw been found satisfactory. The columnTBust _give satisfactory resolution Of"the internal standard from p-xylene and the impurity peaks. Complete resolution of ethylbenzene and m-xylene from p-xylene is difficult and can be considered adequate if the distance from the baseline to the valley between peaks is not greater than 50 % of the peak height of the impurity. Table 1 contains a description oftwo columns that have been found satisfactory. 6.3 Recorder--Electronic integration is recommended. Tangent skimming capabilities are required because of the difficulty in fully resolving impurities from p-xylene. 6.4 Microsyringe, 100-p.L capacity. 6.5 Volumetric Flask, 100-mL capacity. 7. Reagents 7.1 Purity ofReagent--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that ail reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem- 702 DU P050296264 D 3798 j-ABLE 1 Instrument Conditions for p-Xylene Analysis ' g Ijig fused silica |jnary phase polyethylene glycol'4 sntratlon (weight not applicable stainless steel diisodecylphthalate 3.5 %)3.5 % |s support ihsize ft thickness, p. h, m jpa diameter, mm crossllnked not applicable 0.25 50 0.32 flux-calcined diatomitec 60 to 80 not applicable 6.1 3.2 nature, C: 200 200 60 200 200 60 n-undecane n-octane arbowax 20M, a trademark of Union Carbide Corp., 39 Olde Ridgebury Rd., ISiry, CT 06817, has been found satisfactory for this purpose. Bentone 34, a trademark of National Lead Co., has been found satisfactory pis purpose. * hromosorb W, a trademark of Manville Sales Corp. Filtration and Minerals, (Box 5103. Denver, CO 80217-5108, has been found satisfactory for this Society, where such specifications are available.6 Other pies may be used, provided it is first ascertained that the gent is of sufficiently high purity to permit its use without lening the accuracy of the determination. 7.2 High Purity p-Xylene (99.99 % or greater purity)-- ibst p-xylene is available commercially at a purity less than p weight %, but can be purified by recrystallization. To pare 2 qt of high purity p-xylene, begin with approxi- pely 1 gal of reagent grade p-xylene and cool in an ilosion-proof freezer at --10 10C until approximately |to 3A of the p-xylene has frozen. This should require about I. Remove the sample and decant the liquid portion. Allow Is p-xylene to thaw and repeat the crystallization step on the Imaining sample until the p-xylene is free of contamination ^indicated by gas chromatography. 1.3 Carrier Gas--Chromatographic grade nitrogen or he lm. '.4 Pure Compounds for Calibration, shall include mllene, o-xylene, toluene, ethylbenzene, isopropylbenzene nene), and K-nonane. The purity ofall regents should be or greater. If the purity is less than 99 %, the concen- |ttion and identification of impurities must be known so at the composition ofthe standard can be adjusted for the |esence of the impurities. r.4.1 InternalStandard--K-Undecane (NC11) is the recamended internal standard of choice for Conditions A and loctane (NC8) for Conditions B in Table 1. However, other Impounds may be found acceptable provided they meet the literia as defined in Sections 5 and 7.4. > Hazards 8.1 Consult current OSHA regulations and supplier's K 6 "Reagent Chemicals, American Chemical Society Specifications," Am. fjbemical Soc.. Washington, DC. For suggestions on the testing of reagents not Sited by the American Chemical Society, see "Reagent Chemicals and Standards," |y Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY. and the "United pates Pharmacopeia." TABLE 2 Typical Calibration Blend Component p-Xylene (see 7.2.1) Toluene Ethylbenzene m-Xylene o-Xylene Isopropylbenzene rj-Nonane 572.0 0.058 0.579 1.163 0.116 0.058 0.070 Density'4 0.857 0.662 0.863 0.860 0.876 0.857 0.714 Weight, g '490.2 0.050 0.500 1.000 0.102 0.050 0.050 Concentration, weight % 99.64 0.010 0.102 0.203 0.021 0.010 0.010 A Numbers are density in grams per millilitre at 25C. Material Safety Data Sheets for all materials used in this test method. 9. Sampling 9.1 Refer to Practice D 3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this test method. 10. Preparation of Apparatus 10.1 The method used to prepare packed columns is not critical provided that the finished column produces the desired separation. 10.2 Follow manufacturer's instructions for mounting and conditioning the column into the chromatograph and adjusting the instrument to the conditions described in Table I. Allow sufficient time for the equipment to reach equilib rium. See Practices E 260 and E 355 for additional informa tion on gas chromatography practices and terminology. 11. Calibration , 11.1 Prepare synthetic mixtures ofp-xylene with represen tative impurities on a weight basis. Weigh each hydrocarbon impurity to the nearest 0.0001 g. Refer to Table 2 for an example of a typical calibration blend. -Nonane will repre sent the nonaromatic fraction. 11.2 Using the exact weight, or alternatively the exact vol umes and densities (see Table 2), calculate the weight % con centration for each impurity in each calibration, blend of II.l. -- 11.3 Into a 1.00:mL volumetric flask, add 100.0 pL of n-undecane to 99.90 mL of the calibration blend; mix well. Assuming a density of 0.861 g/mL for the p-xylene blend and 0.740 g/mL for NCI 1, the resulting NCI 1 concentration will be 0.086 weight %. 11.4 Inject the resulting solution from 11.3 into the chro matograph. A typical chromatogram is illustrated in Fig. ,1. 11.5 Determine the response factor for each impurity relative to NCI 1 by measuring the area under each peak and calculate as follows: ' ~ (QW,) where: R, = response factor for impurity i relative to the internal standard, Ai = peak area of impurity i, As = peak area of the internal standard, Cs = concentration of the internal standard, weight %, and Q = concentration of impurity i, as calculated in 11.3, weight %. 703 DUP050296265 # D 3798 P-XU. 13.is H-XYL ifi/sa MNCll 12.44 \ E-0EWZ 15.49" 3 N-AfW 6^1 TX. 10\74 C9MW lj/2S -A t -t -t -t 7.0 9.0 11.0 r~T"'" 13.0 i--|--i--r-- I--T r~ ss.o 17,0 MINUTES i--t -t - 19.0 FIG. 1 p-Xylene Analysis using Conditions A In Tattle 1 21.0 r-7-T 23.0 11.6 Calculate the response factors to the nearest 6.001. 12. Procedure 12.1 Pipet 100.0 jxL of internal standard into a 100-mL volumetric flask and dilute to the mark with the sample to be analyzed. Mix well, 12.2 Depending upon the actual chromatograph's oper ating conditions, charge an appropriate amount of sample into the instrument, 12.3 Measure the area of all peaks except p-xylene. Measurements on the sample must be consistent with those made on the calibration blend. Sum and report the nonaro matic fraction as a total area. A poorly resolved peak; such as m-xylene will often require a tangent skim from the neigh boring peak. Make consistent measurements on the sample and calibration chromatograms for tangents or poorly re solved peaks. A typical chromatogram is shown in Fig. 1. 13. Calculation 13.1 Calculate the amounts of each individual impurity. Total the concentration of all impurities. Calculate the p-xylene purity by the difference from 100.00. 13.2 Calculate the impurities as follows: r (WHQ 'W C, = 2C, where: C, = total concentration of all impurities, weight %. - ]?, 13.3 Calculate the purity ofp-xylene, P, in.weight percent^ as follows: 14. Report___ P-- 100.00 -- C, ~"'T~ 14.1 Report the following information: 14.1.1 Individual impurities to the nearest 0.001 weight%, . 14.1.2 For concentrations of impurities less than 0.001 weight %, report as <0.001 weight %, and consider as 0.000, in summation of impurities, 14.1.3 The total impurities to the nearest 0.01 weight %, J and 14.1.4 p-Xylene content to the nearest 0.01 weight %. 15. Precision and Bias 15.1 The following criteria should be used to judge the acceptability (95 % probability level) of results obtained by this test method. The criteria were derived from a round robin among 13 laboratories. The data were run on 2 days using different operators and three samples ranging in con centration from 99.0 to 99.8 weight %. Results of the round robin were analyzed in accordance with Practice E 691. 15.1.1 Results in the same laboratory should not be 704 DUP050296266 D 3798 ed suspect unless they differ by more than the ; shown in Table 3. On the basis of test error alone, Sference between two test results obtained in the same Story on the same material will be expected to exceed jue only about 5 % of the time. 1.2 Results submitted by each of two laboratories : not be considered suspect unless they differ by more : amount shown in Table 3. On the basis of test error the difference between two test results obtained in ent laboratories on the same material will be expected ed this value only about 5 % of the time. Bias--The results from the analysis by 13 different itories of a gravimetrically prepared blend ofp-xylene ates this procedure does not contain a measurable TABLE 3 Repeatability and Reproducibility No t e--This data was calculated after the removal of outliers using Method E 691. Variation of the p-xylene purity was determined from the variation of the calculated total purity. Precision was shown to be dependent upon purity of the material. Component Concentration Weight S Repeatability Reproducibility p-Xytene Nonaromatics Toluene Ethylbenzene m-Xylene o-Xytene 99.510 0.030 0.014 0.110 0.250 0.100 0.026 0.014 0.003 0.011 0.018 0.011 0.093 0.058 0.009 0.029 0.043 0.020 amount of bias nor systematic error that could contribute to a difference between a population mean and the accepted true value. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted m connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any sueh 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 reapproved or withdrawn. Yourcomments are invited eitherfor revision oftills standard or foredditlonal standards and should be addressed to ASTM Headquarters. Yourcomments 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. DUP050296267 i Designation: D 3799 - 89 Standard Test Method for Purity of Styrene by Freezing Point Method1 ;t -,( i This standard is issued under the fixed designation D 3799; 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 reapprovak. .. 1. Scope 1.1 This test method is used for determining the purity of styrene expressed as weight percent. All impurities are consictered to be ethylbenzene, ' ' 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 Us use. It is the responsibility of the user, of this, standard id establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 5 and 7.5. - 2. Referenced Documents 2.1 ASTM Standards: D 1015 Test Method for Freezing Point of High-Purity Hydrocarbons2 D1016 Test Method for Purity of Hydrocarbons from Freezing Points2 D1193 Specification for Reagent Water3 D3437 Practice for Sampling and Handling Liquid Cyclic Products4 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12005 * 3. Summary of Method 3.1 The purity of the styrene is determined by a measure ment of the freezing point of the sample in equilibrium with air at atmospheric pressure. The presence of small amounts of impurities causes a depression of the freezing point which is proportional to the molal concentration of the contami nating substances. The freezing point is the highest tempera ture obtained after the supercooling of the liquid. For purities over 99 % it is not necessary to plot a timetemperature curve. 3.2 The freezing point "methods. Methods D 1015 and D 1016, specified a platinum resistance thermometer for measuring the temperature. For routine work, mercuryin-glass thermometers are used. Other temperature-mea suring devices can be utilized in this method provided that they have temperature resolution to 0.0 PC or better. They must be calibrated since small differences in the tempera readings are significant. They must be .recalibrated aty once per week to correct for differences which may devekjl w\th.age arid handling.,To simplify the multiple calibiafiol the freezing point of,a lajge sample, of styrene is detg with a platinum resistance thermometer and the mere in-glass or other thermometers calibrated against standard styrene. Styrene may be kept in a deep freeze J$p8 several months with no appreciable change in the freezing,^ point. ', 4.' Significance and. Use. 4.1 Purity can be calculated by measuring the freeziu point and relating to' a freezing point for zero impurities. 4.2 This test method is in wide use for both producer and,? consumer for determining purity and is suitable for estab- fishing specifications. 4.3 All impurities are considered to be ethylbenzene. 5. Hazards < 5.1 Consult current OSHA regulations and suppliers Material Safety Data Sheets for all materials used in this tesf method. 6. Apparatus 6.1 Temperature-Measuring Devices--Temperature-mea suring devices can be used, provided they have temperature resolution to 0.01C or better, are operable in the range from -20 to -40C, and are calibrated against a platinum resistance thermometer. 6.2 Styrene Freezing Point Thermometer*?--Special de sign for determination of the freezing point of styrene as shown in Fig. 1 and described in Table 1 specification. 6.3 Freezing Point Apparatus7--See Fig. 2 which consists j of a 665-mL Dewar flask of borosilicate glass, a nest of three test tubes (16 by 150,20 by 150, and 25 by 150 mm), and a mechanically operated stirrer. All corks should fit tightly, and the hole for the stirrer shaft should be as small as practical. 6.4 Reciprocating-Type Stirrer8--A `/Win. rod formed into a coil of four turns of diameter to fit inside the 16 by 150-mm test tube and over the thermometer for immersion 1 This method is under the jurisdiction of ASTM Committee D-l6on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcom mittee DI6.0H on Styrene, Ethylbenzene, Cumene, and Naphthalene. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 3799 - 79. Last previous edition D 3799 - 84. 2 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book cfASTM Standards, Voi 06.03. 5 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 6 A thermometer meeting the specification is manufactured by the Precision Thermometer and Instrument Co., Southhampton Industrial Park, Southhampton, PA 18966, catalog No. 0230 (range: --33'C to -30*0. An equivalent may be used. 7 Available from Central Scientific Co., 1700 Irving Park Road, Chicago, IL. Catalog No. 15835B. An equivalent may be used. sCenco Catalog No. 18860 Vacuum Type Stirrer or Research Appliance Co., Allison Park, PA 15101, No. 601, portable reciprocating stirrer (not explosionproof), have been found suitable. An equivalent may be used. 706 DU P0502 96268 it:qilid above mercury 'nge and subdivision Intervals with auxiliary scale from ;ai length lersion ijatance from bottom of bulb to -33C mark fistance from top of thermometer to -30C mark ngth of unchanged capillary between the enlargement and the graduation f next below ngth of unchanged capillary above or below the 0C point pension chamber Jfnish (tap) Graduation Upeclal marking ale error mercury nitrogen gas -33.02 to --2S.98C ir O.C2C -0.2 to 0.2C 405 to 410 mm total plain front, enamel back, suitable thermometer tubing, diameter, 6 to 7 mm. Coming Normal or equally suitable thermometer glass, diameter 6 to 7 mm but not greater than that of stem; length, 50 to 60 mm. 125 to 140 mm ! 125 to 135 mm notless than 5 mm not lass than'15 mm to permit heating to at least 50C plain All lines, figures; and letters to be clear-cut and distinct. The graduation marks to be Sne, straight, of uniform width and perpendicular to the axis of the ... thermometer. Each degree and tenth degree tine to be longer than the intermediate ones. Graduations to.be numbered in fun at each degree mark : and In decimals at other multiples of0.2C. The- manufacturer's name or trademark, a serial number, and the words "total immersion"` shall bs etched on the stem. The error at any point on the scale shall not exceed 0.1 C. * The accuracy attainable with mercuty-in-glass thermometers, based on performance when al precautions are taken, for measurements of the kind for which these tlermometefs were designed, is from 0.01 C to 0.03C, and calibration corrections are stated to the nearest 0.01C. Subdivision In 0 D2C intervals, therefore, serves rindpally for the purpose of facilitating reading. |n styrene is used with either of these mechanical aids. 6.5 Thermometer, alcohol-type, used to read the tempera ture of the cooling bath. It should read as low as --70"C and be graduated in 1C subdivisions. Reagents 7.1 Purity ofReagents--Reagent grade chemicals shall be |ised in all tests. Unless otherwise indicated, it is intended at all reagents shall conform to the specifications of the tommittee on Analytical Reagents of the American Chem- 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 determination. 7.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Specification D 1193. 7.3 Carbon Dioxide, solid (dry ice), for cooling bath. 7.4 Cooling Liquid--1,1,1-trichloroethane is recom mended because it is nonflammable. No t e--A mechanical cooling device may also be used. 9 Reagent Chemicals, American Chemical Society Specifications, Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards,'' by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 7.5 Styrene Monomer Standard--Caution: While a standard inay be stored for several months in a deep freeze, it should be restandardized on a regular basis in accordance with Test Method D 1015. Standards maintained at 40C will change the purity in days. 8: Sampling ~ 8.1 Sample in accordance with Practice D 3437. 9. Procedures 9.1 Add approximately 10 mL of styrene to the sample tube and adjust the liquid level so that the top of the thermometer bulb will be immersed 20 mm when the bottom ofthe bulb is placed 10 mm above the bottom of the sample tube. Place sample tubes in the Dewar flask, con taining 1,1,1-trichloroethane cooled to about --45C. The 1,1,1-trichloroethane level should be at least 20 mm above the level ofthe styrene in the cooling cell. Maintain the bath temperature between -42 and -45C during the determina tion by cautiously adding dry ice, a small piece at a time. 9.2 Adjust the stirrer to 100 to 150 strokes per minute and maintain this rate throughout the determination. Adjust the stirring rod so that the bottom of the coil just touches the bottom ofthe test tube at full downward stroke. With proper adjustment, the top of the coil will not break the surface of the styrene at top of the upward stroke. 9.3 Alternative methods of cooling can be utilized other 707 DU P0502 96269 i # D 3799 STIRRER No. U NICHROMi WIRE COIL 11 x 16 MM. CORKS : TEST TUBES 16 x 150, 20 x ISO AND 25 x 150 MM. OEWAR UNSILVERED STYRENE MIXTURE FIG. 2 Styrene Freezing Point Apparatus 708 DUP050296270 D 3799 Jjfied in Section 9 provided that they yield a cooling Be styrene of 0.3 to 0.8C/min near the freezing Jicord the highest temperature obtained after the ag. Make readings to the nearest 0.0 TC. This is Irrected freezing point of the sample, btain the mercury or other thermometer corrections The freezing point of the standard styrene . with platinum resistance thermometer) is deter} above with the mercury or other thermometer. The between the freezing point of the standard styrene maximum temperature observed after freezing sithe correction to be applied to the thermometer. Example: at of standard styrene as determined by {resistance thermometer: bint ofstandard styrene as determined with | thermometer. Ixo be applied: -30.82'C --30.90C 0.08*C check a thermometer in constant use twice a week After being in use for six months or more, Ethe standardization about once a week. It has been 8 at the correction does not fluctuate up and down but es to move in one direction gradually giving lower j points. fhe thermometer correction is applied to the freezing ad the corrected freezing point is then converted to aty. fijculation ^ Calculate the styrene content of the sample as Styrene, weight % = 100 + 2.47 (t + 30.61) where: t - corrected freezing point of sample in *C. . 10.1.1 This equation is based on a value of --30.6 TC for the freezing point of pure styrene saturated with air at 1 atm (101 kPa). The factor 2.47 was calculated by assuming that all of the impurity in the styrene is ethylbenzene. The impurities may vary some according to the process and the ethylbenzene feed. Since most impurities are similar in structure with no wide variation in molecular weight the deviation from 2.47 is small. Some companies use 2.5, but this change makes little difference in the calculated purity. 10.2 Sample Calculation: Uncorrected freezing point Thermometer correction -30.84"C +0,08C -30.76-C Styrene, weight % = 100 + 2.47 (-30.76C + 30.61) = 99.63 11. Precision and Bias 11.1 The following data should be used for judging the acceptability of results (95 % confidence level): 11.1.1 Repeatability--Duplicate results by the same oper ator should not be considered suspect unless they differ by more than 0.043 % of actual amount. 11.1.2 Reproducibility--The results between two labora tories should not be considered suspect unless they differ by more than 0.092 % of actual amount. TheAmerican Society for Testing and Materials takes noposition respecting the validity ofanypatent 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, 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 It notrevised, either reapproved or withdrawn. Yourcomments are Invited either for revision of this standardor (or 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, 1316 Race St., Philadelphia, PA 19103. .1 709 DUP050296271 Designation: D 3852 - 90 Standard Practice for Sampling and Handling Phenol and Cresylic Acid1 This standard is issued under the fixed designation D 3852; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (() indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice is provided to ensure that phenol and cresylic acid are properly sampled to provide representative samples for quality assurance analyses and that they are handled in a safe manner. In general, this practice also applies to cresols, xylenols, and some other alkylated phe nolic materials; however, specific information regarding these materials should be sought and used if available. No t e 1: Precaution--Any person sampling or handling these prod ucts should have specific first aid instructions and equipment available for use in the event of personal contact or exposure. 1.2 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 Imitations prior to use. For specific hazard statements, see Section 8 and Notes 1 and 3. 2. Referenced Documents 2.1 ASTM Standard: E 300 Practice for Handling Industrial Chemicals2 2.2 Other Documents: Toxic Substances List Appendix I, 19753 OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 19I0.12004 U.S. DOT Regulations, 49 CFR Transportation, Subchap ters B and C, Parts 171 - 1794 3. Significance and Use 3.1 This practice is issued to provide information useful in establishing sampling and handling procedures. It is expected that this information will only be utilized in conjunction with an existing health and safety program. The information provided cannot be used as a substitute for expert safety and medical advice, but rather as*a supplement to such advice. 4. Description of Product 4.1 Phenol is a colorless to light pink crystalline material which melts at 40 to 4 TC (104 to 106"F). Technical and USP grades melt at lower temperatures. Interstate Commerce Commission Regulations list phenol as a Class B poison 1 This practice is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0J on Handling and Sampling. Current edition approved May 25, 1990. Published August 1990. Originally published as D 3852 - 79. Last previous edition D 3852 - 83. 2 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 3 United States Department of Health, Education and Welfare. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. material and further describe it as "Carbolic liquid." 4.2 Phenol is both extremely hygroscopic and,sH discoloration. Therefore, it cannot be overemphasj proper precautions must be undertaken when unl| __ sampling the product. Moisture must be excluded. TL of sampling devices that contain metals that may ca? discoloration (iron, copper) must also be avoided. 4.3 Cresylic acid is a common chemical name app mixtures of alkyl-substituted phenols. Included are mi\ of cresols, xylenols, and higher alkylated phenols M cresylic acid mixtures contain measurable amount phenol. 4.4 Most cresylic acid mixtures are liquids at amb3 temperatures. However, at low temperatures (<0Cj sometimes become very viscous and difficult to pour.! mixtures containing high concentrations of high me isomers may form thick slurries or become solids temperatures. 4.5 While phenol or cresylic acid is highly da when handled improperly, particularly at the elevate peratures sometimes required to unload tank cars oil trucks, handling and sampling need not be ha provided the dangers are recognized. Proper precautio measures must be provided and scrupulously adhered 1 5. Hazards 5.1 Consult current OSHA regulations and su; Material Safety Data Sheets (MSDSs) for information ctmKj ceming safety, health, and personal protective equipment WSsk all materials utilized in this practice; -- 5.2 HealthsPhenol is very corrosive to the skin an, produces painful and dangerous burns in a very short time. Since phenol is a skin anesthetic, the first reaction is not pain, but a whitening of the exposed area. It is readily, absorbed through the skin and mucous membranes or lungs, and severe exposures may prove fatal unless prompt first aid'1 and medical treatment are exercised. Safety limits have been defined for phenol vapor as 5 ppm or 19 mg/m3 for an 8-h day exposure. Since severe injury or death may result from" excessive exposure to vapor or mist, adequate ventilation of working areas is imperative. It is therefore recommended that tank cars or tank trucks shall be unloaded in the open, rather than inside a closed building and workers shall wear appropriate protective clothing and personal protective equipment. 5.2.1 Qualitatively, cresylic acid is slightly less acute as a health hazard than phenol. However, contact of cresylic acid with the skin can produce painful and serious bums in a short time. It is readily absorbed through the skin and mucous membranes, through the gastro-intestinal tract, or 710 DUP050296272 D 3852 the lungs (either as a vapor or in droplet form), Bally resulting in systemic poisoning. Although no I limits have been defined for cresylic acid vapor, severe jr or death can result from excessive exposure to high otrations of the vapor or mist, or prolonged exposure concentrations. Therefore, adequate ventilation of teas is imperative. In the absence of more definitive | the vapor limit shall be taken to be the same as for |S, that is, 5 ppm (maximum, 8 h "time-weighted e" basis) as listed in Appendix 1 of the 1975 "Toxic nces List." g%Fire--Cresylic acid parallels phenol in its fire hazard ties, being somewhat less hazardous due primarily to : vapor pressure at any given temperature. Phenol is in Category 2 of the NFPA 704M fire hazard Scation system (Note 2) while m- and p-cresols are in 1. Phenol and cresylic acid are combustible and sable; toxic vapor will be given off at elevated temperI should this material become involved in a fire. Water or spray), carbon dioxide extinguishers, foam, and dry Ileal extinguishers are effective in fighting fires involving pi and cresylic acid. |i XE 2--For full description of NFPA categories, see NFPA publi- I; No. 704-969.5 Classification runs from 0 (no hazard) to 4 (very dous). Molten phenol or cresylic acid dissolves carbon diand releases it on solidification. Therefore, special lutions shall be observed if "inert gas" containing fh dioxide is used to agitate or empty containers of bl or cresylic acid to avoid pressure build-up (for ||)le, leave vents open). protective Equipment No personal protection equipment is an adequate litute for safe working conditions and intelligent conduct fie part of employees who work with phenol or cresylic ^Employees who work with phenol or cresylic acid |d be well trained and should maintain safe working Sons. | Persons engaged in the handling of phenol or cresylic ill use protective equipment as dictated by the extent jfeir exposure. The worker shall always wear chemicalpafety goggles and chemically impermeable gloves, as a lum. Depending upon circumstances, additional perprotection may be advisable, including face shield, per shoes or boots, rubber aprons or acid-proofsuits, and itrial gas masks or fresh air masks. Wearing full protecISlothing is recommended when sampling tank cars, tank is, barges, ships, drums, process lines and process Jls. Working areas shall have immediately available ge-type safety showers, easily accessible, plainly marked, ^controlled by quick-opening valves. In addition, there I be at hand a water hose that will deliver clean water at derate pressure. A small stream, such as from an lash fountain, is recommended for washing eyes (see WFPA Publication No. 704.969, National Fire Prevention Assn. 7. First Aid 7.1 The establishment of first aid procedures must be done prior to sampling and handling of phenol and cresylic acid under the guidance of competent safety and medical advice. 7.2 The first aid procedures established should include, but not be limited to, the following considerations: 7.2.1 Speed in removing phenol or cresylic acid from the skin in case of accidental contact is of primary importance. 7.2.2 It is extremely important to immediately place under a physician's care any person injured by skin contact, inhalation, or ingestion of phenol or cresylic acid. 8. Precautions 8.1 Conduct sampling and handling operations only by carefully instructed, experienced, reliable employees, under adequate supervision. 8.2 Accomplish loading, unloading, and sampling opera tions only when adequate lighting is provided. 8.3 Take extreme care to avoid spills and leaks. In case of a spill, wash contaminated areas thoroughly with large quantities of water and collect the liquid in the local chemical waste system. 8.4 Follow shipper's instructions always, and read and observe all caution markings on containers. 8.5 Although the vapor given off at elevated temperatures from phenol or cresylic acid will ignite, these materials can generally be handled with little direct danger of fire. The flash points ofthe liquids are higher than the temperatures at which they are normally handled. In spite of this, carefully restrict open flames and smoking in the vicinity of loading, unloading, and storage operations. 8.6 Do not permit any person ever to enter an empty phenol or cresylic acid tank, tank car, or tank truck until it has been thoroughly washed out with warm water, followed by a thorough steaming. Ensure that oxygen content is acceptable and vessel is free of organic vapors. Require theapproval and observation by a supervisor in every case. Review Sections 6 and 7 in detail. 8.7 Allow no eating or drinking in close proximity to the phenol or cresylic acid handling or sampling-operation. 8.8 Employees shall: 8.8.1 Know the hazards connected with the handling of phenol and cresylic acid; 8.8.2 Be completely acquainted with the purpose, use, and maintenance of personal protective equipment; 8.8.3 Be trained to report promptly to supervision all suspected leaks or equipment failures; 8.8.4 Be trained to recognize and report any symptoms of systemic poisoning or skin contact; be thoroughly trained in the proper procedures for administering first aid and for obtaining professional medical help; 8.8.5 Know and routinely practice the accepted methods of sampling and handling phenol or cresylic acid in order to avoid spilling or splashing, leaks, skin contact, vapor or mist inhalation, or ingestion; 8.8.6 Be completely familiar with the location and opera tion of safety showers, eye baths, hose lines, and all other first aid equipment; and 8.8.7 Know the importance of personal cleanliness and the necessity for immediate removal of clothing contami nated with phenol or cresylic acid. 711 DUP050296273 D 3852 9. Handling and Sampling of Drums 9.1 Before loading, unloading, or sampling of drums of phenol or cresylic acid, carefully read and proceed in accordance with Sections 4 through 8. 9.2 Handle drums carefully when being transported. Block drums in place during transportation to prevent movement and during unloading to prevent spilling. 9.3 Place the drum bung up, loosen the plug slowly to relieve internal pressure, and allow all internal pressure to vent prior to unloading or sampling. 9.4 Most cresylic acids are liquids at ambient tempera tures. Phenol and some cresylic acids are solids at ambient temperatures. If melting is necessary to remove the contents ofa drum, do the necessary heating in a special steam-heated melting chamber, hot-water bath, with steam coils, or with an approved electric drum heater. Never use a flame for melting the drum contents. Properly vent the drum during this operation in order to prevent pressuring. No t e 3: Warning--Do not overheat drums as the danger of spillage caused by thermal expansion and excessive vapors exists. 9.5 Prior to sampling, mix the contents of the drum thoroughly in order to ensure uniformity of the material. This may be accomplished by mechanical agitation or sparging with inert gas (nitrogen is recommended). Exercise extreme caution to prevent pressurization or splashing if inert gas sparging is used. 9.6 Obtain the sample in accordance with Practice E 300. In summary, accomplish sampling by using a clean, dry glass or polypropylene sample tube (see 12.6) and a clean, dry, glass or other appropriate container of appropriate size. The closure shall be a screw cap fitted with a polyethylene or other inert liner. Label the sample bottle to indicate, as a minimum, the date and time, source of sample, type of material, and the name of the sampler and in accordance with OSHA regulations. 9.7 Unload by any convenient, safe method, including gravity flow and pumping. Pressure unloading of drums is not recommended. Take full precautions to protect personnel and equipment from the effects of a possible drum rupture. 10. Unloading of Tank Cars and Tank Trucks 10.1 Before unloading or sampling tank cars or tank trucks of phenol or cresylic acid, carefully read and proceed in accordance with Sections 4 through 8. 10.2 Always follow shipper's instructions, and place, read, and observe all caution markings on the sides of the tank or dome. 10.3 Brakes must be applied, warning signs in place, chocks in place, and ground or bonding wire, or both, attached before any operation begins. Follow normal derail ment procedures. 10.4 In the event of a tank or fitting failure or leak, immediately notify your supervisor. Take whatever appro priate action is deemed necessary to prevent injury to personnel or damage to equipment (see 8.3). 10.5 Top Unloading by Pumping: 10.5.1 Verify that the contents of the tank car or tank truck are designated for storage in the tank you will be unloading to. Verify that adequate storage volume is avail able in the storage tank and that the tank is vented before connecting the unloading line. 10.5.2 Carefully open the vent on the tank car truck and leave the vent open during loading and unload* In case the dome is not equipped with an air inlet \oni ' by carefully opening the manhole cover. Do not confu' air inlet nozzle with the eduction or siphon pipe conm 10.5.3 Verify that no solid has formed in the tank tank truck due to unusually low temperatures oi a concentration of a high melting isomer. In cases ot formation or highly viscous materials, heating of the, tents of the tank is recommended. This is accompli application of low-pressure steam to the heating coils of cars and trucks so equipped or through the use of ins bayonet heaters. If a crust has formed, use insert or heaters to melt the crust prior to proceeding with hearing entire contents of the container. The use of mechajuSj agitation or inert gas (preferably nitrogen) sparging is mended to facilitate this operation. Follow proper provi for venting during this operation. Hold heating and m y to a minimum in order to avoid color degradation ofJi phenol or cresylic acid. Discontinue these operations pnpij unloading or sampling. TM 10.5.4 After completing the recommendations in 19 through 10.5.3, connect the discharge side of the unload pump to the line leading to the storage tank. Connect], suction side of the unloading pump to the eduction orsif* pipe on top of the dome. In the absence of such a perm: pipe, insert a clean stainless steel or nickel pipe of aj, priate size through the manway opening to the bottom off] tank car or tank truck and connect the free end to' suction side of the pump. No t e 4--Transfer lines and associated valves should be preUsjH; with low-pressure steam to facilitate unloading. 10.5.5 Open the appropriate valves in the transfer i between the tank car (or tank truck) and the pumpfl between the pump and the storage tank and start the pi 10.5.6 After all the phenol or cresylic acid has.discharged, shut off the pump and close the unloading valves at the receiving tank and at the tank car (or tn Either drain the lines or blow them clear with compress* or nitrogen to the tank or waste recovery-drain designatf your supervisor-T-If compressed air (or nitrogen) is used, < the air supply when the unloading line is clear and vent| unloading line. Disconnect the compressed air line. Close transfer line valves; disconnect the transfer lines from tl tank car (or truck), pump, and storage tank; and thoroug wash all traces of phenol or cresylic acid from the pipe e^g and fittings. 10.5.7 Disconnect the steam and condensate piping to 1 tank car heating coils. Blow the coils out with compressed s in order to remove condensate and prevent freezing ofpipe* Do not replace steam inlet and outlet caps; let them ha free by their safety chains so as to permit drainage of 1 pipes. Close all tank car dome openings, vents, and bottom j outlet plugs. 10.6 Top Unloading by Pressurization: 10.6.1 As a less desirable alternative to the use of .41 transfer pump for top unloading of material, the pressure#jj tion ofthe tank car or truck with compressed air or nitrogen.jj to force the cresylic acid out may be used where the I pressure of the receiving vessel can be overcome within the jj 712 DU P050296274 # D 3852 ded unloading pressure limits. If this is done, iecial emphasis on the inspection of the tank and its |or evidence of leaks or defects and its maximum fating. Unloading pressure shall never exceed a gage f 25 psi (172 kPa) or the maximum pressure rating, rer is less. The air or nitrogen line must be equipped heck valve and a shut-off valve, a pressure-redudng- ing valve set at 20 psi (138 kPa), a safety relief valve to 25 psi (138 to 172 kPa), and a vent valve. Vent the tank car or truck and inspect for the of solids (see 10.5.3); if solids are present, heat and material until the solids are melted. 6 Connect the discharge line to the eduction pipe. > Make sure the storage tank is vented and has it empty volume. i Close the tank car or truck venting and attach the fessed air or nitrogen supply line to the air inlet nozzle. .6 Open the appropriate discharge line valves and apply air or nitrogen pressure to the tank car or truck, the air or nitrogen pressure to 20 psi (138 kPa) and n it until the tank car and discharge lines are empty. 7 Close the receiving tank valve, shut off the air or in supply line valve, and open the relief valve. 8 Verify that the lines are depressurized, then disconie air or nitrogen supply line, the discharge line, and ighly wash all material from pipe ends and fittings. 9 Close the tank car or truck dome openings. .10 Disconnect the steam and condensate piping to ik car or truck heating coils. Blpw out the coils with issed air in order to remove condensate and prevent up during cold weather. Do not replace steam inlet itJet pipe caps; let them hang by their safety chains so srmit drainage of the pipes. Bottom Unloading by Pumping: .1 Bottom unloading of molten phenol or cresylic gncreases the possibilities of spillage or spraying the Itor. Observe extra caution to prevent this occurrence. 2 If it is necessary to unload molten phenol or ic acid through the bottom outlet, install an auxiliary iff valve in the bottom outlet leg. 3 Verify that the unloading line is properly attached designated storage tank, that the storage tank is and that sufficient storage volume is available to hold [intents of the car or truck being unloaded. ',7.4 Carefully open the vent on the tank car (or track) iase any pressure that may have IniHt up. .5 Open the manway and visually inspect the contents ie presence of solids. If solids are noted, proceed as icted in 10.5.3. '.7.6 Be sure the bottom interior valve is closed tight by :ng the top operated valve rod clockwise on top of the [Verify this by placing a container under the plug on the |om outlet leg and loosening the plug. Allow any trapped hoi or cresylic acid to drain into the container. Do not pve the plug entirely until you are certain that the inside | is holding. 1.7.7 Ifthe outlet leg is equipped with an auxiliary valve, it it carefully to allow any trapped phenol or cresylic acid in into the container. If there is no bottom auxiliary |e, connect one to the bottom outlet leg. Close the iliary valve. 10.7.8 Attach the unloading line to the auxiliary outlet valve. This line must have a drain valve. Make sure the drain valve is closed. 10.7.9 Open the outside auxiliary shut-off valve. 10.7.10 Open the inside bottom outlet valve and pump or drain molten phenol or cresylic acid from the tank car (or truck). 10.7.11 Close the inside bottom outlet valve; open the drain valve and drain the bottom outlet leg into the container. 10.7.12 Close the outside auxiliary shut-off valve and the receiving-tank valve, drain the unloading lines or blow them clear of phenol or cresylic acid with compressed air or nitrogen to the tank or waste-recovery drain designated by your supervisor. If compressed air (or nitrogen) is used, close the air or nitrogen supply when the unloading line is clear and vent the unloading line. Disconnect the compressed air or nitrogen line. 10.7.13 Close all transfer-line valves; disconnect the transfer lines from the tank car (or truck), pump, and storage tank; and thoroughly wash all traces of phenol or cresylic add from the pipe ends and fittings. 10.7.14 Disconnect the steam condensate piping to the tank-car heating coils. Blow the coils out with compressed air or nitrogen in order to remove condensate and prevent freezing of pipes. Do not replace steam inlet and outlet caps; let them hang free by their safety chains so as to permit drainage of the pipes. Close all tank-car dome openings, vents, and bottom-outlet plugs. 10.8 After unloading is completed, by whatever means, remove chocks, safety signs, and ground wire. 10.9 Tank Cars--Turn the "Poison" placards for empty phenol tank cars to "Residue Poison." Turn the "Corrosive" placards for empty cresylic add tank cars to "Residue Corrosive." 10.10 Tank Trucks--Return tank tracks with "Poison" placards (for phenol) or "Corrosive" placards (for cresylic add) in place as received. 11. Sampling of Tank Cars and Tank Trucks 11.1 Sample tank cars or tracks in accordance, with Practice E 300. Any method of sampling therein described that provides a representative sample is acceptable. Among these are "Average Sample," "All-Level Sample," "Con tinuous Sample," and "Running Sample." 11.2 A suitable sample bottle is a 1-pt (0.4-L) narrow neck glass bottle known as a "Boston Round." The closure shall be a screw cap fitted with a polyethylene or other inert liner. 11.3 Sampling shall be done after heating or mixing,, or both, or during unloading (in the case of a continuous sample). 11.4 Place emphasis on the use of clean and dry sampling equipment and sample bottles. 11.5 Immediately after the sample bottle is filled, screw the cap on tightly before making any attempt to rinse off phenol or cresylic add from the outside. Label the sample as with dram samples (See 9.6). 12. Storage 12.1 Refer to Sections 4 through 8 regarding the haz ardous properties of phenol or cresylic acid before at tempting any storage. 713 DUP050296275 # D 3852 12.2 Heat tracing of tank vents and relief devices is recommended to keep vapors from solidifying and blocking those devices. Heat tracing of storage vessels is recom mended to keep material in liquid form. 12.3 The choice of construction materials for storing phenol or cresylic acid depends on the color requirements in conjunction with the end use. 12.4 Preservation of color of high-purity phenol or cresylic acid is best accomplished in vessels constructed of stainless steel or lined carbon steel (glass, nickel, inorganic zinc coating, or baked phenolic resins are suitable materials for linings).. 12.5 When color of the phenol or cresylic acid is not important, vessels of ordinary carbon steel serve satisfacto rily. Phenol and cresylic acid have no appreciable corrosive activity on mild steel at the temperatures Son tered in transportation and storage. 12.6 Hot phenol and cresylic acid readily at' such as copper, aluminum, magnesium, lead Therefore, these metals and their alloys are mended for use in phenol cresylic add storage^!.,, 12.7 Molten phenol and cresylic acid dissolved many organic polymers. It is recommended that i testing be done to determine the stability andi-1 resistance of any polymer prior to its use as a lining 13. Barges and Tankers 13.1 Barges and tankers are sampled and han' manner similar to top unloading of tank cars and tar (10.5). The American Society tor Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly 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 committeB and must be reviewed every five years and ifnot revised, altherreapproved or withdrawn. Yourcomments are invited eitherfor revision ofthis standard orfor,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 feel that your comments have not received a fir hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. :n 714 DUP050296276 n Designation: D 3961 - 89 Standard Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry1 This standard is issued under the fixed designation D 3961; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. pope This test method covers the determination ofsulfur in nge from 0.5 to 100 mg/kg in aromatic hydrocarbons. The test method may be extended to higher sulfur entrations by appropriate dilution. This standard may involve hazardous materials, oper<s, and equipment. This standard does ndt purport to fess all ofthe safety problems associated with its use. It is ^responsibility of the user of this standard to establish Jopriale safety and health practices and determine the mobility of regulatory limitations prior to use. For flic hazard statements, see Section 7. Referenced Document ^ ASTM Standards: >329 Specification for Acetone2 3437 Practice for Sampling and Handling Liquid Cyclic oducts2 'Other Document:3 SHA Regulations, 29 CFR, paragraphs 1910.1000 and P1910.12003 ummary of Test Method |.~1 A liquid sample is injected into a combustion tube ntained at about 800C having a flowing stream of gas lining about 80 % oxygen and 20 % inert gas (for nple, nitrogen, argon, etc.). Oxidative pyrolysis converts fsulfttr to sulfur dioxide which then flows into a titration Iwhere it reacts with triibdide ion present in the electro|. The triiodide thus consumed is coulometrically replaced the total electrical work required to replace it is a sure of the sulfur present in the sample injected. 1:2 The reaction occurring in the titration cell as sulfur xide enters is: If + S02 + H20 -> S03 + 31- + 2H+ t triiodide ion consumed in the above reaction is gener1 coulometrically thus: 31- . If + 2e" 1.3 These microequivalents of triiodide (iodine) are equal he number of microequivalents of titratable sample ion I This test method is under the jurisdiction of ASTM Committee D-16 on >matic Hydrocarbons and Related Chemicals and is the direct responsibility of [committee D16.0E on Instrumental Analysis. at edition approved Nov. 24, 1989. Published January 1990. Originally ishcd as D 3961 - 80. Last previous edition D 3961 - 80 (1985)`!. Annual Book ofASTM Standards, Vol 06.03. Available from Superintendent of Documents, U.S. Government Printing !, Washington, DC 20402. entering the titration cell. The unknown sample is compared to a known sample and the appropriate calculations made to report the sulfur concentration. It is important that the sulfur content ofthe known sample be within a factor of two ofthe unknown sample. 4. Significance and Use 4.1 Total sulfur concentrations are typically required for benzene, toluene, and xylenes used as chemical intermedi ates in solvents. This test may be used for both final product inspections and process control. 4.2 This test method is believed to be applicable in the presence of total halide concentrations of up to 10 times the sulfur concentration and total nitrogen concentrations of up to 1000 times the sulfur concentration. 4.3 This test method is not applicable in the presence of total heavy metal, concentrations (for example, Ni, V, Pb, etc.) in excess of 500 mg/kg. No t e 1--To attain the quantitative accuracy of which method is capable, stringent techniques must be employed to prevent all possible sources of contamination. ^ 5. Apparatus4 5.1 Pyrolysis Furnace--The sample shall be pyrolyzed in an electric furnace having at least two separate and indepen dently controlled temperature zones, the first being an inlet section that can maintain a temperature sufficient to vola tilize all the organic sample. The second zone' Shall be a pyrolysis section that can maintain a temperature, sufficient to pyrolyze the organic matrix and oxidize all the organically bound sulfur. A third outlet temperature zone is required. A flow diagram of the complete instrument is shown in Fig. 1. 5.1.1 Pyrolysis furnace temperature zones for hydrocar bons should be variable as follows: Inlet zone Center pyrolysis zone Outlet zone up to at least 70CTC up to at least 900"C up to at least SOO'C Precondition the furnace in accordance with manufacturer's instructions. 5.2 Pyrolysis Tube, fabricated from quartz and con structed in such a way that a sample, which is vaporized completely in the inlet section, is swept by an inert gas into the pyrolysis zone where it mixes with oxygen and is burned. 4 The apparatus described in 5.1 to 5.5 inclusive is similar in specifications to equipment available from Rosemont Analytical Division, Dohrmann, Santa Clara, CA 95052. For further detailed discussions, in equipment, see: Preprints-Division of Petroleum Chemistry, American Chemical Society, Vol 1, No. 3, Sept. 7-12, 1969, p. B232, "Determination of Sulfur, Nitrogen, and Chlorine in Petroleum by Microcoulometry." by Harry V. Drushel. 715 DUP050296277 \ # D 3961 FIG. 1 Flow Diagram of Pyrolysis Furnace, Titration Cell, Microcoulometer, and Recorder The inlet end of the tube shall hold a septum for syringe introduction of the sample and side arms for the introduc tion of oxygen and inert gases. The center or pyrolysis section shall be of sufficient volume to ensure complete pyrolysis of the sample. A sketch of the pyrolysis tube is shown in Fig. 2. Pack the quartz exit tube with 0.5 in. (12.7 mm) of quartz wool and fit it into the rear of the pyrolysis tube so that the quartz wool is nearest the hot zone. 5.3 Titration Cell, containing a sensor-reference pair of electrodes to detect changes in triiodide ion concentration and an inlet for a gaseous sample from the pyrolysis tube. The sensor electrode shall be platinum foil and the reference5 TM electrode platinum wire in a saturated triiodide half-cell Tfc*? generator anode and cathode half-cell shall also be platinunjffoif The titration cell shall be placed on a suitable maj i, j n. stirrer. '( 1 No t e 2: Caution--Excessive speed will decouple the stirring bar,' causing it to rise in the cell and damage the electrodes. The creatit n , slight vortex is adequate. ' 5.4 Microcoulometer, having variable attenuation, g control, and capable of measuring the potential of' sensing-reference electrode pair, and comparing this po- Section Section 'B-'B* Section 'C-'C* 12/5 Mole Soil Joint- -IS/9 Female Boll Joint rOuort2 Wool '~T--, mmm /\ * Indents For Quartz Wool Pocking f "0" Ring| 60mm Adopter For Connection of Pyrolysis Tube To Coulometric Ceil 110 mm l otat Length Detoil -`O' Detoit -*E` FIG. 2 Pyrolysis Tube Detail 716 ' "Vi DUP050296278 # D 3961 [a bias potential, amplifying the potential difference orking-auxiliary electrode pair so as to generate a Jso the microcoulometer output voltage signal shall irtional to the generating current. Recorder, having a sensitivity to at least 0.1 mV/in. speeds of xh to 1 in./min (13 to 25 mm/min). Use |able electronic or mechanical integrator is recomt but optional. Rampling Syringe--A microlitre syringe of 10-pL capable of accurately delivering 1 to 10-p.L of |mto the pyrolysis tube. 3-in. by 26-gage (76 by a) needles are recommended to reach the inlet zone olysis furnace. 3--Since care must be taken not to overload the pyrolyzing f the tube by too fast a sample injection rate, means should be Nor controlling the sample addition rate (0.1 to 0.2 gL/s). gents and Materials flinty ofReagents--Reagent grade chemicals shall be all tests. Unless otherwise indicated, it is intended reagents shall conform to the specifications of the litee on Analytical Reagents of the American Chemefety, where such specifications are available.5 Other |!tnay be used provided it is first ascertained that the :is of sufficiently high purity to permit its use without bjg the accuracy of the determination. |Purity of Water--The water used in preparing the cell jjtyfe should be demineralized, distilled, or both. Water Ipurity is essential. i A--Distilled water obtained from all borosilicate glass still, fed Idemineralizer, has proven satisfactory. mcetic Acid (sp gr 1.05)--Concentrated acetic acid 30H). I'Acetone (CH3COCH3), Specification D 329. WiArgon, Helium, dr Nitrogen, high-purity grade (HP) ^5), used as carrier gas. 5--High-purity grade gas has a minimum purity of 99.995 %. Cell Electrolyte Solution--Dissolve 0.5 g of potassium I (KI) and 0.6 g of sodium azide (NaN3) in approxi- 500 mL of high-purity water, add 5 mL of acetic acid !OOH), and dilute to 1000 mL. Gas Regulators--Two-stage gas regulators must be pn the reactant and carrier gas. Hydrofluoric Acid (HF), 1 4-^1 mixture with water, ixact mix is not critical since it is used in cleaning iment. The use of HF should be minimized because of considerations. Iodine (I), 20-mesh or less, for saturated reference ode. Isooctane (Note 6) (2,2,4-trimethyl pentane). 6 --Pesticide test grade such as Mallinckrodt "Nanograde" ne has been found satisfactory. Reference fuel 140 is acceptable i the sulfur concentration is below 10 % of the samples being d. An optional step is to percolate the sample through silica gel. Reagent Chemicals, American Chemical Society Specifications," Am. Chem, Washington, DC. For suggestions on the testing of reagents not listed by nican Chemical Society, see "Reagent Chemicals and Standards," by i Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States nacopeia." No t e 7--The most reliable solvent is a sulfur-free form ofthe sample type to be analyzed. Alternatively, use a high-purity form ofcyclohexane boiling point 80C (!76F). It is desirable that the solvent has some structural similarity to the sample. No t e 8--The analyst may choose other sulfur compounds for standards appropriate to sample boiling range and sulfur type which cover the concentration range of sulfur expected. It is imperative, however, that the sulfur content of the standard is within a factor of 2 of the sulfur content ofthe sample. 6.11 Oxygen, high-purity grade (HP) (Note 5), used as the reactant gas. 6.12 Potassium Iodide (KI), fine granular. 6.13 Sodium Azide (NaN3), fine granular. 6.14 Dim-butyl Sulfide (CH3CH2CH2CH2)2S or dibutyl disulfide (CH3CH2CH2CH2S)2. 6.15 Sulfur, Standard Stock Solution (approximately 300 ppm)--Weigh accurately 0.5000 g of di-n-butyl sulfide into a tared 500-mL volumetric flask. Dilute to the mark with wooctane and reweigh. ,,. D x 0.2187 x 106 S, mg/mg = -- ---------------------- where: D = di-n-butyl sulfide, g, and B = (di-n-butyl sulfide + solvent), g. 6.16 Sulfur Standard Solutions should be prepared at sulfur concentrations within a factor of two of the unknown. For example, for approximately 30 ppm, pipet 10 mL of sulfur stock solution (reagent 6.15) into a 100-mL volu metric flask and dilute to volume with isooctane. 7. Hazards 7.1 Consult the current OSHA regulations and supplier's Material, Safety Data Sheets for all materials used in this test method. 7.2 Aromatics are considered hazardous materials. Prac tice sufficient care to limit the exposure to aromatics so that the OSHA threshhold limit values are not exceeded. In ' addition, other chemicals such as hydrofluoric add and sodium azide are used in the method. 8. Sampling 8.1 Consult guidelines for taking samples from bulk in Practice D 3437. 9. Preparation of Apparatus 9.1 Carefully insert the quartz pyrolysis tube in the pyrolysis furnace and connect the reactant and carrier gas lines. 9.2 Add the electrolyte solution to the titration cell and flush several times. Maintain an electrolyte level of Vs to *lA in. (3.2 to 6.4 mm) above the platinum electrodes. 9.3 Place the heating tape on the inlet of the titration cell. 9.4 Place the titration cell on the magnetic stirring device and connect the cell inlet to the outlet end of the pyrolysis tube. Position the platinum foil electrodes (mounted on the movable cell head) so that the gas inlet flow is parallel to the electrodes with the generator anode adjacent to the generator cathode. Assemble and connect the coulometer and recorder (integrator optional) as designed or in accordance with the manufacturer's instructions. 9,4.1 Turn the heating tape on. 717 DUP050296279 # D 3961 9.5 Adjust the flow of the gases, the pyrolysis furnace temperature, titration cell, and the coulometer to the desired operating conditions. Typical operational conditions are given in Table 1. 10. Calibration and Standardization 10.1 Prepare a series of calibration standards covering the range of sulfur concentration expected. Follow instructions in 6.15,6.16, or dilute to appropriate level with zsooctane. It is important that the sulfur concentration of the standard to be used be within a factor of two of the sulfur concentration of the sample. 10.2 Adjust the operational parameters as shown in Table 1. 10.3 The sample size can be determined either by volume or by mass. The sample size should be 80 % or less of the syringe capacity. 10.3.1 Volumetric measurement can be obtained by tilling the syringe with about 7 j iL of sample, being careful to eliminate bubbles, retracting the plunger so that the lower liquid meniscus fells on the 1-pL mark, and recording the volume of liquid in the syringe. After the sample has been injected, again retract the plunger so that the lower liquid meniscus falls on the 1-pL mark, and record the volume of liquid in the syringe. The difference between the two volume readings is the volume of sample injected. 10.3.2 Alternatively, the sample injection device may be weighed before and after the injection to determine the amount of sample injected. This method provides greater precision than the volume delivery method, provided a balance with a precision of 0.00001 g is used. 10.4 Insert the syringe needle through the inlet septum up to the syringe barrel and inject the sample or standard at an even rate of about 0.1 to 0.2 pL/s. If a microlitre syringe is used with an automatic injection adapter, calibrate the injection rate (volume/pulse) to deliver 0.1 to 0.2 pL/s. 10.5 Repeat the measurement of each calibration standard at least three times. It has been observed that artificially high concentrations have been reported when low sulfur samples follow high sulfur samples. Zsooctane samples TABLE 1 Typical Operational Conditions Gas flow, om3/min Inert gas flow, cm3/min Oxygen gas flow, cm3/mln Furnace temperature, C: Inlet zone Pyrolysis zone Outlet zone Titration cell Coulometer: Bias voltage. mV Gain 200 40 160 750 900 900 stirrer speed set to produce slight vortex 160 low (approximately 200) Approximate Range Settings mg/kg S Ohms 100 5 50 10 10 100 3-5 200 1 400 Recorder Sample injection rate 0.5 in./min chart drive 1-mV span with a sensitivity of 0.1 mV/in. 0.1 pL/s TABLE 2 Satisfactory Standard Mated Sample Type Benzene Cyclohexane Zsooctane Styrene Sulftir Cbmr disbutyl sulfide? dibutyi siilfidet dibutyl suilidp. elemental sal can be used to confirm the absence of sulf equipment. 1 No t e 9--Not all of the sulfur in the sample comes furnace as titratable S02. In the strongly oxidative contlijUjA pyrolysis tube some of the sulfur is converted to S03 which react with the titrant. Accordingly, sulfur standards of n-butvl i'rooctane or sulfur standards appropriate to sample boilm<i suffer type and sulfur concentration should be prepared m i_ adequate standardization. Recoveries ofsulfur as S02 less thatf" to be considered suspect. Low recoveries are an indicating operator that he should check his parameters, his opeutinf tcV and his coulometric system. Ifthe instrument is being operated fin recoveries between 75 and 90 % are to be expected. Sati5li>'-'"->'-" materials6 are given in Table 2. 'YWt uitjgii. 10.6 Ifthe fraction of sulfur converted to S02 drop ' 75 % of the standard solutions, prepare fresh standard low-conversion factor persists, review procedural detaigi 10.7 With direct injection below 5 mg/kg sulfur _l line shift error due to the needle septum blank mavi .... significant. Such error can be avoided by insertin syringe needle into the hot inlet and allowing the** septum blank to be titrated before injecting the samp] 11. Procedure 11.1 Flush the 10-pL syringe several times with unknown sample. Determine the sulfur concentratio accordance with Section 12. See Fig. 3 for exampl typical peaks. The samples were 0.32 mg/kg (0.31 in1 mg/kg (0.44 in.2), and 20.7 mg/kg (0.81 in.2). 11.2 Sulfur concentration may require adjustu sensitivity settings or sample volume or both. 11.3 Peak-tailing may be controlled by decreasin stirring rate or increasing the bias voltage or-gain. Ma adjustments in bias voltage with the-function switc^' "stand-by" or "generator read" positions. 11.4 When an overshoot occurs, increase the stirring or decrease the bias voltage by 2-mV increments or decs the gain until a satisfactory peak shape results. 11.5 Increasing the level of electrolyte in the titration, will also help eliminate overshoot. m 11.6 Any adjustments, such as "bias voltage," "gain,- "range-ohms," are allowable in order to obtain a satisfact peak. 11.7 In some cases of very low-level sulfur sample*; negative peak may be observed. This may sometimes , corrected by injecting larger samples and increasing oxygen content of the flow gases. 11.8 The titration cell may become erratic and desei tized occasionally. Rinse the electrodes with water a' acetone. Blow dry with air or nitrogen. Then, very gently 6 Wallace, L. D,, "Comparison of Oxidative and Reductive Methods for Microcoalometric Determinations of Sulfur in Hydrocarbons," Analytical Chcvt'- isiry, Vol 42, March 1970, p. 393. 1 DUP0502 96280 # 0 3961 Bias 160mv Range 200ti Flow Rates 02 - lOOml/min He - lOOml/min Standard - 0.32 wt - ppm S Recovery - 68% Factor - 14.6118 nanogms/in2 Injection - 20 pi Peak Area - 0.31 in2 Bias 160mv Range 40041 Flow Rates 02 - 160ml/min He - 40ml/min Standard - 1.3 wt-ppm S Recovery - 38% Factor - 13.0941 nanogms/in2 Injection - 6.78 pit Peak Area - 0.44 in2 Bias 160mv Range 3041 Flow Rates 02 160ml/min He - 40 ml/min Standard - 20.7 wt-ppm S Recovery - 54.4% Factor - 121.8678 nanogms/in2 Injection - 6.8 pi Peak Area - 0.81 in2 r FIG. 3 Examples of Typical Peak and Areas at Three Sulfur Levels eat care, slowly heat the electrodes over a flame to a range color. Allow them to cool gradually before ing them to the cell. Allow the cell to stabilize before jng the analysis. 9 Low recoveries may result from inadequate condi|pg of a new pyrolysis tube or having carbon in an old lysis tube. In the case of a new pyrolysis tube, continue conditioning runs until recovery reaches a maxpoint and levels off. In the case of an old pyrolysis remove the tube from the furnace and allow it to cool, cooling, rinse it with acetone to remove any hydrom residue. Blow dry with air or nitrogen and wash with hydrofluoric add solution for 3 to 5 min. Rinse with ir followed by acetone and blow the tube dry. Return the | to the furnace, bring it up to operating temperature and ition it with repeated injections of standards of suitable levels. 10 The exit tube may cause erratic performance, or ng or low recoveries, or a combination thereof. Remove I clean the tube by rinsing it with water, then acetone, and it dry. Repack it with quartz wool and replace it in the vsis tube. 1 Check a standard sample at least before every sample. i Calculation |2.l Calculate the sulfur content of the sample in milli- grams per kilogram as follows: Sulfur, mg/kg = a 2b St j YU where: A i = area under curve for the standard solution, in.2 or mm2. A2 = area under curve for sample, in.2 or mm2, B = total weight of sulfur in the injected standard, ng, . V -- sample volume injected, jxL, R = coulometer range switch setting, D = density of sample, g/mL, V - volume of sample, jiL, and F = recovery, ratio of mg/kg sulfur determined in standard divided by the known mg/kg sulfur in standard. This is not used in the calculations, but is used as an operational check. ,, 1.99 AiB 1& R where: 1.99 = coulometric replacement of triiodide ion consumed in titration cell as determined indirectly by Faraday's law. No t e 10--The calculation equation is valid only when the chart speed is 0.5 in./min and a 1-mV (span) recorder with a sensitivity of 0.1 mV/in. is used. No t e 11--If a disk integrator is used, refer to the manufacturer's instructions for the appropriate equations. 719 IP DUP050296281 Sample Cyclohexane, A Cyclohexane, B Styrene, A Styrene, B p-Xylene # D 3961 TABLE 3 Summary of Statistical Data Repeatability Between Days Within Laboratories Average Degrees of Freedom s. Range max. 0,91 6.28 2.42 28.85 3.58 10 0.11 0.35 11 0.28 0.87 11 0.28 0.87 9 0.94 3.01 11 0.19 0.59 Reproducibility Single Result. An m Degrees of Freedom + b Rand 9 0.23 10 0.57 10 0.70 8 2.25 10 0.47 13. Report 13.1 Report the sulfur content of the sample as described in Section 12. 14. Precision 14.1 The following criteria should be used to judge the acceptability (95 % probability level) of results obtained by this method. The criteria were derived from a round robin between twelve laboratories. The data were run on two days by the same operator. 14.1.1 Repeatability--Results in the same laboratory should not be considered suspect, unless they differ by more than the amount shown in Table 3. TABLE 4 Sample Cyclohexane, A Cyclohexane, B Styrene, A Styrene. B p-Xylene Summary of Statistical Calculations Average Standard Coefficient Deviation Variation 0.91 6.28 2.42 28.85 3.5B 0.214 0.530 0.668 2.147 0.449 23.57 8.44 27.56 7.44 12.56 14.1.2 Reproducibility--The results obtained by two laboratories should not be considered suspctt, they differ by more than the amount shown in Tab ' 14.1.3 For a summary ofstatistical calculations, 4. The American Society tor Testing and Materials takes noposition respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised 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 mustbe reviewed every live years and ifnotrevised, either reapprovedor 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. 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. DUP050296282 Designation: D 3962 - 80 (Reapproved 1989)el Standard Test Method for Analysis of Styrene by Gas Chromatography1 This standard is issued under the fixed designation D 3962; 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. " No t e--Editorial changes were made throughout, including the title in November 1989. ope This test method covers the determination of the ities in, and the purity of, styrene by gas chromatog: It is applicable to styrene in the range from 99 to purity. This test method may be used for lower purity e but because the impurities may not all be readily ied, the use of an internal standard becomes more ilt. This standard may involve hazardous materials, operr, and equipment. This standard does not purport to ;s all ofthe safety problems associated with its use. It is sponsibility of the user of this standard to establish tpriate safety and health practices and determine the \cability of regulatory limitations prior to use. For jfic hazard statements, see Section 5 and Note 2. Referenced Documents |. ASTM Standards: $437 Practice for Sampling and Handling Liquid Cyclic Products2 |60 Practice for Packed Column Gas Chromatography3 Other Document:* WSHA Regulations. 29 C1FR, paragraphs 1910.1000 and i|1910.12004 |ununary of Test Method! |l In this test method, the chromatogram area for each iirity is compared to the area of the internal standard eptane or olher suitable > known) added to the sample, i the response factors of these impurities relative to that |e internal standard and the amount of internal standard the concentration of the impurities are calculated. styrene content is obtained jby subtracting the total liint of all impurities from 100.00. Significance and Use pi This test method is designed to obtain styrene purity tie basis of impurities normally present in styrene and be used for final product inspections and process Strok his method is underthe jurisdiction ofASTM Committee D-16 on Aromatic bcarbons and Related Chemicals and is the direct responsibility of Subcomi D 16.OH on Styrene, Ethylbenzene, Cumene, and Naphthalene. -ent edition approved Oct 31,1980. Published January 1981. 'Annual Book ofASTM Siandardst Vol 06.03. piAnnual Book ofASTM Standards, Vol 14.01. \vailable from Superintendent of Documents, U.S. Government Printing :e, Washington, DC 20402. 4.2 This test method will detect the following impurities: nonaromatics, ethylbenzene, p- and m-xylene, isopropyl benzene, o-xylene, K-propylbenzene, m- and p-ethyltoluene, alpha-methylstyrene, m- and p-vinyltoluene, and others where specific impurity standards are available. 5. Hazards 5.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 6. Apparatus 6.1 Gas Chromatograph--Any instrument having cither a thermal-conductivity or flame-ionization detector may be used,- provided the system has sufficient sensitivity and stability to obtain an area of 2000 mm2/pg of internal standard. The sample size to be used in judging the sensi tivity must be such that the column is not overloaded and the signal to noise ratio is at least 5:1. Typical'operating conditions are given in Table 1. TABLE 1 Instrument Parameters Detector Column: Length, m Outside diameter, mm Stationary phase Temperature, C: Injector Detector Column oven Carrier gas and rate Recorder: Range Chart speed Response time Sample size Total chromatograph run time hydrogen flame ionization stainless steel 6.1 3.18 15% FFAP liquid phase on 60/80 mesh Chromosorb' W--A/W DMCS solid support 200 250 130 helium 20 mL/min 0 to 1 mV 1 cm/min l-s full scale 1 pL 35 min 6.2 Column-- 15 % FFAP liquid phase on 60/80 mesh Chromosorb W5 A/W DMCS 6.1 m by 3.18 mm stainless steel or 20 % Carbowax 40006 liquid phase on 60/80 mesh Chromosorb P5 3.05 m by 0.318 cm stainless steel. Other 5 Registered trademark of Manville Sales CorpM Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108. 6 Registered trademark of Union Carbide Corp., 39 Old Ridgbury Rd., Danbury, CT 06817-0001. 721 DU P050296283 D 3962 ***? FIG. 1 Typical Chromatogram . (See Table 1) columns may be used after.it has been established that such column is capable of separating all major impurities and the internal standard from the styrene under operating condi-, tions appropriate for the column. 6.3 Recorder--A recording potentiometerwith a full-scale deflection of 2 mV or less with a response time of no more than 1 s and sufficient sensitivity to meet the requirements ip 6.1 (see Fig. 1). No t e 1--Other methods of recording detector output such as computer-teletype systems may.be used instead of a recorder, provided precision requirements are met. 7. Reagents and Materials 7.1 Carrier Gas--A carrier gas (minimum purity of99.95 mol %) appropriate to the type of detector used should be employed. '* 7.2 Hydrogen and air if a flame ionization detector (FID) is employed. No t e 2: Precaution--in addition to other precautions, ifhydrogen is used here or as a carrier gas, take special safety precautions to ensure that the system is free ofleaks and that the effluent is properly vented or burned. 7.3 n-Heptane, 99.0 % minimum purity, or other internal standard, such as n-octane previously analyzed to be free of compounds coeluting with impurities in the sample. '7.4 Styrene, highest purity available, but not less than 99.6 % as determined by freezing point. No t e 3--Since the purity of the standard styrene is below 100%, areas for the impurities can be obtained from a chromatogram of rite standard styrene. These values are used for adjusting the impurity areas used in calculating the response factors when using the same sample size. If sample size varies, then correction should be made by ialioin weight and area to the internal standard. 7.5 Typical impurities that may be present in commert styrene. These should be at least 99 % pure as the> are t<j' used for determining response factors. 8. Sampling 8.1 Sample in accordance with Practice D 3437. 9. Calibration __ 9.1 Prepare ^synthetic mixture containing approximai 99.5. weight % styrene.and the expected significant imp at their expected concentration. Weigh all.components to accuracy required to calculate the, concentration of each the nearest 0.001 %. With a microsyringe, add 50 pL o' internal standard to a 100-mL volumetric flask about fourths full of the synthetic mixture. Mix well. Add synthetic.,,^ to mark and again mix well. If n-heptane is used as thq|g| internal standard, using a density of.0.684 for n-heptane and 0.906 for styrene, this solution will contain 0.0377 weight: % n-heptane. -j 1No t e 4--Inject a sample of styrene to be analyzed prior to addition of n-heptane to determine if any peaks will appear where the n-heptane peak appears. If any peaks appear, correct the standard for these. 9.2 Inject an appropriate amount of sample into the chromatograph and obtain a chromatogram. 9.3 Measure the areas of all peaks, including the internal standard, except the styrene peak. 9.4 Calculate the response factors for each impurity rela tive to the internal standard as follows: DUP050296284 D 3962 r , AJF.W, AW response factor relative to the internal standard, area of internal standard, area of impurity peak, attenuation factor for internal standard, attenuation factor for impurity peak, internal standard in synthetic, weight %, and impurity in synthetic, weight %. nple Preparation | fetablish, stable instrument operation at the pre- 1 or selected operating conditions. Reference should be to instructions.;provided by the manufacturer of the aatograph and to Practice E 260. With a microsyringe, add 50 jrL of the internal to a 100-mL volumetric flask about three fourths |f sample. Mix well. Add sample to mark and again mix ; If n-heptane is used as the internal standard, using a of 0.684 for n-heptane and 0.906 for styrene, this |on will contain 0.0377 weight % n-heptane. 3; Inject an appropriate amount of sample into the atograph and obtain the chromatogram. ' Calculation and Report Measure the areas of all peaks, including the internal fd, except the styrene peak. : Calculate the weight percent of the individual impu|jf, as follows: area of impurity, 4A As = area of internal standard, R, - response factor for impurity, relative to the internal standard, Ws = concentration of internal standard, weight %, Fj -- attenuation factor for impurity, and Fs = attenuation factor for internal standard. 11.3 Calculate the styrene content by subtracting the sum of the impurities from 100.00. Styrene weight % = 100.00 sum of impurities. 11.4 Report the concentration of impurities to the nearest 0.001 % and the styrene content to the nearest 0.01 %. 12. Precision and Bias 12.1 Precision--The following criteria should be used to judge the acceptability (95:% probability level) of results obtained by this test method. The criteria were derived from a round robin among five laboratories. Some of the data could be pooled because oftheir relative independence ofthe percent concentration with the variation present at that level. The data were run on two days using different operators. 12.2 Repeatability--Results in the same laboratory should not be considered suspect unless they, differ by more than the amount shown in Table 2. 12.3 Reproducibility--The results by each of two labora tories should not be considered suspect unless they differ by more than the amount shown in Table 2. TABLE 2 Precision for Styrene and impurities at Stated Levels Component Concentration, Weight % Repeatability, % Reproducibility, % Styrene Ethylbenzene Alpha-methylstyrene Isopropylbenzene n-Propyibenzena m- and p-ethyltotuene 99.6 0.05 0.07 0.02 0.02 0.01 0.023 0.005 0.006 0.004 -- --' '0.046 0.005 : 0.013 . 0.004 0.018 0.006 TheAmerican Society for Testing anti Materials takes noposition respecting the validity of any patent rights asserted In connection with any Item mentioned in thfe 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 bythe responsible technical committee and must be reviewed every five years ariS~ Ifnotrevised, either reapproved or withdrawn. Your comments are Invited either for revision ol 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 tbat 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. 723 DUP050296285 Designation: D 4076 - 86 {Reapproved 1990) Standard Specification for o-Xylene 9501 This standard is issued under the fixed-designation D 4076; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers a grade of o-xylene identified as "ortho-Xylene 950." 1.2 Consult latest OSHA regulations and supplier's Mate rial Safety Data Sheets on handling materials listed in this specification. 2. Referenced Documents 2.1 ASTM Standards: D847 Test, Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons2 D 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials2 D1209 Test Method for Color ofClear Liquids (PlatinumCobalt Scale)2 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products2 D 1555 Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons2 D2935 Test Method for Apparent Density of Industrial Aromatic Hydrocarbons2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 D3505 Test Method for Density or Relative Density of Pure Liquid Chemicals2 D3797 Test Method for Analysis of o-Xylene! Chromatography2 D3961 Test Method for Trace Quantities of ,,,, Liquid Aromatic Hydrocarbons by Oxidative" coulometry2 D 4052 Test Method for Density and Relative De Liquids by Digital Density Meter3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.100ftW 1910.12004 3. Properties 3.1 o-Xylene 950 shall conform to the following' quirements: Property Purity, min; weight % ' G, Aromatic hydrocarbons, max, weight % Nonvolatile matter, max, mg/100 mL Sulfur, max, mg/kg Acidity Color, max, Pt/Co scale Total distillation range including the temperature 144.4C at 760 mm Hg (101.3 kPa) pressure, 'C Specification 95.0 1.5 5 5 none delected 20- not more than 2.0`C Mj Uic D3?' D37 No t e--Relative density (specific gravity) in vacuum can be dcftS1 mined using Test Methods D 3505 and D 4052. Apparent density in tur, can be determined using Test Method D 2935. When converting weight, to volume or vice versa, Test Method D 1555 shall bs-employed. 1 This specification is under the jurisdiction of ASTM Committee D-J6 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0A on Benzene, Toluene, Xylene, Cyclohexane, and Their Derivatives. Current edition approved May 30, 1986. Published November 1986. Originally published as D 4076 "81. Last previous edition D 4076 -81. 2 Annual Book ofASTM Standards, Vol 06.03. 4. Sampling / 4.1 The material shall be sampled in accordance with Practice D 3437. 3 Annual Book ofASTM Standards, Voi 05.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, either reapprovedorwithdrawn. Your comments are Invitedeither 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. 724 DUP050296286 Designation: D 4077 - 91 Standard Specification for Isopropylbenzene (Cumene)1 This standard is issued under the fixed designation D 4077; 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 reapprovat. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. eope >lf This specification covers isopropylbenzene (cumene). 2 Consult current OSHA regulations and supplier's erial Safety Data Sheets for all materials used in this 'cation. E 299 Test Method for Trace Amounts of Peroxides in Organic Solvents6 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12007 .eferenced Documents ,1 ASTM Standards: 848 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons2 . . 4209 Test Method for Color of CJear Liquids (Platinum- Cobalt Scale)3 1492; Test Method for Bromine Index of Aromatic Hydrocarbons by Coulometric Titration2 3160 Test Method for Phenol Content of Isopropyl benzene (Cumene)2 > ,3437 Practice for Sampling and Handling Liquid Cyclic Products2 3760 Method for Analysis of Isopropylbenzene (Cumene) by Gas Chromatography2 3961 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Micrp- coulometry2 4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry4 298 Method for Assay of Organic Peroxides5 3. Properties 3.1 Isopropylbenzene (cumene) shall conform to the fol lowing requirements: Property Purity, weight %, min Impurities, Total, weight. %, max Benzene, weight %, max Ethylbenzene, weight %, max n-Propylbetizerie, weight %, max Butylbenzenes, weight %, max Phenols, mg/kg, max Sulfur, mg/kg, max Cumene hydroperoxide, at loading, mg/kg, max Bromine index, max Acid wash color, max Color, Pt/Co, max Appearance Specifica tions 99.9 0.1 0.002 0:02 0.03 0.03 5 1 100 100 pass with 2 . 15 a ASTM Test Method D 3760 D3760 D 3760 D 3760 D 3760 D3760 D 3160 D 3961 or D 4045 E 298 or E 299 D 1492 " D`848 D 1209 visual A Clear liquid, free of sediment andhaze from 18.3 to 25.6"C (65 to 78*F). 4. Sampling 4.1 Sampling of this material shall be in accordance with Practice D 3437. 4.2 If cumene has been exposed to air, cumene hydro peroxide may be in the sample. Suitable precautions should be exercised for handling cumene that may contain cumene hydroperoxide. ! This specification is under the jurisdiction of ASTM Committee D-16 on malic Hydrocarbons and Related Chemicals and is the direct responsibility of ommittee D16.0H.on Styrene, Ethylbenzene, Cumene, and Naphthalene. Current edition approved May 15, 1991. Published July 1991.' Originally fished as D 4077 -81. Last previous edition D 4077 - 81 (1986)*'.' i! Annual Book ofASTM Standards, Vol 06.03. Annual Book ofASTM Standards, Vols 06.01 and 06.03. 4 Annual Book ofASTM Standards, Vol 05.03, 5 Annual Book ofASTM Standards, Vol 15.05. 5. Keyword 5.1 isopropylbenzene (cumene) 6 Annual Book ofASTM Standards. Vols 06.03 and 15.05. 7 Available from Superintendent of Documents, U. S. Government Printing Office, Washington, DC 20402. The American Society for Testing and Materials lakes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination 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 il not revised, eitherreapproved or withdrawn. Your comments are irwited either lor revision of this standard or foradditional 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. ' 725 DUP050296287 Designation: D 4297 - 89 Standard Practice for r Sampling and Handling 4,4'-lsopropylidinediphenoi (Bisphenol A)1 This standard is issued under the fixed designation D 4297; 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 TABLE 1 Typical Physical Properties Product Bisphei 1.1 This practice covers procedures for sampling and handling 4,4'-isopropylidinediphenol, commercially known as bisphenol A, in various solid forms, and as a liquid at 154-157 "sry 240 Solid Forms prills. Hates, crystals, r elevated temperatures from the viewpoints of quality assur ance and safety. 1.2 Any person sampling or handling this product should have specific first aid instructions and equipment available for use in the event of personal contact or exposure. properly, particularly at elevated temperatures, its unloadj need not be hazardous provided the hazards are rccogntj and handling instructions are rigidly observed. 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. See Sections 5, 6, 7, and 8 for specific hazards. 5. Hazards 5.1 Health--Consult current OSHA regulations and suOi plier's Material Safety Data Sheets for all materials useeni this practice. 5.1.1 Aside from the risk of thermal bums in handlf bisphenol A when molten, and a possibility of deimain. from impurities, particularly in crude grades, industrial'^ 2. Referenced Documents does not present a significant health hazard. Howeve. ordinary precautions must be observed to protect personne 2.1 OSGA Regulations: from contact with molten bisphenol A or excessive exposi.'i 29 CFR Labor, paragraphs 1910.1000 and 1910.12002 * * * 5 6to7dusts or high concentrations of vapor. 2.2 U.S. DOT Regulations: 5.1.2 Precautions must be observed to protect personnel 49 CFR Transportation, Subchapteis B and C, Parts from excessive inhalation of vapors and dust. 171-1792 5.2 Fire: 3. Significance and Use 5.2.1 Bisphenol A in both the solid and liquid formj combustible and introduces a potential fire hazard when it iS'>! 3.1 This practice is issued to provide information useful in stored, handled, or used. establishing sampling and handling procedures. It is expected 5.2.2 Bisphenol A vapors or dust can form, explosive that this information will only be utilized in conjunction mixtures with air. -- with an existing health and safety program. The information 5.2.3 Dry chemicals, carbon dioxide, foam, and water can provided herein cannot be used as a substitute for expert all be used in fighting fires involving bisphenol A. safety and medical advice, but rather as a supplement to such advice. 6. Protective Equipment 4. Description of Product (See "fable 1) 4.1 Bisphenol A is not classified as a hazardous chemical by the Department of Transportation, and is, therefore not subject to DOT regulations governing the transportation of hazardous articles. Bisphenol A is normally transported in several types of containers including cloth and paper bags, bulk trucks, and covered hopper cars. (See Table 1.) 4.2 While bisphenol A is dangerous when handled im- 6.1 Employees who work with bisphenol A should be well trained and should maintain safe working conditions. Per sons handling molten bisphenol-A require eye, face, respira tory, body, skin, and hand protection. Handling solid bisphenol A requires hand and respiratory protection such as a dust mask. 6.2 Personal protective equipment is not an adequate substitute for good safe working conditions, proper ventila tion, and intelligent conduct. Correct usage of protective equipment requires education in its proper use. 1 This practice is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0J on Sampling; and Handling Aromatic and Cyclic Hydro carbons. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 4297 - 83. Last previous edition D 4297 - 83. 2 Available from Superintendent of Documents, Government Printing Office, Washington, DC 20402. 7. First Aid 7.1 Skin contact with molten bisphenol A causes third degree bums. In case of skin contact with molten bisphenol A, remove all contaminated clothing, immediately see a physician, and advise him of the type of product causing the bums. 726 DUP0502 96288 4! D 4297 If bisphenol A gets into the eyes, flush eyes with pus amounts of water for at least 15 min, holding eyes , and see a physician at once. fety Precautions Exercise care to prevent spills and leaks. If they do only properly protected personnel should remain in intaminated area. If the spill is large, rope offthe area. Because of fire and dust explosion hazards, do not it open flames in the vicinity of tank carriers, other ing containers, or storage tanks. Provide all electrical with vapor-proof globes and explosion-proof safety Ground tank carriers by an approved method. Bibit smoking. All pneumatic conveying should be done nitrogen or other inert gas. Jnloading Hopper Cars or Hopper Trucks |!1 Observe all safety precautions. Always follow shipper's uctions for unloading, and read and observe all caution ings on both rides of the hopper or dome. Opehing of the hopper car dome cover and attach: of delivery lines should all be done by accepted safety dures. Sampling Solid Bisphenol A 10.1 Bulk Quantities--Take a representative sample, pref>ly from a falling bisphenol A stream, nring a straightsampler. Adjust sampler feed rate, riot width, cutter speed, and frequency to collect 7i lb (227 g) of sample per 10 000 lb (4540 kg) of bisphenol A. 10.2 Bags (50 lb (22.7 kg)): 10.2.1 Using a small thief, 8 to 12 in. (203 to 305 mm), remove about Mi lb (113 g) of sample from 1 bag out of every 40 bags (2000 lb) (907 kg) of bisphenol A. Take the sample from the filling ear or, if necessary, by opening one corner of the bag. Place each sample in a plastic bag. Tightly secure the sample bag to minimize absorption of moisture. Label with proper identification and according to OSHA Regulations. 10.2.2 Make a composite blend from the individual samples and mix thoroughly before analyzing. 10.2.3 Aluminum, polyethylene, polypropylene, or stain less steel-type scoops are recommended for taking samples of product from the bags selected for sampling. Avoid contam inating the sample with iron or rust. 10.3 Extreme care and good judgment are necessary to ensure that the samples truly represent the product. 10.4 Remove approximately 75 g portions from each of the bags selected from a sample unit and place in a plastic bag. Seal the opened bags with suitable tape. 10.5 Label die bags properly for future identification in the testing laboratory. 10.6 Large Bulk Sacks (1100 to 2200 lb (500 to 1000 kg)): 10.6.1 Use a sample thief to collect 'A lb (227 g) samples for each 4000 to 5000 lb (1814 to 2268 kg) of material. 10.6.2 Place samples in plastic bags. Tightly secure the sample bags to minimize absorption of moisture. Label with proper identification and according to OSHA Regulations. TheAmerican Society for Testing andMaterials takes no position respecting the validity of anypatent 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 peitent rights, and the risk of infringement of such rights, are entirely their own responsibility. - This standard is subjsct to revision atany 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 standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting o1 the responsible technical committee, which you may attend. If you feel f/iat 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. 727 DUP050296289 # Designation: D 4471 - 85 (Reapproved 1989)1 Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration1 This standard is issued under the fixed designation D 4471; 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. el No t e--Editorial changes were made throughout in November 1989. 1. Scope 1.1 This test method covers the determination of pyridine and other basic nitrogen impurities in crude and refined cresylic acids streams, including mixtures. This test method is applicable.for pyridine base levels of 0.001 % and 0.5 %. 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 7. 2. Referenced Documents 2.1 ASTM Standard: D3852 Practice for Sampling and Handling Phenol and Cresylic Acid2 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12003 3. Summary of Test Method 3.1 This test method is a direct, nonaqueous titration technique utilizing perchloric acid in acetic acid as titrant and the cresylic acid itself as titration solvent. Endpoints may be established potentiometrically as well as by indicator so that the method is applicable to highly colored as well as lighter colored materials. This test method will detect basic components other than pyridine bases should they be present. All basic compounds detected by this procedure are calculated and expressed as percent pyridine. 4. Significance and Use 4.1 The pyridine base content of cresylic acids is impor tant in certain applications. This test method may be used as a tool for quality control and specification purposes by producers and users. 5. Apparatus 5.1 Titrimeter or pH meter, equipped with glass and 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved March 29, 1985. Published December 1985. 2 Annual Book ofASTM Standards, Voi. 06.03. 3 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. calomel electrodes. The pair of electrodes shall be mouril to . extend, well below the liquid level. Storage in via between titrations is essential because prolonged unmeis in nonaqueous medium significantly deadens response 5.2 Buret, 50-mL capacity. 5.3 Magnetic Stirrer, with TFE-fluorocarbon or _ ___ covered stirring bar. " 5.4 Glassware, titration beakers, pipets and. other appro priate glassware. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall used in all tests. Unless otherwise indicated, it is intunLi/j that all reagents shall conform to the specifications of Committee, on Analytical Reagents of the American Chcngg ical Society, where such specifications are available.4 Otlte grades may be used, provided it is first ascertained that reagent is of sufficiently high purity to permit its: use without,/ lessening the accuracy of the determination. 6.2 Perchloric Acid Titrant (0.02 N in glacial acetic* acid)--Add 1.8 mL of 70 % perchloric add (HC10,,) to 1 of glacial acetic acid and mix well. To standardize, weig, accurately 0.0800 to 0.0950 g of primary standard potassium-^ acid phthalate in gladal acetic acid and titrate potentiomet-.-,^ rically or to the indicator endpoint, as described in 9.2.'.' \ Calculate the normality, N, of the perchloric add solution a&l follows: N- W Vx 0.2041 where: W - weight of potassium acid phthalate, g, and V = volume of perchloric acid titrant consumed, mL. 6.3 Potassium Acid Phthalate (KH CgH804), primary standard--Dry for 2 h at 110C. 6.4 Quinaldine Red Indicator Solution--Dissolve 0.2 g of quinaldine red indicator in 100 g of glacial acetic acid. 6.5 Titration Solvent--Glacial acetic acid (CH3C02H) may be used as an additional titration solvent in order to decrease the viscosity of a particular sample or to keep it from freezing. 4 "Reagent Chemicals, American Chemical Society Specifications," American Chemical Society, Washington, DC. Foi suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Company, Inc., New York, NY, and the "United States Pharmacopeia." 728 DUP050296290 D 4471 zards ('Consult current OSHA regulations and supplier's Sal Safety Data Sheets for all materials used in this test id. apling ' Samples shall be taken in accordance with Practice p. locedure Weigh an appropriate amount of cresylic acid sample ie titration beaker. {A sample size of 100 g is suggested expected pyridine base content is in the range of 0.001 >70 %.) Place a stirring bar in the beaker and, ifdesired, ibout 100 mL of titration solvent. The specimen is titrated with perchloric acid titrant the endpoint determined by either of the following iods: .l Indicator--A few drops of quinaldine red indicator led to the solution. The titration is terminated when the olor disappears and the color ofthe sample returns to its ial hue. 2.2 Potentiometric--The electrodes are inserted into the men and the observed potentials are plotted as a ion of the titrant volume consumed. The point where (/AV is the greatest is taken as the endpoint. 5 Repeat the steps 9.1 through 9.2, but with no spec ie to obtain a reagent blank when titration solvent is used. ^Calculation .1 Results are calculated as weight percent pyridine, P, allows: 7.91 X NX(Vk P= W where: N = normality of the perchloric acid titrant, Vs = titrant consumed for the sample, mL, VB = titrant consumed for the reagent blank, mL, and W = specimen weight, g. 11. Report ! 1.1 Report the percent of pyridine bases to the nearest 0.01 %. 12. Precision and Bias 12.1 Precision--The following criteria shall be used for judging the acceptability of results. 12.1.1 Repeatability (within laboratory)--When using the visual endpoint in this test method, results obtained by different analysts in the same laboratory should be suspect within 95 % confidence limits if they differ by more than 2.8 % of the average of values determined. When using the potentiometric endpoint in this test method, results obtained by different analysts in the same laboratory should be supsect within 95 % confidence limits if they differ by more than 2.2 % of the average of values determined. 12.1.2 Reproducibility (between laboratories)--When using the visual endpoint in this test method, results ob tained by analysts in different laboratories should be suspect within 95 % confidence limits if they differ by more than 6.8 % of.the average of values determined. When using the potentiometric endpoint in this test method, results obtained by analysts in different laboratories should be suspect within 95 % confidence limits if they differ by more than 13.9 % of the average of values determined. 12.1.3 Bias--The bias of this test method cannot be determined because no referee method is available to deter mine the true value. The American Society lor Testing and Materials takes no position respecting the validity ofartypatent 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 neapprovedor withdrawn. Your comments are invitedeither forrevision ofthis standard or for additionalstandards and shoutd be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. K 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. 729 DUP050296291 m Designation:: D 4492 - 85 (Reapproved 1989)f1 Standard Test Method for Analysis of Benzene by Gas Chromatography1 This standard is issued under the fixed designation D 4492; the number immediately following th? 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 ah editorial change since the last revision or reapproval. aNoTE--Editorial changes were made throughout, including the title, in November 1989. 'IP f. 1. Scope LI This test method covers the determination of nor mally occurring trace impurities in, and the purity of, finished benzene by gas chromatography. 1.2 This test method was judged applicable for nonaromatic impurities at levels from 100 to 2000 mg/kg and for benzene purities of 99.80 % or higher. 1.3 This test method is applicable for aromatic impurities from 100 to 1000 mg/kg in benzene. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard'does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D852 Test Method for Solidification Point of Benzene12 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 E 260 Practice for Packed Column Gas Chromatography3 E 355 Practice for Gas Chromatography Terms and Relationships3 2.2 Other Document: OSHA Regulations. 29 CFR, paragraphs 1910.-1000 and: 1910.12004 peak areas. The result is multiplied by 100 to get the weight percent composition. ' 4;. Significance and Use 4.1* This test method is suitable for determining the concentrations of known impurities in finished benzene and for Use as an integral quality-control tool where benzene is either produced or used in a manufacturing procedure. It is generally applied to impurities such as noiiaromatics con taining nine carbons or less, toluene, and C8 aromatics. 1 4.2 Absolute purity cannot be determined if uiikhown impurities are present. Test Method D 852 is generally used3 as a criteria for determining the absolute purity. 5. Interferences 5.1 Benzene is typically resolved from naturally occurring components with boiling points <150CC. Naturally occurring components include nonaromatic hydrocarbons, toluene, and C8 aromatics. An adequate separation of known impu rities from benzene should-he evaluated for the columnselected. 6. Apparatus 6.1 Gas Chromatograph--Any instrument having a hy drogen flame ionization detector that can be operated at the conditions given in Table 1. No t e 1--The air/H2 ratio should be adjusted to obtain not only the maximum response, but also* the maximum linearity over the range from 0.01 to 10Owt%. 3. Summary of Test Method 3.1 A small volume of benzene is injected into a gas chromatograph containing a packed column of tetracyanoethylated pentaerythritol on Chromosorb P. 3.2 Quantitative results are obtained by adjusting the integrated area of each recorded peak with a factor obtained from the analysis of a blend of known concentration. The concentration of each impurity is calculated by dividing the adjusted peak area by the sum of total adjusted individual 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved May 31, 1983. Published October 1985. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vo! 14.01. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington DC 20402. TABLE 1 Typical Instrumental Parameters Detector Column: Length, ft (m) Outside diameter, in. (mm) Stationary phase, wt % Temperature: Injector, C Detector, C Column, C Carrier gas: Flowrate: Air/hydrogen flow rate Reoorder range, mV Chart speed, cm/min Sample size, pL: flame Ionization stainless steel 12.0 (3.6) ys (3.18) tetracyanoethylated pentaerythritol (TCEPE); 10 9S on Chromasorb P, 80/80 mesh 175 200 85 nitrogen 40 mL/min For maximum response, (10:1 air to hydrogen ratio is commonly employed. See Note 1). 0 to 1 full scale 1 0.6 730 DUP050296292 D 4492 2--Alternative columns including capillary-type columns and ative stationary phases may be used if they produce at least the 1 aromatic separation and elute C-9 nonaromatic impurities before iene. Column, 12 ft by Vs-in. stainless steel tubing. Recorder, Strip Chart--0 to 1-mV full scale. Microsyringe--10-pL capacity. Reagents and Materials .1 Carrier Gas--Chromatographic grade nitrogen or hel is recommended. ',2 Solid Support--Clhromosorb Ps, 60/80 mesh. 13 Stationary Phase--Tetracyanoethylated pentaerythl(TCEPE). |L4 Pure compounds for calibration should include tol ls, benzene, ethyl benzene, normal heptane, and methyl ?lopentane of a purity not less than 99 %. If the purity of ^calibration compounds is less than 99 %, the concentraand identification of impurities must be known so that / composition of the final weighed blends can be adjusted : the presence of the impurities. (Hazards 8.1 Consult current OSHA regulations and supplier's aterial Safety Data Sheets for all materials used in this test aethod; 18.2 Benzene is considered a hazardous material. The npling and testing of benzene should follow safety rules in der to adhere to all safety precautions as outlined in rent OSHA regulations. Sampling 9.1 Refer to Practice D 3437 for proper safe sampling and adlirig of benzene. Preparation of Apparatus ; 10.1 The method used to prepare the TCEPE column is pt critical provided that the finished column produces the red separation. ' P<j.2 Follow manufacturer's instructions for mountingthe mlumn into the chromatograph and adjusting the instru- |ent to the conditions described in Table 1. Allow sufficient file for the equipment to reach equilibrium. See Practices 260 and E 355 for additional information on gas chroma- pgraphy practices and terminology. Calibration 11.1 Prepare four synthetic mixtures of benzene and Representative impurities on a weight percent basis according go Table 2. J 11.2 Dilute 1.000 g of each stock standard solution into >9.00 g of benzene. Mix well. 11.3 Inject 0.6 pL of the resulting solution into the Chromatograph and determine the response factor relative to benzene for each impurity. The pure benzene used in the ilibration blend must also be analyzed and corrections nade to the composition ofthe calibration blend as required. 11.4 Integrate the area under each peak. Appropriate s Chromosorb P is a registered trademark of Manville Sales Corp., Filtration |and Minerals, P.O. Box 5108, Denver, CO 80217-5108. TABLE Z Preparation of Stock Standard Solutions Solution Number Component(s) WtS'' 1 toluene 5.00 z mixed xylenes 9.00 3 ethylbenzene 5.00 4 normal heptane 10.00 methyl cyclopentane 10.00 A Mixtures should be accurate to 0.01 % for each component. skimming techniques may be used on compounds appearing on the tails of skewed peaks. No t e 3--The nonaromatic fraction is customarily calculated collec tively by summing the areas of all the nonaromatic peaks, The nonaromatic fraction is generally the first group of peaks emerging before benzene. 11.5 Repeat 11.3 at least twice, and calculate the average response factors as follows: RPt = (AB)(ic)/(Ai -- Ao)(Bc) (1) where: RF, = response factor for impurity i, AB = average area of benzene peak, = concentration of impurity /, weight %, Ai = average area of impurity peak in.calibration blend, Ao = average area of impurity peak in pure benzene, and B,, concentration of benzene, weight1 11.6 Calculate response factors to nearest 0.001. No t e 4--The response factor for benzene will always be 1.000. 12. Procedure 12.1 Charge 0.6 pL of specimen Into chromatograph. 12.2 Measure the area of all peaks. The measurement of the specimen peak areas should be consistent with the method for measuring peak areas in the calibration blends; A typical chromatogram is shown in Fig. 1. 13. Calculation . 13.1 CalculateJhe amounts of each individual impurity as required. Sum the areas of all the nonarortiatic peaks. 13.2 Calculate, the weight percent conpentration, x, as follows: x = (Ax )(RFx W0)/At (2) At= >XRPx KAx) (3) where: Ax = area of component x, RFX = response factor of component x, and At = total adjusted peak area of the chromatogram, in cluding benzene. 13.3 Calculate the weight percent impurities, i, as follows: i = 100.00 - Bc (4) 14. Report 14.1 Report the following information: 14.1.1 Benzene and the total impurities to the nearest 0.01 %, and 14.1.2 Individual impurities to the nearest 0.001 %. DUP050296293 # D 4492 & retp FIG. 1 Benzene Analysis 15. Precision and Bias6 15.1 The following criteria should be used to judge the acceptability of results obtained by this test method (95 % confidence level). The precision criteria was derived from the round-robin data submitted by eight different laboratories. Each sample was run twice in two days by two different operators. 15.2 Repeatability--Duplicated results by the same oper ator should not be considered suspect unless they differ by more than the amount shown in Table 3. 6 Supporting data are available from ASTM Headquarters. Request RR: D16-I005. TABLE 3 Benzene Purity Repeatability and Reproducibility4'^'! : Added Impurity, wt % Concentration Average Concentration, Repeatability Reprod&fJ Blank (0.000) Toluene (O.OS4) Xylenes (0.099) Ethylbenzene (0.060) Nonaromatics (0.15B) 99.96 99.92 .99.88 99.92 99.84 0.0,10 0.024' 0.019 &023 0.020 0.021 0.123 '1 0.108 0.046 -.Hl&sgjs 0.055 * Data obtained from roind-robin study involving eight laboratories with fouffl replicate analyses of five samplss. ifVgj dm 15.3 Reproducibility--The results between two laborato-, ries should not be considered suspect unless they differ by more than the amount shown in Table"3. The American Society for Testing andMaterials takes no position respecting the validity ofanypatent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity ofany 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, eitherreapproved or withdrawn. Your comments are invitedeither torrevision ofthis standard or for additional standards- and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 732 DUP050296294 Designation: D 4493 - 89 Standard Test Method for Solidification Point of 4,4'-lsopropylldenediphenol (Bisphenol A)1 This standard is issued under the fixed designation D 4493; 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 (t) indicates an editorial change since the last revision or reapproval. ope [This test method describes the procedure for determiof the solidification point of 4,4'-isopropylidene hoi, commercially known as Bisphenol A, between 150 157C. This standard may involve hazardous materials, oper as, and equipment. This standard does not purport to r all ofthe safety problems associated with its use. It is Responsibility of the user of this standard to establish bpriate safety and health practices and determine the ficability of regulatory limitations prior to use. For Ic hazard statements, see Section 9. Referenced Documents ASTM Standards: 11493 Test Method for Solidification Point of Industrial | Organic Chemicals2 >4297 Practice for Sampling and Handling 4,4'-Isopro' pylidenediphenol (Bisphenol A)2 1 Specification for ASTM Thermometers3 ; 77 Method for Inspection and Verification of Liquid?h- in-Glass Thermometers3 1.2 Other Document: JSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 I Terminology 3.1 Definition: 3.1.1 solidification point--the temperature at which the |uid phase of a substance is in approximate equilibrium gath a relatively small amount of the same substance in its flid phase. Summary of Test Method 4.1 Bisphenol A is melted, and then cooled slowly with mstant agitation. When crystallization begins, and superoling occurs, the temperature falls to a minimum, rises to maximum, and then falls again. The maximum tempera- attained after crystallization begins is the solidification iSoint of Bisphenol A. 1 This test method is under the jurisdiction of ASTM Committee D-16 on jomatic Hydrocarbons and Related Chemicals-and is the direct responsibility of ubcommittee D16.0C on Oxygenated Aromatics. Current edition approved Nov. 24, 1989. Published January 1990. Originally ublished as D 4493 - 85. Last previous edition D 4493 - 85. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards. Vol !4.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 5. Significance and Use 5.1 The solidification point of Bisphenol A is a direct indication ofits purity, although it gives no information as to the nature of any impurities present. 5.2 High purity Bisphenol A has a solidification point of approximately 157C. 5.3 This test method can be used for internal quality control or for setting specifications. 6. Interference 6.1 Bisphenol A under test that is not stored or packaged properly may adsorb moisture. Adsorbed moisture will lower the solidification point. 7. Apparatus 7.1 Nessler Tubes5, borosilicate, 100 mL, short form, 32-mm diameter. 7.2 Electric Heat Block6, thermostatically controlled, ca pable of reaching I70C; having flat-bottom holes 34 mm in diameter by 172 mm deep. No t e 1--A suitable size block is 100 by 1.10 by 175 mm high, and made of aluminum. No t e 2--A thermostatically controlled hot oil bath may be used. 7.3 Erlenmeyer Flask, 500-mL. - No t e 3--The melted sample may be copied in an air jacket-cpoling bath, as specified in Test Method D 1493. ' 7A Thermometer--ASTM 102Q having a range from 123 to 177C and conforming to the requirements for thermometer 102C as prescribed in Specification El. No t e 4--Thermometers should be calibrated in accordance with Methods E77 or calibrated from 154 to 157C versus an NBS thermometer or platinum resistance thermometer. Preferably, thermom eters should be calibrated and certified by a thermometer manufacturer. An alternative thermometer is a platinum resistance thermometer7 with digital read-out. 7.5 Electric Heater8, stir plate, capable ofreaching 150C. 7.6 Magnetic Spinner9, starhead. 5 Fisher Scientific Co., No. 7-052 B, available from the local Fischer supplier, or its equivalent, has been found satisfactory for this purpose. 6 Model 60100 heater available from Precision Scientific, Div. of GCA Corp., 3737 W. Counland St, Chicago, IL 60647, or its equivalent, has been found satisfactory for this purpose. 7 No. 21282-4, available from Brooklyn Thermometer Co., 90 Verdi St., Farming-dale, NY 11735, or its equivalent,,has also been found satisfactory for this purpose. 8 Corning, Model PC-351, available from most laboratory supply houses, or its equivalent, has been found satisfactory for this purpose. 9 Fisher Scientific Co., No. 14-511-98C, or its equivalent, has been found satisfactory for this purpose. 733 DUP050296295 # D 4493 No t e 5--A wire stirrer, as specified in Test Method D 1493, may be used. 7.7 Chloroprene Rubber Stopper10, number 6, with hole to fit thermometer. If wire stirrer is used, an additional hole is needed. No t e 6--Stoppers made of cork or other materials should not be used. 7.8 Ring Stand and Clamp. 8. Reagents and Materials 8.1 Methyl Silicone Oil, suitable for continuous use at 200C. 9. Hazards 9.1 Consult current OSHAt Regulations and supplier's Material Safety Data Sheets for all materials used in this test method. 9.2 When handling molten solids in open tubes, adequate ventilation must be provided and proper protection should be used to prevent thermal bums. It is preferable to perform this test in a fume hood. 10. Sampling 10.1 Collect the sample as directed in Practice D 4297. 11. Procedure 11.1 Place a Nessler tube, filled with Bisphenol A, and 10 Fisher Scientific Co., No. 14-135 I or its equivalent has been found satisfactory for this purpose. containing the magnetic spinner, the stopper, and thermo eter, in an electric heat block, preheated to 170 5C,ji melt Bisphenol A. No t e 7--The solidification point is determined on the specimen received, with no drying procedure. r 11.2 As the Bisphenol A melts, add more to the Nessler tube, if necessary, so that the Immersion requirement of the thermometer will be met. It takes approximately 30 to '45 min to melt enough Bisphenol A to mn the test. In order to -fciB minimize the loss of volatile components, it is advisable to begin the solidification point determination as soon as possible after the Bisphenol A is molten, that is, within 5,,, min. 11.3 After the Bisphenol A has melted, remove the. Nessler tube from the heat block and place in the Erlenmeyer flask, which has been clamped to a ring stand (see Fig. 1). It may be necessary to wrap aluminum foil around the top portion of the Nessler tube, before placing in the Erlenmeyer flask, to prevent the tube from turning in the flask. The flask contains 400 mL of silicone oil that has been preheated to 140 2C , and is on a heater-stir plate. It is advisable to set the flask in a small aluminum foil pan to catch the oil in the event of a flask failure. 11.4 Submerge the thermometer to the immersion mark and ensure that the bulb of the thermometer is approxi mately 20 mm above the bottom of the Nessler tube, clearing the magnetic spinner. 11.5 Start the magnetic spinner stirring at a rate to create a vortex, and continue stirring until the liquid becomes solid enough to prevent the spinner from stirring. The cooling rate should be adjusted to maintain a constant temperature for 734 DUP050296296 D 4493 fit 3 min. The cooling rate may or may not be critical, Inding upon the product purity. |.6 Observe and record the thermometer readings at 30-s vals to the nearest 0.1*C until the temperature rises from -minimum, due to super codling, to a maximum, and By begins to drop. Further stirring will be impossible at point. The maximum temperature is the solidification pit. pIOTE g--Taking temperature readings 30 s apart wiil ensure against king a temporary plateau for the maximum temperature. Plotting I temperature readings against time will also help to identify a fijpotmy plateau. (1.7 Correct the observed solidification point for the iferation of the thermometer. Report 12.1 Report the solidification point as the maximum aperature attained after crystallization begins. Report to : nearest O.rc. TABLE 1 Results of Interlaboratory Freeze Point Tests Material 1 2 3 Average Average 155.41 154,23 154.58 154.74 Vr, %A 0.26 ' 0.23 0.15 0.21 VL. %e 0.30 0.42 0.31 0.34 Vr is the estimated relative standard deviation, or coefficient of variation within laboratories. a VL is the estimated relative standard deviation, or coefficient of variation between laboratories. 13. Precision and Bias 13.1 Precision--An interlaboratory study11 was con ducted by four laboratories to determine freeze points on three separate materials. Duplicates were run by each labo ratory on two different days. See Table I. 13.2 Bias--No statement is made about bias of the test method since there is no absolute method available as a referee method. 11 Supporting data are available from ASTM Headquarters. Request RR: D 16-1008. The American Society for Testing and Materials takes no position respecting the velidlty 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 in subject to revision af any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, eitherreapproved or withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you 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. DUP050296297 (jjjTta Designation: D 4534 89 Standard Test Method for Benzene Content of Cyclic Products by Gas Chromatography1 This standard is issued under the fixed designation D 4534; 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 often reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope J|.l This test method covers the determination of the benzene content of specific cyclic hydrocarbon products. 1.2 Benzene may be determined over a range from 5 to 300 mg/kg. 1.3 The products in which benzene can be determined include cyclohexane, toluene, individual C8 aromatics, cumene, and styrene. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address allofthe 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 Imitations prior to use. A specific hazard statement is given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 E 260 Practice for Packed Column Gas Chromatogra phy3 E 355 Practice for Gas Chromatography Terms and Rela tionships3 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Summary of Test Method 3.1 A gas chromatograph with a flame ionization or other detector and a column containing a supported polar liquid phase is used. A reproducible volume of sample is injected. Quantitative results are obtained from the measured area of the recorded benzene peak by using a factor obtained from, the analysis of a blend of known benzene content. 4. Significance and Use 4.1 Knowledge of the benzene content is typically re quired for cyclic products used as chemical intermediates and solvents. This test method may be used for final product 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0E on Instrumental Analysis. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 4534 - 85. Last previous edition D 4534 - 85. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 14.01. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. inspections, process control, establishing specifications; and research work. 5. Apparatus ; 5.1 Gas Chromatograph--Any chromatograph having eiij ther a flame ionization or other detector that is capable of providing a minimum peak height response of 0.1 mV for 20 mg/kg benzene using a maximum sample injection of 2 jrL 5.2 Chromatographic Column--The choice of column is based on resolution requirements. Any column may be used if it is capable of resolving benzene.from the major compo nent and other impurities. The column described in Table 1 has been found satisfactory. 5.3 Integrator--Electronic integration is recommended. 5.4 Recorder, Strip Chart, 0 to 1-mV range recording potentiometer with a response time of l s or less and maximum noise level of 0.3 % of full scale. If electronic integration is not used, a minimum chart width of 200 ram and a minimum chart, speed of 1 cm/min is required. 5.. 5 Microsyringe,, 10-pL capacity. 5.6 Volumetric Flask, 50-mL capacity. - 6. Reagents and Materials 6.1 Carrier Gas, helium or nitrogen, chromatographic grade. 6.2 Hydrogen, zero grade.. 6.3 Compressed Air, oil free. 6.4 Benzene, 99 % minimum purity. 6.5 Specific Cyclic Hydrocarbon,, high-purity (best grade obtainable) benzene content not to exceed 10 % of the level expected in the sample. 1 7. Hazards 'j 7.1 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this test method. TABLE 1 instrument Parameters Detector Column Length Outside diameter Stationary phase Support Temperature. C Sample inlet system Column Detector Carrier gas Row rate Sample size Hydrogen flame ionization Copper 3.7 m (12 ft) 3.175 (nm ('/a in.) TCEPE (Tetracyanoeihytated pentaerythritol), 10 % Chromosorb P,A 60-80 mesh 200 75-85fl 200 Helium or nitrogen 20 mL/min4 0.5-2 pL, reproducible 4 Chromosorb P Is a registered trademark of Johns-Manville Corp. 8 Approximate values, see 10.1. 736 DUP050296298 4534 ,,LE 2 Density of Cyclic Hydrocarbons at 15.56C, g/mL Benzene Cumene Cyclohexane Styrene Toluene 0.8838 0.8655 0.7826 0.9102 0.8711 "ampling l Guidelines for taking samples from bulk are given in Ltice D 3437. Calibration . 1 Prepare a calibration blend or blends of benzene in the 5c cyclic hydrocarbon at the level or levels approxi- ting those in the samples to be analyzed. A separate blend : be made for each specific cyclic hydrocarbon. .2 Calculate the benzene content of the calibration blend t the following equation and the densities listed in Table Benzene, mg/kg ' WXBJ (Si)(S2) GO3) ere: = density of benzene, = volume of benzene added to the cyclic hydrocarbon, pL, = density of cyclic hydrocarbon, and = volume of cyclic hydrocarbon, mL. 9.3 For example, to prepare an 81-mg/kg blend of bene in toluene, fill a 50-mL volumetric flask to the mark th high-purity toluene. With a microsyringe, carefully add JO pL of benzene to the toluene and mix well. i;9.4 Analyze both the blend and the pure cyclic bydro-bon used to prepare the blend as described in Section 10. :btract the area of the benzene found in the pure cyclic . drocarbon from the area of the benzene in the blend to etermine the area represented by the concentration of 'nzene added to the blend, as shown in 11.1. o. Procedure 1 10.1 Install the chromatographic column, and establish ; ble instrument operation at the proper operating condibns as shown in Table 1. Adjust column temperature and *w rate to achieve sufficient resolution. A retention time of to 6 min for benzene has beeif found to yield sufficient solution with the recommended column. Refer to instruc'ons provided by the manufacturer of the chromatograph d to Practices E 260 and E 355. 10.2 Inject a repeatable volume of sample, typically 2 pL r less, into the chromatograph. The volume of sample njected must be exactly the same as the volume of blend ejected. Start the recorder or integration device, or both, nd obtain the chromatogram. No t e--Some samples may contain components significantly heavier an benzene that may have a long retention time. If desired, the Major Component Cumene Cumene Cumene Cyclohexane Cyclohexane Cyclohexane Styrene Styrene Styrene Toluene Toluene TABLE 3 Precision Benzene Concentration, mg/kg Repeatability, mg/kg 51 27 2 222 19 64 4 66 5 277 28 15 2 38 6 204 11 20 2 190 16 Reasonable Range, mg/kg 0-11 22-33 206-256 35-90 55-115 244-310 0-35 25-67 120-250 14-23 147-206 column temperature may be raised after the elution of benzene to shorten the retention time of these components. If this is done, the column must be reequilibrated at the analysis temperature before each subsequent analysis. 10.3 Measure the area of the benzene peak. Units must be consistent with 9.4. 11. Calculation 11.1 Calculate the concentration of benzene in mg/kg in the cyclic hydrocarbon using the following equation: Benzene, mg/kg = AB/(C - D) where: A = area of benzene peak in the sample, B = concentration of benzene added to the blend. Impor tant: Blend must be made in the same cyclic hydro carbon as is being analyzed as the sample, C = area of benzene peak in the blend, and D = area of benzene in the pure cyclic hydrocarbon. 12. Report 12.1 Report the concentration of benzene in the sampleon an absolute basis to the nearest l mg/kg. 13. Precision and Bias5 13.1 The following criteria should be used to judge the acceptability (95 %_probability level) of results obtained by this method. The criteria were derived from a round robin among five laboratories. 13.1.1 Repeatability--Results in the same laboratory should not be considered suspect, unless they differ by more than the amount shown in Table 3. 13.1.2 Reproducibility--It is estimated that results on the same sample run in two laboratories should be considered suspect if they differ by more than the reasonable range shown in Table 3. Because of the round-robin results from this method, these values were taken straight from the research report without statistical reduction. 5 Supporting data arc available from ASTM Headquarters. Request RR: D16-1006. DUP050296299 # D 4534 The American Society for Testing and Materials takes no position respecting ihe validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of. Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and Ifnot revised, either reapproved or withdrawn. Yourcomments are invited either lor 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 fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. r 1 s I 738 DUP050296300 Last ASTM Designation: D 4588 - 87 Standard Guide for Analysis of p-Xylene bis guide is intended to aid in the selection of suitable ASTM test methods for determining the chemical or physical Jcteristics of finished p-xylene. Srmerly under the jurisdiction of D-16 on Aromatic Hydrocarbons and Related Chemicals, this guide was discontinued in land replaced by Specification D 5136, for High Purity p-Xylene.1 frnudl Book of 'AStM Standards, Vol 06.03. I, DUP050296301 Designation: D 4589 - 91 Standard Test Method for Nitrobenzene in Aniline1 This standard is issued under the fixed designation D 4589; 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 (cl indicates an editorial change sinoe the last revision or reapproval. 1. Scope 1.1 This test method covers a polarographic procedure for the determination of nitrobenzene in aniline. 1.2 This test method has been found applicable to the determination of nitrobenzene in aniline containing concen trations of not more than 25 mg/kg nitrobenzene. 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. For specific hazard statements, see Section 9 and Note 3. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D1549 Test Method for Zinc in Lubricating Oils and Additives (Polarographic Method)3 D3436 Practice for Sampling and Handling Aniline4 E 50 Practices for Apparatus, Reagents, and Safety Pre cautions for Chemical Analysis of Metals5 6 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200s 3. Summary of Test Method 3.1 Polarography is an electrochemical method of anal ysis. A quantitative evaluation of an electro-reducible mate rial such as nitrobenzene can be determined by measuring the characteristic current flow, as a function of an increas ingly applied voltage, resulting from the solution undergoing electrolysis. 3.2 The current flowing through the specimen during the analysis is in the microampere, range so several polarograms can be obtained on the same specimen solution without significant differences. 3.3 The nitrobenzene content is determined by mixing four volumes of aniline with one volume of concentrated hydrochloric acid. The diffusion current of nitrobenzene is 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0D on Organic Nitrogen Compounds. Current edition approved Oct. 15, 1991. Published 1991. Originally published as part of D 5264 - 73 T. Last previous edition D 3264-86. 2 Annual Book ofASTM Standards, Vols 06.03 and 1L01. 3 Annual Book ofASTM Standards, Vol 05.01. 4 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 03.05. 6 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. St, NW, Washington, DC 20006. then measured by polarographic technique. A standard calibration graph is developed with various concentrations of nitrobenzene in aniline versus their diffusion currents. A reading of the diffusion current level of the test specimen from the calibration graph determines its nitrobenzene content. 4. Significance and Use 4.1 This test method gives a quantitative means of detec tion of nitrobenzene in industrial grade aniline both for quality control and quality assurance of the product. 5. Interferences 5.1 Since the diffusion coefficient for solutions of organic molecules can possibly increase up to 2 % per degree rise in temperature, the polarographic cell temperature should be relatively the same when comparing specimen analyses with standard calibration analyses. 5.2 The sensitivity of an analysis is affected by the dimensions of the dropping mercury electrode (DME) capil lary and also by the height of the mercury column above the electrode. It is advisable to use the same DME capillary with a constant head of mercury that will -yield a uniform dropping rate during a series of analyses. Recalibrate when the DME is changed. 5.3 Sudden or severe vibrations of the DME system can cause interferences in the resulting polarogram. 5.4 Residual dissolved oxygen in the specimen solution will interfere with the analysis. This test method includes a nitrogen purge to remove dissolved oxygen. 6. Apparatus.... 6.1 Recording Polarograph--However, a nonrecording polarograph may be adapted for this test method. 6.2 Electrodes: 6.2.1 Dropping Mercury Electrode Capillary. 6.2.2 Electrolysis Vessel, with a mercury pool reference electrode. No t e 1--Suitable electrolysis assemblies are shown in Test Method D 1549 and Practices E 50. Any other cell that will perform similarly may be used. 6.3 Nitrogen Bubbler System and Purification Assembly. No t e 2--If the nitrogen being used contains enough oxygen to interfere with the polarogram, it must be purified by passing the gas over copper turnings at 450C. 6.4 Tubing, flexible, vinyl for connections. Rubber tubing should be avoided due to the possibility of oxygen perme ation. Due to the weight and viscosity of mercury, suitable hose clamps must be used for tubing connections to with stand stresses. DUP050296302 # D 4589 iReagents W.1 Purity ofReagents--Reagent grade chemicals shall be |d in all tests. Unless otherwise indicated, it is intended at all reagents shall conform to the specifications of tire ammittee on Analytical Reagents of the American Chem- Society, where such specifications are available;7 Other kdes may be used, provided it is first ascertained that the |agent is of sufficiently high purity to permit its use without sening the accuracy of the determination. |'7.1.1 Aniline, nitrobenzene-free and chemically pure (re- ent grade) for calibration purposes, p. 1.2 Hydrochloric Acid (HQ), concentrated and' chemiIly pure with a specific gravity of 1.19. 17.1.3 Mercury Metal, triple distilled instrument grade. [7.1.4 Nitrobenzene, chemically pure (reagent grade) for Ijibration purpbses. j'7.1.5 Nitrogen, water-pumped and oxygen-free. 7.2 Purity of Water--Unless otherwise indicated, refer- aces to water shall be understood to mean reagent water Informing to Specification D 1193. Standards J.8. l Prepare a master solution by weighing 100 1 mg of fitrobenzene into 1000 g of aniline. This master solution pntains 0.0001 g of nitrobenzene per gram of aniline and is gual to 100 mg/kg of nitrobenzene. Prepare separate andards containing 5, 10, 15, 20, and 25 mg/kg of jitrobenzene by appropriately diluting aliquots of the above paster solution by weight with aniline. Hazards 9.1 Special attention must be given to ventilation, merhandling, and the immediate cleaning of mercury spills. 9.2 Consult current OSHA regulations and supplier's [aterial Safety Data Sheets for all materials used in this test lethod. 10. Calibration and Standardization 10.1 The DME capillary has an average length of approxaately 80 mm and a bore of approximately 0.04 mm. The Height of the mercury column and reservoir will normally r from 400 to 800 mm. The exact length of the capillary nd the height of the mercury column are determined by rial and error to give a mercury drop-time from 3 to 5 when |t is immersed in a solution of the type to be tested. 10.2 Operate the polarograph in accordance with the Instrument manufacturer's instructions. Adjust the polarpgraph to the following specific settings: irect-current electromotive force (EMF) Initial EMF nP*ng opping mercury electrode Span voltage jlnitial voltage Sensitivity for standardization Percentage point span of applied EMF1 3V additive off negative 2.0V 0V 0.010 pA/mm 10 to 50 % 1 "Reagent Chemicals, American Chemical Society Specifications," American jfchemical Society, Washington, DC. For suggestions on the testing of reagents not pisted by the American Chemical Society, See "Reagent Chemicals and Standards," gjby Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopoeia." 10.2.1 The sensitivity setting may vary with individual instruments. 10.3 Develop polarograms for the series of standards in accordance with the analytical procedure described in Sec tion 11. 10.4 Construct a calibration graph by plotting the wave height of the diffusion current- curve versus the percentage value of the nitrobenzene in the standards on linear graph paper. The calibration curve is valid for comparisons with specimens if the standards and specimens are analyzed with the same set of instrument conditions, cell temperature, and a constant dropping rate of mercury. 11. Procedure 11.1 Pipet a 40.0-mL specimen (sampled in accordance with Practice D 3436) into a beaker and add 10.0 mL of HCI by pipeting and then mix thoroughly. No t e 3: Caution--Prepare the mixture in a fume hood and wear standard protective safety equipment. 11.2 Transfer a sufficient quantity of specimen solution to the electrolysis vessel to immerse the DME capillary. Adjust the mercury head to a level predetermined to give the desired constant drop rate, Purge the specimen by bubbling oxygenfree nitrogen through the specimen for 10 min at a moderate rate. 11.3 Shut off the nitrogen purge and determine a polarogram of the test specimen while observing the specific instrument parameters given in 10.2. No t e 4--A nitrogen blanket above the specimen without disturbing the specimen is desirable. 11.4 Clean the electrolysis vessel with water, acetone, and again with water between analyses to prevent cross contam ination. 12. Calculation 12.1 The diffusion current will increase from a small value as the mercury droplet begins to form to a maximum value as the drop falls. After the drop Ms, the diffusion current will also fall to the low value again. This process is repeated each time a mercury drop is formed and falls producing current oscillations that can be recorded. When nitrobenzene is present, an S-shaped saw-tooth wave will be obtained when the current is recorded on a strip-chart recorder as the applied voltage is spanned. Measure the wave height graphically; the height of the wave will be propor tional to the degree of concentration of nitrobenzene present 12.2 Calculate the diffusion current due to nitrobenzene as follows; D = tdy. S where: D = diffusion current, pA, id -- current wave height, mm, and 5 = sensitivity setting of the polarograph, pA/mm. ' 12.2.1 Using the D value of the specimen, the concentra tion of nitrobenzene corresponding to diffusion current may be read from a previously prepared calibration curve of nitrobenzene concentrations versus diffusion currents of various standards. 741 DUP050296303 # 0 4589 13. Report 13.1 Report the following information: 13.1.1 Nitrobenzene content, mg/kg. 14. Precision and Bias 14.1 Precision--The following criteria should be used for judging the acceptability of results: 14.1.1 Repeatability (Single Analyst)--Duplicate results by the same analyst should not be considered suspect unless they differ by more than 0.8 mg/kg (95 % confidence levelV-' 14.1.2 Reproducibility (Multilaboratory)--The average r& suit reported by one laboratory should not be consider? suspect unless it differs from that of another laboratory bv more than 1.00 mg/kg (95 % confidence level). 14.2 Bias--No statement is made about bias since there' no absolute method available as a referee method. 15. Keywords 15.1 aniline; nitrobenzene; polarographic 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 forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 742 f >- DUP050296304 Designation: D 4590 - 86 Standard Test Method for Colorimetric Determination of p-terf-Butylcatechoi In Styrene Monomer by Addition of Alcoholic NaOH1 This standard is issued under the fixed designation D 4590; 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. cope 1.1 This test method is applicable to the determination of fdual 4-tertiary-butylcatechol (TBC) in styrene monomer pie 1 to 100 ppm range. Any other compound known to jlduce color when contacted with aqueous sodium hyBxide solution will interfere. It may be compensated for by lluding it in the preparation of the standard solutions, if its jptity and concentration in the sample are known. \2 This standard may involve hazardous materials, operShs and equipment. This standard does not purport to Idress all ofthe safety problems associated with its use. It is 1? responsibility ofwhoever uses this standard to consult and mablish appropriate safety and health practices and deterIine the applicability of regulatory limitations prior to use. gor specific statements on hazards, see Section 7. ^jf Referenced Documents |2.1 ASTM Standards: pD 1193 Specification for Reagent Water2 I D 3437 Practice for Sampling and Handling Liquid Cyclic Products3 12.2 Other Document: I OSHA Regulations4 Summary of Method : 3.1 Color is developed in the sample by the addition of austic in a methanol-octanol solvent. The pink color ptensity is measured with a spectrophotometer and cornred to a calibration curve for quantitation. Significance and Use 4.1 This test method is suitable for determining the |uantity of TBC inhibitor, both for the protection against olymerization while in transit aftd storage, and for internal |uality control. . Apparatus 5.1 Visible Range Spectrophotometer, equipped with ab|orption cells providing light paths from 1 to 5 cm for use at Approximately 490 nm. 5.2 Volumetric Pipets, 5 mL. 1 This test method is under the jurisdiction of ASTM Committee D-!6 on lAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee DI6.0H on Styrene, Ethylbenzene Isopropylbenzene. il Current edition approved May 30, 1986. Published July 1986. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Available from the Occupational Safety and Health Review Commission, 1825 K St., NW, Washington, DC 20006. 5.3 Pipetors, 0.1 and 0.2 mL. 6. Reagents and Materials 6.1 Purity of Reagents--Where unspecified, chemicals shall be reagent grade and conform to recognized specifica tions if such exist.5 If found to have no adverse effect on accuracy, other grades may be used. 6.2 4-Tertiary-Butylcatechd, Mp 52-55'C. 6.3 Toluene, ACS reagent grade. 6.4 Methanol, reagent grade. 6.5 n-Octanol, reagent grade. 6.6 Sodium Hydroxide Pellets, reagent grade. 6.7 Alcoholic Sodium Hydroxide, approximately 0.15 N. Dissolve 0.3 g NaOH in 25 mL methanol. Add 25 mL of H-octanol and 100 pL of water. Let this reagent mature for two days before use. This solution is stable for two weeks. 6.8 TBC Stock Standard--Weigh 0.5 g of TBC into 500 g of toluene. This solution will contain 1000 ppm TBC. This standard should have a shelf life of one year or better if stored in a refrigerator or freezer. 6.9 Unless otherwise indicated, references to water shall be understood to- mean any reagent water' as defined in Specification D 1193. 7. Hazards 7.1 Consult the latest OSHA regulations regarding all materials used in this test method. 7.2 Handling Precautions--p-fert-butylcatechol, particu larly when molten or in concentrated- solution, is verycorrosive to the skin. It is also a systemic poison when taken orally or absorbed in quantity through the skin. 7.3 Flammable Hazards--Styrene monomer is flam mable and polymerizes exothermally in the presence of peroxide, mineral acids, and aluminum chloride. 8. Sampling 8.1 Collect the samples in accordance with Practice D 3437. 9. Preparation of Calibration Curve 9.1 Prepare standards of 5,10,20,30, 40, 50, 70, and-100 ppm (mg/kg) TBC in styrene by diluting 0.5, 1, 2, 3, 4, 5, 7, and 10 mLs of TBC stock standard to 100 mLs with toluene. 5 "Reagent Chemicals. American Chemical Society Specifications," Am. Chemical Soc., Washington, DC, or, in the UK, proprietary specifications for Analytical Grade Chemicals. 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" or the "British Pharmacopeia." 743 DUP050296305 D 4590 9.2 Determine the absorbance of each standard solution and one reagent blank in accordance with Section 10. 9.3 Plot absorbance versus concentration on standard graph paper. No t e 1--The plot is close to a straight line. Higher concentrations will definitely yield a curve up to about 300 ppm, then it drops off. 10. Procedure 10.1 Zero the spectrophotometer with the sample to be analyzed. 10.2 Add 5 mL of sample to a dean container. No t e 2--Use acetone or the purest methanol available for glassware cleaning as low results are caused by inferior methanol presence. 10.3 Shake the alcoholic NaOH reagent to ensure homo geneity. No t e 3--The turbidity formed, as the sodium hydroxide ages does not appear to be harmful. 10.4 Add 100 pL of alcoholic NaOH reagent to the container and mix vigorously for 30 s. No t e 4--A vortex mixer is beneficial if round cells are used. 10.5 Add 200 pL of methanol to the container and shake for 15 s. No t e 5--If a blue color persists before the methanol is added, the concentration range has been exceeded. Dilute the sample 1:10 with toluene and repeat. 10.6 Measure the absorbance at 490 nm as soon as possible and within 5 min. No t e 6--Color intensity will increase about 15 % per minute the first 5 min. 10.7 Read the concentration in parts per million TBO from the graph. 11. Report 11.1 Report the inhibitor content of the sample as part! per million (mg/kg) of p-fert-butylcatechol. 12. Precision and Bias6 12.1 Precision--Data obtained by this procedure indicale absolute standard deviations of 0.34 and 0.40 ppm (relativstandard deviation of 2.9 % and 0.8 %) at levels of 12 and 48 ppm TBC, respectively. Results obtained by this proc would be expected to vary from the average by no more than 6 % relative at the 12 ppm level and 2 % relative at the 4 ` ppm level (95 % confidence limit). Testing done in one'1 laboratory by one analyst on a sample of styrene indicates a standard deviation of0.17 ppm at the 12 ppm level based on 15 . analyses. Analysis of a series of synthetic mixtures over the range from 7 to 116 ppm gave recoveries that averaged 98 % with a standard deviation of 1.2 %. 12.2 Bias--r-The bias of this test method cannot be, deter mined because no acceptable reference material and value is available. 6 Supporting data are available from ASTM Headquarters. Request HR: D16-1009. The American Society for Testing end Materials takes no position respecting the validity at any patent rights assertedin 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 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 notrevised, either reapproved or withdrawn. Your comments are invitedeither torrevision ot this standard or for additional 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, 1976 Race St., Philadelphia, PA 79103. 744 DUP050296306 Designation: D 4734 - 90 Standard Specification for Refined Benzene-5451 This standard iis issued under the fixed designation D 4734; 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. (Scope .1 This specification covers benzene-545. .2 Consult current OSHA regulations and supplier's terial Safety Data Sheets for all materials used in this Scation. Referenced Documents .1 ASTM Standards: jD847 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aro matic Hydrocarbons2 ' D848 Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons2 : D849 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons2 D 850 Test Method for Distillation of Industrial Aromatic : Hydrocarbons and Related Materials? , D 852 Test Method for Solidification Point of Benzene2 > D1209 Test Method for Color of Clear Liquids (Plati num-Cobalt Scale)2 ; D1685 Test Method for Traces of Thiophene in Benzene by Spectrophotometry2 D2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 D 3505 Test Method for Density or Relative Density of Pure Liquid Chemicals2 D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry3 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 D4492 Test Method for Analysis of Benzene by Gas Chromatography2 1 This specification is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee DI6.QA on Benzene, Toluene, Xylenes. Cyclohexane, and Their Derivatives. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as D 4734 - 87. Last previous edition D 4734 - 87. 2 Annual Book ofASTM Standards, Vol. 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. D4629 Test Method for Organically Bound Trace Ni trogen in Liquid Petroleum Hydrocarbons by Oxidative Combustion and Chemiluminescence Detection3 D 4735 Test'Method for Determination of Trace Thiopene in Refined Benzene by Gas Chromatograph2 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Properties 3.1 Benzene-545 shall conform to the following require ments: Property Benzene, min, weight % Sulfur, max, mg/kg Thiophene, max, mg/kg Toluene, max, weight % Nonaromatic hydrocarbons, max, weight % N-formylmorpholine as nitrogen Acid wash color, max Acidity Copper corrosion Appearance Color, max, Pt-Co scale Relative Density, 15.56/15.56 'C or Density, 20"C, g/cm5 Distillation range including the temperature 80.1 "C at (760 mm Hg) pressure, max, *C Solidification point, anhydrous Specification 99.90 1 0.6 0.05 0.10 ASTM Test Method D4492 D4045 D 1685 or D 4735 D 4492 D 2360 (if needed) pass with 1 none detected pass (la or lb) A 20 0.8820 to 0.8860 D4629 D 848 "D 847 D849 i> 1209 D 3505 or D4052 0.8780 to 0.8820 4.0 A D 850 5.45 D 852 A Clear liquid free ofsediment and haze when observed at IS.3 to 25.6*C (65 to 78'F). ------ n Refer to Method D 850. Sample Section if drying is required. 4. Sampling 4.1 The material shall be sampled in accordance with Practice D 3437. 5. Keywords 5.1 benzene; benzene-545; purity 4 Available from Superintendent of Documents, U.S. Government. Printing Office, Washington, DC 20402. 745 DUP050296307 # D 4734 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. Yourcomments are invited eitherfor 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 theASTM Committee on Standards, 19t6 Race St., Philadelphia, PA 19103. 746 PW I DUP050296308 Designation: D 4735 - 87 (Reapproved 1991)'i Standard Test Method for Determination of Trace Thiophene in Refined Benzene by Gas Chromatography1 This standard is issued under the fixed designation D 4735; 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. " No t e--Keywords were added editorially in September 1991. cope .1 This test method covers the determination of ophene in refined benzene in the range from 0.5 mg/kg to mg/kg. The range of the test method may be extended by difying the sample injection volume, calibration range, or pie dilution with thiophene-free solvent 1.2 This test method has been found applicable to benfe characteristic of the type described in Specification 2359 and may be applicable to other types or grades.of hzene only after the user has demonstrated that the jrdcedure can completely resolve thiophene from the other anic contaminants contained in the sample. :i 1.3 This standard does not purport to address all of the rety problems, if any, associated with its use. It is the __ onsibility ofthe user of this standard to establish appro bate safety and health practices and determine the applicaity of regulatory limitations prior to use. For specific l statements, see Section 7. Referenced Documents 2.1 ASTM Standards: 6 835 Specification for Refined Benzene-4852 D1193 Specification for Reagent Water3 D1685 Test Method for Traces of Thiophene in Benzene by Spectrophotometry2 D2359 Specification for Refined Benzene-5352. D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 E 260 Practice for Packed Column Gas Chromatography4 E 840 Practice for Using Flame Photometric Detectors in ' Gas Chromatography4 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12005 3. Summary of Test Method 3.1 The thiophene concentration in refined benzene is 1 This test method is under the jurisdiction of ASTM Committee ,D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0E on Instrumental Analysis. Current edition approved Oct. 30, 1987. Published December 1987. 2 Annual Book ofASTM Standards, Vol 06.03, 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 14.01. 5 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. determined at the milligram thiophene per kilogram, sample level using conventional gas-liquid chromatography with a flame photometric detector. A reproducible volume of sample is injected. Quantitative results are obtained by the external standard technique using the measured peak area of thiophene. 4. Significance and Use 4.1 This test method is suitable for setting specifications on benzene and for-use as an internal quality control tool where benzene is either produced or used in a manufacturing process. 4.2 This test method was found applicable for deter mining thiophene in refined benzene conforming to the specifications described in Specification D 2359 and may be applicable toward other grades of benzene if the user has taken the necessary precautions as described in the text. 4.3 This test method was developed as an alternative technique to Test Method D 1685. 5. Apparatus 5.1 Gas Chromatograph--Any chromatograph having a flame photometric detector may be used which can operate at the typical conditions described in Table I. the user is referred to Practice E 260 for additional information about gas chromatography principles and procedures: 5.2 Column--The column must provide complete resoliition of thiophene-from benzene and any other hydrocarbon impurities because of potential quenching effects by hydro carbons on the light emissions from the thiophene. The columns described in Table 1 have been judged satisfactory. ` 5.3 Detector--Any flame photometric detector (FPD) can be used, provided it has sufficient sensitivity to produce a minimum peak height twice that of the base noise for a 4-pL injection volume of 0.5 mg/kg thiophene in benzene. The user is referred to Practice E 840 for assistance in optimizing the operation and performance of the FPD. 5.4 Integrator--Electronic integration is recommended. 5.5 Recorder, a-c, 1-mV range strip chart recorder is recommended. 5.6 Microsyringe, 10-pL capacity. 5.7 Volumetric Flasks, 50, 100 and 500-mL capacity. 5.8 Separatory Funnel, 1 -L capacity. 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended 747 g-v'..:. r* DUP050296309 # D 4735 TABLE 1 Thiophene in Benzene Instrumental Conditions A6 Column Tubing Phase Concentration, weight % Support Mesh Detector H,., mL/mln Air I, mL/min Air 11. mL/min Gas chromatographic conditions Inlet, C Detector, C Carrier Gas Row Rate, mL/min Column Temperature. C 6 ft x 1/8 In. Ni Steel TCEPEA 7 Chromosorb P-AW 100/120 140 80 170 ISO 220 helium 30 70 15 ft by 1/8 in. stainless steel SP-1000 10 Supelcoport 60/80 140 80 170 170 220 helium 30 90 * Tetracyanoethylated pentaeiythiitot or pentrile. 6 Chromosorb P Is a registered trademarK of the Manvffle Corp. C 10 ft by 1 /S in. stainless steel OV-351 10 Chromosorb P-AW 80/100 140 80 170 180 250 helium 30 70 that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is ofsufficiently high, purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ence to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 6.3 Carrier Gas, nitrogen or helium, chromatographic grade. 6.4 Hydrogen, zero grade. 6.5 Compressed Air, hydrocarbon-free. 6.6 Cadmium Chloride Solution (20 g/L)--Dissolve 20 g of anhydrous cadmium chloride CdCl2 into 200 mL ofwater and dilute to 1 L. 6.7 Isatin Solution1--Add 0.5 g of isatin to 200 mL of chloroform. Heat under a fume hood to a temperature just below the boiling point of chloroform (61 C) and maintain for 5 min with stirring. Filter the hot solution through hardened rapid-filter paper into a 250-mL volumetric flask and dilute to volume. 6.8 Benzene, Thiophene-Free--Wash 700 mL of benzene in a 1000-mL separatory funnel to which has been, added 5 mL of isatin solution, with successive 100-mL portions of concentrated sulfuric acid until the H2S04 layer is light yellow or colorless. Wash the benzene with 100 mL of water, then twice with 100 mL of cadmium chloride solution (CdCl2). Finally, wash with another 100-mL portion of water and filter the benzene through medium filter paper into a storage bottle, stopper the bottle tightly and save for future use. 6.9 Sulfuric Acid--Concentrated H2S04.* 7 * "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not fisted by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrami Co., inc., New York, NY, and the "United States Pharmacopeia,'1 7 Isatin 2,3-indolinedione such as Aldrich Catalog No. 11,461-8, available from Aldrich Chemical Co., Inc., 940 W. Saint Paul Ave., Milwaukee, Wi 53233, or equivalent has been found satisfactory for this purpose. 6.10 Thiophene*. 7. Hazards 7. L Benzene is considered a hazardous material. Consult current OSHA regulatipns and supplier's Material Safety Data Sheets for all materials used in this method. 8. Sampling and Handling 8.1 Sampling of benzene should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA-regulations. Refer to Practice D3437 for proper sampling and handling of benzene. > 9. Preparation of the Apparatus 9.1 The chromatographic separation of trace level sulfur compounds can be complicated by absorption of the sulfur compounds by the gas chromatographic system. Therefore, care should be taken to properly free the system of active sites where absorption or reactions could take place. 9.2 Follow the manufacturer's instructions for mounting the column into the gas chromatograph and. adjusting the instrument to conditions described in Table 1. Allow , the instrument and detector sufficient time to reach equilibrium. 10. Calibration Curve 10.1 Prepare a 500-mL stock solution of thiophene in benzene at the 100 mg/kg level by adding 0.04.g (38.0 pL) of thiophene to 435 g (500 mL) of thiophene-free benzene. 10.2 Calculate the thiophene content of the stock solution according to the following equation: Thiophene, mg/kg = (A x 103)/B where: A weight of thiopene, mg, and B = weight of benzene, g. 10.3 Prepare five calibration blends ranging from 0.00 to 10.0 mg/kg of thiophene in benzene by diluting the appro priate volume of stock solution into a known volume of thiophene-free benzene. 8 Thiophene such as Aldrich Catalog No. T3,180-1, available from Aldrich Chemical Co., Inc., 940 W. Saint Paul Ave./Milwaukee, WI 53233, or equivalent has been found satisfactory for this purpose. 748 i------- -i DUP050296310 # D 4735 FIG. 1 M I N U I fi Chromatogram Illustrating the Analysis o! 1.10 mg/kg Thiophene in Benzene SiO.4For example, an 87.0 mg/kg stock solution was spared by dissolving 0.0378 g thiophene into 435 g of jnzene. Aliquots of0.00,0.75, 1.0,2.0, and 5.0 mL ofstock Jlution were dissolved in 100 mL ofthiophene-free benzene 1'produce 0.00, 0.65, 0.87, 1.75, and 4.35 mg/kg, respecfyely. |jil0.5 Inject 4.0 |xL of each solution into the promatograph. Integrate the area under the thiophene peak. ch standard solution and the blank should be analyzed in Implicate. Ij JJo t e I--Injection volumes must be consistent and reproducible. ; 10.6 Prepare a calibration curve by plotting the integrated : area versus milligram per kilogram of thiophene on a tieet of log/log graph paper. No t e 2--In the sulfur mode, the FPD will exhibit a response that is nonlinear power law function. Please refer to Practice E840 for tiditional information on the characteristics and usage of the FPD. 11. Procedure 11.1 Charge 4.0 pL of sample into the chromatograph. 11.2 Measure the area of the thiophene peak. The meaement of the sample peak should be consistent with the nethod for measuring peak areas In the calibration blends. A pical chromatogram is shown in Fig. 1 representing 1.10 mg/kg thiophene in benzene. 13. Report 13.1 Report the thiophene concentration to the nearest 0.01 mg/kg. 14. Precision and Bias 14.1 The following criteria should be used to judge the acceptability of the 95% probability level of the results obtained by this test method. The criteria were derived from a round robin between five laboratories. The-data were obtained over 2 days using different operators. . 14.2 Repeatability--Results in the same laboratory should not be considered suspect unless they differ by more than the amount shown in Table 2. 14.3 Reproducibility--The results submitted by two labo ratories should not be considered suspect unless they differ by more than the amount shown in Table 2. 14.4 Bias--The bias in this test method is being deter mined. TABLE 8 Thiophene Concentration, mg/kg 0.80 1.80 Repeatability and Reproducibility Repeatability, mg/kg Reproducibility, mg/kg 0.040 0.078 0.060 0.078 12. Calculation 12.1 Determine the amount of thiophene directly from Ithe calibration curve prepared in 10.6. 15. Keywords 15.1 benzene; flame photometric detector; gas chromatog raphy; thiophene 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 infringement of such rights, are entirely their own responsibility. This standard Is subjeot 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 for revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel thet your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19W3. 749 DUP050296311 Designation: D 4789 - 88 Standard Test Method for Solution Color of 4,4'-lsopropylidenediphenol (Bisphendl A)1 This standard is issued under the fixed designation D 4789; 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. 1. Scope 1.1 This test method describes the procedure for determi nation of the Platinum-Cobalt Color of 4,4'-Isopropylidenediphenol, commercially known as bisphenol A, dissolved in methanol. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8. 2. Referenced Documents 2.1 ASTM Standards: D1209 Test Method for Color ofClear Liquids (Platinum- Cobalt Scale)2 D4297 Practice for Sampling and Handling 4,4'-Isopro- pylidenediphenol (Bisphenol A)3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.I2004 NIST Letter Circular LC1017, Standard for Checking the Calibration of Spectrophotometers (200 to 1000 nm)5 3. Summary of Test Method 3.1 Bisphenol A is dissolved in methanol. This solution is then transferred to a color comparison tube and the color compared to that of the Platinum-Cobalt Color Standards, either visually or by means of a spectrophotometer. The color is reported as that closest to the applicable standard. 4. Significance and Use 4.1 The presence or absence of color in bisphenol A varies in importance, depending upon its application and the amount of color that can be tolerated in that application. The amount of color also is an indication of the degree of refinement ofbisphenol A, but gives no information as to the nature of any impurities present. 4.2 This test method can be used for internal quality control or for setting specifications. 1 This test method is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0C on Oxygenated Aromatics. Current edition approved Sept. 30, 1988. Published November 1988. 2 Annual Book ofASTM Standards, Vols 06.01 and 06.03. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 5 Available from National Institute of Standards and Technology, U.S. Depart ment of Commerce, Gaithersburg, MD 20899. 5. Interferences 5.1 The presence of any turbidity or haze will affect the color reading. t 5.2 A bisphenol A color that is off-hue, with respect to the r` color standards, will interfere with proper color comparison . 6. Apparatus i 1 6.1 Color Comparison Tubes--Matched 100 mL, tall- ,! form Nessler tubes, provided with ground-on, optically clear, I glass caps. Tubes should be selected so that the height of the . 100-mL graduation mark is 275 to 295 mm above the ' bottom of the tube. 6.2 Color Comparator, constructed to permit visual com parison of light transmitted through tail-form, 100 mL ` Nessler tubes in the direction of their longitudinal axis; and so that white light is passed through or reflected off a while glass plate and directed with equal intensity through the * tubes. It should be shielded so that no light enters the tubes from the sides. 6.3 Spectrophotometer, equipped for liquid samples and. I for measurements in the visible region.6 No t e 1--The spectrophotometer must be clean and in excellent operating condition. The instrument should be calibrated in accordance with the instructions given in NIST Letter Circular LC 1017. For good agreement with the visual method, the spectrophotometer should be a filter type instrument, such as a colorimeter, with a large bandpass, j | ! 6.4 Spectrophotometer Cells, matched, having a 10-mm light path. ..... '! 6.5 Filter Paper, glass fiber filter, 1.^m pore retention. * 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 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. 7.2 Methanol--Check for color against deionized water; if the methanol is not water white, redistill in an ail-glass system. j j I f " != f '` l! 6 Beckman Model B, available from Beckman Instruments, 41365 Vincenti Ct., Novi, MI 48050, or its equivalent, has been found satisfactory for this purpose. '"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." 750 DUP050296312 # D'4789 |7.3 Platinum-Cobalt Color Standards--Prepared acag to Test Method D 1209. Hazards 8.1 Consult current OSHA regulations and suppliers' aterial Safety Data Sheets for all materials utilized in this : method. . Sampling 9.1 Collect the sample as directed in Practice D 4297, Q. Procedure 10.1 Weigh 50 g of bisphenol A. Transfer to a 150-mL Irlenmeyer flask. l! 10.2 Measure 70 mL of methanol. Add to the Erienmeyer flask containing the bisphenol A. 10.3 Stir until all the bisphenol A is dissolved. : 10.4 Transfer the methanol solution to a color comparson tube, fill to the 100-mL mark, and cap the tube. 10.5 If there is any visible turbidity, pass the methanol |dlution through a filter and refill the comparison tube, 10.6 Visually compare the methanol solution comparison libe with the color standards. A spectrophotometer can be sed to determine the transmittance at a wavelength of 436 am, which would be an indication of the color intensity. No t e 2: Caution--Use of a spectrophotometer may provide colors ivhich are higher or inconsistent with those colors obtained by using olor comparison tubes. 11. Report 11.1 Report the following information: ip 11.1.1 The number of the standard that most nearly Imatches the specimen. If the color lies midway between two standards, report the darker of the two. 11.1.2 The result to the nearest 5 units. Duplicate runs that agree within 10 units absolute- are acceptable for averaging {95 % confidence level). 11.2 If there is a difference in hue between the specimens and the standards, and a definite match cannot be made, report the range over which an apparent match is obtained, and report the material as "off-hue." 12. Precision and Bias8 12.1 Precision--The precision estimates are based upon an interlaboratory study on three specimens of bisphenol A from three different sources. One analyst in each of six laboratories performed duplicate determinations and re peated on a second day, for a total of 72 determinations. Practice E 180 was used in developing these precision estimates. 12.1.1 Repeatability (Single Analyst)--The standard devi ation of results (each the average of duplicate determina tions), obtained by the same analyst on different days, was estimated to be 2.0 units absolute at 18 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 10 units absolute. 12.1.2 Reproducibility (Multilaboratory)--The standard deviation of results (each the average ofduplicate determina tions), obtained by analysts in different laboratories has been estimated to be 9.0 units absolute at 5 df. Two such averages should be considered suspect (95 % confidence level) if they differ by more than 35 units absolute. 12.2 Bias--The bias of this test method ' lias not been determined. "Supporting data are available from ASTM Headquarters. Request RR.D161010. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and knot revised, eitherreapproved or withdrawn. Your comments are Invited either forrevision -ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 751 DUP050296313 Designation: D 4790 - 89a Standard Terminology of Aromatic Hydrocarbons and Related Chemicals1 This standard is issued under the fixed designation D 4790; 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. absorbance--the logarithm to the base 10 ofthe reciprocal of the relative transmittance, T, expressed as: A = log,0 (1/7) = -logIO T D 1840, D 2269, D 4053; D-2 accuracy--the agreement between the mean of a series of repeated measurements of a property and the accepted reference value of the property. D 3980; D-l acidity--the number of milligrams of sodium hydroxide consumed when 100 mL of the sample are titrated under the conditions prescribed in this method. D847; D-16 acid reaction--a characteristic of materials producing the acid-color of the indicator used under die conditions prescribed in this method. D 847; D-16 acid wash color--the color developed in the separated acid when a sample is agitated with sulfuric acid under the condition prescribed in this method. D 848; D 2279; D-16 aldehydes--a broad class of organic compounds having a generic formula RCHO, and characterized by a carbonyl group. alkaline or basic reaction--a characteristic of the materials producing the alkalicolor of the indicator used under the conditions prescribed in this method. D 847; D-16 alpha-methylstyrene--2-phenyIpropene (QH^) mol weight 119.16; colorless liquid; subject to polymerization by heat or catalysts; freezing point, -23.2rC; boiling point, 165.38C. apparent density--the density calculated whenv the pycnometer volume is calibrated with water, weighed in air, and when the sample is weighed in air and no air buoyancy correction is used for either weighing, even though the density in vacuum of water is used in. calcu lating the volume. apparent density at 60F --the weight in air ofa unit volume of sample at 60"F; in this method, the weight is in pounds and the volume in U.S.. liquid gallons. Average air in this method is assumed to have a density of 0.0012 g/cms. Dis c u s s io n --This definition is not in conflict with that given in the current version of Definitions E 12. D 2935; D-16 benzene--cyciohexatriene, benzol (obsolete) (C6H6) mol weight 78.11; clear, colorless, highly flammable liquid; characteristic odor, solidification point +5.5C; boiling point 80.1C. 1 This terminology is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0F on Editorial and Nomenclature. Current edition approved Nov. 24, 1989. Published January 1990. Originally published as D 4790 - 88. Last previous edition D 4790 - 89. The boldface designations refer to the original source of the definition and the ASTM Technical Committee havingjurisdiction. benzene, carbon disulfide-free--benzene treated with holic sodium hydroxide and used as a spectrophotom reference standard. benzene-535, refined--benzene with impurities limited trace amounts by a solidification point of 5.35C having a total distillation range of no more than 11 Refer to Specification D 2359 for complete specificati benzene-485, refined (nitration grade)--benzene with rities limited by a solidification point of 4.85C and a total distillation range pf no more than l.O'C R- Specification D 835 for complete specifications. benzene, industrial grade--benzene (Including its impu having a total distillation range of no more than 2C used directly or indirectly in processes that are ins to impurities. Refer to Specification D 836 for co" specifications. benzene, thiophene-free--benzene refined by special nient and used as a reagent in ASTM standards, bias--a persistent positive or negative deviation of a method average value from the assumed or accepted i value. D 1129; D 2777; D- bromine index--the number of milligrams of bromine sumed by 100 g of sample under given conditions. D 1492; D-! carbon disulfide (CS2)--mol weight 76.14; clear, colorle flammable, volatile liquid; boiling point, 45.6C; freezing, point, 111.6C. clear--free of turbidity. ! cloud point of phenol--the temperature at which a separate* phase forms when a homogeneous solution.of phenol in | water is allowed to cool at a' prescribed rate from at temperature above that at which phase separation occurs. It may precisely be defined as follows: when a homoge neous solution of phenol and water is allowed to cool at a prescribed rate with stirring, the solution will show a slight cloudiness or turbidity as the cloud point is approached. On further cooling, the cloudiness will increase rapidly and the thermometer bulb, which is centrally located in the test tube, will suddenly become invisible. The temperature at which the thermometer bulb becomes invisible is taken as the cloud point D 2147; D-16 cloudy--qualitative expression of turbidity, confidence limits--the limits on either side ofthe mean value of a group of observations which will, in a stated fraction or percent of the cases include the expected value. Thus the 95 % confidence limits are the values between which the population mean will be situated in 95 out of 100 cases. D 3980; D-l copper corrosion--a qualitative indication of reactive impu rities in aromatic hydrocarbons. An iridescent, gray, or 752 DUP050296314 # D 4790 : discoloration of polished copper strip is considered e for rejection. i!ive substance--in Committee D-16 Standards, matein industrial aromatic hydrocarbons that discolors or hes polished copper. j(s)--methyl phenol, hydroxymethyl benzene (C7HsO) weight 108.13; colorless, yellowish, brownish, yellow, :t,{pinkish liquid; phenolic odor. Three isomeric cresols c acids--commercial mixtures of phenolic materials ich may include phenol, cresols, xylenols, and other ylated phenols, ne--See isopropylbenzene. exane-995--cyclohexane with a purity of 99.5 _ht % minimum determined by analysis by gas chrotography. Refer to proposed specifications for complete uirements. :es of freedom--the number of observations minus the mber of constraints imposed upon the system. In eral, only one constraint (for example, the mean value) imposed and the total degrees of freedom are one less "n the number of observations. D 3980; D-l jty in air--the weight per unit volume in vacuum minus weight of a volume of air equal to the difference "tween the volume of the sample and the volume ofbrass 'rights equivalent to weight in vacuum of the sample, lbenzene (CgHI0)--mol weight 106.16; clear, colorless, amable liquid; freezing point, -94.97C; boiling point, 6C. oration residue--the nonvolatile impurities remaining r vaporizing a substance. jilg point--the temperature at which the liquid and solid ries of a substance are in equilibrium at a given pressure ually atmospheric). For pure substances it is identical 1th the melting point of the solid form. Lange, 10th Ed.2 dme--the time required for the polymerization reaction proceed to a point where the viscous drag on a rotating indie, partially immersed in the reaction mass is suffi- ent to overcome the torsional force exerted on the indie by a constant speed drive assembly, magnetically upled to the spindle by a standard torsion spring. D 2870; D-16 ologues of phenol--compounds of the phenol series hose structure differs regularly by some radical (for xample, -CH3) from that of its adjacent neighbor in the cries. Also cresols and xylenols.- ogen sulfide (H2S)---mol weight 34.08; flammable, "oisonous gas with characteristic odor of rotten eggs, ustrial grade--a quality of aromatic hydrocarbons suit able for many industrial applications that have a tolerance r nonreactive impurities. Dis c u s s io n --The classification covers intermediate levels of purity 'hat may vary over a wide range for different materials. bitor--a substance added to a material to retard or vent deterioration. Lange. N. A., Handbook ofChemistry, 10th Ed., McGraw Hill Book Co. Inc., York, NY. isopropylbenzene--cumene (C,H12) mol weight 120.19; clear, flammable liquid; melting point, -96.0C; boiling point, 152.4C. internal standard--a compound of known behavior added to a sample to facilitate the analysis. D 2908; D-19 ketones--a class of organic compounds possessing a carbonyl group attached to two hydrocarbon groups. Acetone is the first member of this series, meta-xylene--1,3-dimethylbenzene (CgH10) mol weight 106.16; clear, colorless, flammable liquid; freezing point, -47.87C; boiling point, 139.3C. moisture, atmospheric--ambient humidity that may be ab sorbed by hygroscopic material during sampling and testing and may lead to erroneous results, molten state--the liquid phase of a solid substance existing above its melting point temperature, naptha,' aromatic Solvent--a concentrate of aromatic hydro carbons including Cs, C, and C10 homologs. Dis c u s s io n --Distillation end point of individual grades varies between 155 and 220C to provide a range of volatility and solvency characteristics. Color ofsolvents is water-white to dark red depending on refining treatment naphthalene (Qq H^)--mol weight 128.16; monoclinic pris matic plates; commercially available as white scales, powder, balls, or cakes; odor of moth balls; solidification point, 80. TO; sublimes above melting point, nonaromatic hydrocarbons--one or more types of hydrocar bons identified as paraffins,; cycloparaffins (naphthenes), and olefins. Generally, the saturated types, paraffins and cycloparaffins, constitute the impurities in the commercial grades of aromatic hydrocarbons, nonvolatile matter--the oily, gummy, or resinous residue remaining after .evaporating volatile hydrocarbon mate rials. ortho-xylene--1,2-dimethylbenzene (C8H,0) mol weight 106.16; clear, colorless, flammable liquid; freezing point,- -25.18C; boiling point, 144C. para-xylene--1,4-dimethylbenzene (CgH10) mol weight 106.16; clear, colorless, flammable liquid; freezing point, 13.26C; boiling point, 137 to 138C. ' -- peroxides--a class of oxygen-containing compounds pos sessing a peroxyl-functional group. Hydrogen peroxide is the lowest member of this series. - phenol--hydroxy benzene, carbolic acid (C6H5bH) mol weight 94.11; colorless acicular crystals or white crystalline mass; characteristic odor; solidification point, 40.85*0, boiling point, 182C. phenol-405, refined--phenol with impurities limited to trace amounts as indicated by a solidification point of 40.5C minimum refined to improve color stability. Refer to Specification D 2439 for complete specifications, phthalic anhydride--anhydride of phthalic acid (QH4O3) mol weight 148.11; white lustrous needles; odorless; solid ification point, 130.8C; boiling point, 295C; sublimes, phthalic anhydride-1308, refined--phthalic anhydride with impurities limited to ultra trace amounts as indicated by a solidification point of 130.8C minimum refined to im prove color characteristics. Refer to Specification D 2403 for complete specifications. platinum-cobalt color--color measured in reference to color standards prepared with solutions of cobalt chloride and 753 H paps HI DUP050296315 # D 4790 ;Kasg potassium chloroplatinate. Color standards are identical with the description given in APHA publications3 and is referred to as "APHA Color", polymers)--a large molecule formed by the chemical union of reactive units called monomers. Dis c u s s io n --For Test Method D 2121, polymers of styrene are those molecules that are insoluble in methanol. polystyrene--a plastic based on a resin made by polymeriza tion of styrene as the sole monomer. For use as a standard in colorimetry, the polystyrene shall contain no internal or external additives. precision--the degree of agreement of repeated measure ment of the same property, expressed in terms of disper sion of test results about the arithmetical mean result obtained by repetitive testing of a homogeneous sample under specified conditions. The precision of a test method is expressed quantitatively as a standard deviation com puted from the results of a series of controlled determinations. D 2777; D-19 n-propylbenzene--1-phenyl propane (C9H12) mol weight 120.19; used as a reference standard for identifying and determining Cg aromatics; melting point, --99.2C; boiling point, 159.2C. pyridine bases--a mixture of pyridine and substituted pyridines. The pyridine bases in tar acids refer to those that react with 0.02 N perchloric acid, pyridine, refined--pyridine (including its impurities) having a total distillation range of 1.0"C. Refined to improve color characteristics. Refer to Specification D 2323 for complete specifications. quinoline--benzo(b)pyridine (C9H7N) mol weight 129.15; colorless, refractive oil which darkens on storage; hygro scopic; penetrating odor not as offensive as pyridine; freezing point, -- 15C; boilitig point, 237.7C. reagent blank--a reference standard or correction factor obtained by subjecting one or more reagents to test conditions. reducing substances--impurities in pyridine that decolorize a solution ofpotassium permanganate ofspecified compo sition in Method D 2031. reference standard--primary or secondary standards used to calibrate testing apparatus and methods, refined--treated to reduce impurities, relative density (specific gravity)--the ratio of the mass of a given volume of liquid at 15.54C (60F) to the mass of an equal volume of pure water at the same temperature. D1298; D-2 repeatability--the precision of a test method expressed in terms of the agreement attainable between measurements made by a single operator using the same apparatus and techniques. reproducibility--the precision of a test method expressed in terms of agreement expected between measurements made in different laboratories using similar apparatus and the same procedure. 3 Standard Methods for the Examination of Water and Waste Water, 14 Ed. American Public Health Association (APHA), p. 65. slightly cloudy pyridine--quantitative index of t observed with aqueous solution of pyridine, f containing trace amounts of oil. solidification point--an empirical constant defined temperature at which the liquid phase of a subsf"* approximate equilibrium with a relatively small the solid phase. Dis c u s s io n --Solidification point is distinguished from point which is described in Test Method D 1015. An intci pretan mole percent purity in terms offreezing point is given i n Test D 1016. specific gravity in air--weight of unit volume in uirair buoyancy correction applied. (See relative densif standard deviation--a measure of the dispersion of a sei*"' results around their mean, computed as the positiv' eq root of the variance. The standard deviation is the tas'i most statements of precision and may be obtained fro analysis of variance of results of an interlaboratory-ni program. D 3980;-1 styrene monomer-996--styrene with a purity nt weight % minimum, determined by freezing point;r surement. 1 sulfur dioxide (S02)--mol weight 64.07; colorless, n mable gas with strong suffocating odor soluble in and organic solvents. synthesis grade--a quality of aromatic hydrocarbons related chemicals representing the highest purity av on a commercial scale. It encompasses those ma identified with a quantitative index of purity. 4-tertiary butyl catechol--p-/er/-butylcatechol (C,0H,. mol weight 166.2; colorless crystals; polymerization mi itor for styrene, butadiene, and other olefins; boiling jjoif 285<>C; melting point, 52C. thiophene--thiofuran (C4H4S) mol weight 84.13; a cyclic] ,4 organosulfur; colorless, highly reactive liquid; freezing.,''.1 point, --38.5"C; boiling point, 84.12C. toluene--methyl benzene, toluol (obsolete) (C7HS) mol weight 92.13; clear,- colorless, highly flammable liquid;' odor somewhat like benzene; freezing point, -9499C; boiling point,. 110.6C. toluene, nitration grade--toluene with maximum paraffin impurities of 1.5 volume % having a total distillal ionrange of 1C maximum. Refer to Specification D 841 for complete specifications. total distillation range--the temperature range, expressed in degrees Celsius, observed in vaporizing a material under < specified conditions. Dis c u s s io n --In the standard apparatus used for aromatic hydro carbons, this temperature range is the difference between the temper ature at the time the distilling flask becomes dry (dry point) and the temperature at the time the first drop falls into the receiver (first drop, initial). water solubility--the amount of material that is miscible or will dissolve in water at a given temperature. xylene--a mixture of aromatic hydrocarbons. Dis c u s s io n --The concentration range of individual components in xylene samples from coal tar and petroleum sources is indicated in the following tabulation: DUP050296316 D 4790 Component Ethylbenzene p-Xylene m-Xylene o-Xylene C, Aromatics Weight 4-20 9-20 40-63 5-22 0.3-1 nitration grade--xylene consisting principally of the isomer and having a total distillation range of no than 5C. Nonaromatic impurities is limited to a maximum of 4 volume %. Refer to Specification D 843 for complete specifications. xylene, 10C --xylene having a total distillation range of no more than 10C. This range brackets the .boiling points of the three individual isomers and ethylbenzene. Refer to Specification E> 846 for complete specifications. xylenol(s)--dimethyl pheriol(s), hydroxydimethylbenzene (C8H10O) mol weight 122.16; colorless crystalline pow ders, Five isomeric xylenols exist. The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Vourcomments are invited either for revision ofthis standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive carefitl consideration at e meeting of the responsible technical committee, which you may attend. It ydu feel that your comments have not received a fair hearing you should make your views kndwn to the ASTM Committee oh Standards, 1916 Race St., Philadelphia, PA 19103. DUP050296317 (jjjjh Designation: D 4961 - 89 Standard Test Methods for Gas Chromatographic Analysis of Major Organic Impurities in Phenol Produced by the Cumene Process1 This standard is issued under the fixed designation D 4961; 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. 1. Scope 1.1 These test methods cover the determination of major organic impurities in refined phenol manufactured by the cumene (isopropylbenzene) process. Two test methpds are employed to determine the stated major impurities. 1.2 Test Method A determines the concentration of major impurities such as mesityl oxide, cumene, a-methylstyrene, 2-methylbenzofuran, acetophenone, and dimethylbenzyi al cohol. 1.3 Test Method B determines the hydroxyacetone con tent. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D3852 Practice for Sampling and Handling Phenol and Cresylic Acid3 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.12004 3. Summary of Test Methods 3.1 Two test methods are used to determine the major impurities in phenol: 3.1.1 Test Method A, Majgr Impurity Determination--A known amount of internal standard is added to the sample. A portion of the sample is analyzed by gas chromatography. The concentration of each impurity is calculated relative to the known amount of internal standard that is added. 3.1.2 Test Method B, Hydroxyacetone Determination--A measured amount of sample is analyzed by gas chromatog raphy. The concentration of hydroxyacetone in the sample is determined by the ratio of the area of hydroxyacetone in the 1 These test methods are under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of Subcommittee D1G.OC on Oxygenated Aromatics. Current edition approved June 30, 1989. Published August 1989. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 06.03. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. sample to the area in a standard sample containing a amount of hydroxyacetone. 4. Significance and Use 4.1 This test method is useful in setting specifications refined phenol manufactured by the cumene process and process control. Test Method A is useful for individ impurities in the range from 10 to 100 mg/kg. Test Meth` B is useful for hydroxyacetone in the range from 5 to mg/kg. 5. Purity of Reagents 5.1 Reagent grade chemicals shall be used in all t Unless otherwise indicated, it is intended that all ica^ shall conform to the specifications of the Committee S' Analytical Reagents of the American Chemical Social where such specifications are available.3 Other grades may used, provided it is first ascertained that the reagent il sufficiently high purity to permit its use without lessening > accuracy of the determination. 5.2 Purity of Water--Unless otherwise indicated, i! ences to water shall be understood to mean reagent water defined by Type II of Specification D 1193. -i 6. Hazards 6.1 Consult the current OSHA regulations and supplier?' Material Safety Data Sheets for all materials used in thes test methods. 6.2 The materials used in these test-methods are .hi; toxic and flammable. 7. Sampling 7.1 Sample in accordance with Practice V 3852. TEST METHOD A 8. Apparatus 8.1 Chromatograph, equipped with an on-column injector and flame ionization detector. 8.2 Recorder, with a full scale of 1 mV and a response time of 1 s or less. 8.3 Integrating Device--Any device capable of integrating chromatograph peak areas with a repeatability of 1 % relative. 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." DUP050296318 # D 4961 chromatographic Column, glass6 (2-ram inside diam.Nickel 2007 (5.3-mm inside diameter by 3-m length), mn may be purchased or prepared as described in 10. 1: Caution--Other nickel tubing may not be satisfactory -f the catalytic decomposition of compounds of interest that r in tubing other than Nickel 200. gents and Materials 'olid Support 100/120 Mesh--Acid washed, dichlorosilane (DMCS) treated diatomaceous earth.8 Stationary Phase--A combination of 8 weight % polyethylene glycol9 plus 4 weight % Versamid l suitable solvent is 75 volume % methylene chloride volume % toluene. 1Internal Standard--Tetradecane. Pure Components for Calibration--Mesityl oxide, pe, a-methylstyrene, 2-methylbenzofuran, acetopheand dimethylbenzyl alcohol. The purity of each Sment should exceed 99 weight %. %Phenol--High purity phenol. Carrier Gas--Helium or nitrogen. lolumn Preparation H Either glass or nickel columns may be used. Glass gins are preferred because of their superior inertness, [columns are preferred because of ease of handling. If p tubing is used, it must be cleaned with glacial acetic bllowed by water rinsing. p.l Prepare the column packing as 12 weight % of the r mixed phase (see 9.2) to 88 weight % of the solid t. Dissolve the stationary phase in sufficient solvent so he solution will cover the solid support completely in a hallow, glass or porcelain vessel. Place the vessel in a Bating hood and evaporate the solvent to a constant fit, with occasional gentle stirring. Add the free-flowing ng thus obtained, to the column with the aid of a small J, and apply vacuum to draw the packing into place. |r tap or vibrate the column to ensure even distribution : packing in the column. Place a glass-wool plug at the It end of the column before adding the packing, and one |e inlet end after the column is full. Do not pack the ing too tightly; evenly distribute it with no voids. J22 Column Condition--Install the column into the chropgraph and precondition it at the elevated temperature ribed in 10.2.1 through 10.2.4. Do not connect the coli to the detector block until 10.2.2 has been completed. >.2.1 Start the flow of helium or nitrogen carrier gas and r the column to age for 30 min with no heat 3.2.2 Increase the column temperature to 230G at the rate of 2C/min and hold that temperature for at least 24 h. Connect the column to the detector block after this step has been completed. 10.2.3 If a nickel column is used, reduce the temperature to 130C and make fifteen 1-jxL injections of phenol. 10.2.4 Establish the conditions shown in Table 1 and make repetitive phenol injections until two or more injec tions exhibit the same peak configuration. 11. Preparation and Calibration of Standards 11.1 Use high purity phenol in preparing the calibration standards. Determine the residual impurities in the phenol by the procedure outlined in Section 12. 11.1.1 Sample Preparation--The sample must be handled in a molten state at 50'C. Higher temperatures will degrade the sample. 11.2 Prepare a calibration mixture of phenol containing mesityl oxide (MO), cumene (CU), a-methylstyrene (AMS), 2-methylbenzofuran (2MBF), acetophenone (AP), and dimethylbenzyl alcohol (DMBA). All the above impurity levels should be near the anticipated levels in the sample. If any residual impurity elutes with a known impurity, deduct the residual area obtained in 11.1 (adjusted to sample size) from the area of the impurity. 11.3 Standardization Procedure--Determine the relative response factors (RRF) of each impurity by adding known quantities of impurities and internal standard. Prepare stand ards with impurity levels that bracket the dynamic range of interest Use the procedure in Section 12 for standardization. Determine the relative response factor, F, as follows: T = [fTc x A/iAc - Ab)] x Wj ' <i) where: Wc = weight of impurity, g, W} = weight of internal standard, g, At = peak area of internal standard, Ac = peak area of impurity in calibration blend, and = peak area of impurity in phenol base stock. Set the system sensitivity so that all impurity peaks are recorded at adequate levels for data acquisition. Normally, the minimum, peak height will be twice that ofthe baseline ' noise. No t e 2--Phenol produced by processes other than the cumene process may have impurities that elute with tetradecane. Before using this test method, investigate this by analyzing the phenol without the internal standard. Ifinterference exists, use other internal standards such as durene or sec-butyl alcohol. 11.4 See Table 2 for typical response factors and retention times. 12. Procedure 12.1 See Table 1 for chromatographic conditions. glass column such as a Supelco column, available from Supelco Inc., |lco Park, Bcllefonte, PA 16823, or equivalent, has been found satisfactory for pose. Nickel 200 Tubing is available as Catalog No. HGC-345 from Anaiabs Inc., Walnut St, Norwalk, CT 06854. pupelcoport, manufactured by Supelco, Inc., has been found satisfactory for purpose. [000, a trademark of Supelco, Inc., has been found satisfactory for this ? Versamid 900, a trademark of General Mills, Inc., is available from any natcgraphic supplier. TABLE 1 Typical Conditions for Chromatographic Separation (Method A) Column temperature, C injector temperature, C Detector temperature, C Carrier gas Gas flow rate. cm3/min Hydrogen flow rate. cm3/min Air flow rate. cm3/min Specimen size. pL 180 isothermal 180 250 nitrogen or helium 22 30 320 1 757 DUP050296319 TABLE 2 Component Relative Response Factors and Retention Times Impurity Typical Relative Typical Retention Response Factor Time, min Mssityl oxide (MO) Cumene (CU) a-methylstyrene (AMS) Tetradecane (internal standard) 2-methylbenzofuran (2MBF) Acetophenone (API Dlmethylbsnzyt alcohol (DMBA) Phenol 4.8 1.0 6.0 1.0 9.5 1.0 15.1 1.2 19.4 1.1 21.6 1.1 2S.0 36 u Nesityl Oxide ............ ............ 7.075 Cumene 11. Alpha Methyl Styrene 12.2 Add an appropriate amount of internal standard to molten phenol and mix thoroughly. 12.3 Using a preheated chromatographic syringe (approx imately 75C), inject I jxL of molten phenol specimen. Phenol is not diluted with water as in Test Method B, because water may cause ghost peaks. 12.4 Allow approximately 45 min for all components to elute from the column. 12.5 When phenol elutes, raise the column oven temper ature to 235C. The column should remain at 235C for approximately 1 h. Before another chromatograph run is attempted, stabilize the oven at 180C for at least 10 min. 13. Calculation and Report 13.1 Calculation--Determine the concentration of each impurity using the following formula: Mc = (Fc XACX M,)/A, (2) where: Mc = concentration of impurity C, mg/kg, Fc = relative response factor for impurity C versus the internal standard, Ac = area of impurity C, = concentration of interna! standard, mg/kg, and A, = area of internal standard. 13.2 Report the concentration of each impurity to the nearest milligram per kilogram. Tetradecane (Internal strand*r<n 2 ? J ?4 2~M*ehylben2ofuran 7 4.3 U Acetophenone 77.334 Dimethyl Benzyl Alcohol FIG. 1 Typical Chromatograph--Test Method A 15.2 Bias--Bias has not been determined. 14. Component Relative Response Factors and Retention Times TEST METHOD B -- 14.1 See Fig. 1 for a typical chromatogram. 16. Interferences 15. Precision and Bias j 15.1 Precision: 16.1 Hydroxyacetone will readily degrade; therefore, following items are critical to the accuracy of this method: i 15.1.1 Differences within the same laboratory should be i suspect if they differ by more than 31 % of the average value. 16.1.1 Column length of no greater than 0.61 m, 16.1.2 Injector temperature of 150 2C, and 15.1.2 The concentrations of the following compounds ! should be considered suspect if differences between laborato 16.1.3 On-column injector. ries differ by more than the following concentrations: 17. Apparatus Compound Mesityl oxide (MO) Cumene (CU) a-methylstyrene (AMS) Concentration, mg/kg 26 15 11 17.1 Chromatograph--See 8.1. 17.2 Recorder--See 8.2. 17.3 Integrating Device--See 8.3. 2-methylbenzofuran (2 MBF) 10 17.4 Chromatograph Column, glass, 2-mm inside diam Acetophenone (AP) Dimethylbenzyl alcohol (DMBA) 17 24 15.1.3 These values were determined by round-robin anal yses conducted at approximately 50 and 100 mg/kg levels of eter by 0.61-m length. Column lengths greater than 0.61 m should not be employed. Do not use metal columns. 17.5 Syringe Adapter.11 mesityl oxide, cumene, a-methylstyrene, 2-methylbenzo- furan, acetophenone, and dimethylbenzyl alcohol. 11 A Chaney Syringe Adapter has been found suitable for this purpose. 758 DUP050296320 # D 4961 ients and Materials | Stationary Phase--Porous polymer,12 80 to 100 f Acetol (Hydroxyacetone), 50 % purity. Keep refriger- ' Phenol--High purity phenol containing less than 10 *of hydroxyacetone. ition and Calibration of Standards Add water to high purity phenol and make an solution of 90 weight % phenol and 10 weight % 'This solution will remain in the liquid state at room ature. Prepare standards that bracket the dynamic range of by adding hydroxyacetone to the 90% aqueous Note that both the phenol and hydroxyacetone are this solutions and must be corrected in the calculations. |f3 Inject 1.0 p.L (measured) of the standard hydroxyacesolution and record the area generated by hydroxyfpe. Repeat this step at least two times or until repeated Sons vary by no more titan 5 % relative. A syringe may be used to enhance injection accuracy. icedure 1 See Table 3 for chromatograph conditions. j,2 Add 1.0 g of water to 9.0 g of molten phenol. 3 Inject 1.0 pL (measured) of the specimen from 20.2 rd the area generated by the hydroxyacetone. |i4 Wait until all the phenol has eluted from the. column the original baseline is established before the next ion. ilculation 11 Determine the concentration of hydroxyacetone, ! the following formula: CH = (As X Ce)/Ab |fe; = concentration of hydroxyacetone in the specimen, mg/kg, = area generated by the hydroxyacetone in the spec- , imen, f= concentration of hydroxyacetone in the external standard, mg/kg, and = area generated by the hydroxyacetone in the external standard.2 TABLE 3 Typical Conditions for Chromatographic SeparationTest Method B Column temperature, C Injector temperature, C Detector temperature, "C Carrier gas Carrier gas flow rate, cm3/rrtn Hydrogen flow rate, cms/min Air flow rate, cm^/mki Specimen size, pL 165 150 2A 260 nitrogen or helium 30 30 320 1.0 A Critical. 21.2 A typical chromatogram is shown in Fig. 2. 22. Precision and Bias 22.1 Precision: 22.1.1 Differences within the same laboratory should be considered suspect if they are greater than 30 % of the average value. 22.1.2 The concentration of acetol should be considered suspect if differences between laboratories are greater than 34 % of the average concentrations. 22.1.3 The round-robin analyses were conducted at ap proximately 10, 60, and 160 mg/kg acetol. 22.2 Bias--Bias has not been determined. fc.4'38 Hydroxyacetone (Acetol) 2 Chromasorb 102, a trademark of Johns Manville, nitration and Minerals on, and Poropak Q, a trademark of Supelco, Inc., have been found suitable s purpose. Both are available from chromatographic supply houses. FIG. 2 Typical Chromatograph--Test Method 8 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 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 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. DUP050296321 Designation: D 5060 - 90 iZl t 'B Standard Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography1 2 This standard is issued under the fixed designation D 5060; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year ofl^st revision. A number in parentheses indicates the year oflasfreapprovaL A 1 superscript epsiton (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes the analysis of normally occurring impurities in, and the purity of, ethylbenzene by gas chromatography. Impurities determined include nonaro matic hydrocarbons, benzene, toluene, xylenes, cumen, and diethylbenzene isomers. 1.2 This test method is applicable for impurities at con centrations from 0.001 to 1.000 % and for ethylbenzene purities of 99 % or higher. At this level, p-xylene may not be detected. 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 Section 7. 2. Referenced Documents 2.1 ASTM Standards: D3437 Practice for Sampling and Handling Cyclic Products2 D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards3 E 355 Practice for Gas Chromatography Terms and Relationships4 5 2.2 Other Documents: OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200s 3. Summary of Test Method 3.1 A known amount of internal standard is added to the sample. A gas chromatograph equipped with a flame ioniza tion detector and a polar fused silica capillary column is used for the analysis. The impurities are measured relative to the internal standard. Ethylbenzene purity is calculated by subtracting the impurities found from 100.00 %. 4. Significance and Use 4.1 The test is suitable for setting specifications on ethylbenzene and for use as an internal quality control tool 1 This test method is under ithe jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related .Chemicals and is the direct responsibility of Subcommittee D16.0H on Styrene, Ethylbenzene, Cumenet and Naphthalene; Current edition approved May 25, 1990. Published August 1990. 2 Annua! Book ofASTM Standards, Voi 06.03. 3 Annual Book ofASTM Standards^ Voi 05.03. 4 Annual Book ofASTM Standards, Voi 14.01. 5 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. where ethylbenzene is used in manufacturing process may be used in development or research work invofj ethylbenzene. ' 1 4.2 Purity is commonly reported by subtracting these! mined expected impurities from 100%. Absolute, cannot be determined if unknown impurities are presentf 5. Apparatus 5.1 Gas Chromatograph--Any gas chromatograph hflgSjjj] a flame ionization detector and a splitter injector suitableTM use with a fused-silica capillary column ` may be provided the system has sufficient sensitivity to obtain* minimum peak height response of 0.1 mV for 0.010$jj internal standard when operated at the stated condition Background noise at these conditions is not to exceed 31 5.2 Chromatographic Column, fused silica capillary, 60$ long, 0.32-mm inside diameter, internally coated to a 0.5,^ thickness with a bonded (crosslinked) polyethylene gly<joj:|| Other columns may be used after it has been estabiished m such column is capable of separating all major impunlj and the internal standard from the ethylbenzene un operating conditions appropriate for the column. _ 5.3 Recorder, 1-mV, 1 s or less full scale response^ electronic integration with tangent capabilities (r mended). 5.4 Microsyringe, 10-pL. 5.5 Microsyringe, 50-pL. 5.6 Volumetric Flask, 50-mL. 6. Reagents and ^Materials --- . |j 6.1 Carrier Gas, hydrogen or helium, chromatographic! grade. 6.2 Compressed Air, oil-free. 6.3 Hydrogen, chromatographic grade. 6.4 Nitrogen, chromatographic grade. 6.5 Pure Compounds for Calibration--n-Nonane, ben-1 zene, toluene, ethylbenzene, and o-xylene. The purity of the | ethylbenzene should be 99.8 % or better. The ethylbenzene;! must be analyzed and corrections made in the bompositidn' i of the calibration blend as required. The purity of all other compounds should be 99 % or greater. If the purity is less than 99%, the concentration and identification of the impurities must be known so that the composition of the calibration standard can be adjusted for the presence of the impurities. 6.6 n-Undecane, for use as internal standard, 99 % or greater purity. 7. Hazards 7.1 Consult current OSHA regulations and supplier's 760 DUP050296322 I Safety Data Sheets for all materials used in this test npling ^ Guidelines for taking samples from bulk are given in " ; D 3437. flibration [Prepare a calibration blend of each compound listed and n-undecane at the 0.2 weight % level in ene as described in Practice D4307. -Nonane nts the nonaromatic hydrocarbons. A series of cali- . blends that span the concentration range should be ed, one at the expected level of impurities, another at ` the expected level, and a third series at twice the led level. - Analyze the ethylbenzene used in preparing the cali|n blend as described in 10.3. Analyze the calibration blend as described in 10.3. | Calculate response factors as follows: 5i = (Q vA.,i ^s.b/ response factor for impurity relative to internal stan dard, area of impurity peak in calibration blend, > area of impurity in ethylbenzene in calibration blend, ; concentration of internal standard, weight %, |l area of internal standard peak in calibration blend, : area of internal standard peak in stock ethylbenzene, and U= concentration of impurity, weight %. Calculate response factor to the nearest 0.001. ocedure il Install the chromatographic column and establish |g instrument operation at the operating conditions in Table 1. Refer to instructions provided by the icturer of the gas chromatograph and Practice E 355. 2 Fill a 50-mL volumetric flask to the mark with test [men. With a microsyringe, add 30 pL of the standard, well. Using a density of 0.740 for n-undecane and 0.867 Ihylbenzene, this solution will contain 0.0512 weight % al standard. S.3 Inject 0.6 pL of solution into the gas chromatograph obtain the chromatogram. A typical chromatogram is yn in Fig. 1. Calculation 1 Measure the areas of all peaks, including the internal dard, except for the ethylbenzene peak. 1.2 Sum all the peaks eluting before ethylbenzene except TABLE 1 Instrument Parameters Carrier gas Carrier gas flow rate at 210C, mL/min Detector Detector temperature. C Injection port temperature, <'C Hydrogen flow rate, mL/mln Airflow rate, mL/min Make-up gas Make-up gas flow rate. mL/mln Split flow, mL/min Column temperature program: Initial temperature, C Initial time, min Programming rate, C/min Final temperature, C Chart speed, cm/min Sample size, jiL helium 0.9 flame-ionization 240 230 30 275 nitrogen 23 150 70 24 20 210 1 0.6 for benzene, toluene, and the internal standard. Identify this sum as nonaromatic hydrocarbons. 11.3 Calculate the weight percent of the individual impu rities, C;, to the nearest 0.001 %, as follows: 0.0512 A, Jt, ' As where: Ai = area of impurity, Rs = response factor for impurity, and As = area of internal standard. 11.4 Use the response factor determined for o-xylene for all the peaks eluting after ethylbenzene, and the response factor determined for n-nonane for all the nonaromatic hydrocarbon peaks. 11.5 Calculate the purity of the ethylbenzene by sub tracting the sum of the impurities from 100.00. 12. Report 12.1 Report the following information: 12.1.1 The concentration of each impurity to the nearest 0.001 weight %, and 12.1.2 The purity of ethylbenzene to the nearest 0.01 weight %. 13. Precision and Bias . -- 13.1 The following criteria should be used to judge the acceptability of the . 95 % probability level of the results obtained by this test method. The criteria were derived from a round robin between seven laboratories. The data were obtained over two days using different operators. 13.1.1 Repeatability--Results in the same laboratory should not be considered suspect unless they differ by more than the amount shown in Table 2. 13.1.2 Reproducibility--The results submitted by two laboratories should not be considered suspect unless they differ by more than the amount shown in Table 2. 13.2 Bias--No statement is made about bias since no acceptable reference material and value are available. DUP050296323 START D 5060 TABLE 2 Repeatability and Reproducibility Component Concentration, Weight % Repeatability Reproducibility sec-Butylbenzene n-Propylbenzene mja-Ethyltoluenes o-Xylene Cumene Benzene Toluene mjo-Xylene Diethylbenzenes Ethylbenzene 0.002 0.010 0.014 0.013 0.012 0.024 0.592 0.090 0.008 99.05 0.001 0.002 ' 6.003 0.004 , 0.003 0004 0.083 0.024 0.001 0.200 0.003 0.003 0.002 0.007 0.002 0.005 - 0.100 0.019 0.003 0.186 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 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 for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. i? 762 DUP050296324 Designation: D 5135 - 90 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography1 This standard is issued under the fixed designation D 5135; 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. ffhis test method covers the determination of the ||ies in, and the purity of styrene by gas chromatog- lt is applicable to styrene in the range from 99 to purity and to impurities at concentrations of 0,001 to This test method may be used for lower purity but jjlhe impurities may be readily identified and the use of al standard becomes more difficult. |This standard does not purport to address all the safety i associated with its use. It is the responsibility ofthe ' this standard to establish appropriate safety and Ipractices and determine the applicability ofregulatory %ons prior to use. For a specific hazard statement, see 5. derenced Documents ffciSTM Standards: ... 37 Practice for Sampling arid Handling Cyclic oducts2 Tther Document: ' Regulations--29CFR paragraphs 1910,1000 and |10.12003 [unary of Test Method , iln this test method, the chromatogram peak area for npurity is compared to the peak area of the internal id (n-heptane or other suitable known) added to the |b. From the response factors of these impurities : to that of the internal standard and the amount of |al standard added, the concentration of the impurities jculated. The styrene content is obtained by subtracting ptal amount of all impurities from 100.00. gnificance and Use I/This test method is designed to .obtain styrene purity |e basis of impurities normally present in styrene and gbe used for final product inspections and process A. J This test method will detect the following impurities: romatic hydrocarbons containing ten carbons or less, jjbenzene, p- and m-xylene, cumene, o-xylene, nVlbenzene, m- and p-ethyltoluene, alpha-methyl-styrene, End p-vinyltoluene and others where specific impurity Ijiis test method is under the jurisdiction of AST.M Committee D-16 on iStc Hydrocarbons and Related Chemicals and is the direct responsibility of nmittee D16.0H on Styrene, Ethylbenzene, Cumene, and Napthalene. jfrrent edition approved Oct. 26, 1990. Published December 1990. pnual Book ofASTM Standards, Vol 06.03. Available from Superintendent of Documents, U.S. Government Printing , Washington. DC 20402. standards are available. Absolute purity cannot be deter mined if unknown impurities are present 5. Apparatus 5.1 Gas Chromatograph--Any gas chromatograph having a flame ionization detector and a splitter injector suitable for use with a fused silica capillary column may be used, provided the system has sufficient sensitivity to obtain a minimum peak height response of 0.1 mV for 0.010 % internal standard when operated at the stated conditions. Background noise .at these conditions is not to exceed 3 pV. 5.2 Column---Capillary columns have been found to be satisfactory. For example, 60 m of 0.32-mm inside diameter polar-fused silica capillary internally coated to a 0.5-pm thickness with a bonded (cross-linked) polyethylene glycol can be used (see Table 1 for parameters). Other columns may be used after it has been' established that such a column is capable of separating all major impurities and the internal standard from die-styrene under operating conditions appro priate for the column. 5.3 Electronic Integration, with tangent capabilities is recommended. .5.4 100-mL Volumetric Flask. 5.5 .Microsyringes, assorted volumes. 6. Hazards 6.1 Consult the latest OSHA regulations and suppliers' Material Safety Data Sheets for all materials used in this procedure. 7. Reagents and Materials 7.1. Carrier Gas--a carrier gas (minimum purity of99.95 mol %) appropriate to "the type of detector used should.be employed. TABLE 1 instrument Parameters Carrier gas Cartier gaa flow rate at 210C, mL/min Detector Detector temperature, C Injection port temperature, C Hydrogen flow rate, mL/min Air flow rate, mL/min Make up gas Make up gas flow rate, mL/min Split flow, mL/min Column Column temperature, "C Chart speed, cm/min Sample size, pL helium 0.9 flame ionization 240 230 30 275 nitrogen 23 150 60 m x 0.32 mm ID x 0.5 pm bonded polyethylene glycolfused silica capillary 80 1 0.6 763 DUP050296325 D 5135 Precaution--If hydrogen is used, take special safety pre cautions to ensure that the system is free of leaks and that the effluent is properly vented or burned. 7.2 Hydrogen and air for the flame ionization detector (HD). 7.3 n-Heptane, 99.0 % minimum purity, or other internal standard, such as n-octane, previously analyzed to be free of compounds coeluting with impurities in the sample. 7.4 Styrene, the highest purity available, but not less than 99.6 % as determined by freezing point. 7.5 Pure compounds for calibration, shall be those com pounds that are typically present in commercial styrene. These should be at least 99 % pure as they are to be used for determining response factors. 'HI made to instructions provided by the mantriac chromatograph. 10.2 Prepare sample as described jn 9.2. 10.3 Inject appropriate amount of sample^ matograph and obtain the chromatogram. 11. Calculation 11.1 Measure the areas of all peaks, including standard, except the styrene peak. -I 11.2 Calculate the weight percent of the indni rities, C\, as follows: (m (q 8. Sampling 8.1 Take in accordance with Practice D 3437. 9. Procedure 9.1 Prepare a calibration mixture containing approxi mately 99.5 weight % styrene and the expected significant impurities at their expected concentration^ Weigh' all compo nents to the accuracy required to calculate the concentration of each to the nearest 0.001 %. 9.2 With a microsyringe, add 50 pL of internal standard to a 100-mL volumetric flask about three-fourths full of the calibration mixture. Mix well. Add calibration mixture to mark and again mix well. If n-heptane is used as the internal standard, using a density of 0.684 for n-heptane and 0.906 for styrene, this solution will contain 0.0377 weight % n-heptane. 9.3 Also prepare a sample of the styrene used for the calibration blend with and without n-heptane to determine the concentration of existing impurities and interfering compounds with internal standard. If impurities in the styrene emerge with the chosen internal standard, an alter nate internal standard'must be used. ; 9.4 Inject an appropriate amount of sample into the chromatograph and obtain a chromatogram. 9.5 Measure the areas of all peaks, including the internal standard, except the styrene peak. 9.6 Calculate the response factors for each impurity rela tive to the internal standard as follows: where: A =-- area of impurity, As -= area of internal standard, = response factor for impurity, relative to if standard, and Cs = concentration of internal standard, in cent 11.3 Calculate the styrene content by subtracting i of the impurities from 100.00. Styrene weight 100.00 -- (sum of impurities). 12. Report 12.1 Report the concentration of impurities to i 0.001 % and the styrene content to the nearest O.Olf 13. Precision and Bias 13.1 Precision--The following criteria should hajj judge the acceptability (95 % probability level) obtained by this test method. The criteria were derivjj a round robin among six laboratories. The data wei two days using different operators. 13.2 Repeatability--Results in the same lab should not be considered suspect unless they differ^ than the normal amount shown in Table 2 and 2k:t 13.3 Reproducibility--The results by each of two tories should not be considered suspect unless they< more than the amount shown in TaBTe~2 and 2A. 13.4 No statement is made about bias since no acce reference material and value is available. where: RF, = response factor relative to the internal standard, -^si area of internal standard in calibration mixture, A = area of impurity peak in calibration mixture, ^sb ** area of internal standard in styrene used in making calibration mixture, A = area ofimpurity in styrene used to make calibration mixture, Q = weight percent internal standard in calibration mix ture, and C; = weight percent impurity in calibration mixture. 10. Sample Preparation 10.1 Establish stable instrument operation at the pre scribed or selected operating conditions, Reference should be TABLE 2 Precision for Styrene and Impurities at Stated Component Styrene Ethylbenzene a-methylstyrene Isopropylbenzene n-propylbenzene m- and. p-ethyltoluene p, m-xylene o-xylene Concentration, Repeatability, flcpioducitS^ weight % 99.74 0.043 0.028 0.008 0.004 0.014 0.125 0.030 0.017 0.002 0.0001 0.001 0.0003 0.001 0.005 0.001 S.OEt-'fg c.oufas!# . 0.00 0.001 A o.ooi 0.065 if! 0 007 , 1 0.042 If TABLE 2A Precision for High Purity Styrene and impurities at t Component Styrene RepiodisbiMiyStated Levels Concentration, Repeatability, * weight % 99.96 % 0.024 i% 0.033' Ethylbenzene a-methylstyrene 0.014 0.007 0.003 0.002 -is0.004 j 0.003 764 SffiKE? DU P050296326 AMPLITUDE/1000 (E n la rg e d x 5 0 .0 ) # D 5135 ANALYZED. Thu Nov 15, 1990 9.43.06 ant RESULT: /RESULT/RES3 158. RES METHOD.- GFPA FIG. 1 Typical Chromatogram (see Table 1) The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement 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, eitherreapprovedor withdrawn. Yourcomments are invited either forrevision ofthisstandard drforadditionalstandards 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. DUP050296327 I <1 Designation: D 5136 - 90 Standard Specification for High Purity p-Xylene1 This standard is issued under the fixed designation D 5136; 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 specification covers high purity p-Xylene. 1.2 Consult current OSHA regulations and supplier's Material Safety Data Sheets for all materials used in this specification. 2. Referenced Documents 2A ASTM Standards: D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials12 D1209 Test Method for Color of Clear Liquids (Platinum- Cobalt Scale)2 D 3437 Practice for Sampling and Handling Cyclic Prod ucts2 D3798 Test Method for Analysis of p-Xylene by Gas Chromatography2 D3961 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry2 D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry3 2.2 Other Document: 1 These specifications are under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of subcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved Oct. 26, 1990. Published December 1990. 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 05.03. OSHA Regulations, 29 CFR, paragraphs 1910 l'l 1910.12004 3. Properties 3.1 High purity p-Xylene shall conform to the foil requirements: Property Specification Purity, mb, weight % m-Xylene, max, weight % o-Xy)ene, max, weight % Sulfur, max, mg/kg Toluene, max, weight % Ethylbenzene, max, weight % Nonaromatic hydrocarbons, max, weight % Appearance Color, max, Pt/Co scale Distillation range, including the temperature 138.3*0 at 101.3 kPa (760 mm Hg) pres sure, max, C 99.5 0.30 0.10 5.0 0.10 0.30 0.20 10 1.0 ASTM| leil,; D D jn98 03198 d <j D 3798 D 3798 D 3798 j i n D 1209 D 850 jfl A Clear liquid free of sediment and haze when observed at 18.3 to 75 6 1 78"F). No t e 1--Purity, molar %, minimum, will be specified wbanjjj freeze point procedure under development is completed. 4. Sampling 4.1 The material shall be sampled in accordance Practice D 3437. 5. Keywords 5.1 p-Xylene 4 Available frOMrSuperintendent of Documents, U. S. Government I r Office, Washington, DC 20402. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither forrevision ofthis standardor for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1316 Race St., Philadelphia. PA 19103. 766 DUP050296328 Designation: D 5194 - 91 Standard Test Method for Trace Chloride in Liquid Aromatic Hydrocarbons1 This standard is issued under the iked designation D SI94; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revirion. A number in parentheses indicates the year oflast reapproval A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This test method covers the determination of total life (organic and inorganic) in liquid aromatic hydrocarBhd cyclohexane. | The test method is applicable to samples with chloride Iterations of 1 to 25 mg/kg. Bromides and iodides, if present, will be calculated as ties. |j Materials, such as styrene, that are polymerized by pm biphenyl reagent cannot be analyzed by this test la. W'-This standard does not purport to address all of the w problems, if any, associated with its use. It is the msibility ofthe user of this standard to establish approf safety and health practices and determine the applica;of regulatory Imitations prior to me. For a specific l statement, see Section 7. Referenced Documents ASTM Standards: 891 Test Method for Specific Gravity of Liquid IndusJfaial Chemicals2 p 193 Specification for Reagent Water3 *3437 Practice for Sampling and Handling Liquid Cyclic Products4 13505 Test Method for Density or Relative Density of EPure Liquid Chemicals4 |4052 Test Method for Density or Relative Density of jquids by Digital Density Meter5 Other Documents: iA Regulations, 29 CFR, paragraphs 1910.1000 and 11910.1200s Summary of Test Method I! A known amount of hydrocarbon sample is transinto a separatory funnel containing toluene. Sodium jienyl reagent is added to convert organic halogens into aic halides. The excess reagent is decomposed with er and the phases are separated. The aqueous phase is Jjfied, washed, and concentrated. Acetone is added and ^solution is titrated with silver nitrate solution. jjThis test method is under the jurisdiction of ASTM Committee D-16 on atic Hydrocarbons and Related Chemicals and is the direct responsibility of lomroittee D16.0E on Instrumental Analysis. Urrent edition approved Oct. 15, 1991. Published December 1991. Annual Book ofASTM Standards, Vol 15.05. Annual Book ofASTM Standards, VoIs 06.03 and I i.01. Annual Book ofASTM Standards, Vol 06.03. iptfWHa/ Book ofASTM Standards, Vol 05.03. ^Available from Superintendent of Documents, U.S. Government Printing *' , Washington, DC 20402. 4. Significance and Use 4.1 Organic and inorganic chlorine compounds can have a deleterious effect on equipment and reactions in processes involving aromatic hydrocarbons. 4.2 Maximum chloride levels are often specified for process streams and for aromatic hydrocarbon products. 5. Apparatus 5.1 Titrator, potentiometric, recording, + 2000 mV range, 1 mV resolution with dispenser having a volume readout of 0.00 to 9.99 mL or 0.00 to 99.99 mL and 0.01 % resolution. 5.2 Electrode, glass, reference. 5.3 Electrode, silver, billet type. 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Com mittee on Analytical Reagents of the American Chemical Society, 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. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Types II or III of Specification D 1193. 6.3 Acetone, 99.9 % purity. 6.4 Congo Red Paper. 6.5 Detergent,8 6.6 Isobutanol, 99.9 % minimum purity. ...... 6.7 Isooctane. -- 6.8 Nitric Acid, concentrated. 6.9 Nitric Acid, 5-M. Dilute 160 mL concentrated nitric acid to 500 mL with water. 6.10 Potassium Chloride, primary standard. 6.11 Potassium Chloride Solution, saturated. 6.12 Scouring Powder, cleanser. 6.13 Silver Nitrate, 99.99 % minimum purity. 6.14 Silver Nitrate Solution, 0.01 N, standardized to 0.1 %. No t e 1--This solution may be obtained as foilows: (1) Purchase from a laboratory supply company, (2) Weigh to four places, 1.680 to 1.720 g silver nitrate, transfer quantitatively into a 7 "Reagent Chemicals, American Chemical Soeiely 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." 8 Detergent such as Alconox available from Fisher Scientific, 1600 W. Glendale Ave., Itasca, IL 60143, Catalog No. 04-322, has been found satisfactory for this purpose. 767 DUP050296329 D 5194 1000-mL volumetric flask, make to mark with water, and mix well. Weight AgNQ3 Normality of solution = 169.9 or (3) Dissolve 8.5 g silver nitrate in 500 mL water to eve a 0.1 N solution. Weigh 0.09 to 0.10 g ofdried (105C) potassium chloride to the nearest 0.1 mg into a 250-tnL electrolytic beaker, add 100 mL of water and a stirring bar. While stirring, titrate with the silver nitrate solution. Weight KC1 Normality of AgN03 solution = _ ; ; ------ , ":~" 33 0.0746 X mL AgN03 Pipet 50.00 mL ofthe solution into a 500-mL volumetric flask, dilute to mark with water, and mix well. Divide the calculated normality of the 0.1 N solution by 10 to give the, normality of final AgN03 solution, 6.15 Sodium Biphenyl Reagent,9 The reagent is packed in 18-mL vials that contain 13 to 15 mg of active sodium each. 6.16 Toluene, 99,9 % minimum purity. 7. Hazards 7.1 A material, such as styrene, which is polymerized by sodium biphenyl can cause a violent reaction and should never be used as the sample. 7.2 Consult current OSHA regulations and suppliers' Material Safety Data Sheets for all materials used in this test method. S. Sampling 8.1 Refer to Practice D 3437 for proper sampling and handling of liquid hydrocarbons analyzed by this test method. 9. Electrode Preparation 9.1 Clean the surface of the silver electrode with mild detergent and scouring powder, and rinse with water. 9.2 Immerse the electrode in the saturated potassium chloride solution until the electrode tip turns light gray. 9.3 Rinse weil with water and attach to the titrinreter. 9.4 Repeat the electrode preparation when the silver chloride film begins to peel from the surface, or if the film becomes discolored. 10. Procedure for Total Chloride 10.1 Extreme care must be used to prevent contamination and all glassware should be exclusively reserved for this analysis. Just prior to use, the glassware should be rinsed with water followed by acetone and then air dried. 10.2 Place 50 mL of toluene into a 250-mL separatory funnel and pipet in the amount of the liquid sample that corresponds to the estimated chloride content as prescribed in Table 1. No t e 2--It is generally more convenient to measure the liquid samples by volume and then convert to mass using density or relative density. Table 2 lists the relative densities of several pure hydrocarbons. Densities of unknowns may be determined by using Test Methods D 891, D 3505 or D 4052. No t e 3--Alternately, place the sample into a 125-mL bottle and weigh. From the contents of this bottle add the appropriate amount of 9 Sodium biphenyl reagent, available from South Western Analytical Chemi cals, P.O. Box 485, Austin TX 78767, Catalog No. 500, "Organic Halogen Reagent," or equivalent has been found suitable for this purpose. TABLE 1 Specimen Size Estimated chloride, mg/kg 0 to 5 5 to 25 Specimens 10 TABLE 2 Component Benzene Cyclohexane Ethylbenzene Isopropylbenzene Toluene m-Xylene o-Xylene p-Xylene Densities of Hydrocarbons Density 0.879 0.779 0.867 0.864 ' 0.B66 0.864 0.880 0.861 the sarriple to the toluene in the separatory funnel. Reweigh-fljbsf and determine the weight of the analytical specimen. 10.3 Add the contents of one vial of sodium bid reagent, stopper the separatory funnel, and gently, mix thoroughly, venting,the funnel from time to ti resulting solution or suspension is not blue-green, sodium biphenyl reagent (one vial at a time) until green color persists. No t e 4--The sodium biphenyl reagent has a limited shelf$f as six months by the manufacturer. This can be extended, in j to approximately one year by keeping the reagent under refriges this is done, the reagent should be kept at room temperature! days just prior to use to dissolve any sodium biphenyl that i precipitated upon cooling. 10.4 Allow the mixture to stand for approximately min. Slowly add 20 mL wdter and swirl gently wimS funnel unstoppered until the blue-green color change^ white. Stopper the funnel again and rock it gently for' venting the pressure frequently through the stopcock. 10.5 Add 10 mL 5 N nitric .acid, and then isobutanol. Shake gently, releasing the pressure frequ through the stopcock. 10.6 Drain the aqueous phase into another 25(jr^ separatory funnel containing 50 mL jsopetane and sh|' well. Drain the aqueous phase into a~250-mL electro^ beaker. -- ,JjS 10.7 Make a second extraction of the specimen solution with 20 mL water acidified with 6 drops of 5-M nitric gc| and drain the aqueous phase into the separatory containing the isooctane. After shaking, allow the phqsjS separate and drain the aqueous phase into the ,b|| containing the first water extract. 10.8 Test the aqueous solution with Congo red paper, a if it does not test acidic, add 5-N nitric acid dropwise' * stirring until the test paper turns dark blue. 10.9 Evaporate the solution to about 30 mL on a hfL plate. 'll No t e: Caution--Loss of chloride may result if the solution is boil or evaporated below 25 mL. 10.10 Allow the solution to cool, and add 10 mL; acetone. Titrate the solution potentiometrically with st$tj|j dard 0.01 AT silver nitrate solution and determine the volume of titrant used to reach the end point. 10.11 Determine a blank for each group of samples, using 768 DUP050296330 0 5194 |e reagents including as many vials of sodium biphenyl fere used in the analysis of a sample. Follow all the itions of the analysis, except omit the specimen itself. Procedure for Inorganic Chloride 11 Follow the procedure in Section 10 but without ! the sodium biphenyl reagent to either the sample or Hank. cedure for Organic Chloride .1 Follow the procedures given in Sections 10 and 11 to ine the total and inorganic chlorides. Subtract the tic from the total chloride to give the organic chloride. Calculation |.l Calculate either the total or inorganic chloride as iws: Chloride, mg/kg = 35,500 (A - B) N VD . (1) volume of titrant for aqueous phase, mL, volume of titrant for blank, mL, ; normality of silver nitrate solution, l volume of sample, mL, and = density or relative density of sample. 1.2 Calculate organic chloride as follows: Organic chloride, mg/kg = T -1 (2) where: T -- total chloride, mg/kg and I = inorganic chloride, mg/kg. 13.3 Report chloride to the nearest 0.1 mg/kg. 14. Precision and Bias 14.1 Precision: 14.1.1 The data for determining the precision of this test method are based on the analyses of toluene, ethylbenzene, and p-xylene that had been spiked with organic chloride compounds to the 1, 5, and 25 mg/kg chloride levels each. 14.1.2 The following criteria should be used to judge the acceptability (95 % probability) of results obtained by this test method. The criteria were derived from a round robin between three laboratories. Each sample was run on. two different days in each laboratory. 14.1.2.1 Repeatability--Results in the same laboratory should not be considered suspect unless they differ by more than 0.5 mg/kg. 14.1.2.2 Reproducibility--Results from each of two labo ratories should not be considered suspect unless they differ by more than 0.9 mg/kg. 14.2 Bias--The bias of this test method cannot be deter mined because no referee method is available to determine the true value. 15. Keywords 15.1 aromatic hydrocarbons; chloride; cyclohexane; ethylbenzene; p-xylene; toluene The American Society tor Testing and Materials takes no position respecting the validity of any patentrights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. ' This standard.Js 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 of this standard or'for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 769 DUP050296331 Designation: D 5211 - 91 Standard Specification for Xylenes for p-Xylene Feedstock1 This standard is issued under the fixed designation D 5211; 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 1.1 This specification Covers xylenes for p-Xylene feed stock; These xylenes typically acre extracted from reformate. 3.2 Consult current OSHA regulations and suppliers' Material Safety Data Sheets (MSDS) on handling materials used in this specification. 2. Referenced Documents 2.1 ASTM Standards: D847 Test Method for Acidity of Benzene, Toluene, Xylenes* Solvent Naphthas* and Similar Industrial Aro matic Hydrocarbons2 D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials2 D1209 Test Method for Ctilor of Cleat Liquids (Platinum- Cobalt Scale)2 1 D2306 Test Method for Xylene Isomer Analysis by Gas Chromatography2 D2360 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography2 D 3437 Practice for Sampling and Handling Liquid Cyclic Products2 D3505 Test..Method for Density or Relative Density 1 of Pure Liquid Chemicals2 D3961 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry2 D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry3 1 This specification is under the jurisdiction of ASTM Committee D-16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.0A on Benzene, Toluene, Xylenes, Cyclohexane, and Their Derivatives. Current edition approved Oct. 15, 1991. Published December 1991. 2 Annual Book ofASTM Standards, Vol 06.03. 2 Annual Book ofASTM Standards, Voi 05.03. D 4052 Test Method for Density and Relative Dehslf Liquids by Digital Density Meter3 \ D4629 Test Method for Organically Bound Tracd^S trogen in Liquid Petroleum Hydrocarbons by Oxid^J Combustion and Chemiluminescence Detection3 ' i 2.2 Other Document: OSHA Regulations, 29 CFR, paragraphs 1910 1000-a 1910.1200'* 5. Properties 5.1 Xylenes for p-Xylene feedstock shall conform to * following requirements: Property p-Xylene, fan, weight % Ethylbenzene, max, weight % Toluene, max, weight % C9 and higher boiling aromatic hydro carbons, max, weight % Nonaromatic hydrocarbons, max. weight % Nitrogen,,max, mg/kg Sulfur, max, mg/kg Acidity Appearance . Relative density, 15.56/15.56`C or Density, 20"C, g/cm3 Color, max, Pt/Co scale Distillation range, at,101.3 kPa (760 mm Hg) pressure, max, C Initial distillation temperature, min, 'C Diy point, max, C Specification ' 18 , ' 2b 0.5 1.5 - 0.3 1.0 .. 1.0 , , ' no free acid' A 0.865 to 0.875 0.862 to 0.872 20 5 137 143 ASIM .vi ,.Te Method DD22330066 V4f D '*360 *<S D2360 .,,1? D2360 D 4629 Kn D 3961 or 1i#j D 4045 3 D 847 -*j 1** D3505 or D 405' '! D 1209 1 2 D850 ij Clear liquid free of sediment and haze when observed at 18.3 to 2S.6*C (65 tji 78`F). .- 4. Sampling 4.1 The material shall be sampled in accordance witfl Practice D 3437. " 5. Keywords 5.1 feedstock; p-Xylene; Xylenes 4 Available from Superintendent of Documents, U.S. Government Printing | Office, Washington, DC 20402. 770 iWmmmmm.il DUP050296332 # D 5211 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. Year comments are invited either for revision of this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP0502 96333 A Designation: E 299 - 90 Standard Test Method for Trace Amounts of Peroxides In Organic Solvents1 2 3 This standard is issued under the fixed designation E 299; the number immediately following the designation indicates the year m 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 method2,3 covers organic solvents containing active oxygen in the range from 5 to 80 ppm or higher. By using a special reaction-absorption cell, the test method can be extended to cover the range from 0 to 5 ppm. The test method can be used to determine numerous peroxide classes of varying reactivity such as hydroperoxides, diacyl perox ides, diaroyl peroxides, peresters, and ketone peroxides. The stable di-tert-alkyl peroxides do not react under the condi tions of analysis. 1.2 Solvents that can be successfully analyzed include saturated and aromatic hydrocarbons, alcohols, ethers, ke tones, and esters. In addition, the test method is applicable to olefinic solvents and to certain compounds that contain a, ft and conjugated unsaturaition. Solid samples that are soluble in the acetic acid-chloroform solvent can also be analyzed. 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: D1193 Specification for Reagent Water4 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemi cals5 3. Summary of Test Method 3.1 A sample is dissolved in a mixture of acetic acid and chloroform. The solution is deaerated and potassium iodide reagent solution is added. The mixture is allowed to react in the dark for 1 h, thereby releasing an equivalent amount of iodine. The absorbance of the, solution is measured at 470 nm and the amount of active oxygen present in the sample is determined by reference to a calibration curve prepared from iodine. 3.2 For samples containing 0 to 5 ppm active oxygen, a special reaction-absorption cell is employed. The sample is `This test method is under the jurisdiction of ASTM Committee E-15 on Industrial Chemicals and is the direct responsibility of Subcommittee El 5.22 on Functional Groups. Current edition approved July 27, 1990. Published September 1990. Originally published as E 299 - 66 T. Last previous edition E 299 - 89. 2 Baneijee, D. K., and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, 1964, pp. 792-796. 3 Baneijee, D. K,, and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, 1964, pp. 2367-2368. 4 Annual Book ofASTM Standards, Vol H .01. s Annual Book ofASTM Standards, Vol 15.05. de-aerated and the reaction is carried out withiJlL Absorbance measurements are made at 410 nm id irf the sensitivity. 4. Significance and Use 4.1 Dilute solutions of peroxides in various oigajf vents are frequently used as catalysts or reaction m Peroxides can also be formed through autoxidation classes of compounds including ethers, acetals, di alkylaromatic hydrocarbons and present a potemi. hazard. This test method provides a procedure tor mining the peroxide or active oxygen level. 5. Interferences 5.1 Oxidizing or reducing substances present laj sample will interfere. Colored solutions can be anth/ec absorbance correction is made. 6. Apparatus 6.1 Spectrophotometer--Beckman Model DU or i lent with matched 1-cm cells. 6.2 Special Reaction-Absorption Cell (Fig. 1)--Wh nt cell is used, the regular Beckman cell carriage replaced with the attachment provided for measuring'! absorbance in test tubes. 7. Reagents . ,* - 7.1 Purity ofReagents--RsagexA grade chemicals shall used in all tests. Unless otherwise indicated, it is inteni that all reagents shall conform to the specifications of Committee on Analytical Reagents of the American Ch> ical Society, where such specifications are available.6 Othfi grades may be used, provided it is first ascertained that reagent is of sufficiently high purity to permit its use withe lessening the accuracy of the determination. 7.2 Purity of Water--Unless otherwise indicated, ences to water shall be understood to mean Type II or T; III reagent water conforming to Specification D 1193 7.3 Acetic Acid-Chloroform Solvent (2+1)--Mix 2 voi! umes of acetic acid with 1 volume of chloroform. 7.4 Acetic Acid-Chloroform Solvent (Containing Approxijf mately 4 % Water)--Add 40 mL of water to 1 L of solveiij prepared as described in 7.3. 7.5 Iodine. 7.6 Nitrogen Cylinder. 7.7 Potassium Iodide Solution (50 %)--Dissolve 20 g of 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 "Anaiar Standards for Laboratory Chemi cals," BDH Ltd., Poole, Dorset, U.K., and the "United States Pharmacopeia." 772 DUP050296334 E 299 FIG. 1 Absorption Cell for Low-Active Oxygen' ftassium iodide (KI) in 20 mL of de-aerated water. This (gent should be freshly prepared just prior to use. pi Water, De-aerated--Pass nitrogen through distilled for several minutes prior to use- |Procedure , |.l High Range--0 to 400 \ig ofActive Oxygen: .1.1 Preparation of Calibration Curve: .1.1.1 Dissolve 0.1270 g of iodine in acetic acid-chlo- brm solvent (2+1) and dilute to 100 mL in a volumetric k. This solution contains 1.27 mg of iodine/mL, which is iiivalent to 80.0 pg of active oxygen/mL. 11.1.1.2 Transfer 0, 1,2, 3, 4, and 5-mL aliquots of this Ipition to 25-mL volumetric flasks and dilute each to jjurne with the acetic acid-chloroform solvent. Mix thor- fghiy$.1.1.3 Using a hypodermic needle or glass capillary, irge the solution with nitrogen for 1 to 1.5 min, add 1 mL ffreshly prepared KI solution, and continue the nitrogen Iw for 1 min. Stopper and mix well. 118.1,1.4 Measure the absorbance of each solution at 470 a, using 1-cm cells and a water reference. 18.1.1.5 Subtract the absorbance.of the blank and plot the Isorbance of each standard against micrograihs of active itygen per 25 mL. [8.1,2 Analysis ofSample: 18.1.2.1 Transfer a sample containing up to 400 pg of tive oxygen to a 25-mL volumetric flask and dilute to fblume with acetic acid-chloroform solvent (2+1) (Note 1). jfix thoroughly. No t e 1--A sample volume up to 15 mL may be used provided it is ;cible with the amount of acetic acid-chloroform solvent required to |lute the sample to 25 mL. 18.1.2.2 Sparge the solution with nitrogen for 1 to 1.5 min, 1 mL of freshly prepared KI solution, and continue the [itrogen flow for an additional 1 min. , 8.1.2.3 Stopper, mix well, and allow the solution to stand i the dark for 1 h. No t e 2--Very reactive peroxides react within less than 10 min, while less reactive peroxides require up to 1 h for complete reaction. A general reaction time for 1 h is therefore specified. 8.1.2.4 Measure the absorbance of the solution at 470 nm using l-crn cells and a water reference. No t e 3--Depending on the amount and type of sample present, some precipitation of KI may occur. However, the KI crystals readily settle to the bottom in absorbance measurement. 8.1.2.5 Subtract the absorbance of a blank carried through the entire procedure, and obtain the micrograms of active oxygen present in the sample by reference to the calibration curve. 8.2 Low Range--0 to 40 jig ofActive Oxygen: 8.2.1 Preparation ofCalibration Curve: . 8.2.1.1 Dissolve 0.0634 g of iodine in acetic acid-chlo roform solvent (2+1) and dilute to 100 mL. Transfer a 10-mL aliquot to another 100-mL volumetric flask and dilute to volume with acetic acid-chloroform solvent. This solution contains 63.4 pg of iodine/mL which is equivalent to 4.0 pg of active oxygen/mL. 8.2.1.2 .Transfer 0,1, 3, 5, 8, and 10-mL aliquots to 25-mL volumetric flasks and dilute to volume with the acetic acid-chloroform solvent containing 4 % water. Mix well. 8.2.1.3 Transfer a portion of each standard to the special absorption cell (Fig. 1). Admit a flow of nitrogen through the side arm and purge the solution for 3 min. 8.2.1.4 Add 5 drops of freshly prepared de-aerated KI solution and replace the stopper loosely. Continue purging with nitrogen for an additional 3 min. 8.2.1.5 Tighten the stopper and close the stopcock on the inlet tube so that the solution is under a slightly positive nitrogen pressure. 8.2.1.6 The absorption tubes shall be matched and pro vided with a glass ear for reproducible positioning before absorbance measurements are made. Insert the tube into the cell carriage and rotate until the glass ear contacts the side of. the tube holder. Measure the absorbance of the solution at 410 nm against water contained in another matched absorp tion tube. 8.2.1.7 Subtract the absorbance of the-blank and plot absorbance against micrograms of active oxygen per 25 mL. 8.2.2 Analysis ofSample: 8.2.2.1 Transfer a 5.00-mL sample to a 25-mL volumetric flask and dilute to volume with acetic acid-chloroform solvent (2+1) containing 4 % water. Mix well. 8.2.2.2 Transfer a portion of the solution to the special absorption cell and develop the color as described in 8.2.1.3, 8.2.1.4, and 8.2.1.5. 8.2.2.3 Allow the sample to stand in the dark for 1 h. 8.2.2.4 Measure the absorbance of the solution at 410 nm against water contained in the other matched absorption tube. 8.2.2.5 Subtract the absorbance obtained for a blank carried through the entire procedure, and obtain the micrograms of active oxygen present in the sample by reference to the calibration curve. 9. Calculation 9.1 Calculate the active oxygen content of the sample as follows: 773 DUP050296335 E 299 Active oxygen, ppm = AjBC where: A = active oxygen found, pg, B -- sample used, mL, and C = density, g/mL. 9.2 If a specific peroxide is known to be present, convert the parts per million of active oxygen to peroxide by using the appropriate conversion factor. Peroxide X, ppm = active oxygen in sample, ppm x F where F = conversion factor for peroxide X. 9.2.1 Conversion factors for some common peroxides are as follows: Cumene hydroperoxide Benzoyl peroxide /-butyl hydroperoxide Lauroyle peroxide 9.5125 15.1400 5.6328 24.9150 10. Report 10.1 High Range--Report the parts per million of active oxygen to the nearest 1 ppm. Duplicate runs that agree within 2 ppm are acceptable for averaging (95 % confidence level). 10.2 Low Range--Report the parts per million of active oxygen to the nearest 0.1 ppm. Duplicate runs that agree within 0.2 ppm are acceptable for averaging (95 % confi dence level). N 11. Precision and Bias7 11.1 Precision--High Range: 11.1.1 The following criteria shall be used for judging the acceptability of results (Note 4): 11.1.1.1 Repeatability (Single Analyst)--The standard de viation of results (each the average of duplicates), obtained by the same analyst on different days, has been estimated to be 2.9 ppm at 4 degrees of freedom. Two such values should 7 Supporting data are available from ASTM Headquarters Request RR; EI5-1002. be considered suspect (95 % confidence leve.) by more than 9 ppm. - 11.1.1.2 Reproducibility (Muitilaboratory).--Tiu deviation of results (each the average ofduplicates by analysts in different laboratories, has been estiin 4.6 ppm at 5 degrees of freedom. Two such values s considered suspect (95 % confidence level) if i hey more than 17 ppm. No t e 4--The above precision estimates are based on a-,. tory study on three samples containing 30 to 90 ppm of activ One analyst in each of 6 laboratories performed duplicate ( tions and repeated one day later, for a total of 72 deterffi Practice E 180 was used in developing these precision estima- 11.2 Bias--The bias of this test method has determined. 11.3 Precision--Low Range: 11.3.1 The following criteria shall be used for judgi acceptability of results: 11.3.1.1 Repeatability (Single Analyst)--The stand viation of results (each the average of duplicates). pv by the same analyst on different days, has been esiim be 0.11 ppm at 13 degrees of freedom. Two such should be considered suspect (95 % confidence level) differ by more than 0.3 ppm. 11.3.1.2 Reproducibility (Multilaboratory)--The:3 deviation ofresults (each the average ofduplicates), q by analysts in different laboratories, has been estima' 0.49 ppm at 4 degrees of freedom. Two such values^ be considered suspect (95 % confidence level) if thl' by more than 1.9 ppm. No t e 5--The above precision estimates are based on an inter,, tory study on three samples containing 3 to 10 ppm of active o\ One analyst in each of five laboratories performed duplicate dete. tions and repeated one day later, for a total of 60 determina.' Practice E 180 was used in developing these precision estimates. 11.4 Bias--The bias of this test method has not bg determined due to the unavailability of suitable refefe' material. 12. Keywords 12.1 assay; organic; peroxides; spectfophotometric The American Society for Testing and Materials takes no position respecting the validity ot any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. II you feel that your comments have not received a fair hexing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 774 DUP050296336 Designation: E 300 - 86 Standard Practice for Sampling Industrial Chemicals1 This standard is issued under the fixed designation E 300; 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. ope . This practice covers procedures for sampling several : of industrial chemicals. It also includes recommendajfor determining the number and location of such lies, to ensure their being representative of the lot in fdance with accepted probability sampling principles. ! : Although this practice describes specific procedures npling various liquids, solids, and slurries, in bulk or in ges, these recommendations only outline the principles observed. They should not take precedence over lie sampling instructions contained in other ASTM net or method standards. 5 These procedures are covered as follows: Sections al Consideration ....................................................... 5 to 9 ; Liquids............................................................................ 10 to 25 ........................................................................................................ 26 to 34 ............ I............................................................... .. 35 to 40 i --It is intended to add sections on viscous liquids; multiphase sis, partly solidified solids and liquefiable solids; liquefied gases; ries; and gases, when available. This standard may involve hazardous materials, operons, and equipment. This standard does not purport to uress all ofthe safety problems associated with its use. It is fesponsibility ofwhoever uses this standard to consult and blish appropriate safety and health practices and deter the applicability of regulatory limitations prior to use. !ic precautionary statements are given in Sections 4, 18, . 29, 33 and 36. Referenced Documents .1 ASTM Standards: >270 Method of Sampling Petroleum and Petroleum Products2* > 2234 Test Methods for Collection of a Gross Sample of Coal3 |E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chem icals4 Significance and Use f 3.1 This practice outlines the principles to be observed |hen sampling several classes of industrial chemicals. This ' 1 This practice is under the joint jurisdiction of ASTM Committee E-15 on ustrial Chemicals and is the direct responsibility of Subcommittee E15.05 on npling. j Current edition approved Jan. 31, 1986. Published March 1986. Originally |blished as E 300 - 66. Last previous edition E 300 - 73 (1983). 2 Discontinued, see 1983 Annual Book ofASTM Standards, Vol 05.01. * Annual Book ofASTM Standards, Vol 05.05. 4 Annual Book ofASTM Standards, Vol 15.05. practice also covers the statistical considerations in the sampling of industrial chemicals whether they are liquids, solids, slurries, and in bulk or packages. 4. Safety Precautions 4.1 This practice covers procedures and sampling equip ment used to sample industrial chemicals that may be potentially hazardous to personnel. Accordingly, it is empha sized that all applicable safety rules, regulations, and proce dures must be followed in handling and processing the chemicals. 4.2 The characteristics of the material to be sampled will govern the type of protective equipment required. Since sampling may present such hazards as splashing or spilling, protective clothing should be worn when the chemical is capable of producing eye or skin irritation or bums. During such potential exposures, chemical-type goggles or face shield and protective gloves, or combination thereof, should be worn. 4.3 Respiratory protection, where required, must be in good condition and must be suitable to protect against chemicals being handled. 4.4 When sampling chemicals that may be dangerous to life by skin absorption, oral ingestion, or by breathing the vapor, unusual precautions will be indicated. In such cases, full-body protection such as supplied by a gas-tight or one-piece air-supplied suit should be worn. A second man should be continuously present to summon help and render aid in the event of an emergency. STATISTICAL CONSIDERATIONS3 5. Objectives ----- 5.1 The sampling and testing of industrial chemicals may have one or more of the following objectives: 5.1.1 The objective may be to estimate the average quality characteristic of a given lot of material and to establish confidence limits for this average. This would be the main objective, for example, ifa dollar value is to be placed on the material for customs purposes or for sale. 5.1.2 The objective may be to decide whether the average value for the lot meets a specification. This calls for an acceptance sampling plan with the criterion being related to the estimated mean of the lot. 5.1.3 The objective may be to estimate or make decisions about the variability of a quality characteristic within the_lot. 5.1.4 The objective may be to obtain simultaneous esti mates of the mean and variance or to make decisions about 5 Prepared on an Ad Hoc Committee of ASTM Committee E-l I on Statistical Methods. 775 .4 DUP050296337 E 300 9| some joint combination of these estimates. 5.1.5 If the material comes in containers or can be viewed as coming in clearly demarked units, the objective may be that of estimating the number of such units outside of specifications, that is, the "fraction defective." No t e 2--Procedures are given below for estimating average quality and for applying acceptance sampling inspection based on the lot mean. 6. General Sampling Considerations 6.1 To obtain samples that are representative in a statis tical sense, one must consider such factors as physical form, uniformity, type and number of containers, etc. All of these influence the choice of method for performing the mechan ical sampling operation, as well as the number and location of the required samples. Two commonly used practices for selecting the sequence or location of the individual samples are described. 6.2 Random Sampling is achieved when every part of the lot has an equal chance of being drawn into the sample. 6.2.1 Designate all units in the lot, choosing numbers in sequence or other serial code so that sampling by random numbers can be employed. 6.2.2 Preferably, this sequence should be in direct relation to order of manufacture of packaging as an aid to observing, from the sample results, any evidence of stratification. 6.2.3 Random selection of the numbers should be accom plished by chance or preferably by the use of a table of random numbers. - 6.3 Stratified Sampling can be employed to estimate average quality when it is known or suspected that the value of a property of the material varies in nonrandom fashion throughout the lot for the following typical reasons: (a) the lot may contain several production batches, (b) the lot may contain units produced by different procedures, equipment, shifts, etc., or (c) the lot may be nonuniform because of subsequent size segregation, moisture pickup, surface oxida tion, etc. Ifthe assumed pattern is correct, the variance of the population mean estimate will be less than that based on random sampling. If the assumptions are incorrect, the estimate of the mean may be biased. A stratified sample can be obtained as follows: 6.3.1 Based on the known or suspected pattern, divide the lot into a number of real or imaginary strata. 6.3.2 If these sections are not equal in size, the number of samples to be taken from each stratum should be propor tional to the size of the various strata. 6.3.3 Further subdivide the major strata into real or imaginary subsections and select the required number of samples by chance or preferably by means of a table of random numbers. 7. Estimate of Average Quality 7.1 Determination ofthe Variance ofa Sample Mean--If the material comes in, or can be viewed as coming in, realizable primary units, each of which are to be divided into realizable secondary units, then if nb primary units are selected at random from a lot of N primary units, and if nw secondary units are selected from each primary unit with k tests being made on each secondary unit drawn, then the variance of the mean of the results is given as follows (Notes 3 and 4): a* = x [(N ~ nb)/N] + [ow2/(nb X j] + ^ :J\ where: ' ' <7% = variance of the mean, of = variance of primary units (the material m caiS cans, drums, bottles, or other containers) m of = average variance of secondary units (all-levdL r2 _ thief, or similar samples) from a primary unif,*S variance of tests on a homogeneous sample - N = number of primary units in the lot nb = number of randomly selected primary units' which secondary units are drawn, nw -- number of randomly drawn secondary uni each of the nb primary units, and 1' n, = total number of tests made on all units, replicates. 7.1.1 Equation 1 is also applicable when the secondary units are composited into a single sampl testing. If there is no compositing and k tests are __ each secondary unit, X will be an arithmetic average ! k x nb x nw test results. Ifthe secondary units are compc&iti and k tests are made on the composite sample, X willl"uS arithmetic average of nt = kc results. No t e 3--Uniform quantities (weight or volume, as approim* i the primary units and in the secondary units are assumed. If departure from uniformity is such that a material error would introduced by using a simple mean, a weighted average should bi^usai or, if the secondary units are composited, proportional composftifjj must be adhered to. No t e 4--The factor (N - nb)/N is the correction for sampling finite population. A corresponding correction is generally not ncc&St? for secondary units and tests.' 7.1.2 For homogeneous reduces to Eq 2: liquids of = 0, so that IHfi = (^2/a) x m - nb)m + (*>,) i 7.1.3 If nb = N, Eq 1 and 2 reduce, respectively, to E$! and 4: of = [of/(nb x ,,,)) + (at2/n,) "(H ** = &tj 7.2 Determination ofnh, nw, and nt When-Basic Variances' are Known--When reliable estimates -of the variances of. of, and of are. available from experience with lots of thffi'jj type involved; a set ofequivalent combinations of n^ and n, may be calculated from Eq 1, each combination based on'' the same desired or specified variance of the mean, oX2. Similarly, sets of equivalent combinations may be calculated from Eq 2 and 3. No t e 5--If the precision of the test method has been properly evaluated in accordance with Practice E 180, an adequate estimate of a,2 can be obtained from the repeatability standard deviation (sa) based on approximately 30 degrees of freedom. 7.2.1 Choice of a particular combination in a set for a specific lot is optional. In general, one combination in a set is most economical under given cost conditions and is there fore to be preferred. 7.3 Procedure When Basic Variances are Unknown: 7.3.1 Select at random a likely or convenient number, n{ (10 or more), of primary units from the lot, take one secondary unit from each, and test each secondary unit. Estimate the variance of a measurement of a primary unit, r,2 (a variance that includes between and within unit 776 DUP0502 96338  E 300 lability as well as test variability), using Eq 5: s,2 = 1) (5) ire X{ is the mean of the individual test results on the k , |ary units, with one secondary unit per primary unit and ftest per secondary unit. *5.2 Decide to estimate the mean of the lot from single |s on single secondary units from n2 primary units where , and the n2 units include the , preliminary units, the tie on n2 being determined from Eq 6: n2 ~ S12/TSi2 (6) life TSj is the target value of an estimate of the variance "Y. The target value will depend on the width of the 'red confidence interval. If it is hoped to have a 0.95 ifidence interval of width 2A, then for n2 > 30, Tsj Juld be taken as (A/1.96)2. For smaller values of n2, die S should be replaced by the 0.025 values from a /-table. '.3.3 Estimate the variance ofthe mean after n2 tests from ii:7: s/ = 2(X--l)2/n2{n2- 1) (7) |'.4 A Confidence Limits for the Mean ofthe Lot: ||7.4.1 If the basic variances are known and two-stage npling (primary and secondary units) is employed, then 5 confidence limits for the mean of the lot p are given by I 8: 0.95 confidence limits for p = % 1.96 ak (8) |ere ax is obtained from the or/ value given by Eq 1. 7,4.2 If the basic variances are unknown and the variance & is estimated as in 6.3 (ns sample primary units with one Midary unit per sample primary unit and one test per jsondary unit), then 0.95 confidence limits for the mean of : lot p. are given by Eq 9: 0.95 confidence limits for p = X tom5 sx (9) here sx is obtained from the sfi value given by Eq 7 and can be taken as equal to 1.96 if n2 is greater than 30, but herwise should be taken from a table of /-values for n2 - 1 pgrees of freedom. | Acceptance Sampling for a Lot Mean--Basic Variances Unknown. |i! No t e 6--This section describes a simple random sampling plan for |e acceptance inspection ofan isolated lot and provides for buyer's and r's risks of making a wrong decision. If a series of lots is to be Sspected and knowledge of the basic variances is available, significant livings may be realized by testing composites. 8.1 Introduction--If a specification requires, for example, |iat the average purity or assay of a lot be no less than 8.0 %, it it sometimes assumed that the sampling and jesting plan will accept all lots of 98.0 % or higher, but will |ctect or reject any lot falling below this value. This ideal gtuation is not statistically realistic, as the required degree of crimination can be approached only if the lot units are Issentially uniform and the test procedure is capable of attaining a very high level of precision. It is necessary, herefore, that the contracting parties realize that any sam|ling plan based on a low probability of rejecting a lot which, fact, is 98.0 % or higher in purity, may also permit 'acceptance of some lots below this specification minimum. Accordingly, such specifications must be viewed as incorpo rating both a buyer's and seller's risk. The following proce dures are based on this concept. 8.2 Single Lower Specification Limit (L): Simple Random Samplingfrom a Large Lot: 8.2.1 Procedure: 8.2.1.1 Step I--Note the value of the lower specification limit for average lot quality and designate it by L. Assume this value to represent a quality level for which the proba bility of acceptance should be high and the risk of rejection low. In this procedure, the seller's risk is taken to be 0.05. 8.2.1.2 Step 2--Establish a lower value for the barely tolerable lot quality for which the level of acceptance should be low and designate it by L - A. Here, this buyer's risk is taken to be 0.10. 8.2.1.3 Step 3--Take a preliminary sample of n, (equals 10 or more) units at random from the lot and compute "i X-- f'X/nj.and (10) V (X, - *)2/(, - i) (H) Set 3, = s, (12) 8.2.1.4 Step 4--Note the value of A agreed to in Step 2. Compute \[ = A/3'1 and find from Table 1 the value ofn that comes closest to that given by the computed value of X,. Call this n2. 8.2.1.5 Step 5--Randomly select n2 -- n, additional units from the lot. Compute ,, x2 = 2 jSj/Bj, and (13) S2 Vs (Xt-xfKm-x) (14) 8.2.1.6 Step 6--Check on the adequacy of n2 by taking 32 " s2. Compute X2 = A/32. Enter Table 1 and find the value of n corresponding to X2. Call this 3. If n3 is much greater than 2, for example, more than 20 %, randomly select n3 -- n2 additional units from the lot and return to Step 5! If h 3 is not much greater than 2, proceed with Step 7. 8.2.1.7 Step 7--Using the final values obtained above, calculate the following and accept the lot if [(L-X)/(s/M]<taM (15) TABLE 1 Values'4 of Sample Size (n) for Agreed Upon Values of A A= A/ir Sample Size (n) 2.76 2.16 1.61 1.26 1.00 0.79 o.6a 0.54 0.42 0.33 0.29s 3 4 5 7 10 15 20 30 50 75 100 Values of \ were read from Fig. 13.31 of Bowker and Lieberman, Handbook of Industrial Statistics. s For larger size samples, take n = (2.9Z7 - 8.57/x2. 777 DUP0502 96339 E 300 where = nu n2, or 3, whichever is applicable, r0.os *s the upper 0.05 point of a ?-distribution for n -- 1 degrees of freedom, and s = or s, whichever is applicable. Otherwise, reject the lot. 8.2.2 Example: 8.2.2.1 Assume that a contract covered the purchase of a packaged material with a minimum purity specification of 98.0 %. The buyer and seller agreed that the probability of rejecting a lot of 98.0 % purity should be no greater than 0.05 and that of accepting a lot as low as 97.0 % should be no greater than 0.10. In this case, the pertinent levels are: L = 98.0 L A = 97.0 A =1.0 8.2.2.2 On testing samples from ten units, selected at random, the lot standard deviation was estimated to be: 3j = Sj -- 0.8 The values for X and Ai were also calculated: X = 97.5 % A, = A/gS] = 1.0/0.8 = 1.25 8.2.2.3 Entering Table 1, the sample size n for At = 1.25 is found to be 7. Accordingly, no further sampling is required. 8.2.2.4 Substituting the above values in Eq 15; (L - X)f(.s/fn) = (98.0 - 97.5)/(0.8/Vl0) = (0.5 x /10)/0.8 = 1.97 Since 1.97 is greater than 1.833 (the value for the upper 0.05 point of the l-distribution for 9 degrees of freedom), the lot should be rejected. 8.3 Single Upper Specification Limit (U); Simple Random Sampling from a Large Lot--The procedures of 8.2 will apply here except that U will replace L and U + A will replace L - A. The criterion for acceptance will be: (X - U)/(S/Jn) s t0.05 (16) 8.4 Both Lower and Upper Specification Limits: Simple Random Sampling from a Large Lot--Use the following sampling plan: Determine n, X, and s as in 8.2.1. Accept the lot if (L - X)M-fn) < to.05> and (17) (X- U)J(s/fri)<;t0.05 (18) for n - 1 degrees of freedom. Otherwise, reject the lot. 8.5 General Remarks: 8.5.1 If A is small relative to the lot standard deviation, a large sample size will be required to attain the low 0.10 consumer's and 0.05 producer's risks. 8.5.2 If the estimate of the lot standard deviation is less than the true lot standard deviation, the sample size given by the above procedures will produce a sampling plan whose risks will be different from those planned for. There will be a greater seller's risk of having a lot rejected whose mean is equal to the desired L level. Also, the buyer's risk of accepting a lot, whose mean is below the L - A level for barely acceptable quality, will also be greater than 0.10 (how much greater depends on how far off the estimate of the lot standard deviation may be). 8.5.3 If the estimate ofthe lot standard deviation is greater than the true lot standard deviation, then the above proce dures will give a sample size () that is greater than[ n: eSe to yield the agreed upon risks. It will thus unnccessa increase sampling costs. 8.5.4 The risks stated in this practice are based o assumption that variability among units of the lot folio normal distribution and that the total quantity of.mate' subsamples taken for testing does not exceed 10 % of total quantity in the lot. If variability among units sh evidence of considerable skewness, the logarithms ofthe (or other transformation) should be used. 8.5.5 If the sample units are taken from bulk material 1 given sampling device, these risks are also based on assumption that the sampling device is used in taking the preliminary sample and the total sample. 9. Acceptance Sampling for the Mean of a Lot from. Stream of Batched Material for Which the Basic V: ances Have Been Previously Estimated 9.1 Some Basic Considerations--To understand the redommendations of this section, it is helpful to review brief! the nature of an operating characteristic (OC) curve for, acceptance sampling plan. 9.1.1 The OC curve of acceptance sampling plan gives the probability of acceptance of a lot with reference to hypothetical stream of lots. Two types of streams generally considered. These are designated as Type A an Type B. A Type A stream is a stream oflots that are identi in every respect to the lot currently being inspected. A Ty4 B stream of lots of the same size as the lot currently bein inspected that would be generated by a controlled process?' When we are faced with the inspection of an isolated lot, it seems appropriate to view the risks of the sampling inspe# tion with reference to a Type A stream. We have little ot no knowledge of the process from which the lot came and a decision on the lot would seem best based on data from that lot alone. This is the case considered in Section 8 of this practice; the isolated lot with unknown standard deviation,. 9.1.2 In the present section, reference is to a process that is producing a stream oflots in batches. We assume that the within-batch and between-batch variations are independent and random with constant variances and on the basis of these assumptions we run a pilot study of variances that we take to hold valid for subsequent lots from the'process. The current lot being inspected is recognized from the start as being one ofthe stream oflots coming from the given process and, as such, we are willing to use information about within-batch and between-batch variances obtained in the pilot study as part of the total information on which a decision about the lot is based. In this section, therefore, the probability of acceptance will be with reference to a Type B stream oflots, that is, with reference to a stream oflots from a controlled process. It follows in this case that the variance of a sample lot mean will be a function of both the within-batch and between-batch variances. 9.1.3 The recommended procedures of 9.2 call for compositing of increments and reduction for laboratory testing. As in the case of the batch variability, a preliminary study is made of the compositing and reduction processes and preliminary estimates are made of the reduction vari ance and the testing variance. It is again assumed that these same variances continue valid for the reduction and testing 778 DU P050296340 E 300 edure employed in the inspection of the current lot. -mmended procedures for estimating the batch variances the reduction and testing variances are given in the ex. In the sections that follow, it will be assumed these ates have been made. A Word ofAdvice--Before a particular program is ituted, it would be desirable to review it with a statistician be sure that the recommendations of Section 9 are roughly understood. .2 Acceptance Tests Based on Current Samples: .2.1 Introduction--With knowledge of the basic vari- for the product and for the method of reduction and g, the acceptability of a current lot from the given am of material can be determined as follows: 2.2 Formation ofComposite Samples--For the purpose determining the acceptability of a current lot from the en stream oflots, proceed as follows: Let the lot consist of batches of material where n, is an integer. Presumably n, determined by the needs of the purchaser with respect to inventories, production, etc. (Note 7). Let n2 increments material be taken at random from each of the nx batches at make up the given lot and let n2 be an even number. _e determination ofn2 is discussed in 9.2.4). Ifthe batches not distinct, take nxn2 increments at random from the , Form a composite of all the odd numbered increments d another composite of all the even numbered increments. [ the first composite A, the second composite B. Reduce h composite separately and under uniform conditions run ;o tests on each composite. y No t e 7--A fraction ofa batch should be treated as a whole batch in terminingBj, 9.2.3 _Parlance Formula--The variance formula for the ean (X) of the two composite samples with two tests per mposite is ;2 - 2 : fi- + B W 1 H[2 4 . .(1) here: = estimate made in the preliminary study of the between-batch variance, 2 = estimate of the within-batch variance, ? = estimate of the reduction variance, and f -- estimate of the testing variance. 9.2.4 Determination of the Value of n2 with a Single lower Specification Limit (L)--For a single lower specifica tion limit, the procedure for determining the value of n2 is as /fallows: 9.2.4.1 Step 1--Note the value of the lower specification limit for average product quality and designate it by L. Assume this value to represent a quality level for which the probability of lot acceptance should be high and the risk of lot rejection low. In the procedure for determining n2, the seller's risk is taken to be 0.05. 9.2.4.2 Step 2--Determine a barely tolerable product quality for which the probability of lot acceptance should be low and designate this by L - A, Here the buyer's risk is taken to be 0.10. 9.2.4.3 Step 3--Take n2 as the even integer just greater than y. _ 'W ^ ,[(A2/8.5673) _ (or^/a,) - (of/l) - (if/4)] .. .(2) This n2 will for the stated variances make the probability of lot acceptance for product quality L equal'approximately to 0.95 and the probability of lot acceptance for product quality L -- A equal to 0.10. 9.2.5 Determination ofthe Value ofn2 with a Single Upper Specification (U)--The procedure is the same as that of 9.2.4 except that U replaces L and U + A replaces L -- A. The formula for n2 is the same. 9.2.6 Determination ofthe Value ofn2 with Both a Lower and Upper Specification Limit--The procedure is exactly the same as that of 9.2.4 and the formula for n2 is the same. It is assumed that the spread between specification limits is at least 3 crs. 9.2.7 Sample Checks on the. Basic Variances--Before using Eq 1 in an acceptance test, a check should be made to see if die values previously determined for of, aw2, of, and of are still valid. To check on of, compute the difference between the two tests for composite vl and also the difference between the two tests for composite B and plot the two differences on an extension of Control Chart {4) described in the Annex. Proceed only if both of the two differences fell within the control limits. To check the remaining variances, set up a chart called Control Chart (J); the limits for which shall be 0 and 3.686/^ + ^- + of- w \nl l2 and the central line on which shall be (il1.128 2 o,, 3 \ U2 + of + \i n,n2 ' 2 Plot on this chart the absolute' value of the difference between the mean of composite A and the mean of com posite B. Again proceed only if the difference fells below the upper limit and does not, with previous points, yield a run of seven or more above the central line. No t e 8--If a point fells above the upper limit, this means that the purchaser's testing variance is probably greater than if An estimate of the former based on addition data would consequently have to be made. The acceptance procedure could'thus continue wiHrthe purchaser's test variance in place of.the original if. This new estimate should be based on at least 20 degrees of freedom. 9.2.8 Acceptance Test when there is a Single Lower Specification Limit (L): 9.2.8.1 Step I--Compute Xi* " L - 1.645 (ifIn, + if/n,n2 + ifa + if/4)m .. .(3) 9.2.8.2 Step 2--Accept the lot iiXz. 1 9.2.9 The Acceptance Test when there is a Single Upper Specification Limit (U) 9.2.9.1 Step 1--Compute Xua+V+ 1.645 (ifIn, + if/n,n2 + if)2 + 3,2/4)> (4) 9.2.9.2 Step 2--Accept the lot ifX XUa. 9.2.10 Acceptance Test when there are both a Lower Specification Limit (L) and an Upper Specification Limit (U): 9.2.10.1 Step 1--Note whether U - Lis greater than Xofin, + if/n,n2 + if12 + of/4)m If it is, continue to Step 2. If it is not, do not continue. 779 m DUP050296341 # E 300 9.2.10.2 Step 2--Compute and Xua as in 9.2.8 and 9.2.9. 9.2.10.3 Step 3--Accept the lot if XLa < X s XUa. SIMPLE LIQUIDS 10. Scope 10.1 This procedure covers the sampling of industrial chemicals which are single-phase liquids under the condi tions of sampling. No t e 9--This procedure is based on Method D 270. 11. Summary 11.1 Samples of simple liquids are examined using var ious ASTM methods for the determination of physical and chemical characteristics. It is accordingly necessary that the samples be truly representative of the simple liquids in question. The precautions required to ensure the representa tive character of the samples are numerous and depend upon the type of product being sampled, the tank, the carrier or container from which the sample is being obtained, the type and cleanliness of the sample container, and the sampling procedure that is to be used. A summary of the sampling procedures and their application is presented in Table 2. Each procedure is suitable for sampling a number of specific products under definite storage, transportation, or container conditions. The basic principle of each procedure is to obtain a sample or a composite of several samples in such manner and from such locations in the tank or other container that the sample or composite will be truly representative of the product. Although single-phase liquids are homogeneous by definition, it may be desirable to check for this condition by sampling, from various sections of the container. 12. Definitions 12.1 simple liquid--a single-phase liquid having a vapor pressure of less than 16 psi Reid vapor pressure at 100F (830 mm Hg at 37.8C) and. a Saybolt viscosity of less than 10 000 s (2160 cSt) at 25C. 12.2 average sampler--one that consists of proportionate parts from all sections of the container. 12.3 all-levels sample--one obtained by submerging a closed sampler to a point as near as possible to the draw-off level, then opening the sampler and raising it at a rate such that is about three fourths full as it emerges from the liquid. An all-levels sample is not necessarily an average sample because the tank volume may not be proportional to the depth and because the operator may not be able to raise the sampler at the variable rate required for proportionate filling. The rate of filling is proportional to the square root of the depth of immersion. No t e 10--The tube sampling procedure, 20.3, may be obtain an all-levels sample from a drum. 12.4 upper sample--one obtained from the mil upper third of the tank contents (Fig. 1). No t e 11--The taking of samples from various levels l permits the detection ofvariation in composition ofthe cont< by stratification. If it is known that the contents are not:____ variation, the taking ofsamples at multiple levels may be eliminated 12.5 middle sample--one obtained from the middles the tank contents (Fig. 1) (Note 10). -cL 12.6 single-tank composite sample--a blend ofthe UpmPi middle, and lower samples. For a tank of uniform SfKf section, such as an upright cylindrical tank, the bleM consists of equal parts ofthe three samples. For a horizontal cylindrical tank, the blend consists of the three samples^ the proportions shown in Table 3. , ,, : 12.7 compartment-tank composite sample (ship, hdrjft etc.)--a blend of individual all-levels samples from ead, compartment, which contains the product being sampled! proportion to the volume of material in each comparting 12.8 top sample--one normally obtained 6 in. (152 m below the top surface of the tank contents (Fig. 1). <*W 12.9 outlet sample--one normally obtained at the leve- ot' the tank outlet (either fixed or a swing line outlet) (Fig. 1); '% 12.10 continuous sample--one obtained from a pipelined conveying the product in such a manner as to giveii representative average of the stream throughout the period pi transit. 12.11 jar sample--one obtained by placing a jar i.u< (h$ path of a free-flowing stream so as to collect a definii; volume from the full cross section of the stream. 12.12 mixed sample--one obtained after mixing or vigor-1 ously stirring the contents ofthe original container, and thecy pouring out or drawing off the quantity desired. 12.13 tube or thiefsample--one obtained with a sampling. tube or special thief, either as a core sample or spot sample from the specified point in the container. TABLE 2 Summary of Sampling Procedures and Applicability Type of Container Storage tanks (trucks, cars, ships. barges, stationary) Storage tanks (trucks, cars. stationary) Pipe lines, filing fines, transfer lines Drums, carboy, cans, bottles Free or open-discharge streams Type of Sampling Bottle sampling, thief sampling Tap sampling Continuous sampling Tube sampling Jar sampling Section 21, 22 23 24 25 26 DUP0502 96342 E 300 3 Sampling Instructions for Horizontal Cylindrical Tanks Saplh, got ger Sampling Level, Percent of Diameter Above Bottom Upper Middle Lower Composite Sample Proportionate Parts of Upper Middle Lower 80 50 20 fi. 75 50 20 70 50 20 50 20 50 . 20 40 20 20 15 10 5 34 3 34 3 25 3 15 4 55 46 to 10 10 10 fp4 drain sample--one obtained from the draw-off or rge valve. Occasionally, a drain sample may be the > a bottom sample, as in the case of a tank car. 15 bottom sample--one obtained from the material on jttom surface of the tank, container, or line at its lowest |(Fig. 1). (Drain and bottom samples are usually taken feck for water, sludge, scale, etc.). Sampling Equipment A General Requirements--all sampling apparatus and |ures shall be clean, dry, free of contaminants, and fetructed to materials that are inert to the product to be pled. The sampling container and closure shall be clean, land inert to the material being sampled. |l;2 Bottles and Jars--Bottles and jars may be made of or brown glass or polyethylene with necks shaped to Ive a glass stopper or a screw cap made of metal or plastic prial. Use of unprotected corks as closures is not recomlided for general use. Where safety indicates (such as for jfbxides) use corks covered with materials inert to the nple, such as cellophane, polyethylene, or aluminum foil. |ar glass is advantageous because the container may be ained visually for cleanliness and the sample may be |ually inspected for foreign matter. Brown glass affords ne protection for light-sensitive materials. Before using a tie orjar, examine it to see that it is scrupulously clean. A liety of methods for cleaning glass containers may be used: * ling with detergents, chromic acid cleaning solution, er, acetone, etc. The specific method used will depend |on the material to be sampled. Care should be taken that ; of the cleaning agents are removed from the container lor to use. Close containers as soon as they are dry. f13.3 Screw-Neck andPress-Cover Cans--Cans of tin plate i seams soldered on the outside should be used. The neck Siould be shaped to receive a screw cap or pressed cover. should be taken to ensure that cans are clean, even fhen new. They may be cleaned by washing with lowIpiling, nonflammable solvents and blowing dry with clean ` . Cap the containers as soon as they are dry. Time and Place of Sampling 14.1 Finished Products--When loading or discharging finished products, take samples from both shipping and ceiving tanks, and from the pipeline, if required. 14.2 Ship or Barge Tanks--Sample each product immeliately after the vessel is loaded, or just before discharging. 14.3 Tank Cars--Sample the product immediately after the car is loaded, or just before unloading. 15. Number and Location of Samples 15.1 Bulk Containers (Tanks, Tank Cars etc.)--Simple liquids in bulk containers are frequently found to be homo geneous and only limited sampling is usually required. Upper, middle, and lower samples (21.3) or top and outlet samples (21.5) can be individually tested to confirm this, by means of simple physical tests such as refractive index, specific gravity, viscosity, etc. Complete testing can then be performed on a composite prepared as described in 21.4. 15.2 Packaged Materials (Drums, Cans, Bottles, etc.)--In the case of lots of drums, bottles, and cans, the homogeneity of the lot cannot be assumed, and the required number of samples should be determined in accordance with Sections 5 and 6. The specific containers to be sampled for individual testing should be chosen by means of a table of random numbers. 16. Sampling Operations 16.1 Procedures for sampling cannot be made explicit enough to cover all cases. Extreme care and good judgment are necessary to ensure samples which represent the general character and average condition of the material. Clean hands are important. Clean gloves may be worn but only when absolutely necessary, such as during cold weather, or for reasons of safety. Select wiping cloths so that lint is not introduced, contaminating samples. 16.2 When sampling relatively volatile products, the sam pling apparatus shall be filled and allowed to drain before drawing the sample. If the sample is to be transferred to another container, this container shall also be rinsed with some of the volatile product and then drained. When the actual sample is emptied into this container, the sampling apparatus should be upended into the opening of the sample container and remain in this position until the contents have been transferred so that no unsaturated air will be entrained in the transfer of the sample. 16.3 When sampling nonvolatile liquid products, the sampling apparatus shall be filled and allowed to drain before drawing thejictual sample. If the actual sample is to be transferred to another container, the sample container shall be rinsed with some of the product to be sampled and drained before it is filled with the actual sample. 16.4 A sample shall be considered suspect under any of the following circumstances and should be referred to the appropriate supervisor before analysis: 16.4.1 The sample container is damaged or defective. 16.4.2 There is any doubt as to the nature of the contents ofthe sample container: for example, because of the presence of an old label, incorrect markings, or insufficient identification. 16.4.3 There is evidence of an unexpected lack of unifor mity; for example, a separate layer or suspended matter. 16.4.4 Obvious and unusual variations are apparent in the sample. 16.4.5 The container closure is loose, whether or not there is evidence of leakage. 16.4.6 Evidence that the closure or liner has been at tacked. 781 DUP050296343 # E 300 17. Size of Sample 17.1 The quantity of sample should be as specified by the test instructions, or at least three times greater than the minimum necessary for the actual tests. 18. Precautions 18.1 Volatile Samples (2 to 16 psi Reid Vapor Pressure at 100F (105 to 830 mm Hg at 37.8C)) --It is necessary to protect volatile samples from evaporation. Transfer the product from the sampling apparatus to the sample con tainer immediately. Keep the container closed except when material is being transferred. 18.2 Light-Sensitive Samples--It is important that sam ples sensitive to light be kept in the dark if testing is to include the determination of such properties as color, inhibitor content, stability tests, or neutralization values. Brown glass bottles may be used. Wrap or cover clear glass bottles immediately. It is a definite advantage to use covered metal or cardboard containers into which the sample bottles may be placed immediately after collection. 18.3 Materials of High Purity--Protect highly refined products from moisture and dust by placing paper, plastic, or metal foil over the closure and the top of the container. 18.4 Container Outage--Never completely fill a sample container, but allow adequate room for expansion, taking into consideration the temperature of the liquid at the time of filling and the probable maximum temperature to which the filled container may be subjected. 19. Shipping Precautions 19.1 To prevent the loss of liquid during shipment and to protect against moisture and dust, cover the closure of the glass bottle with plastic caps which have been swelled in water, wiped dry, placed over the top of the stoppered bottle, and allowed to shrink tightly in place. Screw-top bottles are recommended. The cap should be lined with material inert to the sample. The screw caps should be secured by use of adhesive tape or similar material. No t e 12--Shipping of any chemical must comply with current federal, state, and local regulations for the specific material being shipped. 20. Labeling Sample Containers 20.1 Label the container immediately after a sample is obtained. Use waterproof and oil-proof ink or a pencil hard enough to dent the tag, since soft pencil and ordinary ink markings are subject to obliteration from moisture, oil smearing, and handling. If gummed labels are used, they should be further secured with transparent sealing tape. Sufficient detail should be written on the label to completely identify the sample. The following information is frequently desired: 20.1.1 Date and time (and for continuous and dipper samples the hour and minute of collection), 20.1.2 Name of sampler, 20.1.3 Name or number and owner of the vessel, car, or container, 20.1.4 Brand name, grade of material, and code number, and 20.1.5 Reference symbol and necessary identification number. 21.Bottle Sampling 2\.\ The bottle sampling procedure is applic sampling simple liquids in tank cars, tank true tanks, ship tanks, and barge tanks. A suitable bottle, as shown in Fig. 2, is required. The diametel openings in the bottles should be %-in. (I9-mm). S and label bottles immediately after taking them and' them to the laboratory in the original sampling bottleT^'" No t e 13--The designs and dimensions which follow are iuferns only as guides to the form that the sampling apparatus may cue metal is required for construction of the sampling apparatus' a mffd sion-resistant type steel should be selected (Type 316L may br sintaftfeL If flammable materials are to be sampled, a nonmagnetic iow-sfiS generating stainless steel is required. When sampling.flammable liquid? extreme care should be exercised not to sharply strike the contain being sampled with the sampling apparatus. Alternative proceduresnta be used if a mutually satisfactory agreement has been reached by * parties involved. 21.2 All-Level Sample--Lower the weighted, stopper bottle as near as possible to the draw-off level, pull out t. stopper with a sharp jerk of the twine or chain (spark-prooYD attached to the stopper, and raise the bottle at such a rati that it is about three-fourths full as it emerges from liquid. 21.3 Upper, Middle, and Lower Samples--Lower weighted, stoppered bottle to the proper depths (Fig. which are as follows: Upper sample Middle sample Lower sample middle of upper third of the tank cantentMfl middle of the tank contents iTjjj$l middle of lower third of the tank contents!; Pull out the stopper with a sharp jerk of the twine or cli (spark-proof) attached to the stopper and allow the bottle u>1 ALTERNATE RIG (CAN BE FABRICATED TO FIT ANT SIZE CLASS-STOPPERED BOTTLE) FIG. 2 Assembly for Bottle Sampling 782 -me- . , ` ........ #5$ DUP050296344 # E 300 knpletely at the selected level, as evidenced by the pn of air bubbles. When full, raise the bottle, pour off [ amount, and stopper immediately. Composite Sample--Prepare a composite sample in laboratory (not in the field) by mixing portions of els samples as specified in 12.7 or by mixing portions i upper, middle, and lower samples as specified in 12.6. Top and Outlet Samples--Obtain these samples (Fig. , the same manner as specified in 12.13, but at the ving depths: ^sample 6 in. (152 nun) below the top surface of the tank contents opposite the tank outlet (either fixed or swing line outlet) lief Sampling The thief sampling procedure is applicable for obig bottom samples (Fig. 1), of liquids of 2 psi Reid ir pressure at 100F (105 mm Hg at 37.8C) or less, in cars and storage tanks. ;,2 Thief--The thief shall be designed so that a sample |be obtained with lh in. (13 mm) of the bottom ofthe car ik. Two types ofthiefs are illustrated in Fig. 3'. One type ered into the tank with valves open to permit the liquid [lush through the container. When the thief strikes the dm of the tank, the valves shut automatically to trap a :pm sample. The other type has a projecting stem on the rod which opens the valves automatically as the stem strikes the bottom of the tank. The sample enters the container through the bottom valve and air is released simultaneously through the top. The valves snap shut when the thief is withdrawn. 22.3 Procedure--Lower the clean, dry thief through the dome of the tank car or tank hatch until it strikes the bottom. When full, remove the thief and transfer the content to the sample container. Close and label the container immediately, and deliver it to the laboratory. 23. Tap Sampling 23.1 The tap sampling procedure is applicable for sam pling simple liquids in tanks which are equipped with suitable taps or lines. The assembly for tap sampling is shown in Fig. 4. 23.2 Tank Taps--The tank should be equipped with at least three sampling taps placed equidistant throughout the tank height and extending at least 3 ft (9 m) inside the tank shell. A standard 'A-in. (6-mm) pipe with suitable valve is satisfactory. 23.3 Tube--A delivery tube which will not contaminate the product being sampled and long enough to reach to the bottom of the sample container is required to allow' sub merged filling. 23.4 Procedure--Before a sample is drawn, flush the tap (or gage glass drain cock) and line until they are purged completely. Connect the clean delivery tube to the tap. Draw upper, middle, or lower samples directly from the respective (a) Bomb-Types Sampling Thief FIG. 3 Sampling Thiefs 783 DUP050296345 E 300 FIG. 4 Assembly for Tap Sampling taps after the flushing operation. Stopper and label the sample container immediately after filling, and deliver it to the laboratory. 24. Continuous Sampling 24.1 The continuous sampling procedure is applicable for sampling simple liquids in pipe lines, filling lines, and transfer lines. The continuous sampling may be done manu ally or by using automatic devices. 24.1.1 Precaution--The sample line should be purged three times before the sample is taken and special precau tions should be taken to minimize exposure to the chemical being sampled. 24.2 Sampling Probe--The function of the snmplit(Sr"k probe is to withdraw from the flow stream portion f hat wilij^ be representative of the entire stream. The apparatus as- " sembly for continuous sampling is shown in Fig. 5. Probe designs that are commonly used are as follows: 24.2.1 A tube extending to the center of the line and- beveled at a 45.angle facing upstream. -24.2:2 A long-radius elbow or bend extending to the center line of the pipe and facing upstream. The end of the- probe should be reamed to give a sharp entrance edge. >3ris 24.2.3 A tube extending across the pipeline with holes or slots facing upstream. The position and size of the pmbe should be such that it will minimize stratification and dropping out of heavier particles within the tube. No t e 14--Although this discussion is limited to simple liquids which are assumed to be uniform in composition, it is possible that under certain conditions, temporary stratification (caused by pressure, temper ature gradients, etc.) may exist and, therefore, certain precautions are m advised to ensure obtaining representative samples.4 24.2.4 To control the rate at which the sample is with drawn, the probe or probes should be fitted with valves or* plug cocjcs. 24.2.5 A clean, dry container of convenient size shall be used to receive the sample. All connections from the sample probe t6 the sample container must be free of leaks. The container shall be constructed in such a way that it retards evaporation loss and protects the sample from extraneous material such as rain, snow, dust, and trash. The construc tion should allow cleaning, interior inspection, and complete, mixing of the sample prior to removal. The container should be provided with a suitable vent. 24.3 Automatic Sampling Devices: 6 Rushton, J. H., and Hillestad, J. G., "Sampling of Nonhomogeneous Flow in Pipes," Preprint No. 52-64. Proceedings, American Petroleum Institute, PPT1A, Vol. 44, Section 3, 1964, pp. 517-534. END REAMED TO /X SHARP EOGE knsw* D i/ef-1/4" p ip e TO RECEIVER OR SAMPLER TO RECEIVER OR SAMPLER CA> (8) NOTE: PROBE MAY 8E FITTED WITH VALVES OR PLUG COCKS. PROSE MAY BE DISPOSED HORIZONTALLY OR VERTICALLY. PROBES FOR CONTINUOUS SAMPLING HOLES OR SLOTS FACING UPSTREAM 1/8"-1/4" PIPE FLUSH OR DRAIN SAMPLE RECEIVER (D) TYPICAL ASSEMBLY FOR CONTINUOUS SAMPLING FIG. 5 Probes for Continuous Sampling 784 DUP050296346 # E 300 Si I/8"(0.3I8''<TM> -- 3"(7.62 cm) 4 3I l/ "( .iecm)DIA. 40"01.6 cm) FIG. 6 Sampling Tube `1.3.1 Time Cycle (Nonproportional) Types--A sampler led and operated in such a manner that it transfers increments of liquid from the pipeline to the sample tainer at a uniform rate of one or more increments per Lute is a continuous sampler. 4.3.2 Intermittent Sampler--A sampler that is designed operated in such a manner that it transfers equal ments of liquid from a pipeline to the sample container i uniform rate of less than one increment per minute. 4.3.3 Flaw-Response (.Proportional) Type--A sampler t is designed and operated in such a manner that it will tomatically adjust the quantity of sample in proportion to rate of flow is a flow-response (proportional) sampler, `ustment ofthe quantity of sample may be made either by ying the frequency or transferring equal increments while 'ntaining a constant frequency of transferring the increents to the sample container. 24.4Procedure: 24.4.1Nonautomatic Sample--Adjust the valve or plug from the sampling probe so that a steady stream is n from the probe. Measure and record the rate of nple withdrawn as gallons per hours. Divert the sample am to the sampling container continuously or intermitly, to provide a quantity of sample that will be sufficient for analysis. Label the: sample and deliver it to the ratory in the container in which it was collected. 4.4.2 Automatic Sampling--Purge the sampler and the mpling lines immediately before the start of a sampling -ration. If the sampler design is such that complete Urging is not possible, circulate continuous stream from s probe past or through the sampler and back into the line, ithdraw the sample from the side stream through the utomatic sampler using the shortest possible connections, djust the sampler to deliver not less than 1 and not more an 40 gal of sample during the desired sampling period. time-cycle samplers, record the rate at which sample crements were taken per minute. For flow-reSponsive aplers, record the proportion of sample to total stream. 1 the samples and deliver them to the laboratory in the ontainers in which they were collected. No t e 15--For time-cycle samplers, deviations in quantity of the pie taken should not exceed 5 % of the average rate for a given !ng. For flow-responsive samplers the deviation in quantity ofsample per 42 000 gal of flowing stream should not exceed 5 % of the hosen average. 25. Tube Sampling 25.1 The tube sampling procedure is applicable for sam pling liquids in drums and cans. 25.2 Tube--Either Type 316L stainless steel or other material suitable for the particular liquid may be used. The tube should be designed so that it will reach to within about 'h in. (3 mm) of the bottom and have a capacity of approximately 1 pt (5 m) or 1 qt (9 m). A metal tube suitable for sampling 55-gal (208-m) drums is shown in Fig. 6. Two rings, attached to opposite sides of the tubes at the upper end, are convenient for holding it by slipping two fingers through the rings--thus leaving the thumb free to close the opening. An alternative tube sampling apparatus is shown in Fig. 7. This tube is also designed to reach within l/s in. ofthe bottom. 25.3 Procedurefor Drums: 25.3.1 Stand the drum upright and sample from the top. Ifthe drum does not have a top bung, place the drum on its side with the bung up. Thorough mechanical agitation of the drum prior to sampling will ensure that its contents are uniform. If detection of water, rust, or other insoluble contaminants is desired, let the drum remain in the sampling position long enough to permit the contaminants to collect 0,6cm ('/LI 0D STAINLESS STEEL ... FIG. 7 Alternative Tube Sampling Assembly 785 DUP050296347 E 300 at the top or bottom, and take a top and a bottom sample. Remove the bung and place it beside the bung hole with the wet side up. Close the upper end of the clean, dry sampling tube with the thumb, and lower the tube into the liquid for a depth of about 1 ft (304 mm). Remove the thumb, allowing the liquid to flow into the tube. Again close the upper end with the thumb and withdraw the tube. Rinse the tube with the liquid by holding it nearly horizontal and turning it so that the liquid comes in contact with that part ofthe inside surface which will be immersed when the sample is taken. Avoid handling any part of the tube that will be immersed in the liquid during the sampling operation. Discard the rinse liquid and allow the tube to drain. Insert the tube into the liquid again, holding the thumb against the upper end. (Ifan all-levels sample is desired, insert the tube with the upper end open.) When the tube reaches the bottom, remove the thumb and allow the tube to fill. Replace the thumb, withdraw the tube quickly, and transfer the contents to the sample container. Do not allow the hands to come in contact with any part of the sample. Close the sample container; replace and tighten the bung in the drum. Label the sample container and deliver it to the laboratory. 25.3.2 In using the alternative sampling device, the sample shall be pumped directly into the sample bottle by means of a double-valve aspirator bulb. Samples at various levels may be obtained by adjusting the depth of the tube in the drum or can. Before collecting the sample, thoroughly flush the device with the material being sampled. 25.4 Procedure for Cans--Obtain samples from cans of 5-gal (19-L) capacity or larger in the same manner as from drums (25.3.1) using a tube of proportionately smaller dimensions. For cans of less than 5-gal capacity, use the entire contents as the sample, choosing cans as prescribed by the selected sampling plan section or in accordance with agreement between the purchaser and the seller. 26. Jar Sampling 26.1 The jar sampling procedure is applicable for sam pling liquids where a free or open-discharge stream exists as in small filling and transfer pipelines (2 in. (51 mm) in diameter or less) and filling apparatus for bottles and cans. No t e 16--Jar sampling is particularly subject to contamination of the material being sampled. Great care should be exercised to be sure that foreign matter is not introduced into the sample from the air or surroundings. 26.1.1 Jar--Use a clean, dry, glass jar with screw cap. The cap should be lined with material inert to the sample. 26.1.2 Procedure--Insert ajar in the free-flowing stream so that a portion is collected from the full cross section of the stream. Appropriate safety measures should be observed. Take portions at time intervals chosen so that a complete sample proportional to the pumped quantity is collected. Samples collected may be analyzed individually or com posited to provide an average sample of the material pumped. SOLIDS 27. Scope 27.1 This practice covers equipment and procedures for sampling materials that are solids (see 28.1) at the time of sampling. The equipment and procedures that are descnh in these sections are intended to supplement the expert of the sampler as a guide in selecting methods ihut applicable to the material being sampled. 27.2Subjects covered in these sections appear in the urd shown in Table 4. 28. Description of Terms 28.1 solid--a state of matter in which the relative niotiL. of molecules is restricted and in which molecules tend tL retain a definite fixed position relative to each other. A soltijj may be said to have a definite shape and volume. 28.2 sampling--the process of extracting a small i....... of material from a larger bulk, so that it will be sufficient! representative of the bulk for the intended purpose. 1 28.3 lot--a discrete quantity of material. It may contau? >ci single batch or several batches, or be the products continuous process broken into units on the basis oftirr shipment. It is very desirable that individual batches in j Jo-j be specifically identified so that they may become individuaS or stratified units for inspection. t'ijjjjl 28.4 increments--portions of, material selected from var-,i ious parts of a lot, which may be tested individually o kJ composited and tested as a unit. . 28.5 gross sample--& composite prepared by mixing thpj increments. ' 28.6 subsample--a smaller sample produced in a sj fied manner by the reduction in volume or quantity of gross sample. 28.7 laboratory sample--that portion of the subsai which is sent to the laboratory for testing. 29. General Principles and Precautions 29.1 Every sample should be collected arid prepared strict accordance with a specified procedure. 29.2 Because of many variations in the conditions under! which solids must be sampled, and in the nature of thssjA material being sampled, it is essential that the samples be' "v collected by a trained and experienced sampler. Because of 1 variations in the manner of handling the solid, it is impos- l sible to specify rigid rules describing the-exact manner of j sample collection.. Correct sampling principles must be f applied to conditions as they are encountered. . 29.3 To be able to make probability, or, confidence ; statements about the property of a lot, the sampling proce- dure must allow for some element of randomness in selec tion because of the possible variations in, the quality of the TABLE 4 Summary ot Procedures for Sampling Solids Section Terminology General Principles and Precautions Sampling Equipment Hand Scoop Stream Sampling Cup Shovel Sampler Thief Samplers Soli Sample Auger Machine Samplers Application of Sampling Equipment Preparation of Reduction of Sample Laboratory Sample and Storage Precautions Labeling Sample Containers 28 29 30 30.1 30.2 30.3 30.4 30.5 30.6 31 32 33 34 786 DUP050296348  E 300 j. Generally, where segregation is known to exist, and variation of quality is not possible, the sampling be designed to allow for this. The sampler should ; be on the alert for possible biases arising from the use ticular sampling device or from unexpected segregajp the material. Generally, where sampling is to be Hi to the output of a given process on a continuous it will be desirable before adopting a particular ing plan, to undertake an extensive preliminary study pation in the material and possible biases in sampling Intents and methods of reduction. m The statistical principles governing the number and fion of the samples taken from packaged lots of solid ! are essentially those outined in Sections 6,7, and 8, atistical considerations. Whenever possible, nonpackaged, bulk materials Id be sampled while the material is in motion rather fin static piles, carloads, etc. Such occasions are fre|tly ideal for the application of falling-stream samplers. %6 Sampling of bulk solids from boxcars, barges, etc.,' duces additional problems because of possible |mformity in particle size, moisture, impurities, etc. The tical treatment is complex and beyond the scope of this ice. For a typical example, see Methods D 2234. and w ||7 All auger methods and all scoop methods used on jfrials not being loaded or transferred fail a prime pling requirement--that of random selection of the cles or portions selected as samples. Scoops and shovels Ijmited to use at or near the top surface. Augers and thiefs "normally inserted in a preset pattern. Consequently, cles on the bottoms or along certain sides of containers |r have an opportunity to be included in a sample. For Irogeneous or valuable material, this alone may furnish fclbnt reason to go to a falling-stream sampler. 3.8Because of the above factors, the recommended jfbedures that follow are limited to the mechanical operai of taking the required number of increments called for bother standard or in a purchase contract (1,2). [.9 The sampling equipment, sample preparation equip- , containers, etc., used in sampling must be clean, dry, bntammated, and inert to the material being sampled, l protection from heat, cold, light, loss or gain ofmoisture t be necessary. Sampling Equipment PO.I Hand Scoop, for sampling powders from containers l conveyors: pO.1.1 This implement is used for taking small equal tions at either random or regular intervals from the mass |i material to be sampled. It is most frequently used to iiple drums, bags, barrels, or other containers, but may o be used to take portions from a flowing stream, such as belt conveyor, in a chute, etc. [30.1.2 The scoop can be of any suitable size or shape, ' pending, in part, on the size and shape of the particles in |e material to be sampled and the quantity of sample mired. 30.1.3 A sample of a flowing stream should be taken by a single motion of the scoop in such a way as to take a complete cross section of the stream. The scoop should not overflow during this single motion. 30.1.4 Scoop sampling of static material consists of taking samples at or near the surface, and requires nearly perfect homogeneity, a condition that rarely exists for all character istics of the material. The larger particles, especially if they approach the size of the scoop, will frequently be rejected in the sample taking. 30.2 Stream Sampling Cup, for sampling powders from conveyors and chutes: 30.2.1 The cup is used for selecting samples from a flowing.stream, such as a conveyor, a chute, or a belt. 30.2.2 The size of the cup depends upon the diameter of the particle being sampled and the width of the stream of powder. The mouth width of the sampling cup should be at least three times the diameter of the largest particles being sampled. The mouth length ofthe cup should be sufficient to cut the entire stream of material as the material drops from a transfer belt. Figure 8 indicates a design of a suitable cup. 30.2.3 The cup is passed through the entire stream of material as it drops from a belt or a chute. The approximate discharge time should be predetermined in order to secure a minimum of ten alternating, and equally timed, spaced cuts. The cup should be passed through the entire stream in a uniform motion, at the predetermined intervals throughout the loading operation regardless of the size of the sample or number of passes required. The stream samples is not recommended normally for many materials unless a uniform continuous flow of materials is maintained for at least 3 min while the lot is sampled. 30.3 Shovel, for sampling large bulks: 30.3.1 A shovel is used for taking samples from larger bulk shipments such as freight cars, boats, and truck loads. It is most advantageous when material is being loaded or unloaded, or moved by shoveling. It suffers the same disadvantages as the hand scoop. 30.4 ThiefSamplers: 30.4.1 Split Tube Thief: 30.4.1.1 This instrument is essentially a tube, usually % in. (19 mm) in diameter, with a slot running the entire length 17 The boldface numbers in parentheses refer to the list of references appended [this practice. 787 1 .... DUP050296349  E 300 aw! ljjilffijpifoiif!r FIG. 9 Split Tube Thief FIG. 11 Single-Slot Tube Thief of the cylinder (Fig. 9). The end of the tube has a sharp, angled point. 30.4.1.2 The thief is inserted into the material far enough to reach the opposite side (or the bottom) of the container. The thief is then carefully withdrawn, and the increment is extruded into the sample container. 30.4.1.3 The split tube thief is especially suitable for sticky material, in which case the sample may need to be removed with a spatula or other suitable device. 30.4.2 Concentric Tube Thiefs: 30.4.2.1 This equipment is used for taking samples of free-flowing materials like grains from drums, cans, bags, and other containers. Two types are described. 30.4.2.2 Multi-Slot Tube Thief--This, apparatus consists of two tubes, one fitting snugly inside the other. One end of the outer tube is fitted with a point. Oblong holes about 5 by 1 in. (127 by 25 mm) apart are cut through the tubes in corresponding positions. The holes are opened or closed by rotating the inner tube (Fig. 10). 30.4.2.3 The thief is inserted in the material with the inner tube holes closed. The inner tube is rotated to an open position to extract a sample of the material and in a closed position before the thief is withdrawn from the container. 30.4.2.4 Single-Slot Tube Thief--This apparatus consists of two tubes fitting snugly into each other. The inner tube has a slot running lengthwise and has a pointed end. The outer tube slides over the inner one to expose or cover the slot (Fig. 11). 30.4.2.5 The sample thief is closed so that the lower end of the outer tube rests on the shoulder at the bottom of the inner tube, and the inner tube is locked in position with the thumb screw. The sample thief is then pushed into the material diagonally or horizontally, as applicable. The outer tube is then unlocked and raised a few inches to expose the slot of the inner tube to the material. The slot is facing upward. The drum is shaken orjarred to cause the powder to enter the thief at the level of the slot opening. The container is shaken while the sample thief is opened progressively to allow material from all levels i;o enter the thief. After the sample is in the inner tube, the outer tube should be pushed down to its original position. The thief is then removed from the material and inverted so that the sample drops into the sample bottle through the open end. It may be necessary to rap the thief sharply in order to dislodge the powder. 30.4.2.6 These concentric tube samplers have limited applicability. Material that is not free-flowing or is hard- F1G. 12 Grain Probe packed is excluded, thus usually eliminating fme powL. On the other hand, the sampling of material contain granules or particles exceeding one third of the slot wjJL should not be attempted, or bridging and resulting 'anew favor of the small particles may result. Because of" ' pointed ends, these devices cannot sample the bottoms t. containers. If material has been vertically segregated horizontal strata through vibration, or any other reason lowest strata will be inadequately represented. These prif lems are common to both tubes. 30.4.3 Compartmental Thiefs {Triers): 30.4.3.1 This equipment is used for taking sanq free-flowing materials like fertilizers, grain, and other ] ders from bags, drums, cans, piles, carloads, and bins, types are described. 30.4.3.2 Grain Probe--This apparatus consists of tubes, one fitting snugly inside the other. One end of outer tube may be tapered or fitted with an auger point trier is.63-in. (1600-mm) long, with an outside diameter4 1% in. (34.9 mm); an inside diameter of IVs in. (28.5 with eleven compartments 3Vi-in. (88.9-mm) long; separa by 1%-in. (34.9-mm) long plugs (Fig. 12). The outer tut consists of slots that correspond to the compartments ofthe( inner tube. The outer tube slides over the inner tube. 30.4.3.3 The trier shall be inserted into the mater vertically and should not be pointed toward the center ofthc| load. Open the tube with the slots facing-upward, then closgl the tube, and withdraw the sample. The sample shall be: discharged into a receiver as long as the sampling tube. 30.4.3.4 Missouri Trier--This apparatus consists- of I tubes, one fitting snugly inside the other. The trier is anj interrupted core-compartmental double tube. The trier is? 59-in. (1498-mm) long, with an outside diameter of 1V4 in. (28 mm), an inside diameter of % in. (22 mm), and with: eight compartments 3 in. (76 mm) in size. The outer tube consists of slots that correspond to the compartments of the inner tube. The trier operates in the same fashion as the grain probe. The trier shall be inserted as specified in 30.4.3.3. The slot width shall be at least three times the diameter of the largest particles to be sampled (Fig. 13). FIG. 10 Multi-Slot Tube Thief 788 DUP050296350 # E 300 FIG. 13 Missouri Trier 4.3.5 It has been found that these triers secured samliat were closely comparable and most nearly represen- of the material being sampled. These triers have the Incy to secure samples that are biased to varying degrees jeering more of the smaller size particles and less of the ' particles fraction. The triers are at the present time > used by the fertilizer industry (3). |4.3.6 Because of the close clearances, double-tube i and triers will impart a grinding action to the material ; sampled. Soft granules are affected by such action, and j should not be used for such material ifproduct sizing is Jrtant. f'5 Soil Sample Auger, for sampling compact materials: 1:5.1 This is a screw-dr-worm-type instrument useful for j samples of compacted materials (Fig. 14). 1^.2 The auger is turned into the material and then M straight out. The sampie is removed from the auger It , a spatula or other suitable device. The process is gated at different locations as dictated by the sampling 1.6 Machine Samplers, for sampling powders from Con ors, bins, and containers: Jl.6.1 Vacuum Probe Samplers, for large bulk containers: Bj.6.1.1 This equipment can be used for extracting large Iples from freight cars, barges, bins, boats, and truckloads, flonly where air exposure does not affect significant |perties of the material, such as moisture content. This of sampler develops bias, if sizing is important. It erentially selects fines. 10.6.1.2 The apparatus (Fig. 15) consists of a combination one separator and motor driven blower, a probe and nection tubing (4). 1.6.1.3 This equipment works the same way as a vacuum bier does. The probe burrows its way into the material sampled and sucks the material into the sample lector. FIG. 15 Vacuum Sampler 30.6.2 In general, augering probably offers the best com bination of economy, penetration ability, and sample repre sentation, if the material is packaged in drums or similarly sized containers that are to be moved or transhipped without dumping. Although there are many designs, augers fell into the two general categories of open and enclosed augers. 30.6.3 Powered Open Auger--One of the most useful varieties of the open type is a ship auger about l3/i-in. (30.16-mm) diameter, powered by a hand-operated 3A-in. (19.05-mm) drill. The augering is performed through a hole in a catch pan that collects the sample brought to the top. Contents of the pan are then dumped into a' sample container. Open augering may not give good vertical repre sentation of the container because material at the top may be preferentially removed at the expense of the lower layers. Since many materials are frequently segregated vertically, a biased sample may result. 30.6.4 Enclosed Auger: 30.6.4.1 Enclosed augers may either be the ship-auger type or have a central shaft with one or more flights. In either case, it will be surrounded by a sharpened cylindrical sheath which does not rotate. Material removed in drilling may be discharged through a side hose at the top, or it may be stored in the sheath for discharge by reversing the auger after withdrawal from the drum. 30.6.4.2 Because ofthe power required for the penetration drive and withdrawal, as well as the rotary motion, a fixed, permanent installation is required for an enclosed auger. Therefore, it is applicable only when a large number of similar drums or containers are to be sampled over a long period of time. An enclosed auger Will obtain much im proved vertical representation over an open auger, although it is also deficient in sampling the bottom 1 to 2 in. (25 to 51 mm) of a container. 30.6.5 Gravity-Flow Auger Sampler (4): 30.6.5.1 The equipment is designed for use in conveyor pipes, spouts, or hopper bottoms where material flows bygravity. It is suitable and very convenient for sampling products of nearly perfect homogeneity (Fig. 16). 30.6.5.2 The gravity-flow auger sampler works on the principle of rotating a slotted sample collection tube in a 789 DUP050296351 E 300 FIG. 17 Falling-Stream Samplers FIG. 16 Gravity-Flow Auger Sampler flowing mass. The material captured in the sample tube is augered out of the tube by an internal worm screw. A solenoid switch actuate the motor-driven auger at preset intervals and simultaneously engages a clutch to rotate the auger tube. The combination of auger pitch and rotation must be such as to remove the collected material to a collection chute before the sample can fall out on the opposite side through the more slowly rotating slot. 30.6.5.3 This sampling device has the advantages of relative simplicity and little occupied space. Another varia tion of this design is one in which the open slot is always upward and does not rotate, in which case the rotating auger must carry away the collected sample before bridging or overfilling can occur. For both designs, slot width and length, auger pitch and variation of pitch along axis, rotational speeds, flow rate of the bulk mass, and the amount ofsample required must all be properly matched for accurate sampling. The disadvantage is that such a device cuts only part of the stream part of the time. Therefore, ifthe flowing stream is at all segregated in its cross section, a nonrepresentative sample will result unless all segregated layers are proportionately cut (4). 30.6.6 Falling-Stream Samples: 30.6.6.1 The most reliable method of removing a sample from a bulk mass employs a* falling-stream system where a moving cutter removes all of the falling stream part of the time. Such cutters fall into the two general categories of arc-path and straight-path samplers. Slot widths of the cutter should be at least three times the diameter of the largest particles to be sampled; four times or more is preferable. Obviously, the speed of travel through the stream is one control of the sample size collected, but the speed of the cutter should not be so great as to knock the particles away (Fig. 17). 30.6.6.2 Arc-Path Samples--The most popular and prob ably the best performer of the arc-path samplers is the Vezin-type shown in the left half of Fig. 17. The material falls from a belt or vibratory feeder or is fed through a chute as a vertically falling stream that is cut by the radially rotating oriented slots, of the cutter. Such a device will have ' one the to usually slots falls not more than four slots. Material into the sample chute while the cboulllekcotefdthbey""i! material falls by into the reject stream. Mechanically, the Vezin sampler has the advantage of simple rotary motie^i but it will not cut equal percentage from all parts of a stref "!! ifthe slot sides are not perfect radii. The quantity of samj collected is controlled by slot width, number of frequency of the slots passing through the stream (rotational velocity), and the rate of stream flow. 13$ 30.6.6.3 Straight-Path Samplers--With a straight-path sampler, the bulk material falls from a moving belt or otheF feeder, in a vertical stream through which passes a rectan gular slot as shown in the right half of Fig 17. Sample collected is usually diverted through an angled chute into a sample receptacle, and the gross reject material falls directly downward. The amount of sample collected is controlled by feed rate, slot width, cutter speed, and frequency. 1 hi sampler cuts every part of any shaped stream proportion* ately, and is potentially the most accurate type. Many variations occur in slot design and orientation and in the drive mechanism. The common Geary-Jennings type has s~, drive in which the cutter carriage is actuated by a heavy, motor-driven screw. ,0 30.6.6.4 The. cross-cut sampler is a specific model of ai straight-path sampler intended for installation in a spout ori chute as shown in Fig. 18 (4). Because .of the limiting enclosure, the-material sampled must be free-flowing. The apparatus consists of an air-actuated head in a box, a control box, and an airline connection. Collected sample is dis charged through a flexible tube at the bottom of the sampler. 31. Example of the Application of Sampling Equipment 31.1 ThiefSamplingfrom a Container (5): 31.1.1 Remove a thief sample from each of the shipping containers selected for sampling in accordance with Section 5 on statistical considerations. 31.1.2 Nearly all containers are filled in such a way that segregation occurs in the filling. For example, the large or heavier particles roll to the outside and the small, or light particles remain under the pouring spout where they fall. Additional segregation will probably result from the vibra tion of shipping. Therefore, sampling patterns are devised so that samples are taken in locations to represent as accurately as possible the segregated layers or regions. Cylindrical containers, or structures such as solidified metal pours, will 790 DUP0502 96352 300 FIG. 19 Location of Sampling Points from the Exposed Surface of the Car FIG. 18 Cross-Cut Sampler aonly exhibit radial segregation and occasionally ansegregation (variation is observed along the circular i around the center). Sampling positions are calculated so ||o represent annular rings of constant volume in pro wling from the center to the periphery. Angular or aped segments would be preferred but are usually practical. |1.1.3 Except where a definite sampling pattern as previly described is to be followed, the sample equipment Juld usually be inserted diagonally into the container (3). 1.1.4 Individual samples from a single container may be jpposited if necessary to obtain a sample of adequate size jthat container. fa.2 Machine Samplingfrom a Flowing Stream:. pj 1.2.1 Sampling a material in motion, especially in a ^felling stream, is the preferred method for obtaining the ost representative sample; 51.2.2 Arc-path or straight path samplers may be compted to give a series of two or more stages of sampling. In design and operation of such a system, care must be ken to avoid air flows for dust collection, etc., which might > the sample. |31.2.3 If operations are short term so as not to justify illation of a complete falling-stream system, the felling earn sampling may be attempted manually. The place ould be accessible and safe for the person taking the nple. A scoop or slot (see 30.2) with parallel sides should s swept through the stream at a steady but sufficiently rapid :,so that it does not overfill on one pass, Passes should be tied and made at exactly regular intervals. Sampling under andola cars is particularly difficult and should be replaced |ith sampling from a conveyor belt if possible. 31.3 Auger ofShovel Samplingfrom Cars, Ships, Barges, 31.3.1 The following is a typical example of the top upling of an open railroad car. For a more detailed cussion and other procedures, please refer to the general iterature. 31.3.2 Superimpose an imaginary grid above the material, and take samples at the intersections (Fig. 19), preferably by auger or thiefif practical, or by digging a series of holes (pick and shovel) below the surface of the material before any portion of the contents has been removed. 31.3.3 Collect and identify the individual increments. 31.4 Pattern Sampling ofBulk Material: 31.4.1 Pattern sampling was developed to prevent bias in sampling of material in bulk form. This method of sampling takes into consideration the variation of particle size and composition around the loading point (3), for a particular type of loading. 31.4.2 The core locations of sampling patterns shall be as follows: 1 and 2 within 15 in. (381 mm) of loading point; 3, 4, 5, 6, midway between loading point and side or end; and 7, 8,9, and 10 within 18 in. (457 mm) of comers and aimed toward bottom center (Fig. 20). The sampling device shall be inserted vertically in all locations. 32. Preparation and Reduction of Sample 32.1 Appearance--Visual inspection of the sample is recommended to determine if the material contains gross contamination, or if it is equal to the standard. It may show if the material has picked up excessive moisture, or if further laboratory processing is required to reduce the material to a" more uniform particle size. Unusual appearance should terminate further testing until another sample is. obtained, and the cause for the abnormality has been_established. 32.2 Screening--If extraneous matter is detected, a deci sion must be made, as to whether it belongs in the sample. Tools, gloves, etc., are obviously misplaced. Dirt or other contamination may actually be in the lot and properly belong, in its proportionate part, in the sample. A careful consideration of each individual case must be made, Jo determine if the contaminant should be removed by passing the sample through an appropriate screen. FIG. 20 Pattern Sampling 791 DUP050296353 E300 32.3 Grinding--Coarse or nonuniform samples may re quire grinding in a mortar, a mill, or other suitable mechan ical devices to obtain a more uniform sample. The entire sample may be subjected to grinding; or it may be more efficient to screen offthe oversize, grind it, and then blend all portions together. 32.4 Minimum Sample Size--Where analysis of a com posite sample is specified or permitted, individual sample increments are combined and reduced. Many gross samples are unsuitable for laboratory handling or analysis, because they may be too heterogeneous or too large for the analyst to obtain good representation with his small sample. For every bulk solid, with its particular size distribution, there is a minimum amount of material which must be taken in the sampling operation in order for the sample to adequately represent the solid. This minimum quantity is called the minimum sample size, and the goal of any sample prepara tion is to make this minimum sample size at least as small as the smallest quantity that will be taken for any single analysis. Although a thorough discussion of minimum sample size is beyond the scope'of this practice, an excellent presentation by Benedetti-Pichler may be found in Ref. (6). 32.5 Sample Preparation Scheme--In general, a sample preparation scheme will consist of particle size reduction, blending, splitting, and a repeat of this series of operations until the desired minimum sample size is attained. It is difficult to write a general scheme for the reduction of a sample for all types of material because of the nature of the material and the purpose qf the sample. It is important, however, that any splitting operation be immediately pre ceded by blending. Two standard operations are given by the following procedures: 32.5.1 Cone-and-Quarter Method--Dump the individual increments onto a clean canvas, and shovel into a pile, placing each shovelful on top of the pile. Flatten the apex of the cone with a shovel or a board until it is about one fourth its original height. Divide the pile into four equal parts by drawing a board twice through the center of the pile, making right-angle cuts. Discard the opposite quarters; chosen at random, and combine the remaining quarters into a coneshaped pile. Repeat the above operation until the desired quantity of sample is obtained. Place the final sample on a clean canvas, and mix by alternately raising opposite comers of the canvas. 32.5.2 Sample Splitter or Riffle: 32.5.2.1 The sample splitter or riffle (Fig. 21) should be FIG. 21 Riffle Sampler constructed of a material suitable for use with material under test. It consists of a series of chutes that are directed alternately to opposite sides. The slot width should be at least three or more times the diameter of the largest particle to be passed through to prevent bridging and, therefore, biased splitting. 32.5.2.2 Pass the composite or gross sample through the riffle to divide it into two approximately equal portions. Pass one of these portions, selected at random again through the riffle. Continue this operation until the sample size ir reduced to either that required or the minimum sample size beyond which additional grinding is necessary. 32.6 Blending--Sample homogeneity must be assured by thorough blending prior to analysis. This operation should be performed on all samples in such a way that they will not be changed because of light sensitivity, hygroscopicity, etc. No sample container should be filled more than approxi mately half full, and no container should be opened for sample removal until it has been tumbled on a mechanical blender designed for the purpose or rotated by hand, end over end, at least 25 revolutions. On any sample, blending should be done after screening or grinding, or both. 33. Final Laboratory Sample and Storage Precautions 33.1 At least four times as much reduced sample should be prepared as is required for one laboratory to perform a complete analysis. Retain one portion of the well-blended sample for the manufacturer or seller, one for the purchaser, one for the umpire, if necessary, and one reserve to replace5 breakage or loss. 33.2 Samples that are to be stored over long periods, that may be affected by atmospheric exposure, or that may become seriously contaminated in contact with paper or cardboard should be packaged in widemouth, home-canning type mason jars having two-piece, metal caps. Best results are obtained ifthe sample is compatible, by vacuum sealing such bottles (5). Widemouth, serewcapped glass jars with caps and liners of suitable inert material are generally satisfactory. 33.3 For materials in which water content is important Or composition is subject to change upon atmospheric expo sure, plastic containers are generally unsuitable because of their permeability. In other cases, tight, leakproof paper sample envelopes or cardboard cartons with or without plastic liners or coatings, or even tin cans, may be used to hold samples. 33.4 Where corrosion or atmospheric exposure cause problems it is usually better to use widemouth glass jars with suitable screw caps and liners (see 33.2). 34. Labeling Sample Containers 34.1 Label the container immediately after a sample is obtained. Use waterproof and oil-proof ink or pencil hard enough to dent the tag, since soft pencil and ordinary ink markings are subject to obliteration from moisture, oils smearing, and handling. If gummed labels are used, they should be further secured with transparent sealing tape. Sufficient detail should be written on the label to completely identify the sample. The following information is frequently desired: 34.1.1 Date and time. 34.1.2 Name of supplier. 792 HSPI mi DUP050296354 E 300 |,3 Name or number and owner of the vessel, car, or ner. 1.4 Brand name, grade of material, and code number. 1.5 Reference symbol and necessary identification Hr. SLURRY SAMPLING ope This practice describes equipment and procedures apling materials which are slurries at the time of ling. A slurry is considered to be a suspension of solid Jes in a liquid which can be separated by filtration or ftentation (does not include emulsions). The equipment |procedures that are described in this practice are led to supplement the experience of the sampler and to fas a guide in selecting methods that are applicable to fjiaterial being sampled. eneral Principles and Precautions :.l Quite often the value or quality of material being in the sample is related to particle size. When this is se, any segregation of the particles tends to affect these s. Liquids that carry solid particles must have a certain tty to keep the solids in suspension. To overcome the liem of segregation of materials by size or weight requires fication of certain fundamentals of good sampling prac|The slurry should be stirred rapidly before sampling to ~ : uniform distribution of the solids. 1.2 At the time the sample is taken, all particles should Ihiformly distributed throughout the liquid carrier. This |help to obtain a uniform sample. 1.3 The sampling of slurries with any degree of accuracy |ite difficult. This is particularly true when sampling a (tally static system such as storage tank or vat. Arrarige1 must be made to agitate thoroughly the content of such ge units prior to sampling. The most desirable and enient place to sample a slurry is from a pipeline as the al moves through the line. Even here it is difficult to an accurate sample, because slurries subjected to ing will tend to change in composition due to the loss of Squid. Fittings, bends, and other constructions in the line friend to create nonuniformity in solids content. Lines are smaller than 1 in. in diameter are usually not jable for handling slurries because of frequent plugging, use of a continuous running sample line provided with brifice to reduce slurry velocity seems quite satisfactory. '5.4 Ifonly a portion of any slurry sample can be.used for ilysis, the sample should be shaken and a portion dumped Attempts to pour out a predetermined volume are sfactory because the solids have time to separate ng the pouring. 5 Slurry solids should be washed only with the filtrate, > it has been proven that the proposed wash liquid does : dissolve out any fraction of the solids. Large errors can atroduced by washing out soluble fractions of a slurry. 86.6 Sampling practice adhering to above techniques will |duce a reliable sample. The sample is accepted as resenting the entire stream at the time it was taken. The frequently the subsamples are taken, the more accuely will the sample represent the total stream. 37. Continuous Sampling 37.1 Sample Cutter of a Slurry Stream--Continuous samples are taken at various locations in'the plant by a properly designed sample cutter. The opening in the cutter should be sufficiently large that collision of particles will not restrict their entrance into the cutter. The cutter should hold all of the sample without overflowing, and should move completely through the stream at a uniform speed. 37.2 Stationary Sampling Probe, Horizontal Pipe: 37.2.1 A continuous sample may also be taken in pipes by a stationary sampling probe which should be located at 20 pipe diameters (PD) and preferably 40 PD or more down stream from any elbow, valve, or other fitting. 37.2.2 The probe opening should be placed at the center of the cross-section of the pipe and pointed precisely upstream. 37.2.3 The sample should be withdrawn at a rate such that the velocity of flow (feet per second) through the probes opening is equal to the centerline velocity (isokinetic). However, for practical purposes, the sample can be with drawn at 1.2 multiplied by the average velocity of flow. 37.2.4 The average concentration in the pipe is calculated by dividing the composition of the sample by a value V (determined from Fig. 22). 37.2.5 Openings flush with the pipe wall, elbow wall, (Fig. 23) or pump wall do not yield reproducible results for systems that are difficult to suspend. Such systems are those whose settling ratios, S, are above 1.0 (S is the ratio of bottom to top concentration in a settling device). For systems whose settling ratios, S are below 1.0, and whose concentration gradient, -m is less than 0.1, a side-wall tap will give satisfactory results (8). 37.2.6 Use of a circular port probe under the conditions described in the preceding paragraphs, (see 37.2.1 through 37.2.4) will result in samples whose reproducible average will _ be within 8 % of a stream composition for a wide variety of systems and within 2 % for a large majority of suspensions likely to be encountered in petroleum operations .(8), ... 37.3 Sampling in a vertical pipe, upward flow, pipe precisely vertical. 37.3.1 The sampleprobe opening must be pointed down ward, precisely vertical, and at least 3 PD above any.elbow or fitting. 37.3.2 The probe opening should be placed at the center of the pipe cross-section. Sample divided by K equals average isokinetic sam pling at center only, isokinetic velocity is used as 1.2 limes average velocity. FIG. 22 Average Concentration from Sample Concentration 793 DUP050296355 # E 300 ELBOW c ir c u l ar po r t PITOT TAP IX ELBOW 45' OPENING TAP IN SIDE p ipe FIG. 23 Sampling Probes and Taps 37.3.3 The sample should be withdrawn at a rate su<fi that the velocity of flow through the probe opening is equal to the centerline velocity of the flouring stream. It is satisfactory to calculate centerline velocity as 1.2 multiplied by the average velocity of flow. 37.3.4 Use of a circular probe under the conditions described in 37.3.1 through 37.3.3 will result in samples that will equal the average composition within 0.05 absolute volume percent. It is not necessary to use an adjustment factor as is the case for the condition described in 37.2.4 for the horizontal pipe (8). 37.3.5 The withdrawal probe, used as recommended, will give a sample that can be accurately related to the average composition that flows through the pipe, and deviations in position and withdrawal velocity will result in a change of sample composition. Such changes are primarily the result of the settling rate of the dispersed phase, the rate of withdrawal of the sample, and the rate of flow in the pipe. 37.4 In order to reduce the volume of this continuous primary sample so that the amount of material is correct for the analysis, the primary sample is reduced in size by an automatic sampler to provide an increment sample. This increment is discharged into , a small agitator to keep the solids in suspension until the sample is analyzed (7). No t e 17--The isokinetic sampling (where the linear velocity through the opening of the sampling probe is equal to the linear velocity in the pipe in front of the opening) is recommended for.sampling in both vertical and horizontal pipes. Nonisokinetic sampling can be done with equally accurate results, but a knowledge of concentration gradient (which is a function of settling velocity, pipe size, and rate of flow) is necessary so that the ratio between sample composition and average pipeline composition can be determined. To this end, a method has been found and partially developed whereby a settling ratio can be determined by a static test, and thisln turn related to the distribution of solids, or the concentration gradient, from top to bottom of horizontal pipe cross-section. 38. Sampling of a Slurry in Tanks, Tank Cars, Drums, and Other Storage Containers 38.1 Mixing--Mix the full tank containing the slurry for 1 h by using mechanical agitation with a four-arm and a rake-bottom sweep agitator moving at 4 rpm, so that the slurry is thoroughly uniform. Stop the mixing and take the samples immediately while the contents of the tank are still in motion. 38.2 Sampling: 38.2.1 The sampling bottle is a 32-oz (1000-mL) weighted bottle attached to a chain and a stopper with an attached chain (see Fig. 24). Alt HMffboU -th)14 Uloht Air tilt 3 ii Flvtdhtekt tali Stolalns rl iccUt'"' i) FIG. 24 Missouri and Indiana Weighted Restricted-Fill Fluid Fertilizer Sampling Bottles Designed to Fill While Being Lowered (and Raised) in Storage Tanks 38.2.2 Sample bottles are three 32-oz (1000-mL) widemouth polyethylene jars with proper seals, labeled 1, 2, and 3. 38.2.3 Fill each numbered 32-oz (1000-mL) sample bottle, one third full from the sampling jar (see Fig. 24) in the ' numerical order of 1, 2, and 3. 38.2.4 Refill the sampling jar and fill the sample bottles about two thirds full in the numerical order of 2, 3, and 1. 38.2.5 Fill the sampling jar and fill the sample bottle within about 2 in. (51 mm) of the top in the numerical order of 3, 1, and 2. 38.2.6 Determine the temperature of the slurry to th$ji|| closest 1C during the final sampling step. 38.2.7 Take the three sample battles to the laboratory^! wash them, wipe the lips and seals clean and dry, and reseaU \ 38.2.8 Seal the sample kept as a retainer with a new cap, and then further seal by a plastic wrap, covering the entire" cover. 38.2.9 Drop the weighted stoppered sampling bottle into the slurry to a depth well under the surface and well away from the side of the tank near the center point if practical. Pull the stopper, allow the bottle to fill, and then pull to the surface. Initially, run other location checks to determine uniformity of the slurry. 39. Settling Rate Test (8) 39.1 The settling rate test will distinguish between those suspensions which are easy or difficult to suspend and, consequently, those which are easy or difficult to sample. A suspension can be withdrawn from a flowing stream and used in the test. Low values of the settling ratio means that the suspension is insensitive to the method and rate of sampling, whereas high values show that the recommenda tions given above must be adhered to. 794 DUP0502 96356 E 300 insistency of Slurry Suspensions (9) Scope--The method is applicable to aqueous slurry fusions containing 0 to 1,1 to 4,4 to 15, and 15 to 25% solids. Slurry consistency of more proper "concen|ft" is defined as the weight of oven-dry solids in 100 g of lurry. E2 Apparatus: 1.2.1 Sampling Cup of about 200-mL capacity with a pit approximately equal to its diameter and with a %th lip. If the slurry to be sampled is to be taken from a pe where it is being well mixed, it is preferable to use a sampling cup or jug having a capacity of about 1 L. |,2.2 Beakers, 600 to 1500-mL, fared to the nearest 0.1 9.2.3 Containers--A 10-L (3-gal) bucket and a 40-L |iner, both tared. f.2.4 Mixing Device, for the 10 and 40-L containers, brably a portable electric stirrer. (.2.5 Balances, 40-kg capacity, accurate to 50 g, a 2-kg ;ity accurate to 0.1 g. I.2.6 Buchner Funnel and Flask, 150-mm. J. 2.7 Filter Paper, 150-trnn diameter, coarse texture. 0.2.8 Drier or Steam Cylinder, with wire mesh cover, |e enough to accommodate 15-cm filter papers, controlled fin a range from 110 to 150C (230 to 302<>F). 9.2.9 Laboratory Drying Oven with Balance, oven mainled at 105 3C, the balance having a capacity ofat least 1 and accurate to 0.01 g. 9.3 Sampling--Take the sample at the point of where ^sample is uniform and in such a 'manner as to be esentative of the solid water mixture. 1.4 Procedure: 9.4.1 Mixtures Containing Less Than 1 % ofSolids: 0.4.1.1 Use the sampling cup to withdraw five represenye portions of approximately 100 g each. Each time, iosit the entire contents in the tared 600-mL beaker; lefully dry the outside of the beaker and weigh it and its |tents to the nearest 0.1 g to determine the net weight of ^specimen. 9.4.1.2 Place a tared filter paper in the Buchner funnel, listen with water, then apply suction to the flask and filter ; slurry. Remove the resulting pad and filter paper and |t on the dryer until it ceases to steam. Place the paper and ion the weighing pan of the laboratory oven balance and Ske successive measurements after additional drying until instant weight is obtained. Weigft to the nearest 0;0i g. tO.4.1.3 The percentage consistency concentration of the nple is then: l(w -f)/g] x too where: w = weight of the moisture-free mat and filter paper, g, / = weight of the moisture-free filter papet, g, and g = net weight of the original sample in the 600-mL beaker, g- No t e 18--After removing filter paper and pad from Buchner funnel, be sure all solids are wiped clean from the inside surface of the funnel and deposited onto the pad This can be done with the finger. No t e 19--Drying can be sped up if the pad is pressed between blotters in. a hydraulic press before drying. No t e 20--If the pad tends to stick to the cylinder, place the pad between dry blotters. The surface of the cylinder may be treated with a silicone spray or TFE-fluorocarbon to prevent sticking. 40.4.2 Mixtures Containing 1 to 4% Solids: 40.4.2.1 Use the sampling cup to withdraw ten consecu tive representative portions of solids slurry; fill the cup each time and empty the entire contents into the tared 1500-mL beaker. Weigh the contents to the nearest 0.5 g and deter mine the weight of the specimen. 40.4.2.2 Deposit the specimen into the tared 10-L bucket and dilute to 0.5 % consistency concentration or less, using some of the water to rinse all the solids from the beaker. Weigh and determine the net weight of the contents to the nearest 10 g. 40.4.2.3 Determine the percentage consistency concentra tion of the stock in the bucket as in 40.4.2, stirring the stock vigorously with the sampling cup before withdrawing a portion. The percentage consistency of the original sample is then px(W/w) where: p = percentage consistency concentration of the diluted stock, W = net weight of the contents of the bucket, g and w = weight of specimen, g. 40.4.3 Mixtures Containing 4 to 15% Solids: 40.4.3.1 With the sampling cup, withdraw ten consecutive portions of solids slurry, filling the cup approximately half full each time and emptying the contents into the tared 1500-mL beaker. Weigh the beaker and its contents to the nearest 0.5 g and determine the weight of theSpecimen. 40.4.3.2 Deposit the specimen into the tared 40-L con tainer and dilute to less than 0.5 % consistency using some of the water to rinse all the solids into the beaker. Insert and adjust the electric mixer for thorough agitation of the suspension. 40.4.3.3 Proceed as in 40.4.2. 40.4.4 For mixtures containing 15 to 25 % solids, proceed as in 40.4.3, except instead of ten, take five representative portions of the original stock of approximately 100 g each. REFERENCES I) Duncan, A. J. "Bulk Sampling: Problems and Lines of Attack," I Technometrics, TCMTA, Vol 4, No. 3, August, 1962, p. 319. I) Bicking, C. A. "The Sampling of Bulk Materials," Materials 1 Research and Standards, MTRSA, Vol 7, No. 3, March, 1967, p. | 95. |) Cehrke, C. W,, Baker, W. L., Krause, G. F. and Russell, C. H., i "Sampling of Bulk Fertilizers," Journal of the Association of I Official Analytical Chemists, JANCA, Vol 50, April, 1967. (4) Available from Automated Sampling Systems, P. O. Box 2706, Des Moines, IA 50315, (5) Jones, R. J., Ed., "Selected Measurement Methods for Plutonium and Uranium in the Nuclear Fuel Cycle," Division of Technical Information, U. S. Atomic Energy Commission, 1963, pp. 49-50. (6) Berl, W. G., Ed., Physical Methods in Chemical Analysis, Aca demic Press, Inc., New York, 1956, Vol 3, pp. 183-201. DUP050296357 (7) Cook, P. E., "Continuous Sampling for X-Ray Analysis," Denver Equipment Co., (Bulletin No. S1-B12) 1400 17th St., Denver, CO 80217. (8) Rushton, J. H. and Hillestad, J. G., "Sampling of Nonhomogeneous Flow in Pipes," Paper for Presentation to a session on General Engineering during the 29th Midyear Meeting of the American Petroleum Institute Division of Refming in CfiS3 Plaza Hotel, St. Louis, MO, May 13, 1964. (9) "Consistency (Concentration) of Pulp Suspensions," T~2401 TAPPI Standard 360, Technical Association of Pulp . Industry. One Dunwood Park, Atlanta, GA 30341. (10) Penberthy, Division of Houdaille Industries, Inc,, P, O, Birc Prophetstown, IL 61277. -'4Rr ANNEX (Mandatory Information) Al. DETERMINATION OF THE BASIC VARIANCES FROM AN INITIAL PILOT STUDY OF THE" MANUFACTURING PROCESS Al.l Introduction A 1.1.1 The procedures of this practice assume that the manufacturing process turns out material in batches and that there is variation within batches and between batches. It also assumes that the variation within batches and the variation between batches are both random. Furthermore, it assumes that the variance ofthe within-batch variation is the same for all hatches and the variance of the between-batch variation is constant over time. A preliminary step, therefore, is to determine whether these hypotheses are acceptable for a given process. If they are accepted, then the next step is to estimate the within-batch and between-batch variances. If the hypotheses are rejected, the next step is either (a) to make engineering changes in the process that will lead to the hypotheses becoming valid or (b) to find a more sophisti cated model for describing the process. A1.2 Determination of Randomness of Within-Batch and Between-Batch Variation A1.2.1 Step 1--Take 2 "increments of material" at ran dom for each of 25 consecutive batches produced by the given process. If the material comes in packaged form, the 2 increments of material could be 2 randomly selected pack ages. If it comes in bulk form, the 2 increments could be 2 "shovel fulls" or the like. For packaged material this is piled in order, the 2 packages should be selected by the use of random numbers. Material that comes in bulk is probably best sampled as it is moved, on a conveyor belt or otherwise, and the increments should* then be selected at random intervals of time, random numbers again being employed. In the latter case, the precise nature of the sampling instrument (shovel, etc.) must be specified and also the size of the increment it selects. A 1.2.2 Step 2--Prepare for laboratory testing each of the 50 increments taken as called for in Step 1 and make a single measurement on each under as uniform conditions as possible (same laboratory, same analyst, same day, if pos sible). A 1.2.3 Step 3--Prepare 3 control charts for the 50 mea surements called for above.8 These should be: (7) A range chart for the 2 increments from each batch, * See any standard book on control charts, for example, Duncan, A. J., Quality Control and Industrial Statistics, or Grant, E. L,, Statistical Quality Control. (2) A chart ofthe means of the 2 tests made on each and (5) A moving range chart of the batch means. A 1.2.4 Step 4--If there is no point above the upper on Chart (/) and no run of 7 or more points above or hi] the center line or other evidence of nonrandom variatill accept the hypothesis that the basic within-batch variah is random with the same variance. Al.2.5 Step 5--If on Chart (2) there is no trend, no iu of 7 or longer above the average or no other evidence'1 nonrandom variation and also if on Chart (3) there is' point above the upper control limit or no run of 7 or above the center line or other evidence of nonvu variation, then accept the hypothesis that the variation batch to batch is random with constant variance. A 1.2.6 If the process passes all of the above tests wi exception, the data can be used without modificati measure the basic variances as described in A 1.3. exceptions occur, a statistician should be consulted what information about basic variances may be obtain! from the data and just how this should be done. In !ua.-itt might be helpful even prior to this to have the advice. u, statistician in interpreting the control charts, in Steps 3 and'-' 4. A1.3 Determination of Basic Material Variances Al.3.1 Given that the process meets the randomness requirements of Section A 1.2, a "components of variance analysis" should be performed to estimate the within-batc variance and the between-batch variance. The procedure i as follows: i A 1.3.1.1 Step 1--Compute V* = S, - Af,,)2/25(2 - I) (5)1 sb2 = 2 Z,(XL - X )2f(25 - 1) (6) where: Xb is the mean of the test made on the 2 increments from the i`h batch, and X_ is the mean of the whole A 1,3.1.2 Step 2--Take S-, (225_) (2) = 50 tests. a,2 as an unbiased estimate ofthe within-batch variance where a2 is determined as in A1.4. Al.3.1.3 Step 3--Take cb2 = {(sb2 - s,,2)/2] as an unbiased estimate of the within-batch variance. 796 DUP0502 96358 Determination of Basic Variances of Reduction and Analysis 1.4.1 Step 1--Take 20 increments from each of ties. From physical composites of the 1st, 2nd, 3rd,..., l increments from each ofthe 5 batches making a total of Composites. Reduce each composite to the size of a |ratory sample by whatever method of reduction is for the given material and prepare each pf the 20 juratory samples for testing. Run two tests on the labora; sample from each composite. 11.4.2 Step 2--Construct a control chart on the differfes between the two tests for each of the 20 composites. This is to check on the uniformity of the testing procedure. Call the chart Control Chart (4). A 1.4.3 Step 3--Construct a moving range chart on the means ofthe two tests for each of the 20 composites to check on the uniformity in the reduction procedure. A 1.4.4 Step 4--If the hypothesis of uniformity is satisfied in each case, compute s,2 = 2* 2,(Xki - XtfH20(2 - 1) (7) *,2 = 2 "k(Xk - Xf!(2Q - 1) (8) A 1.4.5 Step 5--Take a,2 = s2 as an unbiased estimate of the testing variance. Al.4.6 Step 6--Take a2 -- [(rr2 -- j ,2)/2] as an unbiased estimate of the variance of reduction. TheAmerican Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, either reapproved or withdrawn. Yourcomments are Invited eitherforrevision ofthisstandard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive caneful 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 Committed on Standards, 1916 Place St., Philadelphia, PA 19103. DU P050296359 Designation: E 691 - 87 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method1 $aM This standard is issued under tbe fixed designation E 691; 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. INTRODUCTION Tests performed on presumably identical materials in presumably identical circumstances do not, in general, yield identical results. This is attributed to unavoidable random errors inherent in every test procedure; the factors that may influence the outcome ofa test cannot all be completely controlled. In the practical interpretation of test data, this inherent variability has to be taken into account. For instance, the difference between a test result and some specified value may be within that which can be expected due to unavoidable random errors, in which case a real deviation from the specified value has not been demonstrated. Similarly, the difference between test results from two batches Of material will not indicate a fundamental quality difference if the difference is no more than can be attributed to inherent variability in the test procedure. Many different factors (apart from random variations between supposedly identical specimens) may contribute to the variability in application of a test method, including: a the operator, b equipment used, c calibration of the equipment, and d environment (temperature, humidity, air pollution, etc.). It is considered that changing laboratories changes each of the above factors. The variability between test results obtained by different operators or with different equipment will usually be greater than between test results obtained by a single operator using the same equipment. The variability between test results taken over a long period oftime even by the same operator will usually be greater than that obtained over a short period oftime because ofthe greater possibility of changes in each of the above factors, especially the environment The general term for expressing the closeness of test results to the "true" value or the accepted reference value is accuracy. To be of practical value, standard procedures are required for determining the accuracy of a test method, both in terms of its bias and in terms of its precision. This practice provides a standard procedure for determining the precision of a test method. Precision, when evaluating test methods, is expressed in terms of two measurement concepts, repeatability and reproducibility. Under repeatability conditions the factors listed above are kept or remain reasonably constant and usually contribute only minimally to the variability. Under reproducibility conditions the factors are generally different (that is, they change from laboratory to laboratory) and usually contribute appreciably to the variability of test results. Thus, repeatability and reproducibility are two practical extremes of precision. The repeatability measure, by excluding the factors a through`Jas contributing variables, is not intended as a mechanism for verifying the ability of a laboratory to maintain "in-control" conditions for routine operational factors such as operator-to-operator and equipment differences or any effects of longer time intervals between test results. Such a control study is a separate issue for each laboratory to consider for itself, and is not a recommended part of an interlaboratory study. The reproducibility measure (including the factors a through d as sources of variability) reflects what precision might be expected when random portions of a homogeneous sample are sent to random "in-control" laboratories. To obtain reasonable estimates ofrepeatability and reproducibility precision, it is necessary in an interlaboratory study to guard against excessively sanitized data in the sense that only the uniquely best operators are involved or that a laboratory takes unusual steps to get "good" results. It is also important to recognize and consider how to treat "poor" results that may have unacceptable assignable causes (for example, departures from the prescribed procedure). The inclusion of such 1 This practice is under the jurisdiction ofASTM Committee E-l 1 on Statistical Methods and is the direct responsibility of Subcommittee 11.04 on Development and Evaluation of Test Methods. Current edition approved Nov. J6, 1987. Published January 1988. Originally published as E 691 - 79. Last previous edition E 691 - 79. 798 DU P050296360 # E 61 results in the final precision estimates might be questioned An essential aspect of collecting useful consistent data is careful planning and conduct of the study. Questions concerning the number of laboratories required for a successful study as well as the number of test results per laboratory affect the confidence in the precision statements resulting from the study. Other issues involve the number, range, and types of materials to be selected for the study, and the need for a well-written test method and careful instructions to the participating laboratories. To evaluate the consistency of the data obtained in an interlaboratory study, two statistics may be used: the "fc-value", used to examine the consistency of the within-laboratory precision from laboratory to laboratory, and the "/z-value", used to. examine the consistency of the test results from laboratory to laboratory. Graphical as well as tabular diagnostic tools help in these examinations. jgcope | This practice describes the techniques for planning, Jutting, analyzing, and treating the results ofan interlabiry study (ILS) of a test method. The statistical tech ies described in this practice provide adequate informafor formulating the precision statement of a test method. |2 This practice does not concern itselfwith the developt of test methods but rather with gathering the informaneeded for a test method precision statement after the llopment stage has been successfully completed. The data ined in the interlaboratory study may indicate, however, further effort is needed to improve the test method. -.3 Since the primary purpose of this practice is the selopment of the information needed for a precision ement, the experimental design in this practice may not 'optimum for evaluating materials, apparatus, or indibal laboratories. ,4 Field of Application--This practice is concerned exIvely with test methods which yield a single numerical |e as the test result, although the single figure may be the come of a calculation from a set of measurements. \4.1 This practice does not cover methods in which the isurement is a categorization, such as a go-no-go alloca) (two categories) or a sorting scheme into two or more jjgories. For practical purposes, the discontinuous nature easurements of these types may be ignored When a test Bt is defined as an average of several individual measureits. Then, this practice may be applicable, but caution is uired and a statistician should be consulted. f'5 The information in this practice is arranged as follows: Section ............................................................ Eenced Documents..................................................... ............................. inology......................... ............................................................ mary of Practice............................................................................................. ificance and Use............................................................................ " ting the Imerlaboratory Study (ILS) 1 2 3 4 5 i Membership.................................. ffiic Design........................................ est Method........................................ (abomories........................................... Igterials............................................. timber ofTest Results per Material .. jjrotocol. Sducting the Testing Phase ofthe ILS 6 7 8 9 10 1! 12 Slot Run Ml Scale Run........................................... rulation and Display ofStatistics 13 14 'alculalion of the Statistics........................ abular and Graphical Display of Statistics . it Consistency 15 16 lagging Inconsistent Results....................... 17 Section Investigation..................................................................................... Task Group Actions.......................................................................... Examples of Interlaboratory Studies................................................. Precision Statement Information 18 19 20 Repeatability and Reproducibility.......................................................... Annexes 21 Theoretical Considerations................................................................ Index to Selected Terms.................................................................... References Tables and Figures A1 A2 Tables Glucose in Serum Example ................................................................ Pentosans in Pulp Example...................................................................... Critical Values of Consistency Statistics, h and k............................... Figures Glucose in Serum Example................................................................ Pentosans in Pulp Example................................................................ Table 1-7 8-11 12 Fig. 1-5 6-10 1.6 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 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods2 E 456 Terminology Related to Quality and Statistics2 E 1169 Guide for Conducting Ruggedness Tests2 ~ 3. Terminology 3.1 Definitions--For formal definitions of statistical terms, see Terminology E 456. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 Test Method and Protocol--In this practice, the term "test method" is used both for the actual measurement process and for the written description of the process, while the term "protocol" is used for the directions given to the laboratories for conducting the ILS. 3.2.2 Observations, Test Determinations and Test Results: 3.2.2.1 A test method often has three distinct stages, the direct observation of dimensions or properties, the arith metic combination of the observed values to obtain a test determination, and the arithmetic combination of a number of test determinations to obtain the test result of the test method. In the simplest of test methods a single direct 2 Annual Book ofASTM Standards, Vol 14.02. 799 DUP050296361 2.5 1.5 - E 691 2.15 0- li L -1 -1.5 -2 -2.5 f- MAT: ABODE ABODE ABODE ABODE ABODE ABODE ABODE ABODE LAB: 1 2 3 4 '5 6 78 FIG. 1 Glucose in Serum: h--Materials within Laboratories observation is both the test determination and the test result. For example, the test method may require the measurement of the mass of a test specimen prepared in a prescribed way. Another test method may require the measurement of the area of the test specimen as well as the mass, and then direct that the mass be divided by the area to obtain the mass per unit area of the specimen. The whole process of measuring the mass and the area and calculating the mass per'unit area is a test determination. If the test method specifies that only one test determination is to be made, then the test determi nation value is the test result of the test method. Some test methods require that several determinations be made and the values obtained be averaged or otherwise combined to obtain the test result of the test method. Averaging of several determinations is often used to reduce the effect of local variations of the property within the material. 32.2.2 In this practice, the term "test determination" is used both for the process and for the value obtained by the process, except when "test determination value" is needed for clarity. 3.2.2.3 The number of test determinations required for a test result should be specified in each individual test method. The number of test results required for an interlaboratory study of a test method is specified in the protocol of that study. 3.2.3 Test Specimens and Test Units--In this practice ji" test unit is the total quantity of material needed for obtaining ' a test result as specified by the test method. The portion of. the test unit needed for.obtaining a single test determination > is called a test specimen. Usually a separate:test specimen is'required for each test determination: 3.2.4 Precision,. Bias, and Accuracy, ofa Test Method; 3.2.4.1 When a test method is applied to a large number of portions of a material, that are as nearly dike as possible^ the test results obtained nevertheless will not all have the * same value. A measure of the degree of agreement among' these test results describes the precision of the test method' for that material. 3.2.4.2 Numerical measures of the variability between such test results provide inverse measures of the precision of the test method. Greater variability implies smaller (that is, poorer) precision and larger imprecision. 3.2.4.3 This practice is designed only to estimate the precision of a test method. However, when accepted refer ence values are available for the property levels, the test result data obtained according to this practice may be used in estimating the bias of the test method. For a discussion of bias estimation and the relationships between precision, bias, and accuracy, see Practice E 177. 3.2.5 Repeatability and Reproducibility--These terras deal with the variability of test results obtained under 800 DU P0502 96362 E 691 TABLE 1 Glucose in Serum 1LS Test Result Data Bioratory E*i i. fife A 41.03 41.45 41.37 B 78.28 78.18 78.49 Material C 132.66 133.83 133.10 D 193.71 193.59 193.65 E 292.78 294.09 292.89 It 2 41.17 77.78 132.92 190.88 292.27 42.00 80.38 136.90 200.14 309.40 r' 41.15 79.54 136.40 194.30 295.08 !r3 41.01 79.18 132.61 192.71 295.53 40.68 79.72 135.80 193.28 290.14 j. 42.66 80.81 135.36 190.28 292.34 |: 4 39.37 84.08 136.50 195.85 295.19 42.37 78.60 148.30 196.36 295.44 42.63 81.92 135.69 199.43 296.83 p5 41.88 78.16 131.90 192.59 293.93 41.19 79.58 134.14 191.44 292.48 41.32 78.33 133.76 195.12 294.28 :6 43.26 78.66 137.21 195.34 297.74 40.50 79.27 135.14 198.26 296.80 42.28 81.75 137.50 198.13 290.33 7 41.08 79.76 130.97 194.66 287.28 41.27 81.45 131.59 191.99 293.76 39.02 77.35 134.92 187.13 289.36 8 43.36 80.44 135.46 197.56 298.46 42.65 80.80 135.14 195.99 295.28 41.72 79.80 133.63 200.82 296.12 fcified laboratory conditions. Repeatability concerns the ability between independent test results obtained within fugle laboratory in the shortest practical period of time by iigle operator with a specific set of test apparatus using H specimens (or test units) taken at random from a single |intity of homogeneous material obtained or prepared for : ILS. Reproducibility deals with the variability between jle test results obtained in different laboratories, each of leh has applied (he test method to test specimens (or test Its) taken at random from a single quantity of homogeIps material obtained or prepared for the ILS. 1.2.5.1 Repeatability Conditions--The within-laboratory iditions specified above for repeatability. The single- ator, single-set-of-apparatus requirement means that for Particular step in the measurement process the same pabination of operator and apparatus is used for every test ilt and on every material. Thtxs, one operator may jepare the test specimens, a second measure the dimensions 6 a third measure the breaking force. "Shortest practical fiiod of time" means that the test results, at least for one aterial, are obtained in a time not less than in normal Isting and not so long as to permit significant changes in test laterial, equipment or environment. - 3.3 For further discussion of the terms discussed above. Practice E 177, and the formal definitions in Practice 1456. ; Summary of Practice |4.1 The procedure presented in this practice consists of t basic steps: planning the interlaboratory study, guiding testing phase of the study, and analyzing the test result TABLE 2A Interlaboratory Study Worksheet for Glucose in Serum Initial Preparation of Test Result Data for Material A Laboratory Number Test Results, x i 23 X s d .. h k 1 41.03 41.45 41.37 41.2833 0.2230 -0.2350 -0.39 0.21 2 41.17 42.00 41.15 41.4400 0.4851 -0.0783 -0.13 0.46 3 41.01 40.68 42.66 41.4500 1.0608 -0.0683 -0.11 1.00 4 39,37 42.37 42.63 41.4567 1.8118 -0.0616 -0.10 1.70 5 41.88 41.19 41.32 41.4633 0.3667 -0.0550 -0.09 0.34 6 43.26 40.50 42.28 42.0200 1.4081 0.5017 0.83 1.32 7 41.06 41.27 39.02 40.4567 1.2478 -1.0616 -1.75 1.17 8 43.36 42.65 41.72 42.5767 0.8225 1.0584 1.75 0.77 * Average of cell averages. X = 41.5183 Standard deviation of cell averages, % = 0.6061 Repeatability standard deviation, sr - 1.0632 Reproducibility standard deviation, s,, - 1.0632 where: x = individual test result, n X = cell average = Z x/n where n number of test results per ceil = 3, p X = average of cell averages = 2 Xjp where p = number of laboratories = 8, s = cell standard deviation = Vz (x - x)2/(n -1) cell deviation X - x Vi standard deviation of cell averages "Vs dz/{p -1) s, = repeatability standard deviationi== Vl:7p Sf, = reproducibility standard deviate = larger of s, and V(s,)2 + (s,f(n - 1)/n h = d/s,, and k - sjsr data. The analysis utilizes tabular, graphical, and statistical diagnostic tools for evaluating the consistency of the data so that unusual values may be detected and investigated, and also includes the calculation of the numerical measures of precision of the test method pertaining to both within- laboratory repeatability and between-laboratory reproduc ibility. 5. Significance and Use ..... .... 5.1 ASTM regulations require precision statements in all > test methods in terms of repeatability and reproducibility. This practice may be used in obtaining the needed informa tion as simply as possible. This information may then be used to prepare a precision statement in accordance with Practice E 177. PLANNING THE INTERLABORATORY STUDY (ILS) 6. ILS Membership 6.1 Task Group3--Either the task group that developed the test method, or a special task group appointed for the purpose, must have overall responsibility for the ILS, in cluding funding where appropriate, staffing, the design of the ILS, and decision-making with regard to questionable data. The task group should decide on the number of laboratories, materials, and test results for each material. In addition, it 3 To facilitate the preparation of the final report on the ILS. the task group can obtain the Research Report format guide from ASTM Headquarters. 801 DUP050296363 E 691 TABLE 3 Glucose in Serum-h*1 Laboratory 1 2 3 4 5 6 7 8 A -0.39 -0.13 -0.11 -0.10 -0.09 0.83 -1.75 1.75 B -1.36 -0.45 0.22 1.85 -0.99 0.21 -0.16 0.67 Material C -0.73 0.10 -0.21 2.14 -0.71 0.56 -1.00 -0.15 D -0.41 0.1 s -1.01 0.96 -0.64 0.97 -1.33 1.31 A Critical value = 2.15. E -0.46 1.64 -0.68 0.49 -0.34 0.17 -1.62 0.79 should specify any special calibration procedures and the repeatability conditions to be specified in the protocol (see 12.3 and 12.4). 6.2 ILS Coordinator--The task group must appoint one individual to act as overall coordinator for conducting the ILS. The coordinator will supervise the distribution of materials and protocols to the laboratories and receive the test result reports from the laboratories. Scanning the reports for gross errors and checking with the laboratories, when such errors are found, will also be the responsibility of the coordinator. The coordinator may wish to consult with the statistician in questionable cases. 6.3 Statistician: 6.3.1 The test method task group should obtain the assistance of a person familiar with the statistical procedures in this practice and with the materials being tested in order to ensure that the requirements outlined in this practice are met in an efficient and effective manner. This person should also assist the task group in interpreting the results of the data analysis. 6.3.2 When a person having adequate knowledge of both the materials and the proper statistical techniques is not available, the task group should obtain the services of a statistician who has experience in practical work with data from materials testing. The task group should provide the statistician with an opportunity to become familiar with the statistical procedures of this practice and with both the materials and the test method involved. The statistician should become a member of the task group conducting the ILS, (task group members need not be members of ASTM). 6.3.3 The calculations of the statistics (see Section 15) for each material can be readily done by persons not having statistical knowledge, (see 15.1.3 and 15.4.2.) 6.4 Data Analyst--This individual should be someone who is careful in making calculations and can follow the directions in Sections 15 through 17. 6.5 Laboratory ILS Supervisor--Each, laboratory must Laboratory 1 2 3 4 5 6 7 TABLE 4 A 0.21 0.46 1.00 1.70 0.34 1.32 1.17 Glucose in Serum-/r Material B c D 0.11 0.22 0.02 0.89 0.79 1.78 0.56 0.63 0.61 1.85 d2D 0.74 0.52 0.44 0.72 1.09 0.47 0.63 1.38 0.77 1.45 A Critical value = 2.06. E 0.18 (HD 0.69 0.22 0.24 1.03 0.64 TABLE 5A Glucose in Serum-h a Laboratory i 2 3 4 5 6 7 8 A -0.39 -0.13 -0.11 -0.10 -0.09 0.83 -1.75 1.75 B -1.36 -0.45 0.22 1.85 -0.99 0.21 -0.16 0.67 Material C -0.86 0.39 -0.08 1.59 -0.84 1.09 -1.28 0.01 D -0&1 0.15 --T;01 0.96 -0164 0.97 -1.33 1.31 A Recalculated values after correcting Cell C4, (see 20.1.4 and 201 M* Critical value = 2.15. ' have an ILS supervisor to oversee the conduct of the.! within the laboratory and to communicate with the* Coordinator. The name of the.supervisor should be ob/ on the response form to the "invitation to participate-1 9.4). 7. Basic Design 7.1 Keep the design as simple as possible in oide obtain estimates of within- and between-laboratcrv vf ability that are free of secondary effects. The basic design-H represented by a two-way classification table in which rows represent the laboratories, the columns represent* materials, and each cell (that is, the intersection ofa row wifi a column) contains the test results made by a partic laboratory on a particular material (see Table 1). 8. Test Method 8.1 Of prime importance is the existence of a ye well-written test method that has been developed in on^ more competent laboratories, and has been subjec ruggedness test prior to the ILS. 8.2 A ruggedness test is a screening procedure for iplj gating the effects of variations in environmental of ' conditions in order to determine how control of such conditions should be specified in the written descriptklj the method. For example, the temperature of the lab or ofa heating device used in the test may have an effect cannot be ignored in some cases but may be much lei others. In a ruggedness test, deliberate variations in ten ature would be introduced to establish the allowable on control of temperature. This subject is discussed mb fully in Refs (1,2 and 3) see also Guide E 1169. 8.3 As a result of canying out the screening procedti and of some experience with the test method in the spbi soring laboratory and one or two other laboratories, a written TABLE 6^ Glucose In Serum-fr Laboratory A Material BCD E 1 0.21 0.11 0.38 0.02 0.18 2 0.46 0.89 1.40 1.78 3 1.00 0.56 1.12 0.61 0.69 4 1.70 1.85 1.02 0.74 0.22 5 0.34 052 0.78 0.72 0.24 6 1.32 1.09 0.83 0.63 1.03 7 1.17 1.38 1.38 1.45 0.34 8 0.77 0.34 0.63 0.94 0.42 * Recalculated values after correcting cell C4. (See 20.1.4 and 20.1.5). Critical value = 2.06. 802 DUP050296364 2.5 +1.5 E 691 2.15 >. 0 -1 -1.5 -2.15 -2.5 LAB: ma t : 12345678 12345678 12345678 12345678 12345678 abc d e FIG. 2 Glucose in Serum: h--Laboratories within materials Irsion of the test method must have been developed (but Ot necessarily published as a standard method). This drift buld describe the test procedure in terms that can be easily [lowed in any properly equipped laboratory by cdiiapetent onnel with knowledge of the materials and the property j be tested. The test conditions that affect the test results [ipreciably should have been identified and the-proper ee of Control of the test conditions specified in the scription of the test' procedure. In addition, the test gethod should specify how closely (that is, to how many Jgits) each observation in the test method is to be measured, jj 8.4 The test method should specify the calibration proceare and the frequency of calibration. Laboratories I "9.1 Number ofLaboratories: 9.1.1 An 1LS should include 30 or more laboratories but his may not be practical and some ILS have been run with fewer. It is important, that enough laboratories be included the ILS to be a reasonable cross-section of the population |fqualified laboratories; that the loss or poor performance of few will not be fatal to the study, and to provide a feasonably satisfactory estimate of the reproducibility. . 9.1.2 Under no circumstances should the final statement bf precision of a test method be based on acceptable test iesults for each material from fewer than 6 laboratories. This would require that the ILS begin with 8 or more laboratories in order to allow for attrition. 9.1.3 The examples given in this practice include only 8 and 7 laboratories, respectively. These numbers are smaller than ordinarily considered acceptable, but they are conven ient for illustrating_the calculations and treatment of the data. 9.2 Any laboratory considered qualified to run the test routinely (including laboratories that may not be members of ASTM) should be encouraged to participate in the ILS, ifthe preparatory work is not e7tcessive and enough suitably homogeneous material is available. In order to obtain an adequate number of participating laboratories, advertise the prqpiosed ILS in where appropriate (for example, trade magazines, meetings, circulars, etc.). 9.3 "Qualified" implies proper laboratory facilities and testing equipment, competent operators, familiarity with the test method, a reputation for reliable testing work, and sufficient time and interest to do a good job. If a laboratory meets all the other requirements, but has had insufficient experience with the test method, the operator in that laboratory should be given an opportunity to familiarize himself with the test method and practice its application before the ILS starts. For example, this experience can be obtained by a pilot run (see Section 13) using one or two trial 803 DUP050296365 E 691 TABLE 7 Glucose In Serum--Precision Statistics No t e--This table (with the column for Sy omitted) Is a useful format for the presentation of the precision of a test method as required by Section A21 of the Form and Style of ASTM Standards. Mate* rial A B C D E X 41.5183 79.6796 134.7264 194.7170 294.4920 ' 0.6061 1.0027 1.7397 2.5950 2.6931 s, 1.0632 1.4949 1.5434 2.6251 3.9350 1.0632 1.5796 2.1482 3.3657 4.1923 r 2.98 4.19 4.33 7.35 11.02 fl 2.98 4.42 6.02 9.42 11.74 samples provided by the task group and returning the raw data and the test results to the task group. The importance of this familiarization step cannot be overemphasized. Many interlaboratory studies have turned out to be essentially worthless due to lack of familiarization. 9.4 Obtain written ensurance from each potential partici pating laboratory that it is properly equipped to follow all the details of the procedure and is willing to assign the work to a skilled operator in a timely manner. The derision of a laboratory to participate should be recorded on a response form to a written invitation. The invitation should include information covering the required time for calibrating the apparatus and for testing all of the materials, and other possible costs. The response form should include the name, address, and telephone number of the person supervising the ILS work within the laboratory, the address and other markings required to ensure the ILS sample material will be promptly delivered to the ILS supervisor, answers to brief questions concerning equipment, environment, and per sonnel, including previous use of the test method, upon which the apparent competence of the laboratory may be judged, and an affirmation that the laboratory understands what is involved and agrees to carry out its responsibilities with diligence. 9.5 The ILS should not be restricted to a group of laboratories judged to be exceptionally qualified and equipped for the ILS. Precision estimates for inclusion in a test method should be obtained through the efforts of qualified laboratories and personnel operating under condi tions that will prevail when the test method is used in practice. 10. Materials 10.1 Material designates anything with a property that can be measured. Different materials having the same property may be expected to have different property levels, meaning higher or lower values of the property. Different dilutions of the same material or compound to be assayed are considered "different materials" for the purpose of this practice. The terminology "different levels of material" may be used, if appropriate. 10.2 The number and type of materials to be included in an ILS will depend on the range of the levels in the class of materials to be tested and likely relation of precision to level over that range, the number of different types of materials to which the test method is to be applied, the difficulty and expense involved in obtaining, processing, and distributing samples, the difficulty of, length of time required for, and expense of performing the test, the commercial or legal need for obtaining a reliable and comprehensive estimate of TABLE 8 Pentosans in Fulp-ILS Test Results Laboratory A B 1 0.44 0.96 1.23 1.25 1.98 0.49 0.92 1.88 1.25 1.92 0.44 0.82 1.24 1.42 1.80 2 0.41 0.83 1.12 1.25 1.99 0.41 0.83 1.12 1.25 1.94 0.41 0.84 1.12 1.26 1.95 3 0.51 0.92 1.11 1.35 2.05 0.51 0.93 1.13 1.35 2.08 0.51 0.92 1.11 1.35 2.03 4 0.40 0.96 1.15 1.29 2.05 0.38 0.94 1.13 1.29 2.04 0.37 0.94 1.13 1.29 2.04 5 0.49 0.82 0.98 1.23 1.94 0.49 0.82 0.98 1.23 1.96 0.49 0.84 0.98 1.23 1.96 6 0.43 0.88 1.11 1.31 2.01 0.41 0.92 1.12 1.30 1.99 0.40 0.88 mi 1.31 1.98 7 0.1 B8 0.866 1.05 1.13 1.98 4.21 5.27 11.5 0.171 0.900 0.962 1.15 1.93 0.153 0.831 0.927 1.15 1.96 precision, and the uncertainty ofprior information on anii these points. 10.2.1 For example, if it is already known that ^ precision is either relatively constant or proportional to average level over the range of values of interest, a sn number of materials wili be needed than if it is mer known that the precision is different at different levels. Thej ruggedness test (see 8.2) and the preliminary pilot progijj (see Section 13) help to settle some of these questions, may often result in the saving of considerable time expense in the full ILS. 10.2.2 An ILS of a test method should include at .lei three materials representing different test levels, andi, development of broadly applicable precision statements or more materials should be included in the-study. 10.2.3 The materials involved in any one ILS differ primarily only in the level ofthe property me the test method. When it is known, or suspected, different classes of materials will exhibit different levelssi precision when tested by the test method, consideration, should be given to conducting separate interlaboratoryj studies for each class of material. 10.3 Each material in an ILS should be made to be or selected to be as homogeneous as possible prior to its subdivision into test units or test specimens (see 3.2.3). Ifthe randomization and distribution of individual test specimens (rather than test units) does not conflict with the procedure for preparing the sample for test, as specified in the test method, greater homogeneity between test units can be achieved by randomizing test specimens. Then each test unit would be composed of the required number of randomized test specimens. (See Section 11 and 14.1 for the quantity of each material needed, its preparation and distribution.) No t e--It may be convenient to use established reference materials, since their homogeneity has been demonstrated. 804 DUP050296366 E 691 2.5 2.06 2 .5 iX: ABODE ABODE ABODE ABODE ABODE ABODE ABODE ABODE US: 12345678 FIG. 3 Glucose in Serum: fr--Materials:within Laboratories ll. Number of Test Results per Material i1lr^' 11.1 In the design of an ILS a sufficient total number of |st results on each material must be specified to obtain a ad estimate of the measure of repeatability, generally the l^peatabifity.standard deviation.. In njany cases, the standard atipn in question will be a.function pf the property,level jfeing measured. When this occurs, the standard deviation ghould be determined separately for each level. It is generally bund to limit the number oftest results on each material in |ach laboratory to a small number^ such as three or four. The rum number oftest results-per laboratory will normally : three for a chemical test and three or four for a physical of bptical test. The number may be as small as two when there |s little danger that a test unit will be lost or questionable test suits obtained, or as niiahy as ten when test results are apt to. vary considerably. Generally, the time and effort invested in an ILS is better spent on examining more materials across more laboratories than on recording a large number of test results per material within a few laboratories. 12. Protocol ..___ 12.1 In the .protocol, cite the name, address, and tele phone number of the person who has been designated ILS coordinator (see 6.2). Urge the laboratories ,to call the coordinator when any questions arise as to the conduct of the ILS. 12.2 Clearly identify the specific version of the test method being studied. If the. test method allows several options in apparatus or procedure, the protocol should specify which option or options have been selected for the | Laboratory 1 1 . 1I 1 I 1 2 3 4 5 6 7 A 0.46 0.05 0.93 --Q.19 0.75 0.08 r-2'OBl * Critical value = 2.05. B 0.35 -1.14 0.88 1.40 -1.28 0.21 - -0,41 TABLE 9 Pentosans in Pulp-h4 Material CDE -0.05 -0.07 0.05 -0.94 -0.09 -0.94 0.56 -0.23 1:21 0.32 -0.57 0.56 --1.65 -1.51 -0.39 1.35 1.16 -0.51 0.23 -0.33 F -0,17 -0.38' -0.18 0.12 1.97 -1.37 0.01 Q 1.73 0.35 -o:o4 0.07 -0.91 -1.42 0.21 H 0.63 -0.75 -0.50 0.57 -0.04 -1.45 1.54 1 0.36 -0.25 -0.32 0.38 -0.69 -1.30 1.84 805 DUP050296367 # E 691 2.06 MAT: A B C D E FIG. 4 Glucose in Seram: k--Laboratories within Materials ILS. Test units and test data sheets must be provided for each option. 12.3 When special calibration procedures are required before every determination or every test result, they should be described specifically in the test method. If the test method specifies calibration only daily or less frequently, the ILS task group must decide whether to require recalibration before obtaining each test result. While doing so will eliminate calibration drift and help ensure relative indepen dence of the test results, changes in calibration may increase the variability between test results. 12.4 Describe any special circumstances that must be addressed in implementing the repeatability conditions, such as the period of time between obtaining die test results for TABLE 10 Pentosans in Pulp-fc'1 Material Laboratory AB CDE FGH 8 1 1 1 1 1.93 0.71 m 0.34 2 0.00 0.16 0.00 0.16 0.67 0.18 0.00 0.72 3 0.00 o.i a 0.08 0.00 0.64 0.89 0.22 0.48 4 1.02 0.36 0.08 0.00 0.15 0.36 0.00 1.21 5 0.00 0.36 0.00 0.00 0.29 1.83 0.17 0.54 6. 1.02 0.72 0.04 0.16 0.39 1.52 0.23 0.15 7 1.10 1.07 0.44 0.31 0.73 0.77 0.87 * Critical value = 2.03. 1 1.53 0.21 0.23 0.61 0.64 0.84 1.76 the same material; that is, not less than in normal testing and'] not so long as to likely permit significant changes in material, equipment or environment 12.5 Specify the required care, handling, and conditio of the materials to be tested. Explain the-eoding system used^S in identifying the. materials and the distinction between tester units and test specimens, where appropriate. ^ 12.6 Supply data sheets for each material for- recording the raw data as observations are made. Give instructions on the number of significant digits to be recorded, usually one more, if possible, than required by the test method. Also, supply test result sheets on which test results can be calculated and reported. In many instances this can be combined with the raw data sheet. Specify the number of significant digits to be reported, usually two more than required by the test method. Request the laboratories send raw data and test result sheets as soon as the testing is completed, and at least weekly if testing will continue over several weeks. 12.7 Request that each laboratory keep a record (or log) of any special events that arise during any phase of the testing. This record, to be sent to the ILS coordinator, will provide a valuable source of information both in dealing with unusual data and in making improvements in the test method in future revisions. 806 DUP050296368 4.5 - # E 691 3.5 ~ S3 S 2.5 1.5 - .5 - 0 50 100 150 200 250 300 350 400 Averages FIG. 5 Glucose in Serum: Standard Deviations of Reproducibility (O) and Repeatability ($) Versus Average 12.7.1 Instruct the laboratories to notify the ILS coordi'or promptly whenever an error in test procedure arises, so t a decision can be made as to whether a new set of test "Is should be sent to the laboratory for a complete retest of .material. >.8 Enclose with the protocol a questionnaire requesting Ormation on specific aspects of the apparatus, reagents, bration, or procedure, as well as any other information t might assist in dealing with data inconsistencies, or e rite task group that the laboratory complied with the ent requirements of the test method. Also obtain any r information that may be needed in preparing the final arch report on the ILS (see Footnote 3). perhaps two, material(s) to determine whether the test method as well as the protocol and all the ILS procedures are clear, and to serve as a familiarization procedure for those without sufficient experience with the method (see 9.3); The results ofthis pilot run also give the task group an indication of how well each laboratory will perform in terms-of promptness and following the protocol. Laboratories with poor performance should be encouraged and helped to take corrective action. 13.2 All steps of the procedures described in this practice should be followed in detail to ensure that these directions are understood, and to disclose any weaknesses in the protocol or the test method. - j CONDUCTING THE TESTING PHASE OF THE ILS j Pilot Run 3.1 Before investing laboratory time in the full scale ILS, usually wise to conduct a pilot run with only one, or TABLE 11 Pentosans in Pulp--Precision Statistics Bterial 5T 0.4048 0.8841 1.1281 1.2686 1.9809 4.1814 5.1843 10.4010 16.3610 Si 0.1131 0.0447 0.1571 0.0676 0.0538 0.2071 0.2172 0.5630 1.0901 sr 0.0150 0.0322 0.1429 0.0375 0.0396 0.0325 0.1330 0.1936 0.2156 Sfl 0.1137 0.0519 0.1957 0.0742 0.0626 0.2088 0.2428 0.5848 1.1042 r 0.04 0.09 0.40 0.11 0.11 0.09 0.37 0.54 0.60 R 0.32 0.14 0.55 0.21 0.16 0.58 0.63 1.64 3.09 14. Full Scale Run 14.1 Material Preparation and Distribution: 14.1.1 Sample Preparation and Labelling--Prepare enough of each material to supply 50 % more than needed by the number of laboratories committed to the ILS. Label each test unit or test specimen with a letter for the material and a sequential number. Thus, for ten laboratories and twcT test results for each laboratory the test units for material B would be numbered from B1 to B30, or, if five test specimens per test unit are required, the test specimens may be numbered B1 to B150. 14.1.2 Randomization--For each material independently, allocate the specified number of test units or test specimens to each laboratory, using a random number table, or a suitable computerized randomization based on random numbers. See Ref. (4) for a discussion of randomization. 807 DU P 050296369 E 691 2.5 2.05 i.5 .5 illiilL A P1 r -1 k : -1.5 -2 -2.05 -2.5 HAT: LAB: ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ,1 2 3 4 5 6 -7 FIG. 6 Pentosans in Pulp: h--Materials within Laboratories 14.1.3 Shipping--Ensure that the test units are packaged properly to arrive in the desired condition. When the material is sensitive to the conditions to which it is exposed (light, heat, humidity, etc), place special directions for opening the package on a label outside the package.' Clearly indicate the name of the person who has been designated as ILS supervisor at the laboratory on the address of each package. Follow each laboratory's instructions for ensuring prompt delivery of the package. 14.1.4 Follow-up--Once the test units have been shipped, the ILS coordinator should call each laboratory ILS super visor within a week to ten days to confirm that all test units have arrived safely. If the task group has derided to inter mingle test units from different materials in the order of testing, the testing should not start until all the test units have arrived at the laboratory so they can be tested in the specified order. 14.1.5 Replacement Sets of Test Units--As the ILS progresses, a laboratory may discover that the test method was not used properly on some test units. The laboratory ILS supervisor should discuss this with the ILS coordinator, who may send a replacement set of test units, replace the misused test units, or do nothing, as may seem desirable. 14.2 Checking Progress--From time to time, at intervals appropriate to the magnitude of the ILS, the coordinator should call each ILS supervisor to ascertain how the testing is progressing. By comparing the progress of all laboratories the coordinator can determine whether some laboratories-# * lagging considerably behind the others and so advise the laboratories. 14.3 Data Inspection--The completed data sheets shou be examined fey the coordinator immediately upon recripfirr order to detest, unusual values or other deficiencies ' should be questioned. Replacement sets of test units or q_ specific test units may be sent when- there is missing of obviously erroneous data. The task group can decide later whether or not the additional data should be used in the estimation of the precision of the test method. * CALCULATION AND DISPLAY OF STATISTICS i 15. Calculation of the Statistics 15.1 Overview--The analysis and treatment of the ILS test results have three purposes, to determine whether the collected data are adequately consistent to form the basis for a test method precision statement, to investigate and act on any data considered to be inconsistent, and to obtain the precision statistics on which the precision statement can be based. The statistical analysis of the data for estimates of the precision statistics is simply a one-way analysis of variance (within- and between-laboratories) carried out separately for each level (material). Since such an analysis can be invali- 808 DU PD5Q296370 2.5 +1.5 -- E 691 2.05 .5 . 0 -.5 T1"^ -1.5 -2.05 -2.5 LAB: MAT: 1234567 1234567 1234567 1234567 1234567 1234567 1234567 1234567 1234567 B C DE EGH FIG. 7 Pentosans in Pulp: ft--Laboratories within Materials dated by the presence of severe outliers, it is necessary to first nine the consistency of the data. The following para- aphs show, in terms of a numerical example, how the fenfire program is carried out 15.1.1 The calculations are illustrated with test results im an ILS in which the concentration of glucose in serum `see Table 1) was measured at five different concentration levels by eight laboratories. Each laboratory obtained three it results at each concentration level. 15.1.2 For extended calculations it is usually necessary to retain extra significant digits in Order to ensure that statisti cally important information is not lost in calculation by rounding off too soon. As a general rule, retain at least two more digits in the averages than in the reported test results and at least three significant figures in the standard devia tions. 15.1.3 While the calculations described in this section are arranged for use of a hand calculator, they also can be readily programmed for the computer. If necessary, contact Com mittee E-ll for advice on computational matters, (see 15.4.2). 15.2 Table ofILS Test Results--The test results received from the laboratories are usually best arranged in rows and columns as in Table 1. Each column contains the data obtained from all laboratories for one material, and each raw contains the data from one laboratory for all materials. The test results from one laboratory on one material constitute a cell. Thus, the cell for Laboratory 2 and Material C contains the test results 132.92, 136.90 and 136.40. This cell is called C2, by material and laboratory. It helps in the interpretation of the data to arrange the materials in increasing order of the measured values. ' ~ .. 15.3 Worksheets--Generally, it facilitates the calculations to prepare a separate calculation worksheet for each material, using Table 2 as a model but making appropriate changes for different numbers of laboratories, and test results per mate rial. Enter the test result data for one material (from one column of Table 1) on a worksheet. Also enter the results of the following calculations for that material on the same worksheet, as illustrated in Table 2. Work on. only one material at a time. 15.4 Cell Statistics: 15.4.1 Cell Average, x--Calculate the cell average for each laboratory using the following equation: x = 2 x/n ! where: x = the average of the test results in one cell, x = the individual test results in one cell, and n = the number of test results in one cell. -O) 809 DUP050296371 Thus from Table 2 for Material A, Laboratory 1 (that is, for Cell Al): x = (41.03 + 41.45 + 41.37)/3 = 41.2833. 15.4.2 Cell Standard Deviation, s--Calculate the standard deviation of the test results in each cell using the following equation: '= s/iix-x) xf/(n - 1) (2) The symbols have the same meaning as for Eq 1. Thus for Cell Al: s = / (41.03 - 41.2833)2 + (41.45 - 41.2833)'-' V + (41.37 - 41.283.3)2)/(3 - 1) = 0.2230 While Eq 2 shows the underlying calculation of the cell standard deviation, inexpensive pocket calculators are avail able that calculate both the average and the standard deviation directly. Check to be sure the calculator uses (n 1) as the divisor in Eq 2, not n, and has adequate precision of calculation. 15.5 Intermediate Statistics: 15.5.1 Average of the Cell Averages, x--Calculate the average of all the cell averages for the one material using Eq 3. X-'gx/p i (3) where: x = the average of the cell averages for one material, x = the individual cell averages, and p = the number of laboratories in the ILS. Thus for material A: x = (41.2833 + 41.4400 + 41.4500 + 41.4567 + 41.4633 + 42.0200 + 40.4567 + 42.5767)/8 = 41.5183 15.5.2 Cell Deviation, d--For each laboratory calculate the cell deviation by subtracting the cell average from the average of the cell averages using the following equation: d-x-x (4) Thus for cell Al: d = 41.2833 -- 41.5183 = -0.2350 15.5.3 Standard Deviation of the Cell Averages, sx-- Calculate this statistic using the.following equation: %= sj d2/(p - 1) (5) Thus for material A: ^ [(-0.2350)2J-,(-0.0783); + (-0.0683)2 + (-0.0616)2 + (-0.0550)2 + (0.5017)5 + (--1.0616)2 + (1.0584)2]/(8 - 1) = 0.6061 15.6 Precision Statistics--While there are other precision statistics, introduced later in this practice, the fundamental precision statistics of the ILS are the repeatability standard deviation and the reproducibility standard deviation. The other statistics are calculated from these standard deviations. 15.6.1 Repeatability Standard Deviation, s, C<u*3 this statistic using the following equation: where: r= VI f/P 111 i sr = the repeatability standard deviation, N. s = the cell standard deviation (p of them from Eq 2)," p = the number of laboratories. Thus for material A: = / [(0.2230)2 + (0.485 IT + (1.0608)F: ~ V +(1.8118)2 4- (0.3667)2 + (l.440j81)2 + (I.2478)2 + (0.8225)2]/8 = 1.0632 I 15.6.2 Reproducibility Standard Deviation, sR--Caicula a provisional value of this statistic using the foLowmS equation: (S*)* = V(^)2 +(Jr)2( - 1)/ g where: ss and sr are obtained from Eqs 5 and 6. The symbo * indicates provisional value, (for more information sfe'. Al.1.2). Thus for Material A: (sRf = V(0.6061)2 + (1.0632)2 (3 - l)/3 - 1.0588 Enter the larger of the values obtained by the use of Eqs.' and 7 as the final value of sR to be used for precision statements. In this case, Eq 6 yields the larger valii Therefore, sR = 1.0632. 15.7 .Consistency Statistics, h andk: 15.7.1 For each cell, calculate a value of h using the following equation: h - d/s, (r where: h -- the between-laboratory consistency statistic, d = the cell deviation (i.e., the deviation, of the cell aver from the average of the cell averages, from 15.5.2),, sx = the standard deviation of the cdl averages (fro 15.5.3). Thus for Cell Air h = -0.2350/0.6061 = -0.39 Retain two decimal places in the computed values of ft. 15.7.2 For each cell, use the following equation to calcu- f late a value of ft. k = s/sr (9) < where: k -- the within-laboratory consistency statisdc, s -- the cell standard deviation for one laboratory (from 15.4.2), and sr ~ the repeatability standard deviation of the material (from 15.6.1). Thus for Cell Al: k= 0.2230/1.0632 = 0.21 Retain two decimal places in the computed values of k. 15.8 Other Materials--Repeat the steps described in 15.4 through 15.7 for each material, entering the calculation results on separate worksheets. 810 DUP050296372 # E 691 TABLE 12 Critical Values of fi and k at the 0.5 % Significance Level-4 K. Critical if value of p Critical values of k Number of replicates, n ft 2 3456 789 Bp 1,1* 11 1 44 m -f 74 m 1.92 K 9.H5 W 9.15 ij 2.23 ilf 9 29 life 9 SR m 9.4i m 2.44 H___2.47 Hitr ?-4d 9 SI HI 9 53 RS 2 54 P 2 56 H 9 57 HIf 9.59 P ?.fi0 If 5>.B1 H 9.62 ft 2.62 ft- 2.63 1 2.64 1 2-84 3 1.72 1.67 1.61 1.56 152 1.49 1.47 1.44 4 1.95 1.82 1.73 1.66 1.60 1.56 1.53 1.50 5 2.11 1.92 1.79 1.71 1.65 1.60 1.56 1.53 6 2.22 1.98 1.84 1.75 1.68 1.63 1.59 1.55 7 2.30 2.03 1.87 1.77 1.70 1.65 1.60 1.57 8 2.36 2.06 1.90 1.79 1.72 1.66 1.62 1.58 9 2.41 2,09 1.92 1.81 1.73 1.67 1.62 1.59 10 2.45 2.11 1.93 1.82 1.74 1.58 1.63 1.59 11 2.49 2.13 1.94 1.83 1.75 1.69 1.64 1.60 12 2.51 2.14 1.96 1.84 1.76 1.69 1.64 1.60 13 2.54 2.15 1.96 1.84 1.76 1.70 1.65 1.61 14 2.56 2.16 1.97 1.85 1.77 1.70 1.65 1.61 15 2.57 2.17 1.98 1.86 1.77 1.71 1.66 1.62 16 2.59 2.18 1.98 1.86 1.77 1.71 1.66 1.62 17 2.60 2.19 1.99 1.86 1.78 1.71 . 1.66 1.62 18 2.61 2.20 1.99 1.87 1.78 1.72 1.66 1.62 19 2.62 2.20 2.00 1.87 1.78 1.72 1.67 1.62 20 2.63 2.21 2.00 1.87 1.79 1.72 1.67 1.63 21 2.64 2.21 2.00 1.88 1.79 1.72 1.67 1.63 22 2.65 221 2.01 1.88 1.79 1.72 .1.67 1.63 23 2.66 2.22 2.01 1.83 1.79 1.72 1.67 1.63 24 2.66 2.22 2.01 1.88 1.79 1.73 1.67 1.63 25 2.67 2.23 2.01 i 1.88 1.79 1.73 1.67 1.63 26 2.67 2.23 2.02 1.89 1.80 1.73 1.68 1.63 27 2.88 2.23 2.02 1.89 1.80 1.73 1.68 1.63 28 2.68 2.23 2.02 1.89 1.80 1.73 1.68 1.63 29 2.69 2.24 2.02 1.89 1.80 1.73 1.68 1.64 30 2.69 2.24 2.02 1.89 1.80 1.73 1..68 1.64 ; a nie above critical values tor the ft and k consistency statistics were calculated from Student's t and the F-ratlo using the following relationships: |=(p-1)Np(t!!-hp --2) (with p - 2 degrees of freedom, and Vp/[1 + (p- 1)/F1 F with n -1 'and Ip - IXn - 1) degrees of freedom. here p = number of laboratories. See Annex A1.2 for derivations of these relationships. 10 1.42 1.47 1.50 1.52 1.54 1.55 1.56 1.56 1.57 1.57 1.58 1.58 1.58 1.58 1.59 1.59 1.59 1.59 1.59 1.59 1.59 1.60 1.60 1.60 1.60 1.60 1.60 1.60 6. Tabular and Graphical Display of Statistics | 16.1 Material Order--It is often useful to arrange; .the yorksheets in order of increasing values of x , the material verages. This order may facilitate interpretation. 16.2 Tables--From the Table 2 results for each material, repare tables of ft and k as shown in Tables 3 and 4 for the |ucose in serum example. 16.3 Graphs--Prepare bar graphs for h and k in two ways: iterials grouped by laboratory as in Figs. 1 and 3, and joratories grouped by material as shown in Figs. 2 and 4. arrange the laboratories and materials within and between Bach grouping in the same order as used in Table 1, Thus the aterials will be arranged in ordgr of increasing x from left i right, and the laboratories in order of laboratory code number. DATA CONSISTENCY 17. Flagging Inconsistent Results 17.1 Critical Values of the Consistency^ Statistics--Table 12 lists critical values of the h and k consistency statistics at he 0.5 % significance, level. The critical values for h (first olumn) depend on the number of laboratories (p, second ..olurnn) participating in the ILS and the critical values for k {(columns headed 2 through 10) depend both on the number Jof laboratories (p) and on the number of repUcate test results |(n) per laboratory per material. The 0.5 % level was chosen phased on the judgment and experience that the 1.0 % [resulted in too many cells being flagged and the 0.1 % level in too few. For further discussion see Annex A1. 17.1.1 Obtain from Table 12 the appropriate critical values. For the glucose in serum example, the respective critical h and k values are 2.15 and 2.06. In Tables 3 and 4 circle those values that exceed the critical values and underline those values that approach the critical values. On. each graph draw a horizontal line for each critical value: two for h, since there are both positive and negative values of ft, and one for k, as shown in Figs. 1 to 4. - 17.1.2 The ft and k graphs and the marked tables give a picture of the overall character of the variability of the test method as well as singling out particular laboratories or cells that should be investigated. 17.2 Plots by Laboratory--In order to evaluate the differ ences between laboratories, use the following guidelines. 17.2.1 ft Graph--There are three general patterns in these plots. In one, all laboratories have both positive and negative ft values among the materials. In the second, the individual laboratories tend to be either positive or negative for all. materials and the number of negative laboratories equals the number of positive laboratories, more or less, Neither of these patterns is unusual or requires investigation, although they may tell something about the nature of the test method variability. In the third pattern, one laboratory, with all ft values positive (or negative), is opposed to all the other laboratories, with substantially all the ft values negative (or positive). Such a pattern calls for an investigation of that laboratory. 811 mj*. DUP050296373  E 691 2.03 ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI ABCDEFGHI 1 2345 6 7 FIG. 8 Pentosans in Pulp: ft--Materials within Laboratories 17.2.1.1 Another kind of pattern to look for occurs within one laboratory, in which the h values for low property levels are of one sign, and for high property levels are of the opposite sign. If the values are extreme, this behavior should be investigated. 17.2.2 k Graph--Here the primary pattern to look for is that of one laboratory having large k values (or very small k values) for all or most of the materials. High k values represent within-laboratory imprecision. Very small k values may indicate a very insensitive measurement scale or other measurement problem. 17.3 Plots by Material--When a plot by laboratory shows several h or k values near the critical value line, look at the corresponding plot by material to see how that laboratory differs from the rest for a given material. Often a vertical line that seems strong in the plot by laboratory, because of its relation to the lines for the other materials, will turn out to be reasonably consistent with the other laboratories for the same material. Contrarywise, the h or k value for the one laboratory may be revealed as strongly different from the values for the other laboratories in the plot by material. If so, this behavior should be investigated. 18. Investigation 18.1 Clerical and Sampling Errors--Examine the labora tory report for each flagged cell. Try to locate where each test result in the flagged cell begins to deviate from the others. IsvrI it in the original observations? Are the data rounded prema turely? Are the calculations correct? Then, look for signs oPj mislabeling of test units such that the test result for oner' material was reported as belonging to .another material. Check these errors with the laboratories: do not assume them to be so. 18.2 Procedural Errors: 18.2.1 Study the laboratory reports again looking for deviations from either the test method or the protocol. For instance, variations in the number of significant digits reported in the test results may be a sign of incorrect rounding, or that the equipment in one laboratory is different from the rest. Also, study the event log for special comments relating to the flagged cells. 19. Task Group Actions 19.1 General--If the investigation disclosed no clerical, sampling or procedural errors, the unusual data should be retained, and the precision statistics based on them should be published. If, on the other hand, a cause was found during the investigation, the task group has several options to consider. If the laboratory clearly and seriously deviated from the test method, the test results for that laboratory must be removed from the ILS calculations. However, despite the danger of the recalcitrant laboratory having prior knowledge, 812 wmmmrt IP DUP050296374 # E 691 2.5 1.5 ORO 2.03 .5 XL Li 111 ill ill LAB: MAT: 1234567 1234S67 1234567 1234567 1234567 1234567 1234567 1234567 1234567 AB CD E FGHX FICi. 9 Pentosans in Pulp: k--Laboratories within Materials iy be appropriate to ask the laboratory to retest one or materials following the correct procedure, and then ilude the new set of test results in the ILS calculations. Of se, ifthe data have changed, recalculation ofthe h and k ues must be made and the data consistency examined i.2 Exception--When a large number of laboratories s participated in the ILS and no cause for some unusual I values have been found during the investigation, it may appropriate to delete a cell from the study if all of the fier laboratories are in substantial agreement. The number laboratories that can be considered large enough to Upport deletion of data without an identified cause cannot stated , exactly. Any action which results in discarding tore than five percent of the ILS data likely will lead to the I'resentation of precision data that the test method cannot eliver in routine application. 19.3 Test Method Vagueness--One of the important ings to be on the alert for during a laboratory investigation : for vagueness in the test method standard that permits a ide range of interpretation leading to loss of precision. Particular elements to check are lack of measurement iterances, diversity of apparatus and insufficient direction operator technique. These problems can be the basis for a Revision of the standard. 20. Examples of Interlaboratory Studies 20.1 Glucose in Serum--The ILS is described in 15.1.1. 20.1.1 h Statistic--The overall impression given by Figs. 1 and 2 and Table 3 is one of reasonable consistency for variation among laboratories. Only Laboratory 4'stands out with large values for Materials B and C.' The. graph for Material C, in Fig.-2, shows that Laboratory 4 is distinctly different from the other laboratories. The graph for Material B, however, does not single out Laboratory 4. . 20.1.2 k Statistic--Laboratories 2 and 4 stand out in Fig. 3 and Table 4. The laboratory plot, in Fig. 3, indicates Laboratory 4 has three high values, but a look at the material plots (Fig. 4) for A and B suggests that Laboratory 4 is not out of line for these two materials. On the other hand, the plot for Material C shows Laboratory 4 is different. Simi larly, the plot for Material E shows Laboratory '2 is different for this material. 20.1.3 Cells and Test Results--Cells C4 and E2 should be investigated. A look at Table 1 reveals that the second test results of 148.30 in C4 and of 309.40 in E2 are the particular values to be investigated. 20.1.4 Action--If the data from Laboratory 4 were typed, the result 148.30 in Cell C4 could have been a typographical error. We have no way of knowing this today, many years after this study was made. We will suppose, however, that the task group did indeed call the laboratory and did find that DUP050296375 # E 91 1.2 0 2 4 6 8 . 10 12 14 16 18 20 Averages FIG. 10 Pentosans in Pulp: Standard Deviations of Reproducibility (O) and Repeatability () Versus Average the number should have been 138.30. However, let us suppose that for Cell E2 the task group could find no explanation ofthe apparently high value of309.40. In such a case they should retain the value. 20.1.5 Recalculation--Tables 5 and 6 show the recalcu lated consistency statistics resulting from correcting Cell C4. The discussion of the glucose in serum data is continued in Section 21. 20.2 Pentosans in Pulp--Seven laboratories tested nine materials, obtaining three test results per material as shown in Table 8. 20.2.1 h Statistic--At first glance no one laboratory is singled out for attention by Fig. 6 or Table 9. For Material A Laboratory 7 is different and for Material C, Laboratory 1. On further inspection of the laboratory plot for Laboratory 7 we note the first five materials are negative and the last four positive. Keeping in mind that the first five materials are close together in property level while the last two are much higher in property level, one can see that Laboratory 7 has a different response to property level than the other laborato ries. Laboratory 6 shows the reverse response, but not as strongly. 20.2.2 k Statistic--From Fig. 8 and Table 10, it is obvious that Laboratory 1 is different from the rest with five materials greatly exceeding, and one near, the critical value line. In addition. Laboratory 7 is different for Material H. 20.2.3 Cells and Test Results--Both Laboratories 1 and 7 should be investigated in depth. Examination ofthe cell data for Laboratory 1 in Table 8 suggests special attention should be given to test results 2 in A, 3 in B, 2 in C, 3 in D, 3 in E, and 1 in G, but there appears to be an overall problen within-laboratory variability. On the otherhand. Labor 7 has a different problem in not agreeing with the <. laboratories at the two extremes of property level. , Materia] A the Laboratory 7 test results are less than halft values obtained by the other laboratories, while for Mai I the test results are about 10 % higher than the rest, variation with property level should be explored. 20.2.4 Action--Note that Laboratory 7 reported test ,; suits to three significant digits for all property Jevels whi the other laboratories reported to two decimal places, difference in reporting would have been a good place to t._ the inquiry of this laboratory. It might be the-indication ! apparatus differences, or perhaps a sign that the laborator may have disregarded other requirements ofthe test methou or interlaboratory protocol. The apparently poor withinlaboratory precision of Laboratory 1, ifdetermined to be due to improper test equipment or poor maintenance of test environment might have required omitting this'laboratory's data from the analysis, but with so few laboratories in the ILS and no physical evidence, the task group should retain, this laboratory's data in the analysis. PRECISION STATEMENT INFORMATION 21. Repeatability and Reproducibility 21.1 General --Once the task group has concluded which cells are sufficiently inconsistent to require action, and action has been taken, the statistics of 15.4 through 15.6 are recalculated (see also 20.1.5). Using the corrected statistics, 814 SfUSPEP DUP050296376 E 691 Sculate for each material the 95 % repeatability and producibility limits (see Practice E 177) according to the lowing Eqs 10 and 11: r = 2.8 sr (10) it = 2.8 sR (ll) 21.2 Prepare a table for the corrected precision statistics as Ihown in Tables 7 and 11. 21.3 Variation ofPrecision Statistics with Property Level: 21.3.1 Quite often the values of sr and sR will be found to |ary with the values of the property level x. This type of sponse is the case for both examples as can be seen in Figs. ; and 10, that are based on Tables 7 and 11 respectively. The janner in which the statistics vary with the property level hould be shown in presenting the precision information in he precision statement of the test method. The statistician Hhould recommend the most appropriate relationship to present, using Practice E 1.77 as a guide. 21.4 Precision Statement--Table 7 or 11 (with the Jcolumn for sx omitted) is a useful format for the presentaItion ofthe precision statement ofthe test method as required (by Section A21 of the "Form and Style of ASTM Standards nBluebook)". Having obtained the required precision infor mation in accordance with this practice, the final form of the precision statement may be prepared in accordance with Practice E 177. 21.5 Conclusion--The precision statistics obtained by an ILS such as described in this practice must not be treated as exact mathematical quantities which are applicable to all circumstances and uses. The small number of laboratories and of materials included in the usual ILS guarantees that there will be times when differences greater than predicted by the ILS results will arise, sometimes with considerably greater or smaller frequency than the 95 % probability limit would imply. The repeatability limit and the reproducibility limit should be considered as general guides, and the associated probability of 95 % as pnly a rough indicator of what can be expected. If more precise information is needed in specific circumstances, those laboratories directly involved in a material comparison must conduct interlaboratory studies specifically aimed at the material of interest.4 4 Following the ASTM Research Report format guide, prepare a research report on the ILS to be filed at ASTM Headquarters. ANNEX (Mandatory Information) Al. THEORETICAL CONSIDERATIONS I AI.1 Underlying Assumptions of ILS A1.1.1 Withm-Laboratory Variability--The cell standard | deviation is a measure of the within-laboratory variability of j each individual laboratory. All laboratories are assumed to I have essentially the same level of variability when following the specified repeatability conditions. This assumption is not I always fulfilled. However, the shorter the period of time in which the test results for a particular material are to be j obtained by the laboratories the more likely the validity of j this assumption. Therefore, the laboratory cell variances can generally be pooled by averaging the squares of the cell standard deviations. The square root of this average withinlaboratory variance is the repeatability standard deviation sr A 1.1.2 Between-Laboratory Variability: A1.1.2.1 Variability of Laboratory Means--The test re sults obtained on a particular material at any particular laboratory are considered part of a population having a normal distribution with a standard deviation equal to the repeatability standard deviation but with a mean that may be different for each laboratory. The laboratory means are also assumed to vary according to a normal distribution, whose mean is estimated by the average of all ILS test results for a given material, and whose standard deviation is designated by sL. (The effect of a single outlying laboratory on this assumption will be less if there are enough laboratories.) For the ILS calculations, sL is estimated from the standard deviation of the cell averages, sx, and the repeatability standard deviation, sr is as follows: (%)2 == (S[f + (sr)2/n (A l. 1) Where (sr)2 is the pooled variance for the cell averages of one material, and n is the number of test results per cell. (ss)2 is the observed variance of the average of the cell averages. When fo)2 calculates to less than zero, sL is taken equal to zero. A1.1.2.2 Reproducibility Standard Deviation--The vari ance among individual test results obtained in different laboratories is the sum of the within-laboratory variance and the between-laboratory variance of the laboratory means. Thus, the reproducibility variance is given by Eq Al:2 as follows: is*)2 = (Sr)2 + fe)2 . (A1.2) Substituting Eq A 1.1 into Eq A 1.2 produces Eq A 1.3: (sff = (srf + fe)2 - (sr)2fn (A 1.3) Simplifying and taking the square root gives Eq A 1.4 as follows (and Eq 7): = V(%)2 + (srF( - 1)/ (A 1.4) When sR calculates to less than sn sR is set equal to sr. A1.2 Consistency Statistics Al.2.1 Critical Values--The derivation of the equations for calculating critical values of h and k are given in A 1.2.2 and Al.2.3. In each case critical values were calculated at three significance levels, 1 %, 0.5 %, and 0.1 %. Of these three only the 0.5 % critical values were chosen for flagging as described in Section 17. This choice is based on the judgment from experience that the 1 % values are too 815 DUP050296377 E 691 sensitive (flag too many) and the 0.1 % values are not sensitive enough for flagging adequately in the analysis of ILS data. A 1.2.2 Between-Laboratory Consistency: Al.2.2.1 The consistency statistic h is an indicator of how one laboratory's cell average,, for a particular material, compares with the average of the other laboratories. The critical values for the comparison are calculated with an equation derived from an unpaired r-test as given by Eq A 1.5 as follows: ! = C*c - **)/ %* V[1 + l/(p- 1)] .. (At.5) where: t = observed Student's t value, xc = cell average being tested, x* = average of all cell averages except the one being tested, sx*= standard deviation of all the cell averages except the one being tested, and p == number of laboratories in the ILS. In this relationship t has p-2 degrees of freedom. Three further equations are required in order to express h in terms oft from Eq A1.5. These follow as Eqs A1.6, A1.7, and A1.8: x* = (px - xc)/( p - 1) (A1.6> (sx)2 = (/>- Dte)2/(p - 2) p&-xcf/{(p- l)(p-2)\ (A 1.7) djsx = (xc- x)/sx (A 1.8) Each of these equations is derived by simple algebraic operations from the definitions of symbols accompanying Eq A 1.5 and Table 2. Combining them with Eq A 1.5 results in Eq A 1.9 as follows: h = (p- l)t/Mt2 + P~2) (A 1-9) A1.2.2.2 The critical values of k were calculated by Eq A 1.9 using published values of Student's t at the 0,5 % two-tailed significance levels (6). The values obtained are given in Table 12. A 1.2.3 Within-LaboratoryConsistency: A1.2.3.1 The consistency statistic, k, is an indicator of how one laboratory's withiri-laboratory variability, under repeatability conditions, on a particular material, com with all; of the laboratories combined. Values of k larger 1 indicate greater within-laboratory variability than t'la'i! average for all laboratories. Since such variation among laboratories is expected, critical values of k have 1 calculated to aid in the decision of whether the cell stai deviation of one laboratory is sufficiently different from rest of the laboratories as to require investigation. Al.2.3.2 A valid test for determining whether a pai cell variance is inconsistent relative to the variances of other laboratories is to calculate the F-ratio of the one variance to the pooled variance of all the, other labi ries--excluding the variance being tested. This is shown Eq A 1.10 as follows: 'F = ^mui)2)/(p- 1)] (Al.! / where: s2 = cell variance of cell being tested, 2 , = summation of all other variances, i ' *' .^ (Sjf - cell variances other than the one being tested, and ! p == the number of laboratories. `* The consistency statistic k is defined by Eq Al.ll and the repeatability variance by Eq A1.12 as follows: i k = s/sr (Al.ll) (J,)2= (S(*,-)2 + ia)/P (A1.12>! /! Combining Eqs. A 1.10, Al.l 1 and A 1.12 results in Eq A1.13 as follows: k = V[p/(1 + (p - 1)/F)] (A 1.13) Al.2.3.3 The degrees of freedom for Fin Eq Ai.10 are n | -- 1 and (p -- 1) (n -- 1). The upper critical values of k are calculated from the upper critical values of F at the 0.5 1 significance level for selected combinations of numbers , of test results and laboratories. The values of k given- in Tabtesf 12 were obtained using SAS's BETAINV (inverse beta func-. i tion) and using IMSL's routine MDFI (for the F cdf inverse). ; I 816 DUP050296378 # E 691 A2. INDEX TO SELECTED TERMS Term Section accuracy average of the cell averages, x bias cell cell average, x cell deviation, d cell standard deviation, 5 cell statistics, x, s consistency statistics, h, k h k laboratory material observation precision precision statistics, s,, sR property level protocol repeatability repeatability conditions repeatability limit, r repeatability standard deviation, sr reproducibility reproducibility condition reproducibility limit, R reproducibility standard deviation, sR ruggedness test screening procedure standard deviation of.the cell averages, sx test conditions test determination test method test result, x test specimen test unit intro., 3.2.4.3 15.5.1 Intro., 3.2.4.3 7.1 15.4.1 15.5.2 15.4.2 15.4 15.7 Intro., 15.7.1 Intro., 15.7.2 9. 10. 3.2.2 Intro., 3.2.4 15.6 10.1,20.3 3.2.1, 12. Intro., 3.2.5 Intro., 3.2.5.1 21.1 15.6.1 Intro., 3.2.5 Intro. 21.1 15.6.2 8.2 8.2 15.5.3 8.2 3.2.2 3.2.1, 8. 3.2.2. 3.2.3 3.2.3 REFERENCES |Youden, W. J., "Experimental Design and ASTM Committee," }iMaterials Research and Standards, ASTM, November 1961. pp. 1:862-867. J'Pauls, R. G, Marinenko, G., Knoerdel, M., and Koch, W. F., i "Ruggedness Testing--Fart 1: Ignoring Interactions," Journal of Research ofthe NBS, Vol. 91, 1986, pp. 3-8. (3) Paulc, R. G, Marinenko, G., Knoerdel, M., and Koch, W. F., "Ruggedness Testing--Part 2: Recognizing Interactions," Journal ofResearch ofthe NBS, Vol. 91, 1986, pp. 9-15." _ (4) Duncan, A. J., Quality Control and Industrial Statistics, Richard D. Irwin Inc., Homewood IL, 5th edition, 1986. (5) Dunn, O. J. and Clark, V. A., Analysis ofVariance andRegression, John Wiley and Sons, 1974. The American Society tor Testing and Materials takes no position respecting the validity olany patentrights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity ol any such patent rights, and the risk of Infringement of such rights, eve entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and mustbe reviewed every five years and if not revised, eitherreapproved or withdrawn. Yourcomments 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. 817 DUP050296379 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. Up DUP050296380 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.01 Pa in t --Te s t s f o r Fo r mu l a t e s Pr o d u c t s a n d Ap p l ie d Co a t in 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 06.1)2 and Q6.03, see pp. 829 and xxiv A complete Subject Index begins on p. 861 Reifications for: 15098 - 90 1,4302 - 90 1*5067 - 90" (Methods for: 969 -85(1989)" 94399 -90 >1210 -79(1988)" U316 -87 >2243 -90 >2337 -84 >3793 -89 >2574 86 185 -84(1989)" >5062 - 90" 9 869 -85(1989)" >1309 88 >4144- -82(1987) >1849. -80(1987)" >4948 -89 aclice for: >3925-91 few Methods for: 10 4958 - 91 PD 2353 - 83 IID 2801 -69(1981)" PD 4062 - 88 | D 4400 - 89a J- D 2376 - 84(1989) ID 4707 - 87 practicefor: \ D494I -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 Etegree of Electrical Conductivity of 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, Dilutability Settling of Paint, Evaluating Degree of Settling Properties of Traffic Paints During Storage Stability, Package, of Coatings for Ultraviolet Curing, Estimating Stability, Package, of Paint Upper Layer Separated from aViscous Liquid, Determination of Sampling Liquid Paints and Related Pigmented Coatings Application Properties Brush Drag of Latex Paints, Comparison of Flow Ratings of Organic Coatings Using the Shell Flow Comparator (Discontinued 1992f) Leveling Characteristics of Paints by Draw-Down Method (Discontinued I990f) Leveling of Paints by Draw-Down Method Sag Resistance of-PaintsUsinga 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 Depanmenr 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. t Although this standard has been officially withdrawn from Society approval, a brief description is included for information only. 821 DUP050296381 Test Methodsfor: D 1209 - 84 (1988)" D 1544 - 80 (1989)" D 4838 -88 D 2090 - 88 Test Methodfor: D 1475-90 Test Methodsfor: D 562-81 (1990)" D 4359-90 0 2196 - 86(1991)" D4212-88 D 4287-88 D 1200 -88 D 4040 - 91 D 1545-89 Test Methodsfor: D 2697 - 86 D 5145-90 D 5095 - 90 D4713 -87" D 1644-88 Guidefor: D2832-83 (1991)" Test Methodsfor: D4451-85(199i)" D2371 -85 (1990)" D 2698 - 90 D 3723 - 84 (1990)" Test Methods for: D 2369 - 90 D 5200 -91 D 5087-91 Practice for: D 3960 - 91 Test Methodsfor: D 3792-91 D 4017-90 D 4942-89 Test Methodsfor: 0 1639 - 90 LIST BY SUBJECTS, VOLUME 06.01 Color and Clarity ofLiquids Color of Clear Liquids (Platinum-Cobalt Scale) Color of Transparent Liquids (Gardner Color Scale) Tinting Strength, Relative, of Chromatic Paints, Determining Clarity and Cleanliness ofPaint and Ink Liquids (see Vols 06.02, 06.03) Density, Specific Gravity, and Weight per Gallon Density of Paint, Varnish, Lacquer, and Related Products Consistency and Viscosity Consistency of Paints Using the Stormer Viscometer Determining Whether a Material is a Liquid or a Solid Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer Viscosity by Dip-Type Cup 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 Repellabt. 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 822 m DUP050296382 ! Methodsfor: >437.0 -84(1990)" >2348 -91 >3133' -72(1989)" |)3718' 85a >4457- -85(1991)" >2621 87 (3335 -85a (1991)" >3618 -85a (1991)" >4834 88 >3624. 85a(1991)" >4584. -86(1991)" >1542. 60(1988)" >2349. 90 >-4764 -88 >4563 -86(1991)" >2921 -88 WD3432- 89 helices for: >3271-87 >3168-85(1990)" >2372 - 85(1990)" >2743-68(1987) |D 3272-76 (1988)" defor ID 1978-91 fst Methods for: 215-91 pecification for: |d 358-83(1988) Test Methodsfor: |d 4940 - 89 11734 - 63(1980)" >4262 - 83(1988) ID 2201 - 65(1987)" |;D4417-84 |,D 609-90 ;D 2200 - 91 'radicesfor: jfD 1730- 67 (1984)" ID 1731 -67 (1984)" ED 5107-90 'D 4259 - 88 D 4260 - 88 D 4258-83 (1988) |. D4261 - 83 (1988) I D 3891-90 |D 1732 -67 (1984) |jD 2092 - 86 Suidefor: D4610-86 fest Methodsfor: !'D 823-91 D 1212-91 LIST BY SUBJECTS, VOLUME 06.01 Miscellaneous Methods ofAnalysis Acid and Base Milliequivalent Content ofElectrocoat Bath Arsenic in Paint Cellulose Nitrate in Alkyd Lacquers by Infrared Spectrophotometry, Quantitative Determination of Chromium in Paint by Atomic Absorption Spectroscopy, Low Concentrations of Dichloromethane and 1,1,1-Trichloroethane, Analysis for by Direct Injection into a Gas Chromatograph Infrared Identification of Vehicle Solids from Solvent-Reducible Paints Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy, Low Concentrations of Lead in Paint and Dried Paint Films, Detection of Lead in Paint by Direct Aspiration Atomic Absorption Spectroscopy, Detection of Mercury in Paint, Low Concentrations of, by Atomic Absorption Spectroscopy pH, Measuring Apparent, of Electrocoat Baths Rosin in Varnishes, Qualitative Detection of Thinner in Solvent-Reducible. Paints, Qualitative Determination of Nature 'Titanium Dioxide Content in Paint by X-ray Fluorescence Spectroscopy, Determination of Titanium Dioxide Content of Pigments Recovered from Whole Paint, by Atomic Absorption Spectroscopy Water Repellents and Preservatives in Wood Products, Qualitative Tests for the Presence of Free Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography (see Vol 06.02) Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph Polymers in Emulsion Paints, Qualitative Identification of Separation of Vehicle from Solvent-Reducible Paints Uniformity of Traffic Paint Vehicle Solids by Spectroscopy and Gas Chromatography Vacuum Distillation of Solvents from Solvent-Reducible Paints for Analysis Analysis of Electrocoat Bath Samples Systematic Analysis White Linseed Oil Paints, Chemical Analysis of Panel Specifications and Preparation of Surfaces for Painting Wood Panels for Weathering Tests of Coatings Blasting Abrasives, Analysis of Water Soluble Ionic Contamination, Conductimetric Analysis of Concrete and Masonry Panels, Preparation for Paint Testing Concrete Surfaces, pH ofChemically 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 Alumifium 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, of Organic Coatings 823 DUP050296383 Practices for: D4147 - 82 (1987) D4414- 84 (1990)" D4708-91 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)" D 3259 - 84 (1990)" D 2454 - 91 Test Methodsfor: D 4138-88 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: D5I62-91 Test Methodsfor: 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 D1543 - 86 Applying Coil Coatings Using the Wire-Wound Drawdown Bar Thickness, Wet Film, Measurement by Notch Gages Uniform Free Films of Organic Coatings Drying Times of Organic Coatings at Room Temperature Gas Checking and Draft Resistance of Varnish Films Low-Temperature Coalescence of Latex Paint Films No-Fick-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 Thickness of Protective Coating Systems Measurement of Dry Film Thickness on Ferrous' Base Measurement of Dry' Film ThicknesSoriNonferrous Metal Base Micrometer Measurement of Dry-Film Thickness of Organic Coatings Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel Porosity and Permeability Determination of Edge Performance of Composite Wood Products Under Surfactant Accelerated Moisture Stress Porosity of Paint Films Water Vapor Permeability of Organic Coating Films Water Vapor Transmission ofMaterials in Sheet Form (see Vols 04.06, 08.03, and 15.09) Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates ` Appearance Properties Gloss, (Reflectance, and Hiding Power 45-deg 0-deg, Directional Reflectance Factor of Opaque Specimens by Broad-Band Filter Reflectometry Gloss or Sheen Uniformity, Evaluation of Gloss Differences Between Surfaces of Similar Appearance, Visual Evaluation of Gloss of High-Gloss Surfaces Using Abridged Goniophotomefry Gloss, Specular Hiding Power of Architectural Paints Applied by Roller Hiding Power of Paints by Reflectometry Hiding Power, Relative, of Paints by the Visual Evaluation of Brushouts Print Resistance of Architectural Paints Reflection Haze of High-Gloss Surfaces Wet-to-Dry Hiding Change Absolute Calibration ofReflectance Standards (see Vol 14.02) Preparation of Reference White Reflectance Standards Selecting Coating Specimens for Appearance Measurements Color Bleeding, Degree of Traffic Paint, Laboratory Determination of Color Differences, Calculation from Instrumentally Measured Color Coordinates Color Permanence of White Architectural Enamels (Discontinued 1992f) 824 DUP050296384 1 Methods for: 114960 - 89 Micefor: |> 3964 -- SO (1989) 1 ist Methods for: i> 658-91 l> 968-81 (1991Y2 >4060-90 >5181 -91 >4213-87 >3359-90 >2197-86(1991)" >5179-91 >4541 -85(1989)" 10- 83(1988) >2793 - 69(1987) >4946- 89" >4796- 88 1>3170- 87 (1991)" 11642- 70(1987) 522- 88" >5178 - 91 >4145- 83 >3281 - 84(1989) >4146- 83(1989)" >3363- 74(1989)" H474- 85(1991)" 194366- 91 | 14- 88 13- 89 17- 88 ID3003- 71 (1987) |P> 2091 - 88 92794- 90 IP4518- 91 >2370- 82{1987)f2 |D 913 - 88 fst Methods for: >3260-82 (195 >4938-89 |D 3623 |G 8! 42- '1540|D 1308 |G 20ED2933|D 1654 ID 4256 [D3719!'G 19D 2803 |D 1360 !D 3806 D2485 D 3459 iD 2246 [G 18iD 4303 [D 3424 ID 2620 ID 4939- LIST BY SUBJECTS, VOLUME 06.01 CcoJlor for Thermoplastic Traffic Marking Materials, Evaluation of Selecting Physical Strengths and Resistances (Nonchemical) Abrasion Abrasion Abrasion Abrasion Abrasion Adhesion Adhesion Adhesion Adhesion 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 of Pipeline Coatings,(Limestone Drop Test) Penetration Resistance of Pipeline Coatings (Blunt Rod Test) Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates Print Resistance of Lacquers Rapid Deformation (Impact), Resistance of Organic Coatings to the Effects of Static Friction of Coating Surfaces, Measuring Tensile Properties ofOrganic Coatings Wear Resistance of Traffic Paint, Evaluating Degree of Resistances to Chemicals and Environment Acid and Mortar Resistance of Factory-Applied Clear Coatings on Extruded Aluminum Products Antifouling Paints, Erosion Testing, Using High Velocity Water Antifouling Panels in Shallow Submergence, Testing -- Cathodic Disbonding of Pipeline Coatings Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures Chemical Agents, Effect bn 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 1992+) 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 Coatings by Direct Soil Burial Filiform Corrosion Resistance of Organic Coatings on Metal Fire Retardancy of Paints (Cabinet Method) Fire Retardant Paints, Small Scale Evaluation (2-Foot Tunnel Method) High Temperature Service, Evaluating Coatings Humid-Dry Cycling for Coatings on Wood and Wood Products Humidity-Thermal Cycle Cracking, Testing Finishes on Primed Metallic Substrates Joints, Fittings, and Patches in Coated Pipelines Lightfastness of Pigments Used in Artists' Paints Lightfastness of Printed Matter Light Stability of Clear Coatings Marine Antifouling Coating Subjected to Biofouling and Fluid Shear Forces in Natural Seawater 825 SUP DUP050296385 Test Methodsfor D 3274-82 (1988)" E> 3273-86 (199X)el D 5108-90 D 4828-91 D 4082 - 89 B 117-90 D 2486-89 D 2134 - 66 (1980)" D 2792-69 (1987) D 2198 - 84 (1989)" D 1211-87 D 3450 - 90 D1647 - 89 G 9-87 E 84-90 E 162-90 Practicesfor: D 2248-89 D3456 - 86 (1991)" D 3023-88 D4585 - 87" D 870-87 D 2247 - 87 D 1735-87 Test Methods for: D 868-85(1989)" D 714-87 D 659-86" 0 660 - 87 D.661-86" D 662 - 86" 0 772-86" 0 2200 - 85(1989) 0 610 - 85(1989)" Practicefor: 04121-82(1987) Test Methods for: 02830-91 01641-59(1987) 01014 - 83(1988)" 01150-55(1987)" G 11-88 0 1848 - 88 Practices for: 04141-82(1987)" 0 4587 - 91 01006 - 73(1986)" G 23-90 0 822 - 89 G 53 - 88 D 3361 -87 0 5031-90 LIST BY SUBJECTS, VOLUME 06.01 Microbial Growth or Soil and Oirt Accumulation, Evaluating Degree of Surface Disfigurement ofl Films Mold Growth on the Surface of Interior Coatings in an Environmental Chamber, Resistance to Organotin Release Rates of Antifouling Coating Systems in Sea Water Practical Washability of Organic Coatings Radiation, Effect on Coatings Used in Light-Water Nuclear Power Plants Salt Spray (Fog) Testing Scrub Resistance of Interior Latex Flat Wall Paints Softening of Organic Coatings by Plastic Compositions (Oiscontinued 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 Oried' Films of Varnishes Water Penetration into Pipeline Coatings , Surface Burning. Characteristics ofBuilding Materials (see Vol 04.07) *Jj|jj Surface Flammability ofMaterials Using a Radiant Heat Energy Source (see Vol 04.07) Oetergent 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 ofi Chalking of Exterior Paints, Evaluating Degree of (Discontinued 1990f- -Replaced by Test Melh D4214) Checking of Exterior Paints, Evaluating Degree of Cracking of Exterior Paints, Evaluating Degree of Erosion of Exterior Paints, Evaluating Degree of Flaking (Scaling) of Exterior Paints, Evaluating Degree of Pictorial Surface Preparation Standards for Painting Steel Surfaces Rusting on Painted Steel Surfaces, Evaluating-Degree of Photographic Documentation of Coating and Lining Failures and Defects General Tests ! Mg 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-Are Type) With and Without Water for Exposure of Nonmetailic Materials, Operating Light- and Water-Exposure Apparatus, Filtered Open-Flame Carbon-Arc Type, for Testing Pant and Related Coatings and Materials Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetailic Materials, Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Products Using the Dew Cycle, Operating Light- and Water-Exposure, Using Enclosed Carbon-Arc Apparatus, Conducting Tests on Paints and Related Coatings and Materials 826 DUP050296386 LIST BY SUBJECTS, VOLUME 06.01 acticesfor: G 26-90 fD 713-90 est Methodsfor: D 1736-89 D 2338-84 (1989)" D 2199-82 (1987) D 4797-88 Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials, Operating Road Service Tests on Traffic Marking Materials, Conducting Miscellaneous Properties Efflorescence of Interior Wall Paints Particle Size of Multicolor Lacquers Plasticizer Migration from Vinyl Fabrics to Lacquers Thermoplastic Marking, White and Yellow, Containing Lead Chromate and Titanium Dioxide, Chemical Gravimetric Analysis of SCHEDULES OF EXAMINATION FOR TESTING PAINT PRODUCTS est Methodsfor: D 1546-62(1987) D 333-87 1D 466-42(1989) D 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 peticesfor: D3794 - 79ei D3002- 81 (1987) D 3925-81 (1985)" D 3451-76 (1987)" ;D 3322-82 (1991) j D2336-87(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 uidesfor: ID 2833 -89 D 3630 -89 D3129 -91 D2932 -80(1988)" D3730 -78 (1988)" D4712 -87a (1991) D 4540 -91 D 3323 - 80 (1988)" | D 2931 - 84 (1989)" ID 5010 -91 D 5146 -91 D 3425 -80 (1988)" D 3383 -79a (1988)" D 2205 - 85 (1990)el D 154. -85 (1989)" 3358- 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 Printing Inks and Related Materials, Testing Solvent-Borne Architectural Coatings Solvent-Reducible Interior Semigloss Wall and Trim Enamels, Testing Solvent-Reducible Floor Paints, Testing Traffic Paints, Testing Varnishes, Testing Water-Borne Floor Paints, Testing Wood Furniture Lacquers, Testing Purchasing and Application of Paint and Related Coatings Iuidesfor: 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 Verifications for: D4618-87 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 'est Methodsfor: D3912 - 80 (1989) D3911-89 D 4256-89 D4138-88 0 4263 - 83(1988)" D4285-83(1988) 04262-83(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 DUP050296387 LIST BY SUBJECTS, VOLUME 06.01 Practices for: D 4259-88 D 4260-88 D 4787-88 D 4286-90 0 4227 - 83(1989) D 4228-83 (1989) D4619-91 D4121 -82(1987) D 3843-89 D 4257-87 D4258 - 83 (1988) D4261 -83(1988) Abrading Concrete Acid Etching Concrete Continuity Verification of Liquid or Sheet Linings Applied to Concrete Substrates Contractor Qualifications for Nuclear Powered Electric Generation Facilities, Determining Journeyman Painters, Qualification for Application of Coatings to Concrete Surfaces of Safely-] Areas in Nuclear Facilities Journeyman Painters, Qualification for Application of Coatings to Steel Surfaces of Safety-Related Ar 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^ J990f) Surface Cleaning Concrete for Coating Surface Cleaning Concrete Unit Masonry for Coating Guides for: D5161 -91 D 3842- 86 (1991) D 4537-91 D 5163 - 91 Coating and Lining Work (Metal Substrates), Specifying Inspection Requirements for Coatings for Use in Light-Water Nuclear Power Plants, Selection of Test Methods for Qualify and Certify Inspection Personnel for Coating Work in Nuclear Facilities, Establishing Procedures to"*{ Safety Related Coatings in an Operating Nuclear Power Plant, Establishing Procedures to Monitor the Vk Performance of ,-jM Terminology Relating to: D 4538-90a Protective Coating and Lining Work for Power Generation Facilities GENERAL STANDARDS Specifications for: D3924- 80 (1991)1 E 171-87 Standard Environment for Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials Standard Atmospheresfor Conditioning and Testing Materials (see Vol 15.09) Test Methods for: D 5043 - 90 D 5009-89 D 5066 -91 D 95-83(1990) E 306 - 71(1976)(1 E 337 - 84(1990) Practices for: D 5064 - 90 D 3980-88 0 4236 - 91 D 5068 - 90 D 5069 - 90 E 312-80(1986) E 179-90 E 167-77(1987) G 24-87 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 \ !|S Absolute Calibration ofReflectance Standards (see Vol 14.02) 11 Relative Humidity by Wet- and Dry-Bulb Psychrometer (see Vols 07.01, 11.03, and 15.09) : "1 Conducting a Patch Test to Assess Coating Compatibility Interlaboratory Testing of Paint and Related Materials Labeling Art Materials for Chronic Health Hazards -- Paint Brushes for Evaluation, Preparation of Paint Roller Covers for Evaluation, Preparation of Description and Selection ofConditionsfor Photographing Specimens (see Vol 14.02) Geometric Conditions, Selection of, for Measurement ofReflectance and Transmittance (see Vol 14.02) Goniophotometry ofObjects and Materials (see Vol 14.02) Natural Light Exposure Tests (Sunlight and Daylight), Conducting Under Glass (see Vols 07.01 and 14.02) Definitions ofTerms Relating to: E 284 - 90 E 41-86 D 16-91 Appearance of Materials (see Vol 14.02) Conditioning (see Vols 08.03 and 14.02) Paint, Varnish, Lacquer, and Related Products Guides for: D 5065 - 90 D 5063 - 90 Assessing the Condition of Aged Coatings on Steel Surfaces Use of Certification of Coating Conformance Form METRIC PRACTICE Practice for: E 380-91 Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Materia! section) 828 DUP050296388 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. i D 3619-77(1989) i D 603 - 66(1.989) i D 602 - 81 (1991)*' r d 1199-86(1991)*' t D 604 - 81(1989) fD 605-82(1989) i D 867-81(1986)*' iD 607-82(1987)*' D4288 -83 (1989)*' D 476 - 84(1989) D 81-87 ' D 4462-85 (1989) D 79-86 D 210-81a(1991)*` D 561-82(1989) D 769 - 87(1991)*' D 209-81 (1989) 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) D3021 - 82 (1987)*' D 1649 - 82 (1987)*' D 478 - 86 (1991)*' D 211-67(1989)*' D 768-81 (1987)" For Lis! by Subjects of Volumes 06.01 and 06.03, see pp. 821 and xxiv A complete Subject Index begins on p. 861 PIGMENT SPECIFICATIONS Inert dr 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 IV Aluminum Pdwder 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 ofthe Department of Defense and, if indicated on the standard, replaces corresponding Federal or Military document Consult the DoD jj Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. 829 DUP050296389 D 3722 - 82 (1991 )ei D 3724 - 82 (1987)1 D 2218-67 (1989)" D 85-87 (1991)" D 765-87(1991)el D 1648-86 D 763-81 (1988)" D 3722- 82 (1987)l D372I -83 (1991)" D 475-67(1989) D 83-84(1989) D 656-87 Test Methodsfor: D 305-84 (1990)" D 480-88 D 718-86 (1991)" D 2350-90 D 715 - 86 (1991)" r> 1135-86 (1991)el D 4487 -90 D 126 - 87(1991)" D 185-84(1989)" D 1208 - 84 (1989)" D 283-84(1990)1 D 3872 - 86 (1991)" D 280-81 (1987) D4358 - 84(1990)l D 717-86 (1991)I D 284-88 D 716-86 (199I)I D3256-86(1991)1 D 49 -- 83 {1990)c1 D 970-86(1991)l D 719-86 D 1844-86(1991)I D 1845-86 (1991)l D 2351 -90 D 2352-85 (1990)1 D 3720 - 84 D3926 - 80 (1991)1 D 2742-79 0 2448 - 85(1989) D 1301-91 D 1394 - 76(1991)1 D3280-85(1990)1 D 50-90 D 521-81 D 4450 - 85(1990)" D 444-88 Practicefor: D 34-91 Guidefor: 04139 - 82(1991)" Test Methodsfor: 01155-89 01214-89 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.Red Toner Red Lead Toluidine, Pure Red Toner PIGMENT TEST METHODS Analytical Tests Acetone Extract in Black Pigments, Determination of Aluminum Powders and Pastes, Flaked, Sampling and Testing Aluminum Silicate Pigment, Analysis of Antimony Oxide in White Pigment Separated from Solvent-Reducible Paints, Determination of Barium Sulfate Pigment, Analysis of Blue Pigments, Chemical Analysis of Calcium Borosilicate, Analysis of Chromium, Yellow, Orange, and Green Pigments, Analysis of Coarse Particles in Pigments, Pastes, and Paints Common Properties of Certain Pigments Copper and Dry Cuprous Oxide Pigments, Chemical Analysis of Ferrous Iron in Iron Oxides, Determination of Hygroscopic Moisture (and Other Volatile Matter) in Pigments Lead and Chromium in Air Particulate Filter Samples of Lead Chromate Pigment Dusts Magnesium Silicate Pigment, Analysis of Mercuric Oxide Pigment, Chemical Analysis of Mica Pigment, Evaluating Phthalocyanine Blue and Green Pigments, Chemical Analysis of Red Lead, Chemical Analysis of Red Pigments, Para and Toluidine Silica, Diatomaceous Pigment, Analysis of Silicochromate, Basic Lead, Chemical Analysis of , Strontium Chromate Pigment, Chemical Analysis of Sulfide Sulfur in White Pigment Separated from Solvent-Reducible Paints, Determination of Sulfur Dioxide in White Pigment Separated from Solvent-Reducible Paints, Determination of Titanium Dioxide Pigments, Ratio of Anatase to Rutile by X-Ray Diffraction Titanium Dioxide Slurries, Percent Solids in Tribasic Lead Phosphosilicate, Chemical Analysis of (Discontinued I990f) ' Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment White Lead Pigments, Chemical Analysis of White Titanium Pigments, Chemical Analysis of White Zinc Pigments, Chemical Analysis of Yellow, Orange, Red, and Brown Pigments, Chemical Analysis of Ziiic Dust, Chemical Analysis of Zinc Hydroxy Phosphite, Analysis of Zinc Yellow (Zinc Chromate), Chemical Analysis of m 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 Allhough this standard has been officially withdrawn from Society approval, a brief description is included for information only. 830 DUP0S0296390 'ass ^Methods for: 281-84(1989) J3360 - 80 (1989) ' 153 - 84 (1989)" Ecticefor: *U366 - 86(1991)1 gjjit Methods for: 279-87(1991)" >3022 - 84(1989)" 387-86 >2745-89 332-87(1991)" iecifications for: 207 - 55(1987) D 784-83(1987) " 237-91 D 360-89 uide fon ID 4277-83 (1988)" ID 4142-89 ID4143-89 ID 4368 -89 Test Methodsfor: ID 1979-91 D 29-81 (1987)" D 365-84(1989)" I D 411-83(1987) ID 1650-91 |D 1439-83a (1989)" |.D 509 - 70(1987) 'racticefor: D 2689-88 Test Methodsfor: D1926 89 D 2455 89 D1726 - 90 I D1847 87 If D 1652- 90 I D 1398 - 84 ! D 1615- 60(1987) if D 2572 - 91 :: D 2690 - 89 1 D 1013- 88 D46I3- 86(1990)" D 1312- 56(1987)" D4706- 87 D 563- 88 D 1306- 88 D 1396- 73(1987)" D 3680 - 89 D 1469-73(1988)" D 1542-60(1988)" D 3733-78 (1984)" D 1397-88 D 465-82 (1987fl D1063 - 51 (1987) D1585 - 82 LIST BY SUBJECTS, VOLUME 06.02 Oil Absorption of Pigments by Spatula Rub-Out Particle Size Distribution of Common White Extender Pigments Specific Gravity of Pigments Particle Size Characteristics of Pigments, Reporting Color and Opacity Tests Bleeding of Pigments Color and Strength of Color Pigments by Use of a Miniature Sandmill Color and Strength of Color Pigments with a Mechanical Muller Tinting Strength of White Pigments, Relative, by Reflectance Measurements Tinting Strength of White Pigments, Relative, by Visual Observation RESINS AND POLYMERS Lac, Dry Bleached Orange Shellac and Other Indian Lacs for Electrical Insulation Orange Shellac and Other Lacs Shellac Varnishes General Amino Resins, Testing Epoxy Resins, Testing Latex Vehicles, Testing Poly(Vinyl Chloride) Resins, Testing Amino Resins, Free Formaldehyde Content Lac Resins, Sampling and Testing Nitrocellulose Base Solutions, Soluble Shellac for Electrical Insulation, Testing Shellac Varnish, Sampling and Testing Sodium Carboxymethylcellulose Rosin, Sampling and Grading (see Vol 06.03) Alkyd Resins, Testing . Resin Chemical Tests Carboxyl Content of Cellulose -- _ Carboxylic Acids in Alkyd Resins Chlorine Content, Hydrolyzable, in Epoxy Resins Chlorine Content, Total, in Epoxy Resins Epoxy Content of Epoxy Resins - Fatty Adds in Alkyds Glycerol, Glycol, and Pentaerythritol in Alkyds Isocyanate Groups in Urethane Materials or Prepolymers Isophthalic Acid in Alkyd and Polyester Resins Nitrogen, Total, in Resins and Plastics pH, Apparent of Water-Insoluble Phenol-Formaldehyde Resins Phenol, Free, in Phenolic Resins Phenolic Resins, Determining Methylol Group Qualitatively in Fhthalic Anhydride Content of Alkyd Resins and Resin Solutions Phthalic Anhydride in Alkyds and Esters Containing Other Dibasic Acids (Gravimetric) Foly(Vinyl Butyral), Chemical Analysis of Vinyl Chloride Monomer, Residual Content of Poly(Vinyi Chloride) Resins, Compounds,and Copolymers by Solution Injection Technique Rosin Adds Content of Coating Vehicles, Total Rosin in Varnishes, Qualitative Detection Silicon Content of Silicone Polymers and Silicone-Modified Alkyds by Atomic Absorption Unsaponifiabie 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) 831 4 1 -,|ir t `rl 1 m DUP050296391 Test Methodsfor: > 1064 -58(1981) D 464 - 91 D1065 - 82 LIST BY SUBJECTS, VOLUME 06.02 Test Methods for: D 2090 - 88 D 1544 - 80(1989)" Test Methodsfor: D 5097 - 90 D 4758 -87 D 1259-85 (1990)" D4613-86 D 4640 - 86 (1990)" D 4639- 86 (1990)" D 2998-89 D 2456-91 D 3432 - 89 D 4827 - 88 D 4747-87 D 3008 - 90 E 28 - 67 (1982)*1 D 889-58(1987) Practicefor: 0 4209 - 82(1991)" Test Methodsfor: D 3132-84 (1990)" D 1198-88 D 269 - 52 (1987)*1 Definitions Definitions of Terms Relating to: D 804 - 79(1987) Naval Stores and Related Products (see Vol 06.03) CELLULOSE AND CELLULOSE DERIVATIVES 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 D4794- 88 D 914- 72 (1989)" D 2364- 89 D 2363- 79 (1989)" D 1795- 90 D 4085- 81 (1987) D 3876- 79 (1989)" D 1347 - 72 (1989)" D 1348- 89 D4795- 88 D 1787- 89 D 2438- 89 D 1439- 83a (1989)" D 1696-90 D 2929 - 89 D 1343-91 Alcohol-Benzene Soluble Matter in Cellulose (Intent to. Withdraw) Ashing Cellulose Carboxyl Content of Cellulose Cellulose Acetate Propionate and Cellulose Acetate Btityrate, 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 Ethylcellulose Hydroxyethylcellulose ` Hydroxypropyl Methylcellulose . Intrinsic Viscosity of Cellulose ; Metals in Cellulose by Atomic Absorption Spectrophotometry Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography Methylcellulose Moisture in Cellulose Nitrogen Content of Soluble Nitrocellulose--Alternative Method Pentosans in Cellulose Silica in Cellulose Sodium Carboxymethylcellulose Solubility of Cellulose in Sodium Hydroxide Sulfur Content of Cellulosic Materials by X-ray Fluorescence Viscosity of Cellulose Derivatives by Ball-Drop Method 832 ***** m DUP050296392 LIST BY SUBJECTS, VOLUME 06.02 Terminology of: D 1695 -77 (1989)*1 Cellulose and Cellulose Derivatives POLYMERS fj'est Methodsfor: D3536 - 76 (I988)ei D3S93 -- 80 (1986)(1 Molecular Weight Averages and Molecular Weight Distribution by Liquid Exclusion Chromatography (Gel Permeation Chromatography--GPC) (see Vol 08.03) Molecular) Weight Averages and Molecular Weight Distribution of Certain Polymers by Liquid Size- Exclusion Chromatography (Gel Permeation Chromatography--GPC) Using Universal Calibration (see Vol 08.03) Practices for: D37S0- 79(1985) D 2857 - 87 D 4001 - 81 (J986)(1 Number-Average Molecular Weight of Polymers by Membrane Osmometry. Determination cf (see Vol 08.03) Viscosity ofPolymers, Dilute Solution (see Vol 08.02) Weight-Average Molecular Weight ofPolymers by Light Scattering, Determination of(see Vol 08.03) GENERAL STANDARDS |Specifications for: E 100-81(1986) E 1-90 E 133-86 E 11-87 ASTM Hydrometers (see Vol 14.03) ASTM Thermometers (see Vol 14.03) Distillation Equipment (see Vol 14.02) Wire-Cloth Sieves for Testing Purposes (see Vols 04.01, 04.02, 04.06, 05.05, and 14.02) |Tert Methodsfor: E 70-90 pH ofAqueous Solutions with the Glass Electrode (see Vol 15.05) jjPracticesfor: 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 15.05) Standard Solutionsfor Chemical Analysis, Preparation, Standardization, and Storage of(see Vol 15.05) ^jptflnUions 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 `racticefor: 1 E 380-91 Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Material section) 833 DUP050296393 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 separatepublication and which appears in its entirety in Volume 14.02. Deleted are Appendixes XI, X2, XI, and X4. Added is a table ofselected conversionfactorsfrom Appendix X3. CONTENTS Section Scope............................................................................................................................................................. ....................................... SI Units and Symbols........................................................................................................................................................................... Classes of Units................................ Base Units......................................................................................................................................................................................... Supplementary Units .................................................................................................................................................. Derived Units................................................................................................................................................................................... SI Prefixes......................................................................................................................................................................................... Application of the Metric System......................................................................................................................................................... Genera! ............................................................................................................................................................................................. Application of SI Prefixes................................................................................................................................................................. Other Units...................................... Other Recommendations Concerning Units.................................................................................................................................. Style and Usage................................................................................................................................................................................. Rules for Conversion and Rounding................................................................................................................................................... General ............................................................................................................................................................................................. Accuracy and Rounding................................................................................................................................................................... Significant Digits............ .................................................................................................................................................................. Rounding Values.................. Conversion of Linear Dimensions of Interchangeable Parts........................................................ .................................................. Other Units................ .......................................................................................................................................................... ........... Terminology ......................................................................................................................................................................................... Appendixes Development of the International System of Units........................................................................................................................ Organs of the Metre Convention: BIPM, CIPM, CGPM................................................................................................ r-........... Conversion Factors...................................... Supplementary Metric Practice Guides.......................................................................................................................................... Bibliography Index 1 2 2.1 2.2 2.3 2.4 2.5 3 3.1 3.2 3.3 3.4 3.5 4 4.1 4.2 4.3 4.4 4.5 4.6 5 XI X2 X3 X4 1. Scope 1.1 This standard gives guidance for application of The International System of Units (the modernized metric system) developed and maintained by the General Confer ence on Weights and Measures (abbreviated CGPM from the official French name Conference Generate des Poids et Mesures). The name International System of Units and the international abbreviation SI2 were adopted by the 11th CGPM in 1960. 1.2 Information is included on SI, a limited list of non-SI units recognized for use with SI units, and a list of conver sion factors from non-SI to SI units, together with 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 E43.10 on Standards. Current edition approved Oct 3, 1991. Published December 1991. Originally published in 1964 without designation as ASTM Metric Practice Guide, revised 1966. Adopted as standard 1968. Last previous edition E 380 - 89. 2 From the French name, 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- DUP050296394 E 380 TABLE -I Base SI Units Quantity3 Unit length mass time electric current thermodynamic temperature'* amount of substance luminous intensity metre kilogram second ampere kelvin mole candela * For a discussion of Celsius temperature see 3.4.2. Symbol m kg s A K mol cd TABLE 2 Quantity3 plane angle solid angle Supplementary SI Units Unit radian steradlan Symbol rad sionless derived quantities. Therefore, the supplementary units radian and steradian are to be regarded as dimension less derived units which may be used or omitted in the expressions for derived units. 2.4 Derived Units: 2.4.1 Derived units are formed by combining base units, supplementary units, and other derived units according to the algebraic relations linking the corresponding quantities. The symbols for derived units are obtained by means of the mathematical signs for multiplication, division, and use of exponents. For example, the SI unit for velocity is the metre per second (m/s or m*s_I), 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 C-m instead of A-s-m. 2.4.4 Some common derived units are listed in Table 4. 2.5 SI Prefixes {see 3.2 for application): 2.5.1 The prefixes and symbols listed in Table 5 are used to form names and symbols of the decimal multiples and submultiples of the SI units except for kilogram. 2.5.2 Unit ofMass--Among the base and derived units of SI, the unit of mass (kilogram) is the only one whose name, for historical reasons, contains a prefix. Names of decimal multiples and submultiples of the unit of mass are formed by attaching prefixes to the word gram (g). 2.5.3 These prefixes or their-symbols are directly attached to names or symbols of units, forming multiples and submultiples of the units. In strict terms these must be called "multiples and submultiples of SI units," particularly in discussing the coherence of the system (see Section 5). In common parlance, the base units and derived units, along with their multiples and submultiples, are all called SI units. 3. Application of the Metric System 3.1 General--SI is the form of the metric system that is preferred for all applications. It is important that this modernized form of the metric system be thoroughly under- i "Quantity" as used in the headings of the tables of this standard means measurable attribute of phenomena or matter. TABLE 3 Derived SI Units with Special Names Quantity3_________________Unit 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 dose8 dose equivalent hertz newton pascal joule watt coulomb volt farad ohm siemens weber tesla henry degree Celsius'* lumen lux becquerel gray sieved Symbol Hz Formula Vs kg-m/s2 N/m* N-m W/A C/V V/A A/V V.s Wb/ms Wb/A K[sae 3.4.2] cd-sr Im/m2 1/s J/kg 4/kg m * Inclusion In the table of derived SI units with special names approved by the CIPM In 1976. 8 Belated 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--In 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 103 m becomes 12.3 km 0.00t23 fiA becomes 1.23 nA 3.2.2 Selection--When expressing a quantity hy 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, the 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 836 DUP050296395 # E 380 jgggakv' mu?,. Ilk, m Kgpv? mjmff MS. HU:- m HP' 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 field 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 per 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 ] SSiF irradiance | watt per square metre n mb- Ip m?' ' Up iff: H ' 11 1- luminance magnetic field strength molar energy molar entropy molar heat capacity moment of force1' 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 * See 3.4,4. , - candela per square metre ampere per metre ' joule per mole joule pec mole kelvin . joule per mole kelvin newton metre henry per metre farad per metre watt per square metre watt per square metre steradian watt per steradian joule per kilogram kelvin joule per kilogram joule per kilogram kelvin cubic metre perkllogram newton per metre watt per metre kelvin - metre per second pascal second square metre per second. cubic metre 1 per metre Symbol Gy/s m/s2 rad/s3 rad/s mz mo!/m3 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/mol J/(mol-K) J/(mol-K) N-m H/m F/m W/m2 W/fnf-sr) W/sr J/(kg-K) J/kg J/tkg-K) nrykg N/m W/(m-K) m/s Pa-s m2/S'~ m3 1/m Imeasuremeiits and clothing sizes. 3.2.3 Prefixes in Compound Units*--It is Recommended af only one prefix be used in1 forming a multiple of a fcompound unit. Nbrmally the prefix should be attached to a |,unit in the numerator. One exception to this is when the I kilogram occurs in the denominator. \ Examples: : V/m, not mV/mm, and MJ/kg, not kj/g 3.2.4 Compound Prefixes--Compound 'prefixes, formed by the juxtaposition of two or rftore SI prefixes are not to be used. For example, use 1 nm, not l mpm 1 pF, not 1 ppF 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 of Units--An exponent attached to a symbol containing a prefix indicates that the multiple or submultiple of the unit (the unit with its prefix) is raised to the power expressed by the exponent. For example: 4 A compound unit is a derived unit that is expressed in terms of two or more units rather than by a single special name. I cm3 = (10-2 m)3 1 ns-1 = (10-9 s)~` 1 mm2/s = (10--3 m)2/s = 10"6 m3 = 109 s~` -10_6m2/s ~ 3.2.6 Calculations--Errors in calculations- can be mini mized if the base and the coherent derived- SI units are used and the resulting_numerical values are expressed in powers- of-ten notation instead of using prefixes. 3.3 Other Units: -1 3.3.1 Units from Different Systems--To assist in pre serving the advantage of SI as a coherent system, it is advisable to minimize the use with it of units from other systems. Such use should be limited to units listed in this section. 3.3.2 Units in Use with SI (see Table 6): 3.3.2.1 Time--The SI unit of time 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 837 DUP050296396 TABLE S SI Prefixes 3.3.3 Units in Use with SI Temporarily (see Table 7): Multiplication Factor 1 000 000 000 000 000 000 = 10'3 1 000 000 ooo 000 ooo - to16 Prefix exa peta Symbol E p 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 1 000 000 000 000 - 1012 1 000 000 000-= 10 1 000 000 = 10* 1 000 = 10* tera T electric energy. This unit should not be introduced into any glga mega Q M new areas, and eventually it should be replaced by the kilo k megajoule. 100 = 102 10= 101 0.1 = 10-1 0.01 = 10-2 0.001 = 10-* hecto* deka4 deci4 centi* milli h 3.3.3.2 Pressure and Stress--The SI unit of pressure and da d stress is the pascal (newton per square metre) and with . c proper SI prefixes is applicable to all such measurements. m Old metric gravitational units for pressure and stress such as 0.000 001 = 10-* 0.000 000 001 = 10-" 0.000 000 000 001 = 10"12 0.000 000 000 000 001 = 10-'6 micro p kilogram-force per square centimetre (kgf/cm2) shall not be nano pkx> femto n p < used. Widespread use has been made of other non-SI units such as bar and torr for pressure, but this use is strongly 0.000 000 000 000 000 001 = 10-18 atto a discouraged. The millibar is widely used in meteorology, this * To be avoided where practical, except as noted in 3.2.2. usage will continue for the present in order to permit meteorologists to communicate easily within their profes the minute and second is discouraged except for special fields such as cartography. 3.3.2.3 Area--The SI unit of area is the square metre (m2). The hectare (ha) is a special name for square hectometre (hm2). Large land or water areas are generally expressed in hectares or in square kilometres (km2). 3.3.2.4 Volume--The SI unit of volume is the cubic metre. This unit, or one of the regularly formed multiples such as the cubic centimetre, is preferred. The special name /itrc5 (L)6 has been approved for the cubic decimetre, but use of this unit is restricted to volumetric capacity, dry measure, and measure of fluids (both gases and liquids). No prefix other than milli- or micro- should be used with litre. 3.3.2.5 Mass--The SI unit of mass is the kilogram. This unit, or one of the multiples formed by attaching an SI prefix to gram (g), is preferred for all applications. The megagram (Mg) is the appropriate unit for measuring large masses such as have been expressed in tons. However, the name ton has been given to several large mass units that are widely used in commerce and technology--the long ton of 2240 lb, the short ton of 2000 lb, and metric ton of 1000 kg (also railed the tonne). None of these terms are SI. The term metric ton should be restricted to commercial usage, and no prefixes should be used with it. Use of the term tome is deprecated. 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 rases 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 constructedjjy 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 ofthe 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 die unit names formed with- the prefixes ab- and stat-, for example, the abampere, statvolt, etc. 5 See Appendix X1.11.1. 4 The OGPM in October 1979 approved L and 1 as alternative symbols for litre. Since the letter symbol 1 can easily be.confused with the numeral 1, only the symbol L is recommended for USA use. 3.3.4.2 Decimal Multiples of SI Units--Those multiples ofSI 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). TABLE 6 Units In Use with SI______________________3_._3_.4.3 Unit Names to Be Avoided--Special names for Quantity3 Unit Symbol Definition time minute min 1 min 60s hour day h 1 h 60 min = 3600 s d 1 cl * 24 h = 86 400 s week, month, etc. plane angle degree e 1 (ir/180) rad minute4 V (1/60) S3 (r/10 800) rad second4 V * 0/80)' (7t /648 000) rad volume litre L 1 L s 1 dm* = 10-3 m* mass metric ton t 11 = 10*kg area hectare ha 1 ha 33 1 hm2 = 10" m2 A Use discouraged except for special fields such as cartography. sSee 3.3.2.4. TABLE 7 Units In Use with SI Temporarily Quantity3 Unit Symbol Definition ,, energy [see 3.3.3.1] kilowatthour cross section bam pressure [see 3.3.3.2] bar activity (of a radio- curie nuclide) exposure (X and roentgen gamma rays) absorbed dose rad dose equivalent rem kWh b bar a R rd rem 1 kWh = 3.6 MJ 1 b = 10-2* m2 100 fm2 1 bar = 10* Pa 1 Ci - 3.7 X 10' Bq 1 R = 2.58 x 10~4 C/kg 1 rd = 0.01 Gy t rem = 0.01 Sv = 10 mSv DUP050296397 E 380 tiples and submultiples of SI units are to be avoided -pt for the litre (3.3.2.4); metric ton (3.3.2.5), and hectare .2.3). For example, do not use: i........................... I fermi on ........................ 1 micron imicron................. 1 millimicron r............................. 1 are itna........................ 1 gamma '^magnetic flux density) ass)...................1 7 ofume).................IX o........................... 1 mho 'die..........................I candle ilepower..................I candlepower = 1 fm = 10~15 m = 1 pm = 10~6 m = 1 nm = 10-9 m =1 dam2 = 100 m2 = 1 nT = 1 pg = 1 pL = 1 mm3 = 1S = 1 cd = 1 cd 3.3.4.4 Miscellaneous Units--Other non-SI units that are recated include the following: calorie grade {1 grade = (ir/200) rad] kilogram-force langley (= 1 cal/cm2) metric carat metric horsepower millimetre of mercury millimetre, centimetre, metre of water standard atmosphere (1 atm = 101.325 kPa) technical atmosphere (1 at = 98.0665 kPa) torr 3.4 Other Recommendations Concerning Units: 3.4.1 Mass, Force, and Weight: 3.4.1.1 The principal departure of SI from the gravimetric system of metric engineering units is the use of explicitly distinct units for mass and force. In SI, the name kilogram is restricted to the unit of mass, and the kilogram-force (from which the suffix force was in practice often erroneously dropped) should not be used. In its place the SI unit of force, the newton, is used (see Fig. 1). Likewise, the newton rather than the kilogram-force 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 ofa 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 Iks FIG. 1 Illustration of Difference Between Mass (Unit = kilogram = kg) and Force (Unit = newton = N) (see 3.4.1) 839 DUP050296398 / # E 380 the force that, if applied to the body, would give it an acceleration equal to the local acceleration of free fall. The adjective "local" in the phrase "local acceleratidn 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 of gravity") with observed values ofg 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 of gravity acting on a mass may be expressed in mass units. Any other load is expressed in force units. 3.4.2 Temperature--The SI unit of thermodynamic tem perature is the kelvin (K), and this unit is properly used for expressing thermodynamic temperature and temperature intervals. Wide use is also made of the degree Celsius (C), which 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 (/) is related to thermodynamic tem perature (T) by the equation: r-T0 where T0 = 273.15 K by definition. The International Practical Temperature Scale (IPTS) must be recognized in temperature work of extreme precision. See ASTM STP 565, Evolution of the International Practical Temperature Scale of 1968. 3.4.3 Linear Dimensions: 3.4.3.1 Nominal dimensions name the item; no SI equiv alent is required (see Section 5 for definition of "nominal value"). For example, there is nothing "1 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, in Sch Sch 40 80 ScJ> /:`lj 1 1.315 0.133 0.179 ojsfg <33AO) (3.38) (4.55) .(6.351.' Likewise, a "2 by 4" is that in name only and refers to I approximate dimensions in inches of a rough-sawn pie green lumber, the finished dimensions of which are con erably less. A >/4-20 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 minor7 diameters of a screw thread, should be converted to SI valued * in accordance with 4.1 and 4.2. 3.4.3.2 Surface texture should be expressed in microm-1 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 oe 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 (/ = 2mrz). Its SI unit is kg-m2. 3.4.4.4 Angular Momentum (moment of momentum) is linear momentum (kg-m/s) titties 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 <u (rad/s or 1/s). 3.4.4.5 Rotational Kinetic Energy of a rotating body is equal to 'hlu2. 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). Its SI unit is N -m/rad. 3.4.4.8 Centripetal Acceleration, v2/r or o>2r, where v is the tangential Unear velocity (m/s), r the radius (m), and v the angular velocity_(rad/s) is, Uke any other Unear acceleration, measured in SI units m/s2. No t h --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: 840 DUP050296399 E 380 3.4.7.1 The values of so-called dimensionless quantities, as for example refractive index and relative permeability, are xpressed by pure numbers. In these cases the corresponding $1 unit is the ratio of the same two SI units and may be Ixpressed by the number 1. If 3.4.7.2 Terms such as percent, parts per thousand, and parts per million may also be used, y 3.4.7.3 In all cases, the meaning must be unequivocal. lExpressions like "The mole fraction of C02 in the sample Jwas 1.2 parts per million" or "The mass fraction of C02 in lithe sample was 1.2 parts per million" are permissible, but jpvould 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 psymbols properly, and international agreement provides f'uniform rules. Handling of unit names varies because of 1 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 35mm, and 2.37 lm (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.! With unit names: Product, use a space (preferred) or hyphen: newton metre or newton-metre In the case of the watt hour the space may be omitted, thus: watthour Quotient, use the word per and not a solidus: metre per second, not metre/second Powers, use the modifier squared or cubed placed after the unit name: metre per second squared In the case of area or volume, the modifier may be placed before the unit name: square millimetre, cubic metre This alternative is also allowed for derived units'that include area or volume: watt per square metre * No t e--To avoid ambiguity in complicated expressions, symbols are preferred over words. 3.5.3.2 With unit symbols: Product, use a raised dot: N-m for newton metre In the case of W-h, the dot may be omitted, thus: Wh An exception to this practice is made for computer print outs, automatic typewriter work, etc., where the raised dot is not possible, and a dot on the line may be used. Quotient, use one of the following forms: m/s or m*s * orj In no case should more than one solidus be used in the same 841 DUP050296400 E 380 expression unless parentheses are inserted to avoid ambi guity. For example, write: J/(mol-K) or J-raor'-K-1 or(J/mol)/K, but not J/mol/K 3.5.3.3 Symbols and unit names should not be mixed in the same expression. Write: joules per kilogram or J/kg or J-kg~` but not joules/kilogram nor joules/kg nor joules: kg-1 3.5.4 Numbers: 3.5.4.1 The recommended decimal marker is a dot on the line. When writing numbers less than one, a zero should be written before the decimal marker. 3.5.4.2 Outside the United States, the comma is often used as a decimal marker. In some applications, therefore, the common practice in the United States of using the comma to separate digits into groups of three (as in 23,478) may cause ambiguity. To avoid this potential source of confusion, recommended international practice calls for separating the digits into groups of three, counting from the decimal point toward the left and the right, and using a small space to separate the groups. In numbers of four digits on either side of the decimal point the space is usually not necessary, except for uniformity in tables. Examples: 2.141 596 73 722 7372 0.1335 Where this practice is followed, the space should be narrow (approximately the width of the letter "i"), and the width of the space should be constant even if, as is often the case in printing, variable-width spacing is used between words. Exceptions: In certain specialized applications, such as engineering drawings and financial statements, the practice of using a space for a separator is not customary. 3.5.4.3 Because billion means a thousand million (prefix giga) in the United 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 of cubic feet, or in MCM for thousands ofcircular mils, ofMM 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" symbol followed by a space and the modifier in pa- ei;i'h For example: V (ac) and V (dc); kPa (gage) and'5$&g& (absolute). - eSST- 3.5.6 Pronunciation--Some recommended PTonuvdmmtions in English are shown in Table 8. 4. Rules for Conversion and Rounding 4.1 General; 'flL, nii* 4.1.1 Conversion factors to change a value of a quantities expressed in non-SI units to the corresponding value of thah$t quantity expressed in the International System ofUnits ihay^'- be exact or approximations adequate for the particular^sfcf;$; 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 concerning significant digits see 4.3.) For example, a length of 125 ft converts exactly to 38.1 m. If, however, the 125-ft length had been obtained by rounding to the nearest 5 ft, the conversion should be given as 38 m; and if it had been obtained by rounding to the nearest 25 ft, the conversion should be given as 40 m. 4.1.3 Proper conversion procedure is to multiply a value by a conversion factor that is more accurate than is required; the result is then rounded to the appropriate number of sig nificant digits. For example, to convert 3 feet 29/i6 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 PrefixPronunciation (USA)* - exa................. ........................................ex' a (a as in about) peta....................................................... pet' a (e as in pet, a as in about) tera....................................................... as in terra firma _ giga....................................................... jig' a (/ as irl j/g, a as lit about) mega.....................................................as in megaphone kilo......................................................... kill' oh hecto.....................................................heck' toe deka....................................................... deck' a (a as in about) ded....................................................... asindac/mal centi....................................................... as in centipede milll......................................................... as in mfl/tary micro..................................................... as in microphone nano....................................................... nan' oh (an as in ant) pico....................................................... peek' oh femto.....................................................fern' toe (fem as fit feminine) atto....................................................... as in anatomy_______ _________ Selected Units Pronunciation candela................................................... can dell' a joule....................................................... rhyme with too/ kilometre.................................................kffl' oh metre pascal..................................................... rhyme with rascal siemens................................................. 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, not the second. 842 DUP050296401 I value may be expressed by a multiple or submultiple unit of I by the use ofan appropriate prefix, for example, 979 mm. 4.2Accuracy and Rounding--A conversion obtained by ultiplying a value by a seven-digit factor usually gives a roduct with more digits than the original value. The onverted 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 he original value. The practical aspect of measuring must be onsidered when using SI equivalents. If a scale having ''`vision of Vie inch was suitable for making the original 'easurements, a metric scale having divisions of 1 mm is bviously suitable for measuring in SI units. Similarly, a gage ;r caliper graduated in divisions of 0.02 mm is comparable one graduated in divisions of 0.001 in. Analogous situations exist in mass, force, and other measurements. any techniques are 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 bf 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 iretain. This precision should relate to the number ofdigits 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 lVi6 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 lh 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/in? (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; V/t in = 47.625 nun exact 47.6 mm normal rounding 47.S 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 rounded from 999.7, in which case all three zeros are significant. -- 4.3.4 Occasionally data required for an investigation must 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 The total 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 DUP0502 96402 # E 380 The total is then rounded to All 000 000 as called for by the rule. Note that if the second of the figures to be added had been 217 985 000, the rounding before addition would have produced 218 000 000, in which case the 0 following 218 would have been a significant digit. 4.3.4.2 The rule for multiplication and division is that the product or quotient shall contain no more significant digits than are contained in the number with the fewest significant digits used in the multiplication or division. The difference between this rule and the rule for addition and subtraction should be noted; the latter rule merely requires rounding of digits that lie to the right of the last significant digit in the least precise number. The following illustration highlights this difference: Multiplication: 113.2 x 1.43 = 161.876, rounded to 162 Division: 113.2 -4- 1.43 = 79.16, rounded to 79.2 Addition: 113.2 + 1.43 = 114.63, rounded to 114.6 Subtraction: 113.2 - 1.43 = 111.77, rounded to 111.8 The above product and quotient are limited to three signifi cant digits since 1.43 contains only three significant digits. In contrast, the rounded answers in the addition and subtrac tion examples contain four significant digits. 4.3.4.3 Numbers used in the above illustrations have all been estimates or measurements. Numbers that are exact counts are treated as though they consist of an infinite number of significant digits. More simply stated, when a count is used in computation with a measurement the number of significant digits in the answer is the same as the number of significant digits in the measurement. If a count of 40 is multiplied by a measurement of 10.2, the product is 408. However, if 40 were an estimate accurate only to the nearest 10, and hence contained but one significant digit, the product would be 400. 4.4 Rounding Values1: 4.4.1 When a figure is to be rounded to fewer'digits than the total number available, the procedure should be as follows: 4.4.1.1 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 Intercht Parts--The use of the exact relation 1 in = 25,4 mm generally produces converted values containing more dec-' imal places than are required for the desired accuracy. It is therefore necessary to round these values suitably and at toe 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 of the 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: 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 differencehetween 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 % of the tolerance and 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). (c) Round each limit toward the interior of the tolerance, that is, to the next lower value for the upper limit and to the next higher value for the lower limit.8 Examples: 7 Adapted from ISO R370 (7). 8 If the digits to be rounded are zeros, the retained digits remain unchanged. 844 m DUP050296403 E 380 I dimension is expressed in inches as............... 1.950 0.016 he limits are................................................... 1.934 and 1.966 inversion of the two limits into millimetres ; gives............... ......................................... . 49.1236 and 49.9364 Method A--The tolerance equals 0.032 in and P 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 f '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..........................................;........... <. Ulus reduces the tolerance to 0.80 instead of 0.82 mm given by Method A. 4.5.2 Special Methodfor Dimensions with Plus andMinus deviations--In order to avoid accumulation of rounding Hrrors, the two limits of size normally are converted sepaately: thus, they must first be calculated if the dimension ponsists of a basic size and two deviations. However (except vhen Method B is specified) as an alternative, the basic size ay be converted to the nearest rounded value and each of he deviations converted toward the interior of the tolerance, his method, which sometimes makes conversion easier, gives the same maximum guarantee of accuracy as Method 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 Jaccuracy of measurement, limits that are acceptable for (interchangeability must be determined separately for the jdimensions. For example, where accuracy of measurement is llimited to 0.001 mm, study shows that values converted jjfrom 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 Idisadvantage, 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 I 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 i in a plane, the position of which is given by nontoleranced , basic or gage dimension, such as when dimensioning certain f 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. (c) Round these limits in conformity with the rales in 4.4. For example, a cone of taper 0.05 in/in has a diameter of 1.000 0.002 inch in a reference plane located by the nontoleranced dimension 0.9300 in. By virtue of the taper of the cone, the limits of the tolerance zone depend on the position of the reference plane. Consequently, if the dimen 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 or degrees Celsius is given below: Conversion ofTemperature Tolerance Requirements Tolerance, T Tolerance, K or C 2 (1) 4 (2) 10 (5) 20 (10) 30 (15) 40 (20) 50 (25) 1 (0.5) 2(1) 6 (3) 11 (5.5) 17 (8.5) 22 (11) 28 (14) Normally, temperatures expressed in a whole-number of degrees Fahrenheit should be converted to the nearest 0.5 kelvin (or degree Celsius). As with other-quantities, the number of significant digits to retain will depend upon implied accuracy of the original dimension, for example: 100 5F; implied accuracy estimated to be 2T. 37.7777 2.7777C rounds to 38 3*C. 1000 SOT; implied accuracy estimated to be 2QF. 537.7777 27.7777'C rounds to 540 30*C. 4.6.2 Pressure or Stress--As with other, quantities, pj-esr sure or stress values may be converted by the principle given above. Values with an uncertainty of more than 2 % may be converted without rounding by approximate factors: 1 lbf/in2 (1 psi) = 7 kN/m2 = 7 kPa 5. Terminology 5.1 To help ensure consistently reliable conversion and rounding practices, a clear understanding of the related nontechnical terms is a prerequisite. TABLE 9 Rounding Tolerances Inches to Millimetres - Original Tolerance, inches at least less than Fineness of Rounding, mm 0.000 04 0.000 4 0.004 0.04 0.4 0.000 0.004 0.04 0.4 0.0001 0.001 0.01 0.1 1 845 mm DU P050296404 E 380 5.2 Certain terms used in this standard are defined as follows: accuracy (as distinguished from precision)--the degree of conformity of a measured or calculated value to some recognized standard or specified value. This concept involves the systematic error of an operation, which is seldom negligible. approximate value--a value that is nearly but not exactly correct or accurate. coherent system of units--a system of units of measure ment in which a small number of base units, defined as dimensionally independent, are used to derive all- other units in the system by rules of multiplication and division with no numerical factors other than unity (see Appendix XI.9). deviation--variation from a specified dimension or design requirement, usually defining upper and lower limits (see also tolerance). digit--one of the ten arabic numerals (0 to 9). dimension--a geometric element in a design, such as length or angle, or the magnitude of such a quantity. feature--an individual characteristic of a part, such 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 th 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 j. 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. DUP050296405 E 380 E 380 SELECTED CONVERSION FACTORS To convert from nosphere (760 mm Hg) ard foot tu (International Table) tu (International Table)/h tu (International Table) in./s-ft2**F (k, thermal con ductivity) llorie (International Table) ntipoise `entistokes 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 (Fa) 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) multiply by 1.013 25 x 10s ' 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* 10~6 5.067 075 X 10_!0 ;C = (rF- 32)/1.8 3.048 000* x 10"1 9.290 304* 10~2 2.831 685 X 10~2 1.355 818 2.259 697 X 10~2 3.048 000* 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"4 1.638 706 x 10~5 3.376 85 X 103 2.488 4 X 102 9.806 650* X 104 4.448 222 X 103 6.894 757 X 106 2.957 353 X 10~3 2.780 139 X 10_l 2.834 952 x I0~2 3.051 517 x lO-1 31390 575 x 10"2 7.489 152 . 4.731 765 x 10~4 4.448 222 4.535 924 X 10_1 6.894 757 x 10? 2.767 990 x 104 -1.601 846 x. 10 9.463 529 X I O'4 9.071 847 X 102 1.333 22 x 102 3.600 000* X 103 9.144 000* X 10_1 8.361 274 X 10_l 7.645 549 X 10"1 847 Condensed Index of Committee D-l Standards--1992* 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 biast abrasive test, 1X558(1) falling sand/abrasive test, D968(l> Taber Abraser test, D4060( 1) wear resistance, of traffic paint, D913{1) wet abiasion/scrubbing, D2486,4213(1) Accelerated exposure tests See Exposure - accelerated Acetaldehyde acetaldehyde, spec., D47M)(3) acidity, test, D2086(3> Acetate ester solvents purity, alcohol content, 03545(2) Sa Amyl acetate n*Butyl acetate Ethyl acetate Hexyl acetate Isobutyl acetate Isopropyl acetate Methyl amyl acetate n*Propyl acetate Sa Glycol ether acetates Acetic acid (glacial) formic acid in glacial acetic acid. 53546(3) specification, D362CK3) Acetone acetone tolerance, of bodied oils, D1950C3) alkalinity, test, D1614(3) permanganate time, lest, D 1363(3) specification, D329(3) Acetylene black, See Carbon black Acidity/alkalinity, (pH) acetaldehyde, spec., D4710<3) acetone, test, D1613,1614(3) chemically cleaned/etched concrete, 04262(1) electrocoat baths, 04584(1) fatty quaternary ammon. chlorides, 02081(3) formaldehyde solutions, test, D2379(3) hydroxypropyl methylcellulose, 02363(2) milliequivalence, electrocoat baths, D4370(l) phenol-formaldehyde, D4613(3) pigments, D1208(2) volatile solvents, D1613(3) Acid number (value) fatty acids, D1980{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, D803(3). turpentine and pinene, test, 0233(3) 5 a Saponification number Add resistance (of paints/related coatings) dear coatings on aluminum, test, 03260(1) Acrylate esters, purity, 03362(3) Acrylic acid dimer content, 04415(3) specification, 04416(3) Acrylic emulsion paints, See Artists' Paints Adhesion/Cohesion by cut tape test,D3359(l) Dillon dynometer test; D4796(l) HIPAC coatings, 03730(1) portable tester, puil-off strength, D4S4K1) prepainted fabricated metal, 04145(1) scrape test on smootjrsurfaces, 02197(1) traffic marking paints, materials,.D4796{1) zinc-rich primer on steel, 04146(1) Air blast abrasion fester, 0658(1) Alcohol resistance, furniture lacquer, 02571(1) Alcohol solvents See Amyl alcohol, D319(3) n-Butyl alcohol (1-Butanol), 0304(3) sec-Butyl alcohol (2-Butanol), 01007(3) 2-Ethylhexanol, D500SO) Isobutyl alcohol (isobutanol), 01719(3) Isopropyl alcohol (isopropanol), 0770(3) Methyl isobuty! carbinol, 02635(3) Methanol (Methyl alcohol), 01152(3) n-Propyl alcohol (n-propanol), D3622(3) Aldehydes, purity, test, 02192(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 acid content, D2690(2) phthalic anhydride content, 0563, 01306(2) polyhydric alcohol, 01615, 2456, 2998(2) Alkyds/alkyd resins (cont'd) rosin add content, D1469(2) silicon content, 03733(2) ^ test methods, selection of, 02689(2) unsaportifiable matter content, 01397(2) Sa Paints, solvent-reducible Aluminum (metal surfaces) add/mortarresistance^/ coatings,D326(Xl) preparation for painting, 01730,01731(1) Aluminum powder and paste sampling /testing, 0480(2) specification, 0962(2) Aluminum silicate (anhydrous) analysis, 0718(2) specification, 03619(2) 5 a Pigments, general propertied Aluminum silicate (hydrous) * analysis, 0718(2) specification, 0603(2) $ a Pigments, general properties Amidoamines, See Fatty amines Amino resins free formaldehyde content, 01979(3) test procedures, practice, 04277(2) nitrogen content, 01013(2) solvent tolerance test, 01198(2) Amines/amine values See Fatty amines Fatty quatemary/amine chlorides Amyl acetate, synthetic primary, 03540(3) Amyl alcohol (synthetic), spec., 0319(3) Analysts See Chemical analysis Aniline sampling and handling, practice, 03436 (3) specification, 03264(3) 848 DUP050296407 Condensed Index of Committee D-1 Standards Aniline point j dipentenev related terpene solvents, D801(3) < petroleum hydrocarbon solvents,D611(3) iAnti-corrosion pigments $ ee Basic lead siHcochromate Red lead Strontium chromate Tribasic lead phosphosilicate Zinc chromate Zinc dust Zinc hydroxy phosphite ; Anti-fouling pigments See Copper powder Cuprous oxide Mercuric oxide Anti-fouling paints, submergence test D3263(l) erosion test, high velocity water, D4938(l) erosion test, rotating drum, D4939(l) organotin release rate, D5108(l) Anti-fungal pigments S ee Calcium borosilicate Zinc Oxide Antimony oxide analysis, D2350(2) analysis by spectrophotometry, 03717(1) $a Pigments,general properties Anti-sag meter, multinotch blade, D4400(1) Applicators, film See% Film application/applicators Architectural paints and coatings block resistance, 04946(1) color permanence, white enamels, 01543(1) brushability (brush drag), D4958(l) efflorescence of wall paints, D1736C1) film failures, exterior latex paint, 01848(1) film porosity, 03258(1) freeze-thaw resistance, 02243(1) gloss or sheen uniformity, 03928(1) gloss terminology & definitions,in prep, guides for testing architectural coatings: exterior paints, solvent-borne, D3323(1) water-borne, 03129(1) flat paints, solvent-borne, 03323(1) water-borne, 02431(1) floor paints, solvent-borne, 03383(1) water-borne, 03358(1) gloss and S/G, solvent-bome, 03425(1) water-borne, 04540(1) high performance (HIPAC), 03730(1) solvent-bome (general), 05146(1) water-borne (general), in prep, guide for purchasing: state and institutional, D3927(l) hiding power: brush application, visual, D344?l) drawdown, reflectometric, D28050Q roller application, visual, in prep, wet-to-dry hiding change, 05007(1) leveling, D4062(l) minimum film formation temp., D2345(l) package stability, 01849(1) porosity of films, 03258(1) print resistance, D4207(l) roller spatter, resistance to, 04707(1) sag resistance, 04400(1) washabiiity: soilant, mechanical test, 03450(1) practical multi-stain test, 04828(1) wet abrasion (scrub) resistance: scrub-to-failure test, 02486(1) weight-loss test, 04213(1) Aromatic hydrocarbon solvents See High-flash aromatic naphtha Toluene Xylene Arsenic content, in paint, 02348(1) Artists' paints drawdowns, preparation of, 04941(1) labeling for health hazards, 04236(1) lightfastness of pigments, 04303(1) specifications acrylic emulsion, D5098(1) oil, acrylic, alkyd, resin-oil, 04302(1) water colors, D5067(l) tinting strength, 04838(1) Asbestine See Magnesium silicate Atlas Weatherometer, 05031(1) Automotive painting spray transfer efficiency, 05066(1) Bacterial resistance See Biodeterioration Baking, effect of overbaking, 02454(1) Ball drop method, for viscosity ,01343(2) Barium sulfate (barite, barytes) analysis, 0715(2) specification, 0602(2) S a Pigments, general properties Basic carbonate white lead analysis, 01301(2) specification, 081(2) S a Pigments, general properties Basic lead silicochromate analysis, 01844(2) specification, 01648(2) S a Pigments, genera! properties Basic sulfate white lead analysis, 01301(2) 5 a Pigments, general properties Bend testing mandrel bend test, 0522(1) Berlin white See Basic carbonate white lead Biocidal pigments See Anti-fouling pigments Anti-fungal pigments Biodeterioration (microbiological attack) emulsion paints in container, 02574(1) paint films: discoloration - exterior exposure, D3456(l) mold - environmental chamber, 03273(1) removal of fungal/algal growth, 04610 (1) soil/dirt/fungal accumulation, 03274(1) Sj j Anti-fouling paints Bituminous materials water content, by distillation, D95(l) Black box exposure test accelerated outdoor exposure, D4141(l) 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, 04417(1) Bleeding (bleed resistance) See Pigments-general properties Traffic paint Blistering (Blister resistance) pictorial standards/evaluation, D714(l) water condensation test, D4585U) water fog test 01735(1) Blocking (block resistance) of architectural coatings, 04946(1) lacquers on metal substrates 03003(1) on wood substrates 02793(1) Blue pigments, mixture, analysis of, D1135(2) Sa Iron blue Phthalocyanine blue Ultramarine blue Boiled oils (drying) See Linseed oil Bonding strength. See Adhesion/cohesion Bone black solvent extractable matter, 0305(2) spec., 0210(2) 5a 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,raw and burnt 5 a Pigments, general properties Brunswick blue See Iron blue Brunswick green See Chrome green Brushability (Brush drag) Manual application test, 04958(1) High shear (ICI) viscosity, 04287(1) Brushes,paint See Paintbrushes Bubble time method See Viscometers Burning Characteristics of liquid ingredients Equilibrium method, closed cup fiash/no Bash, 03934(3) flash point, 03941(3) Pensky-Martens (closed cup), 093(1,3) Seta flash tester (closed cup), 03278(3) Seta flash tester (open cup) 04206(3) Sustained burning test, 04206,4207(3) Tag,closed cup, flash point, 056(3) Tag, open cup, flash/fire point, 01310(3) Wick test, 04207(3) of paints/coatings char index, cabinet method, 01360(1) 2-foot tunnel method, 03806(1) Burnt sienna/umber Sec Sienna, burnt and raw Umber, burnt and raw 1- Butanol See n-Butyl alcohol 2- Butanol See scc-Methyl ethyl alcohol 2-Butanone See Methyl ethyl ketone 2-Butoxy ethanol, spec., 0330(3) Butyl acetate alcohol content/purity, 03545(3) specification, 04615(3) Butyl acrylate _` purity tes t, D3362(3) specification, D3547(3) Butyl acrylate/methacrylate monomer content of latexes, 04747(2) n-Butyl alcohol, specification, D304(3) v sec-Butyl alcohol, spec., 01007(3) Butyl glycol See 2-Butoxyethano! Butyral content cellulose acetate butyrates, test, D817(2) Cadmium content in low concentrations in paint, D3335(l) Calcium borosilicate analysis, 04487(2) specification, 04288(2) 5 a Pigments, general properties Calcium carbonate specification, Dll99(2) Sa' Pigments,genera! properties Calcium content cellulose pulp (from wood/cotton), 04085(2) paint driers, by EDTA method, 02613(3) Calcium paint driers See Driers 849 DUP050296408 Condensed Index of Committee D-1 Standards Carbon-arc lamps See Exposure, accelerated Carbon black pigment for paint, spec., D561(2) solvent extractable material, 0305(2) Sa Pigments, general properties Carboxyl content of cellulose, 01926(2) Carboxymethyl cellulose, sodium, D1439(2) Carboxylic acids, identification in alkyd resins, D2455(2) Castor oil, dehydrated specification, 0961(3) <Sene value, 01358(3) 5a Fatty oils Castor oil, raw specification, P960(3) hydroxyl content, 01957(3) Sa Fatty oils Caulking/glazing compounds and sealants viscosity, falling-rod-viscometer, 04040(1) Cellulose and cellulose derivatives acetate, butyrate and proprionate, DS17<2) alcohol-benzene-soluble content, 01729(2) ashing, test methods, D3516(2) carboxyl content, test, D1926(2) cellulose acetate, test, 0871(2), 0365(2) cellulose nitrate, See Nitrocellulose chain length uniformity, 01716(2) chlorine content test, 02641(2) chromatographic analysis, 01915(2) cold check resistance, lacquers, 01211(1) definition of terms, D1695(2) dichloromethane-soluble matter, 03971(2) ethoxyl substitution in cellulose, D4794(2> ethyl cellulose (EC) plastics, 0914(2) ethyl cellulose pulp, metals content 04085(2) hydroxyethyl cellulose, D2364(2) hydroxypropyl methylcellulose, D 2363(2) hydroxypropyl substitution, D3876(2) methoxy substitution, 03876(2) methylcellulose, test methods, 01347(2) moisture content, test, 01348(2) nitrocellulose. See Nitrocellulose silica content test 02438(2) sodium carboxymethylcellulose, D1439(2) solubility in sodium hydroxide, 01696(2) sulfur content, D2929C2) viscosity, ball-drop method, 01343(2) viscosity, intrinsic, 01795(2) volatile/non-volatile of solutions, D4209(2) Centrifuge, See Vehicle separation Cerium paint driers. See Driers Certification of conformance, form, D5063(l) Chalk, See Calcium carbonate Chalking, exterior paints, D659, D4fl4(D Channel black See Carbon black Char index See Burning characteristics Checking (check resistance) exterior paints, test 0660(1) 5 a Cold checking Chemical Analysis See Pigments, analysis White pigments, analysis Chemical resistance, to: acid & mortar, of coated aluminum, 03260(1) alkali, of varnish films, D1647(1) alcohol, of wood furniture lacquers, 02571(1) household chemicals, of coatings, 01308(1) 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, 0913(1) Chlorinated phenol preservative content in wood products, 02921(1) Chlorine content cellulose, test, 02641(2) epoxy resins/compounds, test, 04301(2) hydro!yzable,of liquid epoxy resins, D1726(2) polyvinyl chloride, D1156(2) toluene diisocyanate, Dl638<3) total, of liquid epoxy resins, 01847(2) Chromaticity, See Color Chromatography See individual analysis references Chrome green analysts, D126(2) spedfication, 0212(2) Sa Pigments (general properties) Chrome yellow and orange analysis, 0126(2) specification, 0211(2) 5a Pigments, general properties Chromium content - low concentrations in air particulate filter samples, D435$(2) in paint, D3718(l) Chromium oxide green analysis, 0126(2) specification, 0263(2) Sa Pigments (general properties) Chromium pigments See Chrome green Chrome yellow and orange Chromium oxidegreen. Lead sUicochromate, Strontium chromate Zinc chromate CIE color system See Color-opaque materials Citron yellow See Strontium Chromate Clarity/cleaniihess of paint and ink liquids, D209O (3) Clay, See Aluminum silicate Cioudpoint aromatic hydrocarbon solvents, 04790(3) Coalescence latex paint films, low temperature, 03793(1) Coarse particle analysis See Dispersion (of pigments) Particle size (analysis/distributioaK Cobalt content paint driers, by EDTA method, 02373(3) paint, in low concentrations, D3335(l> liquid drier, analysis, 0564(3) Coconut oil. See Fatty acids, tests, specs. Coefficient of friction See Slip resistance Coefficient of retroreflection See Retroreflection/retroreflectors Coffee stains, resistance to of furniture lacquer, 02571(1) Cohesion, See Adhesion/Cohesion Coil coatings wire-wound bar application, 04717(1) guide for testing, 03794(1) Cologne yellow. See Chrome yellow Cold checking of nitrocellulose lacquers, 01211(1) Color See Color opaque materials Color retention Color - transparent liquids and solids Color--opaque materials CIE color system, E308&4.02) color difference,instrumental, 02244(1) Colour Index, artist pigments, 04302(1), defining and evaluating'tolerances, D3l34(ij! evaluating color change,gray scales 02616(1) metamerism, visual evaluation, 04086(1) Munsell system, 01535(1) tristimulus values, 02244(1) visual evaluation of differences, Dl729(l) Color retention discoloration: microbiological discoloration, D 3456(1) dear coatings in sunlight, 02620(1) household chemicals, effect of, 01308(1) white architectural enamels, 01543(1) light fastness (fading): . ' pigments in artists paints, 04303(1) ' printed matter, D3424(l) Color - transparent, liquids and solids Gardner color scale, 01544 (1,2,3) standard solutions for color tests: caramel/platinum-cobalt, 0365(2) platinum-cobalt scale 01209(1,3) Compatibility, coatings, Patch test, 05064(1) Concrete and masonry test panels, 01743(1) pH, chemically cleaned/etched, D4262(l) surface cleaning (for coating), D4261,4258(1) Conditioning^nvironment for testing,D3924(l) Conductance and conductivity of electrocoat baths, 04399(1) Cone-and-plate viscometers Sec Viscometers, IC1 Conformance/certification of, 05063(1) Conjugated oils See Dehydrated castor oil Oiticica oil Tung oil Sa Fatty oils, conjugateddiene value Consistency, by Stormer viscometer, 0562(1) Contrast ratio , .^ hiding power by reflectometry, 02805(1) Copal content, of lac resins See Shellac-copal resin content Copper content cellulose pulp (from wood/cotton), D4085(2) copper pigments, test, 0283(2) pine tars and pine tar oils, 0856(3) Copper-corrosion ....... in aromatic solvents^0849(3) in dipentene-& related terpenes, 0801(3) ' in petroleum products,D130(3) Sa Exposure tests Copper phthalocyanine blue and green See Phthalocyanine blue < Phthalocyanine green Copper powder analysis, 0283(2) specification, 0964(2) Sa 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 Paint rollers, covers Cracking (crack resistance) exterior paints, evaluating, 0661(1) mandrel bend test, 0522(1) Cross-cut, cross-hatch tape test adhesion of paint, test, 03359(1) Cuprous oxide analysis, 0283(2) specification, 0912(2) See Pigments, general properties 850 DUP050296409 Condensed Index of Committee D-1 Standards pre time, thermosetting resins, D4640(2) Sa Drying/curing pairtain coating, water reducible,, D4712<1) lark chrome yellow See Chrome yellow and orange itions of terms related to paint, varnish, etc., D16<1,2,3) hydrated castor oil See Castor oil, dehydrated Fatty acids - tests, specifications msity--apparent (bulk) hydroxyethelcellulose, 02364(2) I hydroxypropyl methylcellulose, D2363(2) methylcellulose, D1347(2) 1 sodium carboxymethylcellulose, D1439(2) nsity-true f dipentene/terpene solvents, D801(3) industrial aromatics, D2935(3) ] paints and related coatings, D1475(1) | paint liquids, 01963(3) pigments, tests, D153(2) pine oil, D8C2(3) pine tars and oils, D856(3) turpentine and pinene, D233(3) Deposition efficiency of powder coatings, D3451(l) ^Detergent resistance, D2248(l) ;Dewcycle. See Exposure tests-accelerated Diacetone alcohol, spec., D2627(3) Diamines, See Fatty diamines Diatomaceous silica. See Silica Ipibutyl phthaiafe, spec, D608(3) Dichlormethane, determination of by gas chromatography, D44S7(1) Diethlene glycol, spec. D2694(3) !i Dilion Dynamometer^ See Adhesion/cohesion Dilution ratio/DilixtabUity cellulose nitrate solutions,Dl720(3) cellulose nitrate, with toluene, 0301(2) resin solutions, 05062(3) } Dimethyl ketone. See Acetone Dip application water reducible coatings, D4717<1) Dipentene (and related terpene solvents) sampling and testing, D801(3) Dipropylene glycol specification, D2696(3) Dipropylene glycol monomethyl ether (DPGME) specification. 04836(3) purity, D4773(3> Dip-type viscosity cups. See Viscometers Directional reflectance See Reflectance and reflectivity Dirt/Soil resistance exterior white coatings, D3719(l) practical washability, D4S28C1) ivashability, mechanical test, D3450 Disbonding--cathodic pipeline coatings, cyclic temperatures, C42(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, phthalo blue, D963(2) in pigment-vehicle systems, D1210(l) in printing inks, NPERI grindometer, D1316(l) in titanium dioxide slurries, D3926(2> Distillation dipentene, terpene solvents, 0801(3) distillation range, D1078C3) ethyl acetate, spec.,D4614(3) in vacuum, solvent-type paints, D3272(l) petroleum products, 086(3) pine oil, D802(3) pine tars and tar oils, D856(3) turpentine and pinene, D233(3) Dolomite, See Calcium carbonate Draft test, varnish films, 01643(1) Drawdown bars and rods Sec Film application/applicators Draw-down tests, multi-notch applicators leveling characteristics of paints, D4062(l) leveling of paints, D2801 (discontinued) sag resistance of paints, D440CK1) Driers calcium/zinc content, EDTA, D2613(3) cerium content, test, D3970(3) clarity/cleanness, visual, 02190(1,3) cobalt content EDTA method, 02373(3) iron content EDTA method, D2374(3) manganese content EDTA method, D2375{3) rare earths content, EDTA method, D3989(3) selection of test methods, D564C3) specification, D600(3) vanadium content, EDTA method, D39S8(3) volatUe/nonvolatile content, 04140(3) zirconium content EDTA method, D3969(3) Drop black. See B one black Dry film thickness,5er Film, thickness, dry film Drying oils. See Fatty oils Drying/curing cellulose nitrate, D301(2) MEK resistance, zinc-rich primers, D4752(l) room temperature, film formulation, Dl643(1) shellac varnish, D1650(2) temperature during curing by I.R., D3259(l) 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 EDTA method, paint driers calcium content, D2613(3) cobalt content, 02373(3) iron content, 03904(3) lead content, D2374(3) manganese content, D2375(3) rare earths content, D39390) vanadium content, D3988(3) zinc content, D2613(3) zirconium content/ 03969(3) Efficiency See Deposition efficiency (powder coatings) Transfer efficiency-spray application Efflorescence exterior latex paints, Dl848(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-reducible coatings, D4712(l) Elongation mandrel bend test, 0522(1) tensile strength/stiffness,free films, D2370(1) Emulsion vehicles (for paints/related coatings) freeze-thaw resistance, D2243(l) minimum film formation temp., 02354(2) 5a Latex vehicles Environment, standard conditioning for testing coatings, D3924(l) thermosetting (molding) compounds, 01013(2) Erosion resistance of exterior paints, D662(l) Sa 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 01847,4301(2) epoxide equivalent wt., 01652(2) epoxy content, D1652(2) guide for testing, D4142(2) hydrolyzable chlorine content, 01726(2) Ester value of solvents and thinners, D1617{3) Ether-alcohols See Clycol ethers 2-Ethoxy ethanol, specification, D331(3) 2-Ethoxyethyi acetate alcohol content/purity, 03545(3) specification, D3728(3) Ethyl acetate alcohol content/purity, 03545(3) specification, D4614C3) Ethyl acrylate ethyl acrylate, spec., D3548(3) purity, D3362(3) Ethylene glycol specification, 02693(3) Ethyleneglycol monobutyl ether See 2-Butoxyethanol Ethylene glycol monoethyl ether '** " See 2-Ethoxy ethanol Ethylene glycol monomethyl ether See 2-Methoxy ethanol 2-Ethylhexanol, analysis, 05008(3) 2-Ethylhexyl acrylate, spec., D3541<3) Ethyl silicate, zinc-rich primer MEK resistance, D4752(l) Evaporation rate, volatile liquids, 03539(1) Exposure - accelerated-corrosive environment cyclic salt spray/humidity/cold D2933U) filiform corrosion on steel, D2803C1) method for evaluating corrosion, D1654(l) Exposure - accelerated -water/humidity/light black box/Fresnel reflector rack, 04141(1) carbon arc lamp - dew cycle, 03361(1) carbon arc lamp/unfiltered, D822<1) carbon arc lamp, enclosed. Atlas, D5031(l) controlled condensation, D4585(l) fluorescent UV/condensation, 04587(1) 100% humidity chamber, D2247 (1) wood pane! substrates, D358 (06. xenon arc/water spray, G26(l) 851 P DUP050296410 Condensed Index of Committee D-1 Standards Exposure testing-exterior house paints on new wood, 01006(1) paints on steel surfaces, D1014, 5065<1) quantifying dijt collection, D37190) recording results on standard forms, D1150(l) wood panel substrates, 0358(1) Extenderpigments See Aluminum silicate (clay) Barium Sulfate (barytes) Calcium carbonate (whiting) Magnesium silicate (talc) Mica Pumice Silica, diatomaceous Exterior paints and coatings See Architectural paints and coatings. Exposure testing Factory applied finishes See Industrial finishes, water-borne Wood finishes See Color retention Falling-rod viscometer See Viscometers Fatting sand method. See Abrasion resistance Fatty adds--general definition of terms, D1467(3) sampling, 01466(3) testing methods, 02575(3) Fatty acids--specifications coconut oil, D1841(3) com oil, 01842(3) cottonseed cal, 01843(3) dehydrated castor oil, 015390) Unseed oil, D1538<3) soybean oil, 01537(3) tall oil, D19S4(3> Fatty acids--tests add value, 01980(3) ash content, 01951(3) darity/cleanness, 02090(1, color after heating, D1981(3) fish oil content, D3725(3) Gardner color scale, 01544(1,2,3) hydroxyl content, 01957(3) iodine value, 01959(3) rosin add content, 011240(3) saponification value, 01962(3) solidification point D1982(3) spedfic gravity, test D1963(3) titer test 01982(3) unsaponifiablc matter, 01965(3) Fatty acids content alkyd resins, 01398(2) . methyl esters, 01983, 3457(3) solvent paints, 02245(3) tall oil rosin, test, D155(3) tali oil test, 0803(3) Fatty amines, amidomines, diamines amine content, 02083(3) amine values, D2073,2074(3) iodine value, Wijs, D2075(3) isocyanates test 01638(3) non-amine content, 02082(3) test methods, amidomines, 02071(3) water content, 02072(3) Fatty nitrogen compounds identification in solvent paints, D2245(3) non-amine content, D2082(3) test methods, D207K3) water content test, 02072(3) Fatty oils (drying oils) absorption (by pigments), 0281,1483(2) acetone tolerance (heat-bodied oils), 01950(3) ash content, D195K3) break test, 01952(3) darity/deanliness, visual 02090(1, 3) color after heating, test, 01967(3) conjugated diene value, D13580) content, of solvent paints, 02245(3) definition of terms, 0555(3) film formation rates, drying, 01640(1) Gardner color scale, 01544(1,2,3) gel time, test, 01955(3) iodine value, test, 01959(3) loss on heating, 01960(3) sampling, 01466(3) saponification value, 01962(3) selecting test procedures, guide, D4140(3) specific gravity at 25/25*0, test, 01963(3) Fatty oils (drying oils) - (confc'd) testing methods, D555(3) unsaponifiable matter content, D1965(3) unsaturation, Rosenmund-Kuhnhenn, D1541(3) unsaturation, Wijs method, 01959(3) 5 a Castor oil, raw Castor oil, dehydrated Fish oil linseed oil Oiticica oil Safflower oil Soybean ot! Sunflower oil Tall oil Tung oil Fatty quaternary ammonium chlorides add value, tests, D2976(3) amine value, test, 02076(3) ash content, test, 02077(3) iodine value, 02078(3) nonvolatile matter, 02079(3) molecular weight, 02080(3) pH, test, 02081(3) water content, D2072(3) Ferric oxide/Ferrite See Iron oxide pigments Ferrous iron in iron oxides, 03872(2) Field identification/analysis of structural coatings, 05043(1) Filiform corrosion resistance of organic coatings, 02803(1) S a Exposure tests-accelerated-corrosive Film application/applicators artists* paste paints, practice, 04941(1) blade applicators, D823(l) producing uniform films, D823(l) wire-wound (Meier) rods, 04147(1) Film formation, emulsion vehicles minimum temperature (MFFT), 02354(2) Film porosity. See Porosity Film thickness gages dry films by incision cut, Tooke gage, 04138(1) on non-ferrous metals (eddy), 01400(1) on steel, magnetic gage, 01186 using micrometers, DlOOSfl) wet films eccentric wheel, 01212(1) Interchemical and Pfund gages, 01212(1) notched gages, 04414(1) Films, organic coatings, See Free films Fineness of grind (dispersion) See Dispersion Fire retardancy/flammabUity . See Burning characteristics Fischer reagent method (for watercm^t) See Karl Fischer reagent Btelbnil Fish oil in drying oils and fatty acidsjiij 5 a Fatty oils Flake brass See Gold bronze powder Flaked powders See Aluminum powder and paste Flake white See Basic carbonate White Flaking (flake resistance) exterior paints 0722(1) Flammabiiity/fire retardancy See Burning characteristics Flash point--liquids See Burning characteristics Flat paints, interior solvent-borne, test guide, 03323 water-borne, test guide, D2931 Flexibility impact resistance, 02794(1) mandrel bend test, 0522(1) on prepainted metal sheets,D4145{l> Flocculation - of pigments, test for, 09634 2) Floor paints/coatings clear floor sealers, 01546(1) solvent-borne, test guide, 03383(1) water-borne, test guide, D3358(l> Flow and flow rate See Rheological properties Foots, in raw linseed oil gravimetric method, 01966(3) Volumetric method, 01954(3) Ford cup, See Viscometers Formabiiity Impact-Wedge bend test, 03281(1) zinc-rich primer on steel, D4146<1) Formaldehyde acidity test, 02379(3) in amino resins, 01979(3) iron content, test, D2O870) ' methanol content, test, D2380(3) specification, D237SO) v Forms certification of conformance, 05063(1) recording exposure test results, 01150(1) Fouling See Anti-fouling paints Free films (organic coatings) preparation, tensile properties, 02370(1) preparation of, 04708(1) . . Freeze - thaw resistance^ multicolored lacquers, 02337(3) water-borne paints, 02243(1) French blue See Iron blue French chalk See Magnesium silicate French ocher See Ocher Fresnel reflector rack exposure accelerated outdoor metal exposure 04141(1) Friction, static coefficient. See Slip resistance Fuel oil / solvent resistance of traffic paints, 02792(1) Fungicidal (fungistatic) pigments Se e Anti-fungal pigments Fungus resistance/fungicides See Biodeterioration Furnace black. See Carbon black Galvanized surfaces See Steel panels/pipe/tube/sheet Gardner-Coleman method oil absorption of pigments, D1483(2) Gardner color scale transparent liquids, test, 01544(1,24) 852 DUP050296411 Condensed Index of Committee D-1 Standards sGardner-Holdt viscometer tubes See Viscometers Gas checking, draft test, varnish films, 01643(1) gasoline resistance, of traffic paints, D2792(l) Gei time drying oils, test, 01955(3) tar adds, test 02870(3) Glass panels surface prep for testing coatings, 03891(1) Glass beads (in traffic paint) analysis for D4797(l) sieve analysis, D1214(2) test for roundness of, 01155(2) Gloss (specular) and Sheen change, washability of coatings, 04826(1) effect of household chemicals, 01308(2) gloss differences, visual evaluation, 04449(1) haze of high gloss finishes, 04039(1) high gloss, goniophotometer, test, E430(l) measurement of gloss and sheen, 0523(1) tolerances, conformance evaluation, 03134(1) uniformity of brushoufcs, test, 03928(1) Gloss paints See Architectural paints Glycerin--high gravity sampling /testing, D1256<3) specification, 01257(3) Glycidal ethers chlorine content in epoxy resins, 04301(2) Glycols See Diethylenc glycol, 02694(3) Dipropylene glycol, 02696(3) Ethylene glycol, 02693(3) Hexylene glycol, D2636(3) Propylene glycol, 02695(3) Glycol ethers See Dipropylene glycol monomethyl ether Ethylene glycol bulyl ether Ethylene glycol ethyl ether Propylene glycol monomethyl ether Glycol ether acetates See Ethylene glycol ethyl ether acetate Propylene glycol methyl ether acetate Gold bronze powder analysis, 0283(2) specification, D267{2) Sff Pigments, general properties Green pigments See Chrome green Chromium oxide green Phthalocyanine green Grind, of pigment dispersions See Dispersion/fineness of grind Grindometer, NPERI S ee Printing inks Dispersion/ftneness of grind * Guide for assessing aged coatings on steel, 05065(1) painting inspectors, metal substrates,D3276(l) Guides for testing (selection of methods) See Architectural paints and coatings Coil coatings Electrocoat baths Epoxy resins Industrial finishes Lacquers Latex vehicles Powder coatings Solvents Gum rosin See Rosin Halogenated solvents analysis for, in paint, 04457(1) Halo-silane coated glass plates for preparation of free films, D4708U) Halphen-Hicks test rosin content of varnishes, D1542(l,2) Handling material See Materials handling Hardness testing, of organic films Knoop indentation tester, KHN, 01474(1) Koenig pendulum test 04366(1) pencil test, 03363(1) Persoz pendulum test, 04366(1) Pfund indentation tester, PHN, D1474(l) Sward rocker test, D2134(l) Hazards, fire and health handling analine, 03436(3) handling cresylic add, phenol, 03852(3) handling naphthalene, D3438(3) in protective coatings, 03630(1) labeling art materials, 04236(1) Haze See Gloss Heat resistance of organic coatings on steel, 02485 (1) effect of overbaking, D2454(l) Heatset-type printing inks non-volatile content, 04713(1) Hegman scale fineness of dispersion, pigments, 01210(1) Hematite See Iron oxide red n-Heptane flash/fire point of liquids, test 01310(3) Heptane miscibility See Miscibuty Hexanes commercial, specification, D18360) Hexyl acetate, spec,, 05137(1). Hexylene glycol, specification, 02636(3) Hiding power (of paints/coatings) ! brushouts, visual, relative, D344(l) drawdowns, reflectometry, 02805(1) roller application, practical, visual, In Prep, wet-to-dry change, visual, 05007(1) High-flash aromatic naphthas, 03734(3) High performance (HIPAC) coatings, 03730(1) High-purity (reagent) water, spec., 01193(3) High shear (ICI) viscosity, 04287(1) Sa Brushability . Horizontal pul! test, static friction, 04518(1) Household chemicals, resistance to, of organic coatings, 01308(1) House Paints See Architectural paints Humidity resistance, of coatings humid-dry cycling, on wood, 03459(1) humidity, on steel, 02247(1) humidity-thermal cycle on steel, 02246(1) S a Water resistance Hunter, visual gloss differences, 04449(1) Hydrocarbon solvents See Aliphatic hydrocarbon solvents Aromatic hydrocarbon solvents Solvents, general test procedures Hydroquinone content in vinyl acetate, D2193(3) Hydroxyethylcellulose, testing, D2364(2) Hydroxyl content cellulose acetate, 0871(2) cellulose acetate, butyrate, DS17(1) fatty oils and adds, D1957(3) Hydroxypropyl methylcellulose, 02363(2) Hydroxypropyl substitution in cellulose ether products, 03876(2) ICI cone/plate viscometer, D4287(l) Sa Brushability Impact resistance , flexibility test, 02794(1) Imprinting See Print resistance Inclined plane test, static friction, D4518(l) Indentation hardness See Hardness Testing 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, test guide, 01712(1) Inert pigments See Extender pigments Infrared pyrometry (thermometers) for wood coatings, cure cyde, D3259(l) Infrared spectrophotometry, analysis See Spectrophotometry--infrared Ink, Inkometer, See Printing Inks Inspection of paint application work guide for inspectors, 03276(1) Interchemical Film Thickness Gage See Film thickness gages Interior paints See . Architectural paints Interlab testing See Statistical methods Iodine value, tests Drying oils,Rosehxnund-Kuhnhenn, 01541(3) fatty amines, Wijs test, 02075(3) fatty quaternary ammon. chlorides, 02078(3) lac resins, test, 029(2) Wijs test, 01959(3) Iron blue analysis, 01135(2) specification, 0261(2) Iron oxide black natural/synthetic-analysis, 03872(2) synthetic., spec., 0769(2) See Pigments, general properties Iron oxide brown (natural) analysis, D50(2) specification, 03722(2) 5a- Pigments, general properties Iron oxide brown (synthetic) analysis, D3872(2) specification, D3724(2) Sa Pigments, general properties Iron oxide red (natural) analysis, :D50(2) specification, 03722(2) 5 a Pigments,, general properties Iron oxide red (synthetic) analysts, 050(2) specification, 03721(2) 5a Pigments, general properties Iron oxide yellow analysis, 050(2) specification, 0768(2) 5a Pigments, general properties Iron paint driers See Driers Iron Oxides, ferrous iron content, 03872(2) ISO flow cups. See Viscometers Isobutyl acetate alcohol content/purity, D3545(3)( Isobutyl acetate (95% grade), spec., 01716(3) Isobutyl alcohol, specification, 01719(3) Isocyanates foam raw materials, test methods, 01638(3) isocyanate groups in urethanes, 02572(2) Isophorone, specification, 02916(3) Isophthalic acid content alkyd and polyester resins, test, D2690(2) Isopropanol See Isopropyl alcohol Isopropyl acetate alcohol content/purity, 03545(3) Isopropyl acetate (99% grade), spec., D3131<3) Isopropyl alcohol, specification, 0770(3) Kaolinite, Kaolin See Aluminum silicate Karl Fischer reagent, water content, 04017(1) Kauri-butanol value, 01133(3) 853 HP? DUP050296412 Condensed Index of Committee D-1 Standards Ketones Lieberman-Storch test methyl n-amyl ketone/ spec./ 04360(3) rosin content of varnishes, 01542(1,2) purity, test D2192(3) Lightfastness Ketone solvents of printed matter, 03424(1) See Acetone, D329(3) of pigments used in Artists' Paints, 04303(1) Diacetone alcohol, 02627(3) Sa Artists* paints Isophorone, 02619(3) Color retention Methyl amyl ketone, 04360(3) Limonite See Ocher Methyl ethyl ketone, 0740(3) Linseed oil Methyl isoamyl ketone, 02917(3) boiled, specification. D260{3) Methyl isobutyl ketone, 01153(3) raw, specification, 0234(3) Knife test, for paint adhesion, 03359(1) Sa Fatty oils Knoop hardness tester, 01474(1) Foots in raw linseed oil Koenig pendulum test, hardness, 04366(1) Oil absorbtion (of pigments) $a Hardness testing Fatty adds - tests, specifications Labeling Liquids, - art materials for health hazards, 04236(1) darity/cleanliness, visual, 02090(1, 3) Lacquer color, by Gardner scale, 01544 (1,2,3> cellulose nitrate content, 03133(1) density and specific gravity, 03505(3) definition of, 016(1,2,3) liquid/solid state, characterization, 04359(1) ester value, of lacquer solvents, 01617(3) $<r Burning characteristics freeze/thaw test, multicolored, 02337(1) guide for testing, 0333(1) imprint resistance (of dried films), 02091(1) particle size analysis(muIticolored),D2338(l) Magnesium silicate plasticizer migration, vinyl fabrics, 02199(1) analysis, 0717(2) selection of test methods, 0333(1) stain removal (multicolored lacquer) 02198(1) specification, D605(2) Sa Pigments, general properties temperature-change resistance, test, D121K1) Maleic anhydride testing wood furniture lacquers, 02571(1) color, by platinum cobalt scale, 03366(3) viscosity by dip type viscosity cups, 04212(1) maleic add content, 02930(3) viscosity by Ford viscosity cup, 01200(1) sampling and handling, practice, 03438(3) Lac resins See Shellac spedfication, 03504(3) Lampblack solvent extractable matter, test, 0305(2) Mandrel bend test specification., 0209(2) flexibility of organic coatings, 0522(1) ' Lampblack content test, 0305(2) Manganese content Lapis lazuli See Ultramarine blue Latex paints -- See Architectural paints of drier, D564,2375(2) of cellulose pulp, 04085(2) Latex vehicles Mar resistance filter-retained solids content, 05097(2) under development by 00123 guides to test procedures, 04143(2) Marine coatings See Antifouling paints nonvolatile content, 04758(2) Masonry exposure test panels, prep., 01734(1) unreacted monomer content, 04827,4747(2) Masonry treatments See Water repellents Sa Emulsion vehicles MEHQ content Lead chromate pigments See Methyl ether of hydroquinone See Chrome yellow-and orange Meier rods See Film applicators Chrome green MEK resistance Molybdate orange of ethyl silicate-zinc rich primer, 04752(1) Lead content, analysis Menhaden fish oil See Fatty oils air particulate filter samples, 04358(2) Mercuric oxide basic lead silico-chromate, 01844(2) analysis, 0284(2) - leaded zinc oxide, test, 03260(2) spedfication, 0911(2) paint driers, 02374, 564(3) Mercury content red lead pigments, test, D49(2) in mercuric oxide, 0284(2) traffic marking material, 04797(1) in paint (low concentrations), 03264(1) white linseed oil paints, 0215(1)" Metal powder pigments yellow, orange, and green pigments, 0126(2) See Aluminum powder and paste Copper powder Lead pigments Gold bronze powder See White lead Zinc dust Lead chromate pigments Metal substrates, coatings on Basic lead silicochromate accelerated outdoor exposure, 04141(1) Red lead adhesion, by cut/tape test, 03359(1) Leaded zinc oxide blistering-evaluation of, D714(l) Lead silicochromate coil coatings, 03794(1) See Basic lead silicochromate flexibility/adhesion-deformed, D4145(l) Lead molybdate See Molybdate orange mandrel bend test, D522(l) Lead oxide See Red lead primers, testing practices, 03322(1) Leaded zinc oxide, analysis, 03280(2) Leafing properties aluminum powders/pastes, 0480(2) Metamerism, visual evaluation, 04086(1) Methacrylic acid (glacial 98.5%) Leveling (ropiness) of paints, test, 04062(1) spedfication, 03845(3) Methanol (methyl alcohol) acetone content of, 01612 (3) content, in formaldehyde solutions, 0238 permanganate time, test, 01363(3) spedfication, 01152(3) Methoxyl content hydroxypropyl methylcellulose, 02363(21* methylcellulose, 01347(2) Methoxybhydroxypropyl substitution by Zeisel-gas chromatography, 03876(2) Methyl acrylate, specification, 04709(3) Methyl alcohol. See Methanol Methyl amyl acetate, 02635(3) Methyl amyl alcohol See Methyl isobutyl carbinol Methyl amyl ketone purity, by gas chromatography, 03893(3) 3 Methyl butyl ketone ,^ purity, by gas chromatography, D3893(3) Methylcellulose .*& See Cellulose and cellulose derivatives Methylcydohexane purity from freezing point, test, 01016(3) Methyl esters, fatty add composition, D1983(3) preparation from fatty acids,, 03457(3) preparation from oils, 02800(3) Methyl ether of hydroquinone (MEHQ) content of monmomeric acrylate esters, 03125(3) Methyl ethyl ketone 99.5% grade, spec., D3729(3) purity, by gas chromatography, 02804(3) spec., 0740(3) Methyl isoamyl ketone purity, by chromatography, 03893(3) spec., 02635(3) Methyl isobutyl carbinoL spec., 02635(3) Methyl isobutyl ketone analysis by gas chromatography, 03329(3) spec., 01153(3) Methyl methacrylate unreacted monomer in lathees, 04827,4747(2) Methyl n-amyl ketone 98% grade, spec, 04360(3) Methylol group content in phenolic resins, test, 04706(2) Metric practice--SI Units, excerpts, E380(l, 2; 3) MFFT See Film formation, emulsion vehicles Mica pigment analysis, 0716(2) spec., 0607(2) .___ Microbiological attack See Biodeterioration Mkrocoulometry See Couiometry Micro-organism resistance See Biodeterioration Migration of plasticiser from vinyl fabrics to lacquers, test, 02199(1) Miliiequivalency, add/base See Electrocoat baths Miloriblue See Iron blue Mineral (hydrocarbon) oils moisture content, 0890(3) content in rosin oil, 01131(3) Mineral spirits aromatic content, chromatography,03257(3) specification, 0235(3) Miniature sandmill method- color and strength of pigments, 03022(2) Minimum film formation temperature (MFFT) Sre Film formation, emulsion vehicles Miscibility lacquer solvents, with heptane, 01476(3) water soluble solvents, with water, 01722(3) Mixed aniline point dipentene/terpene solvents, test, D80K3) 854 DUP050296413 Condensed Index of Committee D-1 Standards Modulus of elasticity, 2370(1) Moisture content blue pigments, 01135(2) capillary moisture in concrete, 04263(1) cellulose acetate, test, 0871(2) cellulose, test, 01348(2) ethylceiluJoge, test, 0914(2) hygroscopic moisture in pigments, 0280(2) hydroxyethylcellulose, test, 02364(2) hydroxypropyl methylcellulose, 02363(2) Karl Fischer method, 04017(1) lac resins, test, 029(2) liquid naval stores, 0890(3) methylcellulose, test, 01347(2) pine oil, 0890(3) pine tars and pine tar oils, test D8560) sodium carboxymethyicellulose, 01439(2) tall oil, test 0803(3) Moisture vapor permeability See Permeability Mold resistance See Biodeterioration Molybdate orange analysis, 0126(2) specification, 02218(2) S a Figments, general properties Molybdenum content molybdate orange, 0126,2216(2) Mortar resistance of clear coatings on aluminum, 03260(1) Mottling failure, exterior latex paints, D1648(l) Mud-cracking failure, exterior latex paints, 01848(1) Muller device color/tinting strength of pigments, 0387(2) Multinotch applicator tests sag resistance of paints, D4400(l) leveling of paints, 04062(1) Multi-panel forms far recording results, 01150(1) 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, 03735(3) 5 a Hydrocarbon solvents National Printing Ink Research Institute NPIRI, See Printing Inks Naval stores * def. of terms, 0804(3) volatile/nonvolatile content r 04140(3) water content, 0890(3) 5 a Tezpene solvents Newtonian liquids See Viscometers (viscosity) Nitrocellulose base solutions, test methods, 0365(2) content in alkyd lacquers, 03133(1) dilution ratio for solutions, 01720(3) testing, D3Q1(2) Nitrogen content cellulose nitrate, test 0301(2) nitrogen-containing plastics, 01013(2) resins and plastks(total), test, 01013(2) Nonleafing aluminum pigment See Aluminum powder and paste Nonvolatiie/volatile content aluminum powders/pastes, 0480(2) coatings, by volume, 02697(1) driers/naval stores, 04140(3) emulsions, resin solutions, D4209(2) guide to test methods, 02832(1) latices, test, 04758(2) pigment dispersions, 04139(2) printing inks/resin solutions, test, 04713(1) resin solutions, test 01259(2) shellac varnish, test, 01650(2) silane/siloxane masonry treatments, 05095(1) titanium dioxide slurries, 03926(2) varnishes, test; 01644(1) volatile solvents, test, 01353(3) Notched gages film thickness measurement, 04414(1) Notched film applicators See Multinotch applicator tests NPIRI See Printing inks Ocher analysis, 050(2) specification, 085(2) Odor test volatile solvents and diluents, 01296(3) Oil absorption (of pigments) ' Gardner-Coleman method, D1483(2) Spatula rub-out test, 0281(2) Oil content artists* paints, spec., 04302(1) solvent-borne paints, 02245(3) Oil resistance electrical insulating varnish, P115(1) . wood furniture lacquers, 02571(1) 5 a Fuel oil resistance Oils See Fatty oils (Diying oils) Mineral oil Pine oil Rosin oils Oiticica oil chloroform-insolubles, 01958(3) gel time, 01955(3) specification, 0601(3) Orange pigments See Molybdate orange Chrome yellow and orange Organotin release rate of anti-fouling paints, 05103(1) Overbaking (of paints/related coatings) effects of overbaking, 02454(1) Oxirane epoxy content of epoxy plastics, 01652(2) Package stability coatings for ultraviolet curing, 04144(1) emulsion paints, biodegradation, 02574(1) freeze-thaw resistance, 02243(1) sampling liquid paints, 03925(1) settling of traffic paint, 0869(1) solvent and water-borne paints, 01849(1) Paint brushes preparation for evaluation, D5068C1) Paint inspection See Inspection of paint application work Paint thinners See Thinners Paint rollers, covers preparation for evaluation, 05069(1) Panel forms (single/multi), D1150O) Panel preparation for tests See Steel panels Para (paranitraniline) red analysis, 0970(2) specification, D475C2) 5 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, 01366(2) polymeric powder properties, 03451(1) white extender pigments, 03360(2) Pastes in oil (of pigments) See Pigment dispersions Patch test, coating compatabillty, 05064(1) Pavement marking paint See Traffic paint Pearlescent pigments See Nacreous pigments Peen plating S ee Coatings--mechanically deposited Pencil test film hardness, 03363(1) Pendulum test, hardness of coatings, 04366(1) Penetration--paint films See Porosity Pensky-Martens closed, flash point, 093 (1,3) Pentaerythritol/pentaerythritol content methods for testing, 02195(3) monopentaerythritol content, 02999(3) of alkyd resins, 01615(2) Permanganate time acetone and methanol, test, 01363(3) tricresyl phosphate, test, 01721(3) Permeability, to moisture vapor, of organic films, 01653(1) Peroxide content of styrene monomer, test, 02340(3) Persian gulf oxide See Iron oxide red Pexsozpendulum test See Hardness Perspiration resistance of H1PAC coatings, D3730O) Petroleum spirits See Mineral spirits Pfundgage See Film thickness measurement Pfund indentation hardness See Hardness pH See Acidity/Alkalinity Phenol, in phenolic resins, D1312(2) Phenolic resins (Phenol formaldehyde) apparent pH, 04613(3) free phenols content, 01312(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, 0563,1306(2) sampling and handling 03438(3) specification, 02403(3) Phthalocyanine (phthalo) blue analysis, 01135, 03256(2) specification, 0963(2) Sa Pigments, genera! properties Phthalocyanine (phthalo) green chemical analysis, 03256(2) specification, 03021(2) Sa Pigments, general properties Pictorial stds, steel surfaces, 02200(1) Figment content/paints and dispersions paint/traffic marking material, 04451(1) pigment pastes in oil, test, 01206(2) solvent paints, 02371,2698(1) titanium dioxide slurries, 03926(2) water-based paints, 03723(1) Pigments--analysis and specifications see individual pigment names Sa Pigments-color categories White pigments, chemical analysis DUP050296414 Condensed Index of Committee D-1 Standards Pigments--color categories See Black pigments Blue pigments Blown pigments Glass beads Green pigments Inert pigments (Extenders) Metal powder pigments Nacreous pigments Orange pigments Red pigments White hiding pigments Yellow pigments Figments--composition categories See Earth pigments Iron oxide pigments Lead chromate pigments Chromium pigments Pigments--function categories See Anti-corrosion pigments Anti-fouling pigments Anti-fungal pigments Colorant pigments Extender pigments (inerts) White hiding pigments Pigments--general properties bleeding characteristics, D279(2) composition acidity/alkalinity, D1208(2) ignition loss D1208(2) moisture content, 0280, 01208(2) volatile content, D4139(2) water soluble salts content, D2448(2) lightfastness in artist paints, 04303(1) oil absorption Gardner-Coleman method, 131483(2) Spatula, rub-up test, D2S1I2) , particle size characteristics, reporting of, D1366(2) course particle content, D185(2) fineness of dispersion paint, D1210(l) fineness of grind, printing ink, D1316(l) particle size distribution, 03360(2) specific gravity, 0153(2) tinting strength and color colored pigments -- with mechanical muller, 0387(2) with miniature sand mill, 03022(2) white pigments-- visual method, 0332(2) instrumental method, D2745(2) Pigments--in paints and diversions See Dispersion/fineness of grind . Lightfastness Pigment content Slurries White pigments^hemical analysis Pine oil moisture content, 0890(3) sampling/testing, D802(3) Fine tar/pine tar oils sampling and testing, 0856(3) Pinholing film failures of exterior latex paints, D1848(l) Plasticizer migration vinyl fabrics to lacquers, D2199(l) Plastics coatings for plastic substrates, 03002(1) epoxy content, 01852(2) Platinum-cobalt solutions, color scale See Color Polyester resins See alkyds Polyhexafluoropylene (FEP) substrate for preparation of free films, D4708C1) Polyhydric alcohols content See Alkyds Polymeric powders/powder coatings test procedures, practices, 03451(1) Polymerization cellulose nitrate, test, 01716(2) dipentene/teipene solvents, test, 0233(3) unreacted monomer of latexes, 04747(2) Polymerization inhibitors butylcatechol in styrene, 02120(3) Polymerization time electrical insulating shellac, 0411(2) Polymers silicons,silicon content, 03733(2) solubility range, test, 03132(2) Polyurethanes See Urethanes Polyvinyl butyral resins See Resins--polyvinyl butyral Polyvinyl chloride (F.VQ chlorine content, test, D1156(2) residual vinyl chlopde, 03680(2) test procedures, guide, 04368(2) Porosity, of paint films, 03258(1) Potash blue See Iron blue Powder coatings See Polymeric powders/powder coatings Practices See individual standard practices Sa Guidesfor testing Precision See Statistical methods Primers ethyl silicate - zinc rich MEK resistance, cute test, 04752(1) formability on steel, 04146(1) test guide, on pre-formed metal, 03322(1) Primrose chrome/yellow See , Chrome yellow and orange Print resistance of lacquers, 02091(1) of architectural coatings, in preparation Printed matter evaluating lightfastness, 03424(1) Printing inks and vehicles apparent tack, inkometer test, D436K1) fineness of grind, NIP1RI method, D1316(l) lightfastness, printed matter, 03424(1) nonvolatile content, 04713(1) (inting strength, in prep, viscosity, by falling-rod; D4040(l) water pick-up, 04942(1) Sa Resina Resin solutions 1- Propanol See n-Propyl alcohol 2- Propanone Sec Acetone Proplony1 content cellulose acetate propionates, 0817(2) Propyl acetate, normal alcohol content/purity, 03545(3) 90-92% grade, spec, 03130(3} n-Propyl alcohol, spec, 03622(3) Propylene glycol monomethyl ether PGME, purity, 04773(3) spec, 4837(3) Propylene glycol monomethyl ether acetate PGME acetate, purity, D4773(3) spec, 04835(3) Propylene glycol, spec, 02695(3) Prussian blue See Iron blue Pull-off strength (bond strength) See Adhesion/Cohesion Pull test, static friction, 04518(1) Pumice/pumice stone/pumadte specification, D867(2) Purchasing, state/institutional, D392711) Rare earths content paint driers, by EDTA method, 03989(3) Raw oils (drying oils) 7 See Fatty oils Raw sienna/umber See Sienna, burnt and raw Umber, burnt and raw Reagent water microelectronicprocessing, spec, 01193(3) reagent water, spec, 01193(3) Red copper oxide (77402) See Cuprous oxide Red iron oxide See Iron oxidered Red lead analysis, 049(2) specification, D83(2) Sa Pigments, 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, 02616(1) hiding power by reflectometry, 02805(1) instrumental color difference, D2244(1) Munsell color system, D1535C1) of opaque specimens, E97(l) preparation of reflectance standards, EZ590) specific luminance, traffic coatings, 04061(1) Reflective markers in traffic paint See Glass beads Refractive index dipentene/terpenes, 0801(3) pine oil (natural/synthetic), 0802(3) turpentine and pinene, test, D233(3) Repellents, See Water repellents Reporting paint film failures of exterior latex paints, 01848(1) Reproducibility and Repeatability See Statistical methods Resin solutions, general properties clarity /cleanness, 02090(1,3) cloud point, D5062(3) ....... dilutability (solvent tolerance), 05062(3)' Gardner color scale, D1544(t,2^3) nonvolatile, ink vehicles, 04713(1) nonvolatile matter content, test, 01259(2) std. color solutions, D365(2), Dt209(l,3) unsaponifiable matter, D1397(2) viscosity, test, 01725(2) Resins,general properties softening, ring and ball, E28(3) solubility/range, test, D3132(2) voiatile/nonvolatile, 04209(2) volatile resin adds, D3008(3) water content, Karl Fischer, test, D4017(l) Resins, various types See Alkyd resins Amino resins Epoxy resins Phenolic resins Rosin Shellac (lac) Urethanes Vinyl resins 856 DUP050296415 Condensed index of Committed D-1 Standards Resistance propertles/reslstance to See Abrasion resistance Add resistance Alcohol resistance Alkali resistance Bleeding Biodeterioration Blistering Blocking Checking Chemical resistance Chip (chipping) resistance Coffee stains Corrosion resistance Cracking (crack resistance) Deteigen t 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 Over baking 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 Retroreilection (horizontal coatings) traffic paints, specific luminance, D406K1) Rheological properties/non-Newtonian coatings Brookfield viscometer, 02196(1) ICl cone/plate viscometer, D4287<1) Sa Viscometers (viscosity) Ring-and-ball apparatus softening point, of resins, E2S0) Road service testing See Traffic paint Rocker hardness test (Sward) See Hardness Roller application, of paint hiding power.practical, 05150(1) spatter resistance, D4707(l) Rollers, paint See Paint rollers, covers Ropiness (of paints). See Leveling Rosenmund-Kuhnhenn method iodine value of drying oils, 01541(3) Rosin add number, D465(3) ash, burning residue iron content, D1064(3) sampling and grading, D509{3) saponification number, D464(3) tall oil rosin-fatty adds, D1585(3) unsaponifiable matter, t>1065{3) toluene insolubles, 02693(3) volatile oil content, 0889(3) volatile resin acids content, D30Q8(3) Rosin acid content coating vehides, D1469(2) fatty adds, test, 01240(3) rosin oil, test, D1131(3) tall oil, test, D803(3) lac resins, test, D29(2) Lieberman-Storch test, 01542(1,2) Rosin esters rosin adds content, 01469(2) Rosin oils, testing of, 01131(3) Rouge See Iron oxide red Rub-out test (pigments) See Oil absorption (pigments) Rusting-degree-photographic standards on painted steel surfaces, 0610(1) Safflower oil specification, 01392(3) Sa Fatty oils Sag resistance test Using a multinotch applicator, 04400(1) Salt spray (fog) resistance with acetic acid, B287, 117(1) Sampling liquid paints & pigmented coatings, 03925(1) Sand abrasion test falling sand method), D968(l) Sandstone, architectural preparatory surface cleaning, 05107(1) Saponification number/value drying oils, fatty adds, 01962(3) lac resins, test, 029(2) rosin, test, 0464(3) - tall oil, test, D803(3) 5 a Unsaponifiable matter content Saybolt viscometer See Viscosity Scaling See Flaking Scattering coefficient absolute values (hiding power), 02805(1) white pigments, relative values, 02745(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 Sericite See Mica Setafiash tester See Burning Characteristics Settling traffic paint, accelerated, 01309 traffic paint in containers, 0869(1) Set-to-touch-time See Drying properties Sheen See Gloss and Sheen Sheet metal (with organic coating) flexibility/adhesion of the coating, 04145(1) mandrel bend test, D522(l) Shellac (lac resin) bleached shellac spec., 0207(2) copal resin content, 029(2) for electrical insulation, 0411,784(2) orange shellac and other Lacs, spec., 0237(2) sampling and testing, D29(2) shellac varnishes sampling and testing, 01650(2) specification, 0360(2) volatile/non-volatile content, 04209(2) SI units (International System of Units) metric practice, excerpts, E380,(1,2,3) Sienna (burnt and raw) analysis, 050(2) specification, D765(2) $ a Pigments, general properties Sieve analysis glass spheres, used in traffic paint, 01214(2) pigments, practice for reporting, 01366(2) pigments and dispersions, (0185(2) Silanes, siloxanes See Water repellents Silica, diatomaceous analysis, D719(2) spedfication, 0604(2) Silicate pigments See Aluminum silicate Calcium borosilicate Calcium silicate Magnesium silicate Silicone-coated paper preparation of free films, 04708(1) Silicone polymers silicon content by spectrophotometry, D3733 Skinning See Stability--package Slip resistance, static friction test, 02518(1) Slurries titanium dioxide content, 03926(2) Soapstone See Magnesium silicate Softening point organic coatings, test, 02134(1) resins, ring and ball apparatus, E28(3) Soil accumulation, on paint films degree of surface disfigurement, 03274(1) Soil/dirt resistance (removal) practical washability, 0.4528(1) Solid/Liquid state, characterization, D4359(l) -Solids content See NonvolatUe/voUtile content Solubility tests cellulose in sodium hydroxide, 01696(2) cellulose nitrate, 0301(2) solubility range (resins/polymers), 03132(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) Hatogenated solvents Hydrocarbon solvents Ketone solvents Terpene solvents DUP050296416 Condensed Index of Committee D-1 Standards Solvent resistance alcohol, on furniture lacquer, D257H1) gasoline/fuel oil, on traffic paint D2792(1) Steel surfaces, unpainted pictorial standards of condition, D2200(l) profile of abrasive - cleaned steel, 04417(1) Texture gloss differences of similar surfaces, 04449(1) Thermalvoltaic infrared thermometers MHK, of ethyl silicate primer 04752(1) test panels, preparation of, D609(l) See Infra-red pyrometry Solvents-test procedures, general Steel surfaces, painted Thermistor infrared radiation thermometers analysis, chromotography, D327K1) See Exposure, accelerated See Infra-red pyromeby clarity/cleanness, 02090(1,3) Exposure, exterior Thermosetting resins evaporation rate, D3539 halogenated, in paints, analysis, D4457(1) Stiffness offree films, 02370(1} Stormer viscosity (consistency) stroke cure time of phenolics, 04640(2) Thickness--paints/related coatings hydrocarbon solvents of paint, 0562(1) producing uniform films, 0823(1) acidity, test, D1613(3) of pine tars and pine tar oils, D856(3) S a Film thickness measurement aniline point, 0611(3) Strip (copper tarnish) test Thinness See Mineral spirits. Turpentine, benzene content, D4367(3) coppercorrosion in petroleum products, D130(3)j VM &P Naphtha Kauri-butanol test, 01133(3) Stroke cure time S a Solvents odor (characteristic/residual), D1296(3) thermosetting phenolic resins, D4640(2) Thixotropy sampling/test procedures, 0268(3) Strontium chromate, analysis, D1845(2) water content, by Fischer reagent, D1365(3) Sa Pigments, general properties rotational (Brookfield) viscometer, 02196(1) Sa Viscometers identification in paint, 02349(1) Structural coatings lacquer solvents,heptane miscibility, 01476(3)1 field identification/analysis, 05043(1) Tinting strength chromatic paints, 04838(1) water miscibility, D1722(3) Sulfide content printing inks, in prep, Solvent tolerance See Resin solutions white pigment, from paint, D2351(2) 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 Figments, general properties retired. specification, 01462(3) Sunflower oil Titanium dioxide Sa Fatty oils specification, 03169(3) Sa Fatty oils analysis of and for Fatty acid tests, specifications Surface analysis anatase/rutile ratio, D3720I2) Spattering (spatter resistance) adhesion, tests, D4541(l) atomic absorption spectroscopy, D 4563(1) roller application test, D4707(l) gloss differences, visual evaluation, D4449(l) by X-ray spectroscopy, D 4764(1) Spatula rub-out test gloss gonlophotometer, E430(l) chemical analysis, 01394(2) See Oil absorption, pigments profile, blast cleaned steel, D4417(l) in traffic marking paint; 04797(1) 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, D406K1) add etching of concrete, D4260(l) tinting strength, visual, D332(2) Specific permeability aluminum (hot-dip), D1731<1) Sa Pigments, general properties See Moisture vapor permeability aluminum/aluminum-alloy surfaces, 01730(1). Titer Spectroscopic analysis architectural sandstone, 05107(1) fatty adds, test, D1982(3) acrylic polymer in emulsion paint, 03168(1) concrete/masonry panels, D1734(l) Toluene antimony content (low cone), D3717(l) galvanized steel, non-passivated, 02201(1) industrial grade, spec. 0362(3) cellulose nitrate in alkyd lacquers, D3133(l) glass panels, D389K1) toluene insolubles in rosuvP269(3) chromium content (low cone),D3718(l) magnesium alloys, D1732(l) volume and weight calculations, 015555(3) diene value, dehydrated castor oil, D1358(3) sted test panels, D609(l) Toluidine red identifying separated vehicle solids, D2621(l)| Sustained burning test analysis, 0970(2) iron content (of rosin), 01064(3) Seta-flash tester (open cup), 04206(3) specification, 0656(2) lead/cadmium/cobalt, 03335(1) Wick test, D4207C3) Tooke gage. See Film thickness, dry films lead/chromium in pigment dust, D4356(2) Sward rocker See Hardness testing lead content in paint, 04834(1) mercury contentflow concentration), 03624(1) Traffic paint metal content of cellulose pulp, D4085(2) Taber abraser test. See Abrasion resistance adulteration of vehid^solids, 02743(1) sulfur content of cellulosics, D2929C2) Tack, of printing inks, Inkometer,04361(1) bleeding, over tar and asphalt, D959(l) ' titanium dioxide in paint, 04563,4764(1) Tag cup See Burning Characteristics bleeding, photographic standards D868(l) traffic paint vehicle adulteration, D2743(l) Talc See Magnesium silicate conducting road service tests, D713(l) Specular gloss See Glossand Sheen Tall oil, test methods for, D803 degree of chipping, DS13(1) ,, Spoilage See Biodeterioration Sa Fatty oils degree of settling, D869(l) Package stability Tall oil rosin glass spheres, roundness, D1155(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 acids content, 01585(3) gasoline resistance, D2792(l) hiding power of paints, D344,2805(1) volatile resin adds content, D3008(3) no-pick-up (drying) time, D711(l) Stability--package See Package stability pigment content, by ashing, 04451(1) Stain resistance practices for testing, D2205(l) coffee stains, D 2571(1) Tar See Pine tar/pine-tar oils retroreflectance/specific luminance, D4061C1) of factory applied wood finishes,.D3023(l) Temperature tests settling during storage, D1309C1) of multicolor lacquers, 02198(1) freeze-thaw resistance, 02243(1) wear Ufe/resistance, 0913(1) of organic finishes, D1308(l) low-temperature coalescence, 03793(1) Transfer efficiency-spray application of transportation industry finishes, D154D(1) minimum film formation temp. D2345(2) under laboratory conditions, D5009(l) of wood furniture lacquer, 02571(1) Tensile properties, of free films, 02370(1) under production conditions, D5066(l) So Washability, Porosity Tetpene solvents Tribasic lead phosphosilicate Static friction tests (slip resistance) See Dipentene, Pine Oil, Turpentine analysis, D2742(2) inclined plane/horizontal pull, D4518(l) Terra alba See Coldum sulfate specification 02744(2) Statistical methods Term de sienna See Sienna (bumfandraw) Tributyltin See Organotin release rate for interlaboratory testing, E691(3), D3980C1) Testresults See Forms for recording Trichloroethane determination Steel blue pigment See Iron blue Testing, interlaboratory practice, 03980(1) by gas chromatography, D4457(l) 858 DUP050296417 * Condensed Index of Committee D-1 Standards Tricresylphosphate permanganate time, D 1721(3 specification, 0363(3) unsaponifiable matter content, D1399<3) volatile matter content, 01468(3) | Tristimulus values See Color- opaque materials | Tung Oil gel time, test, D1955<3) quality determination, D1964(3) raw, specification, D12(3) i Tunnel method(two foot tunnel) fire retardancy of paints, D3806(l) Turkey red See Iron oxide red ? Turkish umber See Umber (burnt and raw) ' Turpentine pinene composition, D3009C3) sampling and testing, D233(3) specification,.Dl3(3) || Two-foot tunnel method fire retardancy of paints, D3806(l) Ultramarine blue analysis, 01135(2) specification, 0262(2) 1 Ultraviolet-cured coatings cure time, reporting of, D3732(l) package stability, D4144(l) Ultraviolet exposure, D4587(t) Umber (burnt and raw) analysis, D50(2) specification, 0763(2) Units, 51, metric, 380(1,2,3) Unsaturation (in drying oils and derivatives) Rosenmund-Kuhnhenn method, 01541(3) Wijs method, 01959(3) Urea-formaldehyde resin solutions See Amino resins Urethanes free toluene diisocyanate content, D3432(2) 2-ethoxethyl acetate in, spec., 03728(3) isocyanate group content, 02572(2) isocyanate raw materials, 01638(3) methyl ethyl ketone in, spec., 03729(3) UV See Ultraviolet-cured coatings Ultraviolet exposure Vanadium content paint driers, EDTA method, 03988(3) Varnishes abrasion resistance: air blast, 0658(1) falling sand method, 0988(1) acid value, test, 01639(1) acrylic arid, spec., 04416(3) bleached lac varnish, testing, 01650(2) clarity/cleanness, visual, 02090(1,3) def. of terms, D16{1,2,3) density, test, 01475(1) discoloration (light stability), D2620(l) household chemicals, effect, 01308(1) elasticity or toughness, D1642(l) elongation/tensile strength, 02370(1) exterior durability, test, 01641(1) drying at room temperature, 01640(1) flash point, test, 03278(3) Gardner color scale, D1544(1,2,3) gi gas checking and draft test, D1643(l) humidity resistance, 02247(1) indentation hardness, test, D1474(l) moisture vapor permeability, 01653(1) nonvolatile matter content, 01644(1) preparation of free films, 04708(1) preparing glass panels for testing, D3$91(l) Varnishes (continued) preparing steel panels for testing, D609(l) rosin adds content, D1469(2) rosin content, Lieberman-Storch, D1542(1,2) rosin content, Halphen-Hicks, D154201,2) scrape adhesion test, D2197(l) selection of test procedures, D1S4(1) shellac varnish, testing, D1650(2) specific gravity at 25/25C, 01963(3) test environments, 03924(1) viscosity, dip-type viscosity cups, 04212(1) viscosity. Ford cup, D1200(1) volatile/nonvolatile content, D4209(2) water and alkali resistance, D1647(l) water immersion test, 0870(1) weathering tests on wood, D358(l) wet film thickness, 01212, 4414(1) ` Vehicles, solvent type, pigmented centrifuge for pigment content, 02371,2698(1) centrifuge for vehide separation, 02372(1) non-volatile content, printing inks, 04713 solids identification, infra-red, 02621(1) Venetian red, analysis, D50(2) 5 a Pigments, general properties Vinyl acetate acetaldehyde content, 02191(3) acidity, test, D20S6(3) hydroquinone content, 02193(3) specification, 02190(3) Vinyl chloride monomer (residual) content in polyvinyl chloride resins Vinyl resins polyvinyl butyral, 01396(2) polyvinyl chloride, 04368(2) Viscometers (viscosity} ball drop method, cellulose, 01343(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, 0803(3) 1CI cone/plate (high shear), 04287(1) ISO flow cups, D5125(l) Saybolt, 0856(3) Stormer (Krebs units), 0656(3) Weisseriberg, rheogoniometer, 03451(1) Zahn cups (coil coatings), D3794{1) VM & P Naphtha specification, D3735(3) VOC (Volatile organic compounds) paints and related coatings, D3960CD automotive coatings, abatement, 05087(1) Volatile liquids rate of evaporation, D3539C1) Sa Solvents Volatile matter content See NonvoUtile/volatile content Volatile organic compounds (VOC), 03960(1) Wick test (low viscosity mixtures), 04207(3) Washability, of architectural paints soilant - mechanical washing, 03450(1) stains & soOants - practical test, O 4828(1) Sa Wet abrasion (scrub) resistance Water--high-purity/reagent-grade reagent water, spec., 01193(3) Water-borne paints See Architectural paints Artists1 paints Industrial finishes Water colors See Artists'paints Water content--paints/related materials by gas chromatography, 03792(1) by iodine reagent method, 01631(3) crude cresylic acid, 03439(3) fatty nitrogen compounds, 02072(3) In compressed air, 04265(1) Karl Fischer reagent method, 04017(1) liquid naval stores, 0890(3) petroleum products, by distillation, 095(1,3) pigments, and pigment pastes, 01208(2) solvents, by Fischer reagent method, 01364(3) terpene solvents, 0690 Water fog test, organic coatings, 01735(1) Water immersion test paints on steel, 0870(1) Water miscibility See Miscibility Water pickup test See Printing Inks Water-reducible coatings industrial type, testing guide, 04712(1) Water repellents for wood, evaluation of, D--(1) in prep, masonry treatments,siiane,non vol,05095(1) qualitative test for in wood, D29210) Water resistance of coatings boiling water, of furniture lacquer, 02571(1) controlled condensation, 04585(1) of varnishes, D1647(l) water-fog test, 01735(1) water immersion test, D870(l) Sa Humidity resistance Water-soluble matter, content dry pigments, D1208,2448(2) lac resins, 029(2) pigments (lead chromate type), Dl26(2) salt content, blue pigments, 01135(2) salt content of pigments, 02448(2) Water spotting,exterior latex parints,D1848(l) Water vapor permeability, 01653(1) Wear resistance (Wear life) of traffic paint, 0913(1) Sa Abrasion resistance Weathering See Exposure Weatherometer, See Exposure-accelerated Weissenberg rheogoniometer test viscosity of powder coatings, 03451(1) Wet abrasion (scrub) resistance scrub-to-failure method, D2486(l) weight loss method, 04213(1) Wet film thickness gages See Film thickness gages, wet film Wet ground muscovite mica See Mica Wet-to-dry hiding change of paints, 05009(1) White architectural enamels See Architectural paints and coatings White extender pigments See Extender pigments White hiding pigments Se e 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 859 j st ( r 'J'-' DUP050296418 Condensed Index of Committee D-1 Standards White pigments, analysis extracted from paint antimony oxide content, U2350 combined sulfur, D2351, D23S2(02) general, 0215 (01) practices and methods, list, 034(02) $ a White hiding pigments Extender pigments White zinc See Zinc oxide Whiting S ee Calcium carbonate Wick test See Burning Characteristics Wijs procedure--iodine value drying oils and derivatives, D19590) fatty amines/diamines, test, D2075(3) Wire-wound drawdown bar (Meier rod) coating application method, 04147(1) Wolfe-potentiometric method fatty acids in tall oil rosin, 01583(3) Wood chlorinated phenol in, test for, 02921(1) exposure tests on wood, 01006(1) panels for weathering tests, 0356(1) water repellents for, under devel. by D01.42 water repellents in, test for, D2921{1) Wood finishes blocking test, D2793E1) dry film thickness, 02691(1) exposure tests, practices, 01006(1) factory applied: liquid/fresh film, properties, 02336(1) factory primed, durability tests, D2830(l) humid-dry cycling, 03459(1) preservative, chlorinated phenol, 02921(1) temperature of coating cure cycle, 03259(1) weathering tests, panels for, 0358(1) $tt Factory applied finishes Wood rosin. See Rosin Wood sash glazing compounds See Caulking/glazing/sealant compounds Wood turpentine. See Turpentine Xenon lamps exposure, nonmetallic materials, G26(l) lightfastness of pigments, D4303(l) Xylene ten*degree, spec.,D846<3) Yellow ocher See Ocher Yellow pigments See Basic lead sUicochromate Chrome yellow Iron oxide yellow Ocher Strontium chromate Zinc chromate Zinc driers See Driers Zinc dust pigment analysis, D521(2) specification, 0520(2)- Zinc hydroxy phosphite analysis, 04450(2) specification, 04462(2) Zinc oxide analysis, 03280(2) specification, 079(2) Sa Figments,general properties Zinc-rich primer. See Primers Zinc sulfide analysis, 03280(2) specification, 0477(2) Sa Figments, 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, 04794(2) methoxyl hydroxypropyt sub.,, 03876(2) Zinc chromate analysis, 0444(2) specification, D478(2) Sa Figments, general properties Zinc-coated (galvanized) surfaces preparation for painting, 02092(1) Zinc content driers, EDTA method, 02613(3) white linseed oil paints, 0215(1) white zinc pigments, 03280(2) zinc dust pigment, D521(2) zinc hydroxy phosphite, 04450(2) 860 DUP050296419 ANNUAL BOOK o f ASTM STANDARDS Index 1 Section 6 PAINTS, RELATED COATINGS, AND AROMATICS This index covets the standards, and related material appearing in Volumes 06.01, 06.02, and 06.03. The boldface references are to the 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. 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 issued as Volume 00.01. 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.. In the preparation of indexes, every attempt has been made to index standards on three levels: (1) by main subject, using general and specific search terms; (2) by test methods or other significant sections ofASTM standards; arid (3) by cross-references to locate main subject entry terms. (See also references are abbreviated as Sa and appear under main entry terms.) Specification F451, for Acrylic Bone Cements (Volume 13.01), illustrates ASTM's method of indexing. s: INDEX TERMS FOR MAIN SUBJECT ENTRY Adhesives--surgical implant materials acrylic bone cements (for internal orthopedic prostheses), self-curing, spec., F 45.1 . Orthopaedic medical devices--bone acrylic bone cements (for internal orthopedic prostheses), 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) 861 DUP050296420 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, 0968 (06.01) abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) air blast abrasion tester, A D 658 (06.01) scrub-to-failure of interior latex flat wall paints, test, D 2486 (06111) Taber abraser, test, 0 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 (0601) 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, 0 4838 (06.01) Accelerated testing--paints/related coatings/materials accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure ' apparatus, practice, D 822 (06.01) coatings (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, 01654 (06.01) nonvolatile content of latexes, test, D4758 (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, B117 (06.01) Accelerated testing--wood products wood used as panels in weathering tests of coatings, spec., 0 358 (06.01) Acetaldehyde (AA) Sa Aldehydes acetaldehyde content of vinyl acetate, test, D 2191 (06.03) 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, 03545 (06.03) Acetic add content cellulose acetate, test, 0871 (06.02) Acetic acid (glacial) formic acid in gladai acetic acid, test, 0 3546 (06.03) gladal (99.8 %) acetic add (for use in paint/vamish/ lacquer/related products), spec., 0 3620 (06.03) > < Acetone acetone in methanol (methyl alcohol), test, 0 1612 (06.03> acetone, spec., D 329 (06.03) acetone tolerance of heat-bodied drying oils, test, D1950 (06.03) alkalinity in acetone, test, 0 1614 (06.03) apparent pH ofwater insoluble phenol-formaldehyde resin, test, 04613(06.02) permanganate time of acetone/methanol, test, 0 1363 (06.03) Acetophenone analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 04961(06.03) Acetyl content acetone in methanol (methyl alcohol), test, 01612 (06.03) apparent acetyl content of cellulose acetate proprionate/ butyrate, test, A 0 817 (06.02) combined acetyl/acetic add content of cellulose acetate, test, 0871 (06.02) Acetylene black See Carbon black (headings) Acid content add/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, 0 4370 (06.01) Add-insoluble extenders add-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, 01135 (06.02) Addity, alkalinity, pH--paints/related coatings/materials acetaldehyde, spec., 0 4710 (06.03) add/amine value of fatty quaternary ammonium chlorides, test, 02081(06.03) acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, 04370 (06.01) addity in vinyl acetate and acetaldehyde, test, 0 2086 (06.03) addity in volatile solvents/chemical intermediates (used in paint/varnish/lacquer/related products), test, 01613(06.03) acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, 0 847 (06.03) alkalinity in acetone, test, 01614 (06.03) apparent pH of electrocoat baths, test, 0 4584 (06.01) apparent pH of water insoluble phenol-formaldehyde resin, test, 04613(06.02) cellulose acetate propionates/butyrate, test, A 0-817 (06.02) cellulose acetate; test, 0 871 (06.02) ethylcellulose, test, 0914 (06.02) formaldehyde solutions, ted, 0 2379 (06.03) hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, 0 2363 (06.02) methyl acrylate, spec., 0 4709 (06.03) methylcellulose, test, 01347 (06.02) moisture content of pigments, 01208 (06.02) pH of chemically cleaned/etched concrete surfaces. 04262(06.01) Addity, alkalinity, pH--plastics cellulose acetate propionates/butyrate, test, A 0 817 (06.02) Add number Sa Saponification number/value rosin oil, test, 01131 (06.03) rosin, test, 0 465 (06.03) sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) sampling and testing turpentine, method, 0 233 (06.03) tall oil, methods of testing, 0 803 (06.03) Add pbthalic anhydride See Pbthalic anhydride 862 m DUP050296421 Index of ASTM Standards, Section 6 Alkyds/atkyd resins resistance mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) inluble extenders soluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) value id/amine value of fatty quaternary ammonium chlorides, test, D 2076 (06.03) id value of organic coating materials, test, D1639 (06.01) adds and polymerized fatty adds, test, D 1980 (06.03) ipling/tesdng lac resins (orange shellac/button lac/gamet I iac/bleached lac), test, D 29 (06.02) j<l wash color imatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) ite esters [ty, by gas chromatography, test, D 3362 (06.03) /lie acid jHcrylic acid dimer in acrylic acid/unsaturated organic adds, test, D 4415 (06.03) glacial acrylic acid (99.0 % grade), spec., D 4416 (06.03) 'lie latex paints Sa Latex paints artists' acrylic emulsion paints, spec., D 5098 (06.01) jiartists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) water content of water-redudble paints, by direct injection into gas chromatograph, test, D 3792 (06.01) crylie polymer content qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) :t!ve oxygen content--organic solvents ^ trace peroxides (5-80 ppm), using spectrophotometer, test, E 299 (06.03) hesion--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) dear/pigmented organic coatings, test, D1308 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) mar resistance oforganic 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, 04948(06.01) commercial hexanes, spec., D1836 (06.03) Adhesives--structural trace peroxides (5-80 ppm), using spectrophotometer, test, E 299(063)3) Adulteration See Purity African ocher See Ocher Aged coatings assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Air blast abrasion tester paints and related coatings, test, A D 658 (06.01) Air blast cleaning oil/water presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), 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-soluble content alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) Alcohol content . alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) polyhydiic alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) Alcohol resistance wood furniture lacquers, test, D 2571 (06.01) Alcohols (C4-C]3) 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 cresylate solutions . . __ - cresylic acid content (of alkaline cresylate solut!ons),-cbemical ' analysis, D 3439 (06.03) Alkaline earth carbonates add-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Alkalinity alkalinity in acetone, test, D1614 (06.03) Alkali resistance dear/pigmented organic coatings, test, D1308 (06.01) dried varnish films, test, D1647 (06.01) Alkyds/aliyd 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 add content, test, D1398 (06.02) glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D1615 (06.02) identification of carboxylic adds in alkyd resins D 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (063)2) DUP050296422 s resins Index of ASTM Standards, Section 6 'm ;id content of alkyd/polyester resins, test, (06.02) ydride content (in absence of dibasic acids), test, j`563(06.02) phthalic anhydride content (in presence of dibasic acids), by gravimetric test, D1306 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) roan acids content, test, D1469 (06.02) silicon content of silicone polymers/silicone modified alkyds, by atomic absorption spectrophotometry, test, D3733 (06.02) specific gravity at 25/25"C, test, D1963 (06.03) .testing industrial water-reducible coatings, guide, D 4712 (06.01) unsaponifiable matter content, test, D1397 (06.02) All-day testing See Twenty-four'hour testing Alternative indicator method total, primary, secondary, and tertiary amine values offatty amines, test, D 2074 (06.03) Alumina acid-soluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) alumina/iron oxide in magnesium silicate pigment, test, 0717(06.02) Alumina hydrate acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Aluminum acid/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (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) Aluminum alloys preparation of aluminum/aluminum-alloy surfaces (for painting), practice, D1730 (06.01) preparation of hot-dip aluminum surfaces (for painting), practice, D1731 (06.01) Aluminum coatings See Coatings---aluminum Aluminum oxide (A1j 03) content aluminum oxide in aluminum silicate (hydrous/anhydrous) pigment, test, D 718 (06.02) aluminum oxide in titanium dioxide (TiO^pigments, test, D1394 (06.02) Aluminum potassium silicate See Mica pigment , Aluminum powder and paste Set Pigments (headings) aluminum powder/paste pigments for paints, spec., O 962 (06.02) sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) Alnmhmm reduction method total titanium in white titanium pigments, by aluminum reduction method, test, D1394 (06.02)' Aluminum silicate pigments aluminum silicate (hydrous/anhydrous) pigment, analysis, test, D 718 (06.02) aluminum silicate pigments (anhydrous), spec., D 3619 (06.02) aluminum silicate pigments (hydrous), spec., D 603 (06.02) American turpentine See Turpentine Amidoamines See Fatty amidoamines Amine resins Sa Resins (headings) amine resins--solvent tolerance, test, D1198 (06.02) Amines .-us*, See Fatty amines t. Amines content percent of amines (primary/secondary/tertiary) in fatty amines , test, D 2083 (06.03) ? Amine value acid/amine value of fatty quaternary ammonium chlorides., test 02076(06.03) i^ Amine values (total/primary/secoudary/tertiary) fatty amines/arnidoamines/diamines, by referee potentiometnc method, test, D 2073 (06.03) fatty amines, by alternative indicator method, test, D 2074 (06.03) Aminolysis a identification of polyhydric alcohols in alkyd resins, quaiitative/quantitative analysis, test, D 2456 (06.02) Amino resins , amino resins, selecting test procedures, practice, D 4277 (06.02) free formaldehyde content of amino resins, test, D1979 (06,02). Ammonium hydroxide content ammonium hydroxide group (alumina/iron oxide) in magnesium silicate pigment, test, D717 (06.02) Amyl acetate primary (synthetic) amyl acetate (98 % grade), spec., D 3540 (06.03) Amyl alcohol (synthetic) amyl alcohol (synthetic), spec., D 319 (06.03) Anatase-ratile ratio ratio of anatase to rutile in titanium dioxide (TiOJ pigments, by x-ray diffraction, test, D 3720 (06.02) Angle of incidence joss differences between surfaces of similar appearance, method for visual evaluation, p 4449 (Q6.01) Aniline industrial grade aniline, spec., D 3264 (06.03) nitrobenzene in aniline, test, D 4589 (06.03) sampling and handling aniline, practice, D 3436 (06.03) Aniline point aniline point/mixed aniline point of petroleum products/ hydrocarbon solvents, test, D 611 (06.03) . sampling and testing dipentene, method, D 801 (06.03) Animal black See Bone, black ANSI replacement standards use ofprotective coating standards in nuclear power plants, : ,selecting ASTM standards, guide, D 5144 (06.01) Anti-corTO$ion pigments---basic lead silicocSromate - . basic lead 9ilieochromate pigment, spec., D1648 (06.02) chromium trioxide content of basic lead siHco-chromate pigment, test, D1844 (06.02) ,, Anti-corrosion 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) Anti-corrosion pigments--strontium chromate chemical analysis of strontium chromate pigment, test, 0 1845(06.02) strontium chromate pigment, spec., D1649 (06.02) Anti-corrosion pigments--zinc chromate analysis, D 444 (06.02) zinc yellow (zinc chromate) pigments, spec., D 478 (0&02) Anti-corrosion pigments--zinc hydroxy phosphite analysis, D 4450 (06.02) zinc hydroxy phosphite pigment, spec., D 4462 (06.02) Antifouling coating system erosion testing of antifouting 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, O 5108 (06.01) 864 DUP050296423 Index of ASTM Standards, section u Ash content--paints/related coatings/materiais shallow submergence test, D 3623 (06.01) Subjecting marine antifbuling coating to bifouling and fluid ; shear forces in natural seawater, test, 0 4939 (06.01) kifonling paint pigments--copper powder chemical analysis of cuprous oxide/copper pigments, test, j 0283(06.02) jcopper powder (for antifouling paints), spec., D 964 (06.02) Mfouling paint pigments--cuprous oxide chemical analysis of cuprous oxide/copper pigments, test, 0 283 (06.02) cuprous oxide (for antifouling paints), spec., 0 912 (06.02) jtifouiing paint pigments--mercuric oxide fanalysis, D 284 (06.02) mercuric oxide for use in antifou'iing paints, spec., 0911(06.02) ntimony content antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, 03717 (06.01) ntimony oxide Sa Pigments (headings) i antimony content (low concentrations) in solids of liquid I coatings/dried films, by atomic absorption spectroscopy, test, 0 3717(06.01) j antimony oxide content of white pigment (separated from ; solvent-type paints), test, D 2350 (06.02) inti-sag meter ! sag resistance of paints, using a multinotch applicator, test, 04400(06.01) Apparent acetyl content apparent acetyl content of cellulose acetate proprionate/ I butyrate, test, A 0 817 (06.02) Apparent tack. ! apparent tack of printing inks/vehicles,> by inkometer, test, 04361 (06.01) Appearance of materials bleeding characteristics, of dry pigments, test, D 279 (06.02) : blistering (of paints/related coatings), A D 714 (06.01) chalking (of white/lightly tinted exterior paint films), practice, A 0 4214 (06.01) checking (of exterior paints), test, A 0 660 (06.01) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, 0 2090 (06.02, 06.03) | clear/pigmented organic coatings, test, 01308 (06.01) cracking (of exterior paints), test, A 0 661 (06.01) degree of rusting on painted steel surfaces, method, A 0610 (06.01) erosion (of exterior paints), A 0 662 (06.01) evaluating degree of bleeding of traffic/pavement marking paint, test, A D868 (06.01) flaking (of exterior paints), A 0 772 (06.01) gas checking/draft test (of varnish films), 01643 (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, 0 4941(06.01) printing inks/ink films/related materials, selecting test methods, guide, 0 5010 (06.01) selection/preparation of coating specimens, practice, 03964(06.01) testing industrial water-reducible coatings, guide, 0 4712 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, O 5146 (06.01) Application properties testing industrial water-reducible coatings, guide, 0 4712 (06.01) Application viscosity (for paints/related products) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Aqueous coatings sag resistance of paints, using a multinotch applicator, test, 04400(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, 0 4946 (06.01) evaluating architectural paints for purchase by state/local governments, practice, 03927 (06.01) index to selection and use of testing procedures, 0 2833 (06.01) interior latex semigloss/gloss paints, selecting test methods, guide, 04540 (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, 0 4828 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, 0 5146 (06.01) wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) Architectural paints and coatings hiding power of architectural paints applied by roller, test, 0 5150 (06.01) print resistance of architectural paints, test, 0 2064 (06.01) Architectural sandstone preparatory surface cleaning of architectural sandstone, practice, 05107(06.01) Aromatic hydrocarbons See Hydrocarbons (headings) Aromatic potentiometer titrator acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, 0 4370 (06.01) Aromatics content aromatics (ethylbenzene and eight-carbon (C8/heavier) content in mineral spirits, by gas chromatography, test," 0 3257(06.03) chemical analysis of benzene, by gas chromatography, test, D 4492 (06.03) Arsenic content arsenic in paint, test, 0 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, 0 4236 (06.01) lightfestness of pigments (in artists' paints), test, 0 4303 (06.01) preparing drawdowns of artists' paste paints, practice, 04941 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) Asbestine See Magnesium silicate Ash content soluble cellulose nitrate, testing, methods, 0 301 (06.02) Ash content--paints/related coatings/materiais acid/amine value of fatty quaternary ammonium chlorides, lest, 0 2077(06.03) ashing cellulose, test, O 3516 (06.02) cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, 0 871 (06.02) drying oils and fatty acids, test, D1951 (06.03) 865 DUP050296424 Index of ASTM Standards, Section 6 Ash content--paints/related coatings/materials ethylceliulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydioxyethylcellulose, test, D 2364 (06.02) methylcellulose, test, D1347 (06.02) moisture content of pigments, D120S (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 lac/gamet lac/bleached lac), test, D 29 (06.02) tall oil, methods oftesting, 0 803 (06.03) Atmospheres--conditioning/testing standard environments for conditioning/testing paint/ varnish/lacquer/related materials, spec., D 3924 (06.01) Atmospheric analysis 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) Atomic absorption See Spectrophotometry--atomic absorption Atomic absorption spectrophotometry See Spectrophotometry--atomic absorption Atomic absorption spectroscopy See Spectroscopy--atomic absorption Automatic spray producing films of uniform thickness ofpaint/vamish/related products on test panels, test, D 823 (06X11) 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, 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, D5125 (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 (06.01) Bacteria/bacterial control--paints/related coatings/materials 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, 03273 (06.01) Baked coatings nonvolatile content of latexes, test, D 4758 (06.02) Baker-Phiiippoff equation intrinsic viscosity of cellulose acetate, using modified Baker-Phiiippoff equation, test, D 871 (06X12) Baking (paints/related coatings) effects of overbaking on organic coatings, practice, 02454 (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 j:, t, , | viscosity of cellulose derivatives, by ball-drop method, test, D1343 (06.02) ' " i| Bar codes j abrasion resistance of printed matter, by the ga-cat comprehen- 1 sive abrasion test, 0 5181 (06.01) Barite See Barium sulfate pigments Barium sulfate acid-soluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, 01135 (06.02) Barium sulfate content barium sulfate content in barium sulfate pigment, test, 0 715(06.02) Barium sulfate pigments Sa Pigments (general properties) barium sulfate pigment, analysis, test, 0 715 (06.02) barium sulfate pigments, spec., 0 602 (06X12) Barriers comparative corrosion preventive characteristics of materials used for joints/oouplings/fittings/patches in pipeline coatings, test, G18 (06.01) Bartlet white lead See Basic sulfate white lead Barytes barium sulfate pigments, spec., D 602 (06.02) Base content add/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06X11) Basic carbonate white lead basic carbonate white lead pigment, spec., 0 81 (06.02) white lead- chemical analysis, test, D1301 (06.02) Basic lead silicochrvmate basic lead silicochromate pigment, spec., D1648 (06.02) chromium trioxide content of basic lead silico-chromate pigment, test, 01844 (06.02) Basic sulfate white lead white lead- chemical analysis, test, D1301 (06.02) Beilstein analysis field identification of coatings, test, D5043 (06.01) Bend testing--coatings effects of outdoor weathering on pipeline coatings, test, Gil (06.01) mandrel bend test of attached organic coatings, test, D522 (06.01) ........... specific bendability of pipeline coatings,-test, G10 (06.01) - Benzene ----- acidity of benzeneAoluehe/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color, test; D 848 (06.03) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocatbons/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 of benzene, by gas chromatography, test, ' D 4492 (06.03) commercial density (ofpure liquid chemicals), test, D 3505 (06.03) cyclic hydrocarbon products, by gas chromatography, test, D 4534 (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) 866 DUP050296425 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, D3437 (06.03) solidification point, test, D 852 (06.03) thiophene content of benzene, by spectrophotometry, test, D1685 (06.03) thiophene content of refined benzene, by gas chromatography (with Same photometric detection), test, D 4735 (06.03) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toiuene/niixed zylenes, by gas chromatography, test, D 2360 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06j 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) Blsphenol 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'-isopropyiidenediphenol (dissolved in methanol), test, 4789 (06.03) Bituminous materials (general) 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) water in petroleum products/bituminous materials, by distillation, test, D 95 (06.01,06.03) Black box exposure test accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06.01) 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/garnet 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 (06.01) laboratory evaluation of degree of bleeding of traffic/pavement marking paint, test, D 969 (06.01) Blended sllane-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 (06.01) testing water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) Blocking blocking resistance of trade sales paints, test, D 494$ (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) Blotching repenting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Blue-light reflectance See Reflectance and reflectivity (headings) Blue pigments Sa Iron blue/Phtbalocyanine blue Ultramarine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) Blunt rod test penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Boiled oils (drying) See Oils (headings) Boiling point industrial aromatic hydrocarbons, test, D 850 (06.03) Boiling water resistance wood furniture lacquers, test, D 2571 (06.01) Bonding . .- comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Bond strength bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Bone black bone black pigment, spec., D 210 (06.02) solvent extractable material in black pigments, test, D305 (06.02) Bone-dry bleached lac See Bleached lac--dry Book covers abrasion resistance of printed matter, by the gsucat comprehen sive abrasion test, D 5181 (06.01) Boron trioxlde (Bj Oj ) calcium borosilicate, test, D 4487 (06.02) Brabender moisture tester moisture content of (iron/copper phthalocyanine/ultramarine) blue pigments, by Brabender test, D1135 (06.02) Break drying oils, test, D1952 (06.03) Breaks cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) Brick bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Brightening power See Tlnthig strength Broad-band filter reflectometry directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) DUP050296426 Index of ASTM Standards, Section 6 Bromide content Bromide content titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D 4764 (06.01) Bromine index aromatic hydrocarbons, by coulometric titration, test, 01492 (06.03) Bronze blue See Iron blue 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, D50 (06.02) iron oxide black (natural)- chemical analysis, test, 03872(06.02) natural red/brown iron oxide pigments, spec., 0 3722 (06.02) synthetic brown iron oxide pigment, spec., D 3724 (06.02) Brunswick blue See Iron blue Brunswick green See Chrome green Brush-application behavior testing industrial water-reducible coatings, guide, 0 4712 (06.01) Brush drag comparison of the brush drag of latex paints, test, D 4958 (06.01) Brushes preparation of paint brushes for evaluation, practice, 05068(06.01) Bubble test viscosity of transparent liquids, by bubble time method, test, 0 1545 (06.01, 06.02, 06.03) Bulk density See 0ensity--apparent (bulk) Burning characteristics--paints/related coatings/materials fire retardancy of paints, by cabinet method, test, A 0 1360 (06.01) small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, 0 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, 0 4207 (06.03) Burnt sienna Sa Pigments (headings) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, 0 50 (06.02) raw/bumt sienna pigments, spec., 0 765 (06.02) Butadiene purity of hydrocarbons from freezing points, test, D1016 (06.03) Butane purity of hydrocarbons from freezing points, test, 0 1016 (06.03) 1- Butanol See n-Butyl alcohol 2- Butanol See rec-Butyl alcohol 2-Butanone See Methyl ethyl ketone (MEK) Butoxyethano! 2-butoxyethanol, 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, 0 29 (06.02) ij-Butyl acetate alcohol content/purity of acetate esters, by gas chromatogtaohv test, 03545 (06.03) 1 n-butyl acetate (all grades), spec., 0 4615 (06.03) n-Butyl acrylate n-butyl acrylate, spec., 03547 (06.03) purity, by gas chromatography, test, 0 3362 (06.03) unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06,02) n-Butyl acrylate/methacrylate unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) o-Butyl alcohol n-butyl alcohol (butanol), spec., 0 304 (06.03) sec-Butyl alcohol sec-butyl alcohol, spec., 01007 (06.03) Butylated melamine-formaldehyde resins See Resins Butylcatechol inhibitor content p-tert-butylcaiecbol (TBC) in styrene monomer, test, 02120(06.03) residual p-/ert-butyIcatechol (TBC) in styrene monomer, by addition of NaOH, test, 0 4590 (06.03) Butyl glycol See Butoxyethano] n-Butyl methacrylate unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06.02) Butyraldehyde Sa Resins (headings) poly(vinyl butyral)- chemical analysis, test, 01396 (06.02) Butyryl content cellulose acetate propionates, test, A 0 817 (06.02) c C4-C]3 alcohols chemical/physical analysis, selection/use oftest procedures, E 852 (06.03) Cabinet method fire retardancy of paints, by cabinet method, test, A 01360 (06.01) Cadmium content lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test^0 3335 (06.01) Calcium borosilicate analysis, 04487(06.02) calcium borosilicate pigments, spec., 0 4288 (06.02) Calcium carbonate calcium carbonate pigment, spec., 01199 (06.02) Calcium content calcium/zinc content, by EDTA method, test, 0 2613 (06.03) metals (iron/copper/manganese/calcium) content ofcellulose pulp (from wood/cotton), by atomic spectrophotometry, test, 0 4085 (06.02) zinc dust (metallic zinc powder), test, 0 521 (06.02) Calcium oxide (CaO) content calcium borosilicate, test, 0 4487 (064)2) calcium oxide in magnesium silicate pigment, test, 0717(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 (06411) 868 i. DUP050296427 Index of ASTM Standards, Section 6 Chain length uniformity Calibration--paints/related coatings instrumentation equipment/standards for measuring purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) viscosity of printing inks/vehicles, by falling-rod viscometer, test, 04040 (06.01) Capacitance comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Capillary gas chromatography analysis of styrene by capillary gas chromatography, test, 05135(06.03) unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06.02) . Capillary-moisture relations capillary moisture in concrete, by plastic sheet method, test, D 4263 (06.01) Carbon-arc lamps accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, 0 822 (06.01) conducting tests on paint/vamish/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 nonmetallic materials, practice, G 23 (06.01) operating unfiitered apparatus (for testing paints/related coatings), using the Dew cycle, practice, D 3361 (06,01) Carbonate content acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, 0 1135 (06.02) Carbon black carbon black pigment for paint, spec., 0 561 (06.02) solvent extractable material in black pigments, test, 0305(06.02) Carbon black content solvent extractable material in black pigments; test, 0305(06.02) Carbon disulfide content carbon disulfide content of aromatic hydrocarbons, using spectrophotometry, test, D 2324 (06.03) Carboxyl content carboxyl content of cellulose, test, 01926 (06.02) Carboxylic acid identification of carboxylic adds in alkyd resins 0 2455 (06.02) Carboxylic acids content alkyd resins, test, 0 2455 (06.02), Castor oil dehydrated castor oil, spec., 0 961 (06.03) hydroxyl value of fatty oils/acids, test, D1957 (06.03) raw castor oil, spec., 0 960 (06.03) spectrophotometric diene value of dehydrated castor oil/derivatives, test, 0.1358 (06.03) Cellular plastics See Urethanes {headings) Cellulose and cellulose derivatives alcohol-benzene soluble matter in cellulose, test, 01794 (06.02) ashing cellulose, test, 0 3516 (06.02) carboxyl content of cellulose, test, 0 1926 (06.02) cellulose/cellulose derivatives, terminology, 0 1695 (06.02) cellulose (chemically refined), composition by chromatographic analysis, method, 0 1915 (06.02) chain length uniformity, by fractional predpitation of cellulose nitrate, test, 0 1716 (06.02) chlorine content, test, 0 2641 (06.02) dichloromethane/l,l,!-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) dichloromethane-soluble matter content of cellulose, test, 0 3971(06.02) ethoxyl substitution in cellulose ether products, by gas chromatography, test, 04794 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, tesi 0 2363 (06.02) hydroxyethylcellulose, test, 0 2364 (06.02) in cellulose ether products methoxyl and hydroxypropyl substitution, by Zeisel-gas chromatographic technique, test, 0 3876(06.02) intrinsic viscosity of cellulose, test, 0 1795 (06.02) methylcellulose, testing, 01347 (06.02) moisture in cellulose, test, 01348 (06,02) nitrogen content of soluble nitrocellulose, by ferrous sulfate procedure, test, D 4795 (06.02) pentosans content of cellulose, test, 01787 (06.02) silica content, test, D 2438 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, 0 1439 (06.02) . solubility in sodium hydroxide, test, 0 1696 (06.02) soluble nitrocellulose-base solutions, methods of testing, 0 365(06.02) sulfur content, by X-ray fluorescence, test, 0 2929 (06.02) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, 01211 (06.01) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, 04209 (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, 03133 (06)01) dilution ratio for solutions, test, 0 1720 (06.03) soluble cellulose nitrate, testing, methods, 0 301 (06.02) Cellulose and cellulose derivatives--ethylcellulose (EC) etbylcellulose, methods oftesting, 0914 (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, A 0 817 (06.02) Cement bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, 04796 (06.01) Cementitious linings inspection of linings in operating flue gas desulfurization systems, practice, O 4619 (06.01) Centrifuge (high-speed for vehicle separation) See Vehicle separation--solvent-type paints Ceramic whitewares directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Cerium content cerium content (of paint driers), by EDTA method, test, 03970(06.03) Cerium paint driers See Oriers Certification form certification of coating conformance form, D 5063 (06111) Chain length uniformity cellulose, by fractional precipitation of cellulose nitrate, test, 01716(06.02) 869 DUP050296428 Index of ASTM Standards, Section 6 Chalk Chalk See Calcium carbonate Chalking white/lightly tinted exterior paint films, practice, A D 4214 (06.01) Change in color See Color (headings) Channel black See Carbon black (headings) Char index fire retardancy of paints, by cabinet method, test, A D1360 (06.01) Checking exterior paints, test, A D660 (06.01) Chemical analysis--paints/related coatings/materials calcium borosilicate, test, D4487 (06.02) CrC,j alcohols, chemical/physical analysis (selection/use of test procedures), 852 (06.03) chemical analysis of yeDow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) ethyl methyl pentanol content/purity value of2-ethyihexanoi, 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, D4797 (06.01) zinc hydroxy phosphite, test, D4450 (06.02) 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 (06111) 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., D 4835 (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/materials ethylcefiulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D1347 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, 01439(06.02) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) Chlorinated hydrocarbons dichloromethane/1,1,1 -trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(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, X> 4301 (06.02) hydrolyzable chlorine content of liquid epoxy resins, test, D 1726(061)2) 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 fonnahility/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 (06.02) Chromatography--gas (detergents) methoxyl/hydroxypropyl substitution (of cellulose ether products), by Zeisel technique, tefl, D3876 (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, qnaiitative/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, D3962 (06.03) analysis ofp-xylene, method, D 3798 (06.03) ' ' analysis ofstyrene 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/l,l,l-trichloroethanecdSrent in paints/ ' coatings,-by direct injection gas chromatography, test, D 4457 (06.01) ethoxyl Substitution in cellulose ether products, py gas r; chromatography, test, D 4794 (06.02) ethyl methyl pentanol content/purity value of 2-ethyihexanoi, 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 adds 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; 0 2195(06.03) phenol content (of tar add mixtures), by gas liquid chromatog raphy, test, D 3626 (06.03) pinene composition (ofwood/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, D 3054 (06.03) 870 DUP050296429 Index of ASTM Standards, Section 6 Coatings purity of methyl (amyl ketone/isoamyl ketone), test, D3893 (06.03) purity of methyl ethyl ketone, using gas chromatography, test, D2804 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) qualitative identification of polymers in. emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) solvent composition analysis (of solvent-type paints), direct-injection technique, practice, D 3271 (06.01) thiophene content ofrefined benzene, with flame photometric detection, test, D4735 (06.03) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, test, D 2360 (06.03) uniformity (of traffic paint vehicle solids), practice, D 2743 (06.01) unreacted monomer content of latexes, test, D4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) unreacted toluene diisocyanate content of urethane prepoly mers/coatings, test, D3432 (063)2) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) xylene, purity of ortAo-xylene, test, D 3797 (06.03) Chromatography--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 1 cellulose (chemically refined), composition by chromatographic i analysis, method, D1915 (06.02) l Chrome green j Sa Pigments (general properties) chemical analysis of phthalocyanine blue/green pigments, test, \ D3256 (06.02) | chrome green pigment, spec., D 212 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) | Chrome yellow and orange I chrome yellow/orange pigment, spec., D 211 (06.02) I yellow/orange/green pigments containing lead chromate/ | chromium oxide green, analysis, test, D126 (06.02) I 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 ofstrontium 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, D4358 (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 green/Lead silicochromate Zinc chromate (yellow} Chromium trioxide content chromium trioxide content of basic lead silico-chromate pigment, test, D 1844 (06.02) Chronic health hazards See Hazards--health CIE color system degree of rusting on painted steel surfaces, method, A D 610 (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, D5043 (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 (06313) Cleaning solvents See Solvents Closed-cup flash point methods See flash point (headings) Cloud point aromatic hydrocarbons/related chemicals, terminology, D4790 (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, D 3359(063)1) organic coatings, applied to smooth panel surfaces^ by scrape adhesion test, D 215)7 (06.01) Coating capacitance water penetration into pipeline coatings, test, G9 (06.01) Coating contractors See Nuclear reactor vessels--qualifications for painters Coating industry design/use of safety alert system for hazardous work locations in coating/lining industry, practice, A D4257 (06.01) Coating leveling See Leveling characteristics Coatings accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D3717 (06.01) DUP050296430 Index of ASTM Standards, Section 6 Coatings assessing the condition of aged coatings on steel surfaces, guide, D5065 (06.01) certification of coating conformance form, D 5063 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D3718 (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, D5064 (06.01) dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) dry film thickness, by microscopical measurement, D2691 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (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 (clear/pigmented) coatings for rigid/semirigid plastics substrates, practice, D 3002 (06.01) exposure of paints/related coatings to fluorescent UVeondensation 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, D1210 (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, D 4121 (06.01) porosity of paint films (to indicate coating penetration), test, 03258(06.01) presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) producing films of uniform thickness of paint/varnish/related products on test panels, test, 0823 (06,01) pull-off strength of coatings, using portable adhesion testers, test, D4541 (06.01) purity of methyl isobutyl ketone, by gas chromatography, test, D 3911 (06.01) sag resistance of paints, using a multinotch applicator, test, 04400(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, D3259 (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 clear/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, D 4147 (06.01) coil coatings, testing, practice, D 3794 (06.01) Coatings--enamel amount of liquid separated as upper layer from a viscous sblution/dispersion containing dispersed solids, test, D 4948 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D S031 (06.01) gloss of high-gloss metaliic/nonmetallic surfaces, by goniophotometry, method, 430 (06.01) Coatings--epoxy subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06411) Coatings--organic See Organic coatings Coatings--ultraviolet-cured cure time, practice, D 3732 (06.01) estimating package stability of coatings for ultraviolet curing, test, D 4144 (06.01) Coatings 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, hy direct soil burial, test, G19 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Cobalt content lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) paint driers, by EDTA method, test, D 2373j (06.03) Cobalt paint driers Sa Driers liquid paint driers, selection of test methods, D 564 (06.03) Coconut oil coconut oil, spec., D1841 (06.03) -- Coefficient of friction static friction of coating surfaces, test, D 4518.(06.01) Coefficient of retroreflection (of retroreflectors) See Re.troreflection/retroreflectors . Coffee stains wood furniture lacquers, test, D 2571 (06.01) _ . Cohesive strength bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Coil coatings application using a wire-wound drawdown bar, practice, 04147(06.01) coil coatings, testing, practice, D 3794 (06.01) Cold-check resistance temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D 1211 (06.01) Cold resistance temperature-change (high-low) resistance of dear nitrocellulose 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) 872 DUP050296431 I Index of ASTM Standards, Section 6 Conformance Color--discoloration dear coatings, by sunlight-through-glass test, D 2620 (06.01) clear/pigmented organic coatings, test, 01308 (06.01) surfaces of paints/related coatings (by microbiological attack), practice for determining by exterior exposure tests, 03456(06.01) Color--light exposure operating carbon-arc light-exposure apparatus with and without water for exposure of nonmetallic materials, practice, G 23 (06.01) Color--lightfastness lightfastness of pigments (in artists' paints), test, D 4303 (06.01) printed matter, D 3424 (06.01) Color--organic/inorganic chemicals acetaldehyde, spec., D 4710 (06.03) cellulose acetate propionates/butyrate, test, A D 817 (06.02) color of cresylic acids ("C" series standards), test, . D 3627 (06.03) fatty acids (after heating), test, D1981 (06.03) maleic/phthalic anhydride (in molten state/after heating), by platinum-cobalt scale, test, D 3366 (06.03) methyl acrylate, spec., D 4709 (06.03) sampling and testing dipentene, method, D 801 (06.03) Color--paints/reiated coatings/materials aluminum silicate (hydrous/anhydrous) pigment, analysis, test, D718 (06.02) artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) benzene/toluene/xylenes/refined solvent naphthas/similar industrial aromatic hydrocarbons, test, D 848 (06.03) cellulose acetate, test, 0 871 (06.02) clarity/deanness of (nonpigmented) paint and ink liquids, by visual examination, test, 0 2090 (06.02,06.03) dear liquids, by platinum-cobalt scale, test, 01209(06.01,06.03) color differences from instrumentally measured color differences of opaque materials, test, D 2244 (06.01) colored pigments (dry/pastes in oil), with a mechanical miiller, test, 0 387 (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, AD 3022 (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/platinum- cobalt), 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, 0 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 Iac/garnet lac/bleacbed lac), test, 0 29 (06112) solid aromatic hydrocarbons/related materials (in molten state), by platinum-cobalt scale, test, D1686 (06.03) solution color of4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) testing industrial water-redudble coatings, guide, 0 4712 (06.01) Colorfastness lightfastness of printed matter, D 3424 (06.01) Colorimeter relative tinting strength of printing ink dispersions, test, 0 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, 05009 (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/abrasive blast cleaning! D 4285 (06.01) Concentration (of elements) concentration of formaldehyde solutions, test, D 2194 (06.03) Concrete--paint applications sample preparation for qualification testing of coatings (used in nuclear power facilities),.spec., 05139 (06.01) Concrete--surfaces abrading concrete, practice, D 4259 (06.01) acid etching concrete, practice, 0 4260 (06.01) capillary moisture, by plastic sheet method, test, D 4263 (06.01) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) _ making and preparing concrete/masonry panels for testing paint finishes, method, D1734 (06.01) pH of chemically cleaned/etched concrete surfaces, 0 4262(06.(11) surface cleaning concrete (for coating), practice,JO 4258 (06.01) surface cleaning concrete unit masonry (for coating), practice, 04261 (06.01) Condensation ,,. water resistance ofcoatings, using controlled condensation, practice, 0 4585 (06.01) Conditioning standard environments for conditioning/testing paint/ vamish/lacquer/related materials, spec., 03924 (06X11) Conductance and conductivity (electrical) cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) conductimetric analysis ofwater-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) continuity verification of liquid/sheet linings applied to concrete substrates, practice, 04787 (06.01) electrical conductivity of electrocoat baths, test, 0 4399 (06.01) Conductivity bridge/cell electrical conductivity of electrocoat baths, test, 0 4399 (06X11) Cone-and-plate viscometers Sa Viscometers (headings) high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Conformance certification of coating conformance form, 0 5063 (06X11) 873 m DUP050296432 Index of ASTM Standards, Section 6 Conical mandrel apparatus Conical mandrel apparatus mandrel bend test of attached organic coatings, test, D 522 (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, D 5161 (06.01) Consistency consistency of paints, using Stormer viscometer, test, D 562 (06.01) Containers--aerosol volatile organic compounds (VOC) of solvent reducible paints in aerosol cans, test, D 5200 (06.01) Containers--fiberboard abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Containers--tank cars/wagons sampling and handling aniline, practice, D 3436 (06.03) sampling/bandling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) sampling procedures--for paints/pigmented coatings, practice, D 3925 (06.01) sampling/unloading procedures--for cresylic acid/phenol, practice, D 3852 (06.03) sampling/unloading procedures--for naphthalene/maleic anhydride/phthalic anhydride, practice, D 3438 (06.03) Contamination--nuclear use of protective coating standards in nuclear.power plants, selecting ASTM standards, guide, D 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, D4940 (06.01) decontaminability of coatings used in light-water nuclear power plants, test, D 4256 (06.01) Continuity verification continuity verification ofliquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) Contractors coating contractor qualification (for nuclear-powered generation facilities), practice, D 4286 (06.01) Contrast ratio hiding power of paints, by reflectometry, test, A D 2805 (06.01) Copal content sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 25k (06.02) Copper--corrosion copper corrosion of industrial aromatic hydrocarbons, test, D 849 (06.03) detection of copper corrosion from petroleum products, by copper strip tarnish test, A D130 (06.03) sampling and testing dipentene, method, D 801 (06.03) Copper content chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) sampling and testing pine tars/pine-tar oils, method, 0856(06.03) Copper phthalocyanine blue Sa Phthalocyanine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) Copper phthalocyanine green See Phthalocyanine green Copper powder chemical analysis of cuprous oxide/copper-pigments, test, D 283 (06.02) copper powder (for antifouling paints), spec., D 964 (06.02) Copper strip test detection ofcopper corrosion from petroleum products, by copper strip tarnish test, A D130 (06.03) Copy materials/products--lithographic water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, D 4942 (06.01) Corn oil com oil, spec., D1842 (06.03) Corrosion--atmospheric testing evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) Corrosion--electrodeposited 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, D 849 (06.03) detection of copper corrosion from petroleum products, by copper strip tarnish test, A D130 (06.03) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) filiform corrosion resistance, test, D 2803 (06.01) sampling and testing dipentene, method, D 801 (06,03) water resistance of coatings, using controlled condensation, practice, D 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 for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06.01) Corrosion--pitting/crevice salt spray (fog) testing, method, B117 (06.01) Corrosivity * detection ofcopper corrosion from petroleum product^ by copper strip tarnish test, A D130 (06,03) Corrugated fiberboard boxes abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Cotton metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) Cottonseed oil Sa Fatty adds--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, D 3961 (06.03) Coulometry--microcoulometry sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, D 3961 (064)3) Couplings comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) 874 .. .. V ^ b DUP050296433 Index of ASTM Standards, Section 6 Degradation--paints/related coatings/materials Cracking--coatings continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) edge performance ofcomposite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) exterior paints, evaluating, test, A D 661 (06.01) mandrel bend test ofattached organic coatings, test, D 522 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) Cresol water content, by iodine reagent method, test, D1631 (06.03) Cresyllc acid and phenol, sampling and handling, practice, D3852 (06.03) color of cresyllc adds ("C" series standards), test, D 3627 (06.03) cresyllc add content (of alkaline cresylate solutions), chemical analysis, D 3439 (06.03) pyridine base content in cresylic add, by direct titration, test, D 4471 (06.03) Gross-cut tape test adhesion of coating films to metallic substrates, by tape test, D 3359 (06.01) Cross-hatch tape test adhesion of coating films to metallic substrates, by tape test, D3359 (06.01) Cross index 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) Crude tar acids See Tar adds--crude/refined Crystallization solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) C(T) specimen testing adhesion of coating films to metallic substrates, by tape test, D 3359 (06.01) Cumene (isopropylbenzene) See Isopropylbenzene (cnmene) Cumene process analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (06.03) Cuprous oxide chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) cuprous oxide (for antifouling paints), spec., D 912 (06.02) Curing characteristics MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Curing of organic coatings See Drying or curing Curing time stroke cure time of thermosetting phenol-formaldehyde resins, test, D4640 (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-redudble coatings, guide, D 4712 (06.01) Cut tape test adhesion ofcoating films to metallic substrates, by tape test, D 3359 (06.01) Cyanoacrylate adhesive adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) Cyclohexane apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) benzene content 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, D 3437 (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) Cyclohexane 995 cyclohexane 99S, spec., D 3055 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, D 3054 (06.03) Cylindrical mandrel apparatus mandrel bend test of attached organic coatings, test, D 522 (06.01) Damping hardness test hardness of organic coatings, by Kdnig/Persoz pendulum hardness tests, D 4366 (06.01) Dark chrome yellow See Chrome yellow and orange Data analysis--recording/reporting results recording results on single-/multi-panel forms, method, AD 1150(06.01) Daylight Sa Reflectance and reflectivity (headings). ... directional reflectance factor (45-deg 0-deg) ofopaque specimens, by broad-band filter reflcctometry, test, E 97(061)1) Decomposition points industrial aromatic hydrocarbons, in distillation tests, D850(06.03) Decontamination decontaminability of coatings used in light-water nuclear power plants, test, D4256 (06.01) use ofprotective coating standards in nuclear power plants,' selecting ASTM standards, guide, D 5144 (06.01) Defects--coatings... photographic documentation of coatings/lining defects and failures, D 4121 (06U1) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Definition of terms naval stores/related products, def. of terms, D 804 (06.03) protective coating/lining work for power generation facilities, terminology, D4538 (06.01) Deformation--paints/related coatings/materials flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) mar resistance of organic coatings, using balanced beam scrape adhesion and mar test, D 5178 (06.01) penetration resistance of pipeline coatings, by blunt rod test, 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) 875 7W DUP050296434 Index of ASTM Standards, Section 6 Degradation--paints/related coatings/materials 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 UV- condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) Degree of cure See Curing characteristics Degree of dispersion See Dispersion Degree of settling evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) Degrees of freedom aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) , Degummed soybean oil See Soybean oil Dehydrated castor oil See Castor oil Densitometer relative tinting strength of printing ink dispersions, test, D 2066 (06.01) Density--paints/related coatings/materials apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) calculating formulation physical constants of paints/coatings, practice, D 5201 (06;01) commercial density (of pure liquid chemicals), test, D 3505 (06.03) hydrogen sulfide/sulfur dioxide (qualitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) methyicellulose, test, D 1347 (06.02) paint/vamish/lacquer/related products, test, A D1475 (06.01) sodium glycolate content of sodium carboxymethylcellulose, test, 0 1439(06.02) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Density--petroleum products volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Dental tin foil substrate preparation of free films of organic coatings, practice, D 4708 (06.01) Deposition deposition efficiency of polymeric powders/powder coatings, practice, D 3451 (06.01) Depth of color See Color (headings) Depth of penetration penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Design--building applications design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) Design basis accident (DBA) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Destructively-distilled wood turpentine See Turpentine Destructive testing--coatings dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) Desulfurization systems ^j design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D4618 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) Detergent materials/systems--drycleaaing mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) Detergent resistance organic finishes, practice, D 2248 (06.01) Deterioration water penetration into pipeline coatings, test, G 9 (06.01) Deterioration--biodeterioration microbiological discoloration (of paint film surfaces), by exterior * exposure tests, practice, D 3456 (06.01) paint films, evaluating degree of surface disfigurement, AD3274 (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) Dew cycle operating light- and water-exposure apparatus (unfiltered carbon-arc type), in testing paints and related coatings, practice, D3361 (06.01) Diacetone alcohol diacetone alcohol, spec., D 2627 (06.03) Diamines See Fatty diamines Diatomaceous silica pigment Sa Silica (diatomaceous) diatomaceous silica pigment, analysis, test, D 719 (06.02) Dibasic adds (absence or presence) See Phthalic anhydride content Dibenzal method monopentaerythritol in commercial pentaerythritol, test, D 2195 (06.03) Dibutyl phthalate '' dibutyl phthalate, spec., D 608 (06.03) Dichloromethane dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) dichloromethane-soluble matter content of'cellulose, test, D 3971 (06.02) Dielectric constant (permittivity)/disslpation-fact6r comparative corrosion preventive characteristics of materials used for'jomts/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) water penetration into pipeline coatings, test, G 9-(06.01) Diethylbenzene isomers impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) Diethylene glycol diethylene glycol, spec., D 2694 (06.03) flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Difatty secondary amines See Fatty amines Differences in color See Color (headings) . Diffraction intensity (of x-rays) See X-ray diffraction Dillon dynamometer bond strength of thermoplastic traffic marking materials, using cement bricks/steei cubes, test, D4796 (06.01) Diluents paint/related coatings- odor (characteristic/restdual), test, D 1296 (06.03) 876 DUP050296435 Index of ASTM Standards, Section 16 Driers Dilutafaility value resin solution dilutability, test, D 5062 (06.03) iDilution ratio/value cellulose nitrate solutions, for active solvents, hydrocarbon diluents, and cellulose nitrates, test, D1720 (06.03) soluble cellulose nitrate, testing, methods, D 301 (06.02) Dimer acrylic aeid dimer in acrylic add/unsaturated organic acids, test, D 4415 (06.03) | Dimethyl-benzyl alcohol analysis of major organic impurities in phenol produced by tbe cumene process, by gas chromatography, test, D 4961 (06.03) Dimethyl ketone See Acetone Dip application testing industrial water-reducible coatings, guide, D 4712 (06.01) Dip coater producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) Dipentene (and related terpene solvents) sampling and testing dipentene, method, D 801 (06.03) Dipropylene glycol dipropylene glycol, spec., D 2696 (06.03) propylene glycol/dipropylene glycol, spec., D 5164 (06.03) Dipropylene glycol monomethy] ether (DPM) dipropylene glycol monomethyl ether, spec., D 4836 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol I monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Dip-type viscosity test viscosity (of paints/vamishes/lacquers/related materials), by dip-type viscosity cups, test, D 4212 (06.01) Direct aspiration spectrophotometric-procedure Sa Spectrophotometry (headings) lead content in paint, by direct aspiration atomic absorption spectroscopy, test, D 4834 (06.01) Directionality gloss of high-gloss metallic/nonmetallic surfaces, by goniopbotometry, 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 Sol! accumulation quantifying dirt collection on coated exterior panels, test, 03719(06.01) Dirt resistance See Resistance--soil Disbonding disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) specific bendability of pipeline coatings, test, 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) coarse particles in pigments/pastes/paints, test, D185 (06.01,06.02) copper phtbalocyanine blue pigment, spec., D 963 (06.02) fineness of grind of printing inks, by NPIRI grindometer, test, 01316(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, D86 (06.03) distillation range (between 30 and 350"Q 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, D3272 (06.01) Distillation--petroleum products distillation of petroleum products, method, D 86 (06.03) water in petroleum products/bituminous materials, by distillation, test, D95 (06.01,06.03) Distilled fatty adds See Fatty adds--specifications Distilled water addity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) Doctor test mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) Dolomite See Calcium carbonate Double rub method MEK. resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Douglas fir wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Draft test varnish films, test, D1643 (06.01) Drag comparison of the brush drag of latex paints, test, - - - - D 4958 (06.01) ____ Drawdowns preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) Draw-down test 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, D4707 (06.01) sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) Driers calcium/zinc content, by EDTA method, test, D 2613 (06.03) cerium content, by EDTA method, test, D 3970 (06.03) clarity/cleanness of (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, D 3804 (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) 877 DUP050296436 Index of ASTM Standards, Section 6 Driers vanadium content, by EDTA method, test, D 3988 (06.03) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D4140 (06.03) zirconium content, by EDTA method, test, D 3969 (06.03) Drop Mack See Bone black Drop tests impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Dry bleached lac See Bleached lac Dry Him thickness See Film--dry film thickness Drying oils See Oils--drying Drying or curing coatings, by ultra-violet techniques, practice for reporting cure time, D 3732 (06.01) MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) organic coatings, at room temperature, determination of film formation rates, test, D1640 (06.01) sampling and testing shellac varnish, D1650 (06.02) soluble cellulose nitrate, testing, methods, D 301 (06.02) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259(063)1) Drying time sampling and testing shellac varnish, D1650 (06,02) Dry red lead See Red lead Durability accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) comparison of the brush drag of latex paints, test, D 4958 (06.01) exterior durability (of varnishes), test, D1641 (06.01) factory-primed wood products with finish coatings, test, 0 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, D 4796 (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, 0 4958(06.01) Eccentric center wheel wet film thickness gage wet film thickness of organic coatings, D1212 (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 (063)3) cobalt content in paint driers, test, D 2373 (06.03) iron content in paint driers, test, D 3804 (06.03) lead content in paint driers, test, D2374 (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, D1736 (06.01) reporting paint film failures characteristic of exterior latex S paints, classification, D1848 (06.01) * J. | i i Efflux cups I viscosity of paints/related materials, by ISO Bow cups, test, D 5125 (06.03) : | Elasticity elasticity/toughness of varnishes, test, D 1642 (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, G 8 (063)1) 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 (063)1) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) impact resistance of pipeline coatings, by falling weighttest, G14 (06.01) impact resistance of pipeline coatings, bylimestone drop test, G13 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) j j f j j ;j j J j j : : | i | Electrical stress cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) " 'j Electrochemical measurements nitrobenzene in aniline, test, D 4589 (06.03) j 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 batfisTtest.D4399 (06.01) nonvolatile- and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (063)1) 1 'j Electrostatic spray 1 evaluating and comparing transfer conditions-laboratory conditions, test, D 5009 (06.01) Electrostatic spray application testing industrial water-reducible coatings, guide, D 4712 (06,01) Elongation mandrel bend test of attached organic coatings, test, 0 522(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, D 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) 878 DUP050296437 Index of ASTM Standards, Section 6 Exposure tests--carbon-arc apparatus testing industrial water-reducible coatings, guide, D 4712 (06.01) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (06.02) Enamel coatings See Coatings--enamel English china clay See Aluminum silicate Epoxide equivalent weight (EEW) epoxy content of epoxy resins, test, D 1652 (06.02) Epoxy content epoxy resins, selecting test procedures, practice, D 4142 (06.02) Ethylbenzene aromatics (ethylbenzene and eight-carbon (Q/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, D 5060 (06.03) purity ofhydrocarbons from freezing points, test, D1016 (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) Epoxy (EP) plastics--coatings subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Epoxy resins selecting test procedures, practice, D 4142 (06.02) Equilibrium method flash point of liquids, test, D 3941 (06.03) Erosion erosion testing of antifouling paints, using high velocity water, test, 04938 (06X11) exterior paints, method for evaluating, A D 662 (06.01) practical wasbability of organic coatings, test, D 4828 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D4213 (06.01) Ester content alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) Esters n-butyl acetate (all grades), spec., D 4615 (06.03) ester value of solvents and thinner*, test, D1617 (06.03) ethyl 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) n-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) I Ester value ester value of solvents and thinners, test, D 1617 (06.03) Etching acid etching concrete, practice, D 4260 (06.01) Etherification sodium glycolate content of sodium carboxymethylcellulose, test, 01439 (06.02) Ethoxy ethanol 2-ethoxyethanol, spec., D 331 (06.03) Ethoxyethyl acetate 2-ethoxyethyl acetate (99 % grade), spec., D 3728 (06J)3) alcohol content/purity of acetate esters, by gas chromatography, test, D3545 (06.03) Ethoxyl content ethylcellulose, test, D914 (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., D4614 (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, 0 1615 (06.02) Ethylene glycol monobutyl ether See Bntoxyethanol Ethylene glycol monoethyl ether See Ethoxy ethanol Ethylene glycol monomethyl ether See Methoxy ethanol 2-Ethylhexanol 2-ethylhexanol (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., 0 3541 (06.03) Ethyl iodide ethoxyl substitution in cellulose ether products, by gas chromatography, test, D4794 (06.02) Ethyl methyl pentanol content ethyl methyl pentanol content/purity value of2-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, D3539 (06.01)' Exempted solvents ~ Sa Solvents (headings) dichloromethane/l,l,I-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (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 D4257 (06.01) Exposure tests freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) water resistance of coatings, using controlled condensation, practice, D4585 (06.01) Exposure tests--carbon-arc apparatus accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc iight/water exposure apparatus, practice, D822 (06.01) carbon-arc light- and water-exposure apparatus, unfiltered, by Dew cycle, practice for operating, D 3361 (06.01) 879 DUP050296438 Index of ASTM Standards, Section 6 Exposure tests--carbon-arc apparatus conducting tests on paint/vamish/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 nonmetallic materials, practice, G 23 (06.01) Exposure tests--corrosive environments evaluating filiform corrosion resistance of organic coatings on metal, test, D 2803 (06.01) evaluation of painted/coated specimens subjected to Corrosive environments, method, D1654 (06.01) Exposure tests--exterior accelerated outdoor exposure tests 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, G 11 (06.01) quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) Exposure tests--fluorescent-UV apparatus exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) operating iight-/water-exposure apparatus (flubrescent-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) Exposure tests--light accelerated testing Of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, 0 822 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) lightfastness of pigments (in artists' paints), test, D 4303.(061)1) lightfastness of printed matter, D 3424 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) operating ligbt-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) Exposure tests--organic coatings detergent resistance, practice, D 2248 (06.01) effect of chemical agents on organic finishes (user) in transportation industry), practice, D 1540.(06.01) effects of overbaking on organic coatings, practice, 02454(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, AD 1150(064)1) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (06.01) testing finishes on primed metallic substrates for humidity- thermal 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., D358 (06.01) Exposure tests--ultraviolet-cured coatings cure time, practice for reporting, D3732 (06.01) estimating package stability of coatings for ultraviolet curing test, D 4144 (06.01) Exposure tests--water erosion testing of antifouling paints, using high velocity water test, D 4938(061)1) subjecting marine antifouling coating to bifouling and Quid 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 nonmetallic materials, practice, G 26 (06.01) Extender pigments Sa Aluminum silicate/Barium sulfate/Calcium carbonafe/Calcium sulfate Magnesium silicate Pigments (general properties) Silica (diatomaceous) particle size distribution, by hydrometer of common white extender pigments, test, 0 3360 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, 0126 (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 0 661 (06.01) degree of erosion, evaluation, A D 662 (06.01) degree of flaking, evaluation/ A D 772 (06D1) house and trim coatings, solvent-based, practices for selecting/using test procedures, practice, D 2932 (06.01) latex house paints, selecting/using test procedurejs-practice, 03129(06.01) quantifying dirt collection on coated exterior panels, test, D3719 (06.01) " reporting paint film failures characteristic of exterior 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, testrD 1065 (06.03) Extractives content.. dichloromethane-soluble matter content of cellulose, test, D 3971 (06.02) ` F Fabrication design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D4618 (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, D 4121 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D4541 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D 1848 (06.01) 1 I < 1 i 3 j j 1 I j { 1 -j j j ? i j ! j j j DUP050296439 Index of ASTM Standards, Section 6 Fiber-optic light Falling rod viscometer viscosity ofprinting inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) Falling sand abrasion test abrasion resistance of organic coatings, by falling abrasive, test, 0968(06.01) Falling stones impact resistance of pipeline coatings, by limestone drop test, G 13 (06.01) Falling weight test impact resistance of pipeline coatings, by falling weight test, G 14 (06.01) Fan coat testing industrial water-reducible coatings, guide, D 4712 (06.01) Fatty adds--general fatty acid composition, by gas-liquid chromatography of methyl esters, test, D1983 (06.03) fatty adds used in protective coatings--terminology and selecting test methods, guide, D1467 (06.03) identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) sampling liquid oils/fatty adds (commonly used in paints/ vamishes/related materials), test, D1466 (06.03) Fatty acids--specifications coconut oil, spec., D1841 (06.03) com oil, spec., D1842 (06.03) cottonseed oil, spec., B1843 (06.03) dehydrated castor oil, spec., B1539 (06.03) linseed oil, spec., D1538 (06.03) soybean oil, spec., D1537 (06.03) tall oil, spec., D1984 (06.03) Fatty acids--tests acid value of fatty adds/polymerized fatty acids, test, D1980 (06.03) ash content, test, D1951 (06.03) clarity/deanness of (nonpigmected) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) color after heating, test, D1981 (06.03) color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) fatty acids used in protective coatings--terminology and selecting test methods, guide, D1467 (06.03) fish oil content, by gas-liquid chromatography, test, D 3725 (06.03) hydroxyl value of fatty oils/adds, test, D1957 (06.03) iodine value, test, D1959 (06.03) polymerized fatty acids, selecting test methods, D 2575 (06.03) rosin add content, test, D1240 (06.03) saponification value of drying oils/fatty adds/polymerized fatty adds, test, B1962 (06.03) solidification (titer) point of fatty adds, test, D 1982 (06.03) spedfic gravity at 25/25*C, test, D1963 (06.03) unsaponifiable matter in drying oils/fatty adds/polymerized fatty acids, test, D1965 (06.03) Fatty acids content alkyd resins and alkyd resin solutions, test, D1398 (06.02) fatty acid composition, by gas-liquid chromatography of methyl esters, test, D1983 (06.03) oleic add content of tall oil rosin, test, B1585 (06.03) . preparation of methyl esters from fatty acids, for fatty add composition analysis, test, D 3457 (06.03) tail oil, methods oftesting, D803 (06.03) Fatty amidoamlnes fatty nitrogen compounds, selection of test methods, D 2071 (06.03) iodine value, by Wijs procedure, test, B 2075 (06.03) total/primary/secondary/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 amines 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) 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, B 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, B 2082 (06.03) total/primary/secondapf/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, D 480 (06.03) Fatty nitrogen compounds identification ofoils 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, B 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, B 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 gnd Testing"), ' (Related Material) (06.01, 06.02, 06.03) Feedstock xylenes for p-xylene feedstock, spec., D 5211 (06.03) Ferric chloride methylol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) Ferric oxide Sa Iron oxide pigments ferric oxide in barium sulfate pigment, test, D 715 (06.02) Ferrite pigments See Iron oxide black Ferrous iron content iron oxide black (natural)- chemical analysis, test, 03872(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 881 DUP050296440 Fibrous magnesium silicate Index of ASTM Standards, Section 6 Fibrous magnesium silicate See Magnesium silicate Field testing--paints/related coatings/materials assessing die condition of aged coatings on steel surfaces, guide, D5065 (06.01) conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) conducting a patch test to assess coating compatibility, practice, D 5064 (06.01) field identification of coatings, test, D 5043 (06.01) profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) Filiform corrosion resistance Sa Corrosion (headings) organic coatings on metal, test, D 2803 (06.01) Film exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) film hardness (of factory-applied organic coatings on metal substrates), by pencil test, D 3363 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) preparing drawdowns of artists' paste paints, practice, 0 4941 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (064)1) 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 nonconduciive coatings (applied.to nonferrous metal base), nondestructive measurement, test, 01400 (06.01) dty-film thickness of organic coatings, using micrometers, test, D1005 (06.01) dry film thickness of protective coating systems, by destructive means, test, D4138 (06.01) erosion testing of antifouling paints, using high velocity water, test, >4938 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) nonmagnetic coatings (paint/varnish/lacquer), applied to a ferrous base, > 1186 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, 04939 (06.01) Film--electrical conductors soluble cellulose nitrate, testing, methods, D301 (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 ofpigment-vehicle systems, test, D1210 (06.01) printing inks, by NP1RI method, test, D1316 (06.01) Finger-rub test field identification of coatings, test, 0 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, 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 (06411) sustained burning (of liquid mixtures), by' Seta-flash tester (open cup), test, 0 4206 (064>1, 06.03) sustained burning (oflow viscosity liquid mixtures), by Wick test, 04207 (06.03) Fire testing--petroleum products flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) First aid handling/sampling phenol and cresylic acid, pfactice, 03852(06.03) sampling and handling aniline, practice, 0 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 oorrosion 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, 04541 (06.01) Flake brass See Copper powder/Gold bronze powder Flaked powders sampling/testing flaked aluminum powders/pastes, "methods, 0480(06.03) . Flake White ----- See Basic carbonate white lead Flaking ' exterior paints, A 0 772 (06.01) Flame cleaning standard pictorial surface preparation standards for painting steel surfaces, A 0 2200 (06.01) Flame photometric detectors (FP0) thiophene content of refined benzene, by gas Chromatography (with flame photometric detection), test, D 4735 (06413) Flame spread small-scale evaluation of fire-retardant paints, by 2-foot tunnel'-, method, test, D 3806 (06.01) - Flammability--paints/related coatings/materiais fire retardancy of paints, by cabinet method, test, A 01360 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, 01310(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) 882 iWfWiiigi DUP050296441 Index of ASTM Standards, Section. 6 Fungal influence--paints/related coatings/materials sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) lammability--petroleum products flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Flash/no flash method compliance by liquids of closed-cup flash point specifications, D 3934 (06.03) lash point--liquids equilibrium method, test, D 3941 (06.03) flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) flash/no flash equilibrium method, D 3934 (06.03) flash point by Tag closed tester, test, D 56 (06.03) flash point (of fuel oils/lube oils/suspension ofsolids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) 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) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) tall oil, methods of testing, D 803 (06.03) Flat interior latex paint See Latex paints Flexibility mandrel bend test of attached organic coatings, test, D 522 (06.01) organic coatings (paints) on prepainted deformed metallic sheets, test, D4145 (06.01) Floor paints/coatings clear floor sealers, performance tests, D 1546 (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/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) shellac (dry/powdered) used for electrical insulation, selecting test methods, D411 (06.02) testing industrial water-reducible coatings, guide, D4712 (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, by ISO flow cups, test, 05125(06.03) viscosity of paints/varnishes/lacquers, by Ford viscosity cup, test, D 1200 (06.01) Flue gas desulfurization system design/fabrication (for protective lining application), spec., D4618 (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, D 1966 (06.03) foots in raw linseed oil, by volumetric method, test, D1954 (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, D3281 (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 (inhibited/unhibited), 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, D 5201 (06.01) Fractionated and distilled fatty adds See Fatty adds--specifications Free formaldehyde See Formaldehyde Free monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) Free phenols See Phenol Free silica content See Silica content Free toluene diisocyanate content __ urethane prepolymers/coating solutions, by gas chromatography, test, 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 (06.01) Freezing point freezing points of high-purity hydrocarbons, test,JD 1015 (06.03) purity of hydrocarbons from freezing points, test; D1016 (06.03) purity of styrene, by freezing point method, test, D 3799 (06.03) French blue See Iron blue French chalk See Magnesium silicate French ocher See Ocher Fresnel reflector rack exposure method accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, 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, A D3274 (06.01) 883 ^5- DUP050296442 Index of ASTM Standards, Section 6 Fungal influence--paints/related coatings/materials presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (06.01) Fungicidal pigments See Calcium borosilicate/Zinc oxide Furnace black See Carbon black (headings) Furnaces chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (064)1) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) Furniture finishes temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test D1211 (06.01) GA-CAT comprehensive abrasion test abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 0 5181 (06.01) Gages wet film thickness of organic coatings, by notched gages, practice, 04414 (06.01) Galvanized surfaces See Steel panels/Steel pipe/tube/Steel sheet Gamma radiation effects of radiation on coatings (for light-water nuclear power plants), test, D 4082 (06.01) Gardner-Coleman method oil absorption of pigments, test, 01483 (06.02) Gardner color scale color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) Gardner-Holdt viscometers See Viscometers--Gardner-Holdt Garnet lac orange.shellac and (button lac/garnet lac), spec., D 237 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) Gas black pigment See Pigments--carbon black Gas checking draft test varnish films, test, D1643 (06.01) Gas chromatography See Chromatography--gas (headings) Gelled vehicle laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) Gel time drying oils, test, D1955 (06.03) tar acids, test, D 2870 (06.03) Generic resin field identification of coatings, test, D5043 (06.01) Glacial acetic acid 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) Glacial acrylic add See Acrylic acid Glacial methacrylic acid See Methacrylic add (glacial) Glass panel reading surface wet film thickness of organic coatings, 01212 (06.01) Glass panels directional reflectance factor (45-deg G-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) surface preparation (for testing paints, varnish, lacquer & related coatings), 03891 (06.01) Glass spheres (in traffic paint/marking material) chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, 0 4797 (06.01) sieve analysis of glass spheres (for retroreflective pavements markings/industrial uses), test, 01214 (06.02) test for roundness of, 01155 (06.02) Glazing compounds--metal sash slump of face glazing/bedding compounds on metal sash, test, 0 2376 (06.01) viscosity of printing inks/vehicles, by felling-rod viscometer, test, 04040 (06.01) Gloss dear/pigmented organic coatings, test, 01308 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, 0 4449 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metry, method, E 430 (06.01) gloss/sheen uniformity evaluation, test, 0 3928 (06.01) practical washability of organic coatings, test, 0 4828 (06.01) reflection haze of high gloss surfaces, test, 0 4039 (06.01) specular gloss of nonmetallic specimens, test, 0 523 (06411) Gloss paints interior latex semigloss/gloss paints, selecting test methods, guide, 0 4540 (06.01) Glne gas desulfurization (FGD) inspection of linings in operating flue gas desulfurization systems, practice, 0 4619 (06.01) Glycerin--high-gravity high-gravity glycerin, spec.; 01257 (06.03) sampling/testing high-gravity glycerin, test, D'1258 (06.03) Glycerol and ethylene glycol content glycerol/ethylene glycol/pentaerythritol in aUcyd resins, test, 01615(06.02) Glyddyl ethers total chlorine content in epoxy resins/compounds, test, 04301(06.02) ---- Glycol ethers purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, 0 4773 (06.03) . 1 Glycols See Engine coolants Gold bronze powder chemical- analysis ofcuprous oxide/copper pigments, test, 0283(06.02) gold bronze powder, spec., 0 267 (06.02) Government specification fire retardancy of paints, by cabinet method, test, A 01360 (064)1) Grading sampling/grading rosin (delivered in commercial bags/ barreis/drums), test, 0 509 (06.03) Graphics abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 0 5181 (06.01) Graphitic mica See Stone--mica Gravimetric method resin solution dilutability, test, 0 5062 (064)3) water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 04942 (06.01) white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, 0 4797 (06.01) 884 DUP050296443 Index of ASTM Standards, Section 6 i Green pigments Sa Chrome green/Chromium oxide green { Phthalocyanine green 1 yeUow/orange/green pigments containing lead chromate/ i chromium oxide green, analysis, test, D126 (06.02) : Grind (pigments) See Fineness of grind (dispersion) Grit filter-retained solids content of polymer latexes, test, D 5097 (06.02) Grit content grit content of mica pigment, test, D 716 (06.02) Ground dolomite/iimestone/oyster shell I See Calcium carbonate Guides for testing paints/related coatings/materials alkyd resins, practice, D 2689 (06.02) < amino resins, selecting test procedures, practice, D 4277 (06.02) ' analysis of electrocoat bath samples, guide, D 1978 (06.01) ( architectural paints/coatings (solvent-/water-thinned), 02833(06.01) chemical analysis of white pigments, selection of test methods, guide, X> 34 (06.02) clear/pigmented lacquers, D 333 (06.01) j coil coatings, testing, practice, D 3794 (06.01) | drying oils, selecting test methods, guide, D 555 (06.03) J epoxy resins, selecting test procedures, practice, D 4142 (06.02) \ evaluation of (clear/pigmented) coatings for rigid/semirigid I plastic substrates, practice, D 3002 (06.01) : exterior latex house paints, practice, D 3129 (06.01) exterior solvent-based house/trim coatings, practice, D 2932 (06.01) fatty acids used in protective coatings--terminology and selecting test methods, guide, D1467 (06.03) fatty nitrogen products, D 2071 (06.03) floor paints (solvent-thinned), practice. D 3383 (06.01) floor paints (water-thinned), practice, D 3358 (06.01) interior flat wail paints (latex), practice, D 2931 (06.01) interior flat wail 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, D3425 (06.01) latex vehicles, selecting test procedures, practice, D4143 (06,02) nonvolatile matter content (of paint/raw paint materials), practice, D 2832 (06411) polymeric powders/powder coatings, practice, D 3451 (06.01) polymerized fatty acids, selecting test methods, D 2575 (06.03) poly(vinyl chloride) resins, guide, D 4368 (06.02) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) sampling/testing volatile soivents/chemical intermediates (for paints/lacquer/varnish/related jnaterial), selecting test methods, D 268 (06.03) testing industrial water-reducible coatings, guide, D4712 (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 spectroscopy/gas chromatography, practice, D 2743 (06.01) varnish, D154 (06.01) volatile/nonvolatile content (of ceUulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (064)2) f volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, j 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, D3960 (06.01) Heating tests--paints/reiated coatings/materials Gum content artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) Gum rosin See Rosin Gum spirits of turpentine See Turpentine H Halo-silane coated glass plates preparation of free films of organic coatings, practice, D 4708 (06.01) Halphen-Hicks test qualitative detection of rosin in varnishes, by Lieberman- Storch/Haiphen-Hicks tests, D1542 (06.01,06.02) Handling materials See Material handling Hardness (indentation) indentation hardness of organic coatings, by Knoop and Pfond 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 Knoop and Pfund methods, test, D1474 (06.01) Hazardous constituents analytical procedures for determining hazardous constituents in protective coatings, selecting test methods, guide, D 3630 (06.01) Hazard potential--health analytical procedures for determining hazardous constituents in protective coatings, selecting test methods, guide, D3630 (06.01) design/use of safety alert system for hazardous work-locations in coating/lining industry, practice, A D4257 (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 diphenol (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/nonmetailic 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 D 817 (06.02) chemical/gravimetric analysis of white/yeilow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) distillation of industrial aromatic hydrocarbons/reiaied 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, D1960 (06.03) 885 DUP050296444 Index of ASTM Standards, Section 6 Heating tests--paints/related coatings/materials stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D4206 (06.01,06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D 1211 (06.01) water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) Heatset-type printing inks nonvolatile content of printing inks/resin solutions/vehicles, test, D4713 (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, D1347 (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, 01310(06.03) heptane miscibility of lacquer solvents, test, 01476.(06.03) purity of hydrocarbons from freezing points, test, 01016(06.03) Heptane miscibility Sa Miscibility heptane miscibility of lacquer solvents, test, D1476 (06.03) Herring content fish oil content (ofdrying oils and their fatty acids), by gas-liquid cbrpmatography, 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, 05150(06.01) Hiding power--paints/coatings comparison of the brush (bag of latex paints, test, 04958(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, D 4958 (06.01) High-speed centrifugal vehicle separations See Vehicle separation High velocity water erosion testing of antifouling paints, using high velocity water test, 0 4938 (06.01) High voltage continuity testing continuity verification of liquid/sheet linings applied to concrete 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 substrates, practice, 04787 (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, G13 (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, O 2246 (06.01) Humidity--relative testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) Hunter appearance gloss differences 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, 02306 (06.03) Hydrocarbons acidity in volatile solvents/chemical intermediates (used in paint/vamish/lacquer/related products); test, - D1613 (06,03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, D4534 (06.03) dichloromethane/1,1,1-trichloroethane content in'paints/ coatings, by direct injection gas chromatography, test, D 4457(061)1) 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, D4747 (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, D 1492 (06.03) color (ofsolid aromatic hydrocarbons/related materials in molten state), by platinum-cobait scale, test, D1686 (06.03) solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, D4493 (06.03) 886 DUP050296445 Index of ASTM Standards, Section 6 Industrial aromatic hydrocarbons total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zytenes, by gas chromatography, test, D 2360 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic, hydrocarbons, test, D 5194 (06.03) Hydrocarbons--high-purity commercial density (of pure liquid chemicals), test, D 3505 (06.03) freezing points of high-purity hydrocarbons, test, D 1015 (06.03) purify of hydrocarbons from freezing points, test, D1016 (06,03) solidification point of industrial organic chemicals, test, D1493 (06.03) Hydrocarbons--industrial aromatic acidity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D847 (06.03) acid wash color, test, D 848 (06.03) apparent density ofindustrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) copper corrosion of industrial aromatic hydrocarbons, test, D 849 (06.03) distillation, test, D850 (06.03) hydrogen sulfide and sulfur dioxide content (qualitative), test, D 853 (06.03) solidification point of industrial organic chemicals, test, D1493 (06.03) sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcouiometry, test, D3961 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Hydrocarbons--fight volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Hydrodynamic stress subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Hydrogen sulfide content industrial aromatic hydrocarbons, test, D 853 (06.03) Hydrolyzable chlorine content hydrolyzable chlorine content of liquid epoxy resins, test, D1726 (06.02) Hydroqninone content hydroquinone in vinyl acetate, test, D 2193 (06.03) Hydroxyacetone content analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) Hydroxyethylcellulose hydroxyethylcellulose, test, D 2364 (06,02) Hydroxy] (hydroxide ion) content .* hydroxyl content of cellulose acetate, by spectrophotometry, test, D 871 (06.02) hydroxyl content of pyridine-soluble cellulose esters, by spectrophotometry, test, A D817 (06.02) hydroxyl value of fatty oils/acids, test, D1957 (06.03) pentaerythritoi (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) Hydroxypropoxyl content hydrogen sulfide/suffiir dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) Hydroxypropyl methylcellulose hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) Hydroxypropyl substitution methoxyl/hydroxypropyl substitution in cellulose ether products, by Zeisel-gas chromatography, test, 03876(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) I 1CI cone/plate viscometer high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Identification field identification of coatings, test, D 5043 (06.01) Ignition--loss on ignition moisture content of pigments, D1208 (06.02) Ignition residues of drying oils See Ash content Immersion chemical resistance of pipeline coatings, test, G 20 (06.01) comparative corrosion preventive characteristics ofmaterials used for joints/couplings/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, 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) Impressed current system cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) Imprinting print resistance of architectural paints, test, I> 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-xylene, by gas chromatography, method, D 3798 (06.03) chemical analysis of benzene, by gas chromatography, test,' ' D4492.(QfL03) 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, D4773 (064)3) pyridine base content in cresylic acid, by direct titration, test, 04471 (06.03) styrene, by gas chromatography, test, D 3962 (06.03) Inclined plane method static friction of coating surfaces, test, D 4518 (06.01) Inclusions continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) Index of refraction (refractive index) See 'Refractive index Indian ocher See Ocher Indian red See Iron oxide red Industrial aromatic hydrocarbons See Hydrocarbons--industrial aromatic 887 DUP050296446 Index of ASTM Standards, Section 6 Industrial grade benzene/toluene/xylene Industrial grade benzene/toluene/xylene See Benzene/Tolueqe/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 ofpolymers in emulsion paints, by ' infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) Infrared (IR) analysts--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 ctuing cycle, by infrared radiation thermometers, practice, D 3259 (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-te/r-butylcatechol (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) Ink apparent tack of printing inks/vehicles, by inkometer, test, D 4361 (06.01) clarity/cleanness 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 ofprinting inks/vehicles, by inkometer, test, D 4361 (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, D49 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet 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, D5163 (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, D 3276 (06.01) specifying inspection requirements for coating/fining work on metal substrates, guide, D 5161 (06.01) Inspection personnel establishing procedures to qualiiy/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 ofpaints/varnishes/Iacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (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 reflectomctry, test, E 97 (06.01) evaluation of color for thermoplastic traffic marking materials, test, D 4960 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E430 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) testing industrial water-reducible coatings, guide, D4712 (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 bendabilify 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, D4828 (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 fbr selection and use of test procedures, D 3425 (063)1) 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, D3980 (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, D4787 (06.01) 888 \ I W--i DUP050296447 Index of ASTM Standards, Section 6 Isopropylbenzene (cumene) Intrinsic viscosity Sa Viscosity (headings) intrinsic viscosity ofcellulose acetate, using modified Baker-Philippoff equation, test, D 871 (06.02) limiting viscosity number of cellulose acetate propionate/ butyrate, test, A D 817 (06.02) iodine-pyridme-sulfur dioxide reagent water in liquid naval stores, test, D 890 (06.03) Iodine reagent method water content, in phenol and related materials, test, D1631 (06.03) Iodine value acid/amine value offatty quaternary ammonium chlorides, test, D 2078 (06.03) fatty amines, amidoamines, and diamines, Wijs procedure, test, D 2075 (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) Iodine value--drying oils and their derivatives modified Rosenmund-Kuhnhenn method, test, D1541 (06.03) Wqs method, test, D1959 (06.03) Ionic contamination See Contamination (headings) Iron raw/bumt sienna pigments, spec., D 765 (06.02) Iron blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D 1135 (06.02) chemical analysis of phthalocyanine blue/green pigments, test, D3256 (06.02) iron blue pigment, spec., D 261 (06.02) Iron content--paint driers formaldehyde, test, D 2087 (06.03) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) iron in liquid iron paint driers, by EDTA method, test, D3804 (06.03) iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D4085 (06.02) methylcellulose, test, D1347 (06.02) rosin, test, D1064 (06.03) Iron oxide black black synthetic iron oxide pigment, spec., D 769 (06.02) iron oxide black (natural)- chemical analysis, test, 0 3872(06.02) Iron oxide brown (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) Iron oxide brown (synthetic) iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) synthetic brown iron oxide pigment, spec., D 3724 (06.02) Iron oxide content calcium borosilicate, test, D 4487 (06.02) Iron oxide red (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) Iron oxide red (synthetic) analysis, D 50 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) Iron oxide yellow analysis, D 50 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) Iron paint driers See Driers Irradiance/irradiation--paints/related coatings/materials effects of radiation on coatings (for light-water nuclear power plants), test, D 4082 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Isatin thiophene content of benzene, by spectrophotometry, test, D1685 (06.03) Isobutanol See Isobutyl alcohol Isobutene (isobutylene) purity of hydrocarbons from freezing points, test, D1016 (06.03) Isobutyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, D3545 (06.03) isobutyl acetate (95 % grade), spec., D1718 (06.03) Isobutyl alcohol isobutyl alcohol, spec., D1719 (06.03) isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02) ISO cups viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) Isocyanates isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02) ISO (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 ofhydrocarbons,from freezing points, test, D1016 (06.03) Isophorone isophorone, spec., D 2916 (06.03) Isophthalic acid content isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) Isoprene purity of hydrocarbons from freezing points, test, 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., D3131 (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) isopropylbenzene (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) 889 DUP050296448 Index of ASTM Standards, Section 6 4,4' Isopropylidene diphenol 4,4' Isopropylidene diphenol sampling/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 Jaune de zinc See Zinc yellow Joints comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) Jones reductor total titanium in white titanium pigments, by Jones reductor, test, D1394 (06.02) K Kaolinite See Aluminum silicate pigments Karl Fischer reagent method--water content paints/paint materials, test, D4017 (06.01) water in volatile solvents, by Fischer reagent titration method, test, D 1364 (06.03) Kauri-butanol value hydrocarbon solvents, D1133 (06.03) Ketones aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) 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) methyl isoamyl ketone, spec., D 2917 (06.03) methyl isobutyl ketone, spec., D1153 (06.03) meihyl -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, D 3893 (06.03) purity of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) 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, D3359 (06.01) Knoop hardness indentation hardness of organic coatings, by Knoop and Pfund methods, test, D1474 (06.01) Konig pendulum test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D4366 (06.01) Krems white See Basic carbonate white lead Kubelka-Munk equation relative tinting strength of printing ink dispersions, test, D 2066 (06.01) Labeling abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) art materials for chronic health hazards, practice, D 4236 (06.01) Laboratory evaluating and comparing transfer conditions-laboratory 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/varnish/lacquer/related products), test, D1613 (06.03) adhesion (to smooth surfaces), by scrape adhesion test, D 2197 (06.01) amount ofliquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) cellulose nitrate in alkyd lacquers, quantitative determination by infrared spectrophotometry, test, D3133 (06.01) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) clear and pigmented, selection of test methods, D 333 (06.01) clear/pigmented organic coatings, test, D1308 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D5031 (06.01) discoloration (light stability), test, D 2620 (06.01) dry film thickness of nonconductive coatings (applied to nonferrous metal base), nondestructive measurement, test, D1400 (06.01) dry film thickness (of nonmagnetic organic coatings applied to a Ferrous base), D1186 (06.01) " dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01) effects of overbaking on organic coatings, practice, 02454(06.01) elongation/tensile strength/stiffness, test, D 2370 (06.01) ester value of solvents and tbinners, test, D1617 (06.03) 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 point ofliquids, by Setaflash closed-cup apparatus, test, 0 3278(06.03) freeze-thaw stability of multicolor lacquers, test, I> 2337 (06.01) glacial acrylic acid (99.0 % grade), spec,, D 4416 (06.03) heptane miscibility of lacquer solvents, test, D 1476 (06.03) imprint resistance, of dried films, test, D 2091 (06.01) indentation hardness of organic coatings, by Knoop and Pfund methods, test, D1474 (06.01) methyl n-amyl ketone (98 % grade), spec., D 4360 (06.03) moisture vapor transmission of organic coating films, test, D1653 (06.01) paint/varnish/lacquer/related products, terminology, D16 (06.01, 06.02, 06.03) paint/varnish/lacquer/related products, test, A D1475 (06.01) 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) 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 test, D 870 (06.01) 890 DUP050296449 Index of ASTM Standards, Section 6 Lead chromate stain removal (of multicolored lacquer on primed steel panels), test, D 2198 (06.01) standard environments for conditioning/testing paint/ varnish/lacquer/reiated materials, spec., D 3924 (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, D4212 (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) wood furniture lacquers, test, D 2571 (06.01) Lac resins See Resins--lac Lampblack lampblack pigment, spec., D 209 (06.02) solvent extractable material in black pigments, test, 0305(06.02) Lampblack content solvent extractable material in black pigments, test, 0305(06.02) Lapis lazuli See Ultramarine blue Latex 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., 0 5098 (06.01) blocking resistance of trade sales paints, test, 04946 (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, 0 185 (06.01, 06.02) color differences of opaque materials, instrumental evaluation, test, 0 2244(06.01) comparison ofthe brush drag of latex paints, test, 04958(06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, 05031 (06.01) consistency of paints, using Stormer viscometer, test, 0562(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, 01640 (06.01) efflorescence (of interior wall paints), test, 0 1736 (06.01) field identification of coatings, test, 0 5043 (06.01) filter-retained solids content of polymer latexes, test, 05097 (06.02) fineness of dispersion of pigment-vehicle systems, test, 01210(06.01) freeze-thaw resistance of water-borne coatings, test, 02243(06.01) gloss/sheen uniformity evaluation, test, 0 3928 (06.01) ! hiding power of architectural paints applied by roller, test, | 0 5150(06.01) hiding power of paints, by reflectometry, test, A 0 2805 (06.01) hiding power (relative dry), visual evaluation of brushouts, test, 0 344 (06.01) : high shear viscosity (of paints/vamishes/related products), by ' ICI cone/plate viscometer, test, 0 4287 (06.01) i lead/cadmium/cobalt content (low concentrations) in : nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, 0 3335 (06.01) leveling, by draw-down method, test, 0 4062 (06.01) low temperature coalescence, test, 0 3793 (06.01) mandrel bend test of attached organic coatings, test, 0522(06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, 03624 (06.01) nonvolatile content of latexes, test, 04758 (06.02) package stability of solvent-reducible/water-reducible paint, test, 01849(06.01) paint spatter resistance to roller application, test, 0 4707 (06.01) paint/vamish/lacquer/related products, test, A 01475 (06.01) preparing drawdowns of artists' paste paints, practice, 04941(06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, 0 823 (06D1) qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, 0 3168 (06.01) relative tinting strength of chromatic paints, test, 0 4838 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, 01848 (06.01) sag resistance, using multinotch applicator, test, 04400 (06.01) sampling liquid paints/related pigmented coatings, practice, 0 3925(06.01) scrub-to-failure of interior latex flat wall paints, test, 02486(06.01) specular gloss of nonmetailic specimens, test, 0 523 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, 0 2247 (06.01) unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06.02) volatile content, test, 0 2369 (06.01) volatile organic content (VOC) of paints/related coatings, selecting test procedures, practice, 03960 (06.01) volume nonvolatile matter in clear/pigmented coatings, test, 02697(06.01) washability of interior architectural coatings, test, 03450(06.01) water content of paints/paint materials, by Karl Fischer method, test, D4017 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, 0 3792 (06.01) water-thinned floor paints, selection and use of test procedures, practice, 03358 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, 0 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., 0358(06.01) - Latex paints--selection and use of test procedures exterior latex house paint, practice, 0 3129 (06.01) floor paint, practice, 03358 (06.01) interior fiat wall paint, practice, 02931 (06.01) interior latex semigloss/gloss paints, selecting test methods, guide, 04540 (06.01) latex vehicles, selecting test procedures, practice, D4i43 (06.02) Latex vehicles nonvolatile content of latexes, test, 0 4758 (06.02) unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06.02) Leachates/leaching water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, 0 2448 (06.02) Lead chromate chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, 0 4797 (06.01) 891 DUP050296450 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, D 126 (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, 0 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 oflead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) lead content in paint, by direct aspiration atomic absorption spectroscopy, test, 04834 (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 linsedd oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) yellow/orange/green pigments containing lead chromate/ chromium oxide green, test, D126 (06.02) Leaded zinc oxide analysis of white zinc pigments, test, D 3280 (06.02) Lead peroxide content lead peroxide/true red lead content of dry red lead pigments, test, D49 (06.02) Lead salt infrared radiation thermometers temperature ofapplied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) Lead screening test lead content in paint, by direct aspiration atomic absorption spectroscopy, test, D4834 (06.01) Lead siticochromate 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, D 480 (06.03) Leveling characteristics architectural paints/coatings (aqueous/nonaqueous), in white/light tints, by draw-down method, test, D4062 (06.01) Lieberman-Storch test qualitative detection of rosin in varnishes, by LiebermanStorch/Halphen-Hicks tests, D 1542 (06.01, 06.02) Light--exposure accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc ligbt/water exposure apparatus, practice, 0 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, 04587 (06.01) lightfastness of pigments (in artists' paints), test, D 4303 (06.01) lightfasmess 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 2$ (06.01) operating light-/water-exposure apparatus (fluorescem-UV condensation type) for exposure of nonmetallic materials, practice, G53 (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, 02620(06.01) Light--transmission and reflection color changes (ofopaque materials), by instrumental evaluation, test, D 2244 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) light stability of clear coatings, by sunlight-through-glass method, test, D2620 (06.01) Lightening power See Tinting strength Lightfastness artists' acrylic emulsion paints, spec., D 5098 (06.01) Limestone drop test impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Limiting viscosity number limiting viscosity number of cellulose acetate propionate/ butyrate, test, A D 817 (06.02) Limonite See Ocher Linear programmed temperature gas chromatography See Chromatography--gas {headings)' Lining industry continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) _ design/fabrication of flue gas desulfiirization system components (for protective lining application), spec., D 4618 (06.01) design/use of safety alert system for hazardous work locations in coating/lining industiy, practice, A D 4257 (06.01) inspection of linings in operating flue' gas-desulfurization - systemsr^ractice, D 4619 (06.01) Linings continuity verification ofiiquid/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., D 1538 (06.03) raw, foots, by gravimetric method, test, D1966 (06.03) raw, foots, by volumetric method, test, 0 1954 (06.03) raw linseed oil, spec., D 234 (06.03) white linseed oil paints- chemical analysis, selecting test methods, practice, 0 215 (06.01) 892 DUP050296451 Index of ASTM Standards, Section 6 Marine (shipboard) coatings Lipids alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) Liquid chemicals See Chemicals Liquid coating properties testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (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--epoxy epoxy content of epoxy resins, test, D1652 (06.02) Liquids amount of liquid separated as upper layer from a viscous soliition/dispersion containing dispersed solids, test, D 4948 (06.01) chemical resistance of pipeline coatings, test, G 20 (06.01) clarity/cleanness of (nonpigmented} paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) color of transparent liquids, by Gardner color scale, test, D 2544 (06.01, 06.02, 06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) ilash/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 ofsolids/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 (ofliquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01,06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) viscosity of transparent liquids, by bubble time method, test, D1545 (063)1,06.02,06.03) 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, D4541 (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 ofliquid coatings/dried films, by atomic absorption spectroscopy, test, 03717(06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D 3624 (06.01) Low hiding strontium chromate See Strontium chromate Low temperature bake coatings nonvolatile content of latexes, test, D 4758 (06.02) Low voltage 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 of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06311) Magnesium alloys surface preparation for painting, practice, D1732 (063)1) 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., D605 (063)2) Magnesium silicate pigment magnesium silicate pigment, analysis, test, D 717 (063)2) Magnetic flux film thickness ofpipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Magnetic testing film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (063)1) Maintenance--coatings assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) conducting a patch test to assess coating compatibility, practice, D 5064 (06.01) establishing procedures to monitor performance of safety related coatings In operating nuclear power plant, guide, D 5163 (06.01) Maleic acid content maleic add content of maleic anhydride, by potentiometric titration, test, D 2930 (06.03) Maleic anhydride color in molten state/after heating, by platinum cobalt scale, (includes 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/calciunt) content of cellulose 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, 05066(06.01) Marine (shipboard) coatings See Antifouling paint pigments (headings) 893 PW DUP050296452 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, D1734 (06.01) surface cleaning concrete unit masonry (for coating), practice, D4261 (06.01) Masonry water repellents nonvolatile content in silanes/sEoxaries/silane-siloxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) Material handling impact resistance ofpipeline coatings, by falling weight test, G14 (06.01) naphthalene, maleic/phthalic anhydride, practice, D 3438 (06.03) phenol and cresylic acid, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Matter insoluble In chloroform chloroform insoluble matter in oiticia oil, test, D1958 (06.03) Mechanical damage specific bendability of pipeline coatings, test, G 10 (06.01) Mechanical muller See Muller device MEHQ content See Methyl ether of hydroquinone (MEHQ) content MEK (methyl ethyl ketone) resistance See Methyl ethyl ketone (MEK) Menhaden-derived fish oil See Oils--drying 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, 03624 (06111) 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, 0 283(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 paste/Copper powder Sa Gold bronze powder/Zinc dust Metal primer Sa Primer zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) , Metals and metallic materials wet film thickness of organic coatings, D 1212 (06.01) Metals and metallic materials--coating applications accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) adhesion of coating films to metallic substrates, by tape test, 03359(06.01) coil coatings, testing, practice, D 3794 (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, E 430 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D4085 (06.02) painted surfaces- evaluating degree of blistering, AD 714 (06.01) specifying inspection requirements for coating/lining work on meted 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 (06113) solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) Metboxy ethanol 2-methoxyethanol, spec., D 3128 (06.03) Methoxyl content hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylceUulose, test, D1347 (06.02) Mcthoxyi/hydroxypropyl substitution cellulose ether products, by Zeisel-gas chromatography, testT D 3876 (06.02) Methyl acrylate methyl acrylate, spec., D4709 (06.03) ...... - Methyl amyl acetate -- methyl amyl acetate, spec., D 2634 (06.03) . - Methyl amyl alcohol See Methyl isobutyi 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; D 4961 (06.03) Methyl butyl ketone purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) MethylceUulose See Cellulose and cellulose derivatives Methylcydohexane purity of hydrocarbons from freezing points, test, D1016 (06.03) Methylene chloride dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) 894 DUP050296453 Index of ASTM Standards.' Section* 6 Moisture content--paints/related coatings/materials Methyl esters Microscopic examination--paints/related coatings fatty add composition, by gas-liquid chromatograpby of methyl dry film thickness of protective coating systems, by destructive esters, test, D1983 (06.03) means, test, D 4138 (06.01) preparation from oils, for fatty add composition determination reporting particle size characteristics of pigments, practice, by gas-liquid chromatography, D 2800 (06.03) D1366 (06.02) preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) Microwave procedures laboratory preparation of gelled vehicles, using microwave oven, Methyl ether of hydroquinone (MEHQ) content practice, D 5166 (06.02) methyl- ether of hydroquinone (MEHQ) content of colorless monomeric acrylate esters, test, D 3125 (06.03) Migration plasticizer migration from vinyl fabrics to lacquers, method, Methyl ethyl ketone (MEK) D 2199 (06.01) MEK resistance of ethyl silicate (inorganic) zinc-rich primers, MiDiequivalency by solvent rub, test, D 4752 (06.01) acid/base miiliequivalent content of (anodic/cathodic) methyl ethyl ketone, spec., D 740 (06.03) electrocoat baths/their ultrafiltrates, test, D4370 (06.01) purity of methyl ethyl ketone, using gas chromatography, test, Milori blue D 2804 (06.03) See Iron blue Methyl isoamyl ketone (MIAK) Minerals methyl isoamyl ketone, spec., D 2917 (06.03) field identification of coatings, test, D 5043 (063)1) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D3893 (06.03) Mineral spirits aromatics (ethylbenzene and eight-carbon (C8/heavier) content Methyl isobntyl carbinol methyl isobutyl carbinol, spec., D 2635 (06.03) in mineral spirits, by gas chromatography, test, D 3257 (06.03) Methyl isobutyl ketone (MIBK) methyl isobutyl ketone, spec., D1153 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, 03329(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, 04706 (06.02) Methylstyrene analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D 4961 (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) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06313) porosity ofpaint films (to indicate coating penetration), test, D 3258 (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, D1476'(06.03) water miscibility of water-soluble solvents, test, D1722 (063)3) Mixed aniline point sampling and testing dipentene, method, D 801 (06.03) Mixed xylene See Xylene (mixed) MMFT See Film 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 coatings ' discoloration susceptibility (in exterior exposure tests), practice, D 3456 (063)1) paint films, evaluating degree of surface disfigurement, Model 'C wet film thickness gage wet film thickness of organic coatings, D1212 (06.01) Modified Wolfe-potentiometric method -- See Wolfe-pgtentiometric method Moisture analysis--wood products edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) AD3274 (063)1) resistance of emulsion paints (in containers) to attack by Moisture content--paints/related coatings/materials calcium borosilicate, test, D 4487 (06.02) 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) capillary moisture in concrete, by plastic sheet method, test, 04263(06.01) cellulose acetate propionates/butyrate, test, A D817 (06.02) Microbiological examination presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) Microcoulometry See Coulometry--microcoulometry Microelectronic derice processing--water reagent water, spec., D 1193 (06.03) Micrometer cellulose acetate, test, D 871 (06.02) ethylcellulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylceliulose, test, 0 2364 (06.02) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (063)2) methylcellulose, test, 01347 (06.02) moisture content of (iron/copper phthalocyanine/ultramarine) disbonding characteristics of pipeline coatings, by direct soil blue pigments, by Brabender test, D1135 (06.02) burial, test, G19 (06.01) dry-film thickness of organic coatings, using micrometers, test, 01005(06.01) moisture in cellulose, test, D1348 (06.02) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) pine tars and pine tar oils, test, 0 856 (06.03) sampling and testing dipentene, method, 0 801 (06.03) 895 pm ----r DUP050296454 Index of ASTM Standards, Section 6 Mar resistance Mar resistance mar resistance erf 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, D1734 (06.01) surface cleaning concrete unit masonry (for coating), practice, D4261 (06.01) Masonry water repellents nonvolatile content in silanes/siloxahes/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, G 14 (06.01) naphthalene, maleic/phthalic anhydride, practice, D 3438 (06.03) phenol and cresylic acid, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Matter insoluble in chloroform chloroform insoluble matter in oiticia oil, test, 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 hydroqninone (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., D911 (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, D 4961 (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 paste/Copper powder Sa Gold bronze powder/Zlnc 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, D1212 (06.01) Metals and metallic materials--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) coil coatings, testing, practice, D 3794 (06.01) discontinuity (holiday) testing of noncondactive 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 (06X11) mandrel bend test of attached organic coatings, test, D 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 0714 (06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, 05161 (06.01) testing primers/primer surfaccrs over preformed metal, selection/use of procedures, practice, D3322 (06.01) Metaxylene See meta-Xylene Methacrylic add (glacial) glacial (98.5 %) methacrylic acid (for use in paint/vamish/ 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, 0 2380(06.03) methanol (methyl alcohol), spec., 01152 (06X)3) permanganate time of acetone/methanol, test, D1363 (06.03) solution color of 4,4'-isopropyIidenediphenol (dissolved in methanol), test, D 4789 (06.03) Methoxy ethanol 2-methoxyethanol, spec., D 3128 (06.03) Methoxy! content hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, 0 2363 (06X)2) methylcellulose, test, 01347 (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 amyf acetate, spec., 0 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, D 4961 (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, D1016 (06.03) Methylene chloride dichloromethane/l,l,l-trichioroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) 894 DUP050296455 Index of ASTM Standards, Section 6 Moisture content--paints/related coatings/materials * by tape testy1 esters tty acid composition, by gas-liquid chromatography of methyl esters, test, D1983 (06.03) Protective reparation from oils, for fatty acid composition determination >162 (06.0h by gas-liquid chromatography, 0 2800 (063)3) Jn prepainttyparation of methyl esters from fatty acids, for fatty acid , '1) composition analysis, test, 03457 (06.03) by goniopithyl ether of hydroquinone (MEHQ) content methyl ether of hydroquinone (MEHQ) content ofcolorless :st- monomeric acrylate esters, test, D 3125 (06.03) ofceltr.i th>1 etty* ket0M (MEK) hntr, 0!MEK resistance of ethyl silicate (inorganic) zinc-rich primers, -utometr 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, 8 work 0 D2804(06'03> Tlethyl isoamyl ketone (MIAK) tal, methyl isoamyl ketone, spec., D 2917 (06.03) 6.011 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) nish/ Methyl isobutyl ketone (M1BK) ' methyl isobutyl ketone, spec., D1153 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, 5 03329(06.03) Methyl methacrylate unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, 04827 (06.02) Methylol group content methylol group determination (qualitative) in phenolic resin's, test, 0 4706(06.02) Methylstyrene analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 0 4961 (06.03) Metric practice--SI (International System of Units) use of international system of units (SI) (modernized metric system), excerpts, (Related Material--all volumes) (06.01, 06.02, 06.03) Mica pigment grit content of mica pigment, test, 0 716 (06.02) wet ground mica pigments, spec., 0 607 (06.02) Microbiological attack--paints/related coatings discoloration susceptibility (in exterior exposure tests), practice, 0 3456(06.01) paint films, evaluating degree of surface disfigurement, A 03274 (06.01) resistance ofemulsion paints (in containers) to attack by microorganisms, test, 0 25?4 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, 0 3273 (06.01) Microbiological examination presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, 0 4610 (06.01) Microcouiometry See Coulometry--microcouiometry Microelectronic device processing--water reagent water, spec., 01193 (06.03) Micrometer disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) dry-film thickness of organic coatings, using micrometers, test, 0 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, 0 4138 (06.01) reporting particle size characteristics of pigments, practice, 0 1366 (06.02) Microwave procedures laboratory preparation of gelled vehicles, using microwave oven, practice, 0 5166 (06.02) Migration plasticizer migration from vinyl fabrics to lacquers, method, 02199(06.01) Milliequivalency acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D4370 (06.01) Milori blue See Iron blue Minerals field identification of coatings, test, 0 5043 (06.01) Mineral spirits aromatics (ethylbenzene and eight-carbon (Cg/heavier) content in mineral spirits, by gas chromatography, test, D 3257 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., 0 235 (06.03) porosity of paint films (to indicate coating penetration), test, 03258(06.01) Miniature sandmill method color and strength of color pigments, A 0 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, 0 2354 (06.02) Miscibility heptane miscibility of lacquer solvents, test, 01476 (06.03) water miscibility of water-soluble solvents, test,' "01722 (06.03) Mixed aniline point sampling and testing dipentene, method, 0 801 (06.03) Mixed xylene See Xylene (mixed) MMFT See Film Model 'C' wet film thickness gage wet film thickness of organic coatings, 01212 (06.01) Modified Wolfe-potentiometric method See Wolfe-potentiometric method " Moisture analysis--wood products edge performance of composite wood products under surfactant accelerated moisture stress, test, 0 2065 (06.01)- Moisture content--paints/related coatings/materials calcium borosilicate, test, 0 4487 (06.02) capillary moisture in concrete, by plastic sheet method, test, 04263(063)1) cellulose acetate propionates/butyrate, test, A D817 (06.02) cellulose acetate, test, 0 871 (06.02) ethylcellulose, test, 0 914 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, 0 2363 (06.02) hydroxyethylcellulose, test, 0 2364 (06.02) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, 0 280 (06.02) methylcellulose, test, 01347 (06.02) moisture content of (iron/copper phthalocyanine/ultramarine) blue pigments, by Brabender test, 01135 (06.02) moisture in cellulose, test, 01348 (06.02) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, 0 2195 (06.03) pine tars and pine tar oils, test, 0 856 (06.03) sampling and testing dipentene, method, 0 801 (06.03) 895 DUP0502 96456 Index of ASTM Standards, Section 6 Moisture content--paints/related coatings/materials sampiing/testing lac resins (orange shellac/button lac/gamet 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 40! 7 (06.01) water in liquid naval stores, test, D 890 (06.03) Moisture degradation conducting tests on paint/vamish/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, D 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, D126 (06.02) Molybdenum content molybdate orange pigments, spec., D 2218 (06,02). yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Monocyclic aromatic hydrocarbons See Hydrocarbons {headings) Monocyclic terpene hydrocarbons See Dipentene (and related terpene solvents) (headings) Monomeric acrylate esters (colorless) methyl ether of hydroquinone (MEHQ) content of colorless monomeric acrylate estets, test, D 3125 (06.03) Monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) water content of paints/paint materials, by Karl Fischer method, test, D4017 (06.01) Monomer (nnreacted) 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 , :,, i II sag resistance of paints, using a multinotch applicator, test*' - 4 04400(06.01) 1 wet film thickness of organic coatings, by notched gage%: : practice, D 4414 (06.01) . ,, . Multipanel forms *j recording results on single-/multi-panel forms, method, ' A 01150(06X1) i ,i,r N Naphtha and naphtha derivatives acidity of benzene/toluCne/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color of industrial aromatic hydrocarbons, test, 0848(06,03) aromatic hydrocarbons/related chemicals, terminology, 04790(06.03) evaporation residue determination, test, D 2232 (06.03) high-flash aromatic'naphthas, spec., D 3734 (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 (0602) 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., D656 (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 (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) water in liquid naval stores, test, D 890 (Q6.03) Negative Beilstein field identification of coatings, test, D 5043 (06,01). Neutral salt spray test See Salt spray (fog) testing __ , Newtonian liquids 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) Nitration grade/pnre benzene/benzol See Benzene Nitration grade/pure toluene/toluol 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) 896 IPPPSMS DUP050296457 Index of ASTM Standards, Section 6 Nuclear reactor vessels--coatings applications soluble nitrocellulose, by ferrous sulfate procedure, test, 04795(06.02) Nitrogen impurities pyridine base content in cresyiic acid, by direct titration, test, D4471 (06.03) Nonamine component content non-amine component content of fatty amines/nonamines, test, D 2082 (06.03) Nonaromatic hydrocarbons Sa Hydrocarbons (headings) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D 2360 (06.03) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) Nonaromatic impurities chemical analysis of benzene, by gas chromatography, test, D 4492 (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, D 4787 (06.01) Nonconductive protective coatings discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Nonconjugated oils--iodine value ' See Iodine value Noncontact thermometer temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 03259(06.01) Nondestructive evaluation (NOE) 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 Resins (headings) Non-human control--algae See Algae Nonleaiing aluminum pigment ,, See Aluminum powder and paste Nonmagnetic coatings film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Nonmagnetic organic coatings dry-film thickness of organic coatings, using micrometers, test, D 1005(06.01) Nonmetallic materials accelerated testing of paints/varnishes/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 goniophotometry, method, E430 (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) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Non-Nevrtonian 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/vamishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, D4040 (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) ceilulosics/emulsions/resin solutions/sheUac/vamishes, 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, D 5095 (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/vehicles, test, D 4713 (06.01) sampling and testing shellac varnish, D 1650 (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 (06.03) 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, D 4414 (06.01) NPIRI method fineness of grind of printing inks, by NPIRI 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, D4538 (06.01) Nuclear reactor vessels:--coatings applications abrading concrete, practice, D 4259 (06.01) add etching concrete, practice, D 4260 (06.01) capillary moisture in concrete, by plastic sheet method, test, D4263 (06.01) 897 app , DUP050296458 Index of ASTM Standards, Section 6 Nuclear reactor vessels--coatings applications coatings for light-water cooled nuclear power plants, 03912 (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., D 4618 (06.01) design/use ofsafety 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, D 4082 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power,plant, guide, D 5163 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) oil/water presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), D 4285 (06.01) pH of chemically cleaned/etched concrete surfaces, 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., D 5139 (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 masonry (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, D4286 (06.01) establishing procedures to qualify/certify inspection personnel for coating woric 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, D 4227 (06.01) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 4228 (06.01) Ocher chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) ochre pigment, spec., E> 85 (06.02) n-Octane purity of hydrocarbons from freezing points, test, 01016(06.03) Odor field identification of coatings, test, D 5043 (06.01) unreacted monomer content of latexes, by gas-iiquid chromatography, test, D 4747 (06.02) volatile solvents and diluents, test, D 1296 (06.03) Oil absorption calcium borosilicate, test, D 4487 (06.02) pigments, by Gardner-Coleman method, test, D1483 (06.02) pigments, by spatula rub-out test, D 281 (06.02) Oil acids identification of oils and oil adds 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 cleaning/abrasive blast cleaning), 0 4285(06.01) Oil resistance wood furniture lacquers, test, D 2571 (06.01) Oils Sa Hydraulic fluids coconut oil, spec., D1841 (06.03) com oil, spec., D 1842 (06.03) . cottonseed oil, spec., D 1843 (06.03) fish oil content (of drying oils and their fatty adds), gas-/Iiquid chromatography, test, D 3725 (06.03) identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) rosin oils, testing, D1131 (06.03) safflower oil, spec., D1392 (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/derivatives, test, D1358 (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, D1952 (06.03) color after heating, test, D1967 (06.03) color of transparent liquids, by Gardner colot1 scale, test, D1544 (06.01,06.02,06.03) degummed soybean oil, spec., D124 (06.03) dehydrated castor oil, spec., D 961 (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, D 3725 (06.03) foots, by gravimetric method, test, D1966 (06.03) foots, by volumetric method, test, D1954 (06.03) gel time, test, D1955 (06.03) '_ iodine valued-test, D1959 (06.03) loss on heating of drying oils, test, D1960 (06.03) methyl esters, preparation for fatty acid composition analysis by 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., D1462 (06.03) safflower oil, spec., D1392 (06.03) - sampling liquid oils/fatty adds (commonly used in paints/ vamishes/related materials), test, D1466 (06.03) saponification value of drying oils/fatty acids/polymerized fatty acids, test, D1962 (06.03) specific gravity at 25/25'C; test, D1963 (06.03) unsaponifiable matter in drying oils/fatty adds/polymerized fatty acids, test, D1965 (06.03) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) Oils--fatty clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) 898 lififrSiSj DU P050296459 Index of ASTM Standards, Section 6 Organic linings Oils--fuel flash point (of fuel oilsAube 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 oilsAnbe oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (062)3) Oils--mineral mineral oil content, of rosin oil, test, D 1131 (06.03) mineral (petroleum) spirits hydrocarbon drydeaning solvent, spec., 0235(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 (062)3) Oils--soybean degummed soybean oil, spec., D124 (06.03) refined soybean oil, spec., D1462 (06.03) Otis--tali distilled fatty acids, spec., D1984 (06.03) tall oil, methods of testing, D803 (06.03) Oils--tall oil rosin oleic acid content of tall oil rosin, test, D1585 (06.03) volatile resin acids in tail oil/giim/wood rosin, by gas chromatography, test, D 3008 (06.03) 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/testiog flaked aluminum powders/pastes, methods, D480 (06.03) Oleic acid content oleic acid content of tall oil rosin, test, D1585 (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, D 5150 (06.01) Opacity/opaqne 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 flash point methods See Flash point (headings) * Optical materials/properties/tests Sa CIarity/cleanness//Gloss/Haze Hiding power/Lrnninance/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 yellow/orange pigment, spec., D 211 (06.02) molybdate orange pigments, spec., D 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Orange shellac See Shellac Organic coatings abrasion resistance, by Taber abraser, test, D 4060 (06.01) acid 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/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (062)1) detergent resistance, practice, D 2248 (06.01) dry-film thickness of organic coatings, tiring 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, A 0 2485 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D4587 (06.01) filiform corrosion resistance, test, D 2803 (06.01) film formation rates in drying or curing process, test, D1640 (06.01) film hardness, by pencil test, D 3363 (06.01) flexibility/adhesioa 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, D4366 (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, D 4708 (06.01) producing films ofuniform thickness of paint/vamish/related products on test panels, test, D 823 (062)1) 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 spectropEotometry, test,' D 3733 (062)2) testing finishes on primed metallic substrates for humiditythermal cycle cracking, method, D 2246 (062)1)- testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) water immersion test, D870 (06.01) wet film thickness of organic coatings, D1212 (06.01) wet film thickness of organic coatings, by notched gages, practice, D4414 (06.01) Organic compounds acrylic acid dimer in acrylic acid/unsaturated organic acids, test, D 4415 (062)3) alcohol-benzene soluble matter in cellulose, test, D1794 (Q6.02) amount of volatile organic compound (VOC) released from solventbome automotive coatings and available for removal in a VOC control device (abatement), test, 05087(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) 899 ! DUP050296460 Index of ASTM Standards, Section 6 Organic liquids (volatile) Organic liquids (volatile) See Volatile organic compounds (VOQ Organic matter content volatile organic content (VOC) of paints/related coatings, selecting test procedures, practice, 0 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/garnet lac/bleached lac), test, D 29 (06.02) Orthoxylene See ortAo-Xylene Outdoor weathering See Weathering--outdoor Ovens nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) Overbaking (of paints/related coatings) effects of overbaking on organic coatings, practice, 02454(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/vamisb/iacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-v/ater-exposure apparatus, practice for conducting tests, D 4587 (06.01) Package stability estimating package stability of coatings for ultraviolet curing, test, 04144(06.01) freeze-thaw resistance of water-borne coatings, test, 02243(06.01) package stability of solvent-reducible/water-reducible paint, test, D1849 (06.01) resistance of emulsion paints (in containers) to attack by microorganisms, test, 0 2574 (06.01) sampling liquid paints/related pigmented coatings, practice, 0 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/paints 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, 01613 (06.03) clear/pigmented organic coatings, test, 0 1308 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus; practice, 0 5031 (06.01) dichloromethane/1,1,1-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reHectometry, test, E 97 (06.01) dry-film thickness of organic coatings, using micrometers, test, D 1005 (06.01) erosion testing of antifouling paints, tiring high velocity water, test, 04938 (06.01) evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, 0 869 (06.01) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A 0 2485 (06.01) field identification of coatings, test, 0 5043 (06.01) fire retardancy of paints, by cabinet method, test, A 01360 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, 0 1310(06.03) flash point by Tag closed tester, test, 0 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, 0 16(06.01,06.02,06.03) preparation of free films oforganic coatings, practice, 04708(06.01) recording results on ringle-/multi-pand forms, method, A 01150 (06.01) small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, 0 3806 (06.01) standard environments for conditioning/testing paint/ vamish/lacquer/reiated materials, spec., 0 3924 (06.01) titanium dioxide content in paint, by x-ray fluorescence - spectroscopy, test, 04764 (06.01) wet film thickness of organic coatings, 01212 (06.01) _ Paint--industrial water-base pigment content, by low temperature ashing, test, 03723(06.01) testing industrial water-reducible coatings^guide, 0 4712 (06.01) testing water resistance of coatings at 100 % relative 'humidity, ' practice,' 2247 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, 0 3792 (06.01) Paint--inspectors Sa Qualifications painting inspectors (metal substrates), guide, 0 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 thinnets, test, 01617 (06X3) evaporation rate, test, 0 3539 (06.01) nature of thinners in solvent-reducible paints, qualitative determination, method, 0 2349 (06.01) Paint brushes preparation of paint brushes for evaluation, practice, 0 5068(06.01) 900 ____wowamij W- DUP050296461 Index of ASTM Standards, Section 6 Petroleum/petroleum products U Paint roller Pendulum test HI preparation of paint roller covers for evaluation, D 5069 (06.01) hardness of organic coatings, by Konig/Persoz pendulum K Paint spatter resistance hardness tests, D4366 (06.01) H paint spatter resistance to roller application, test, D 4707 (06.01) Penetration--paint film | Paint test results porosity of paint films (to indicate coating penetration), test, I' recording results on $ingle-/multi-panel forms, method, D 3258 (06.01) i A D1150 (06.01) Penetration--pipeline coatings Pale gold bronze See Gold bronze powder Panel evaluation evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01)' mandrel bend test of attached organic coatings, test, D 522 (06.01) Pane! 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 j directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) j lightfastness ofprinted matter, 0 3424 (06.01) Para (paranitraniline) 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) ii Paraxylene ; See para-Xylene Paris red "* ' See Red lead Paris white See Calcium carbonate Paris yellow See Chrome yellow and orange impact resistance of pipeline coatings, by falling weight test, G14 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Pensky-Martens closed tester Sa Flash point (headings) flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Pentaerythritol glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D 1615 (06.02) pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06113) Pentane purity of hydrocarbons from freezing points, test, D1016 (06.03) Pentosans content pentosans content of cellulose, test, D1787 (06.02) Percent dilutabitity resin solution dilutabitity, test, 0 5062 (06.03) Percent epoxide epoxy content of epoxy resins, test, D1652 (06.02) Performance--coatings clear floor sealers, 0 1546 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, 0 5163 (06.01) subjecting marine antifouting coating to bifouting and fluid shear forces in natural seawater, test, D 4939 (06.01) Performance-nuclear materiais/applications . establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, Particle size (analysis/distribution) 05163(06.01) chemical analysis of calcium borosilicate, test, D 4487 (06.02) coarse particles in pigments/pastes/paints, test, D185 (064)1,06.02) multicolor lacquers, test, A D 2338 (06.01) polymeric powder properties, by multiple sieve method, practice, 03451 (06.01) reporting particle size characteristics of pigments, practice, D1366 (06.02) Particle size (analysis/distribution)--distribution particle size distribution, by hydrometer ofcommon white extender pigments, test, 0 3360 (06.02) Paste coarse particles in pigments/paStes/paints, test, D185 (06.01, 06.02) 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--mechiinicaUy deposited Permanent white See Barium sulfate Permanganate time permanganate time of acetone/methanol, test, 01363 (06.03) tricresyl phosphate, test, D 1721 (06.03) Permeability--Aims . moisture vapor transmission of organic coating films, test, 01653(06.01) Permeability absorption reporting particle size characteristics of pigment^ practice, D1366 (06.02) Permeance moisture vapor transmission of organic coating films, test, 01653 (06.01) Peroxides Sa Active oxygen content peroxides in styrene monomer, test, 0 2340 (06.03) trace peroxides (2:5-80 ppm), using spectrophotometer, test, E 299 (06.03) Persian gulf oxide See Iron oxide red Persoz pendulum test hardness of organic coatings, by Konig/Persoz pendulum . hardness tests, D 4366 (06.01) Petroleum--mineral spirits See Mineral spirits Petroleum/petroieum products Pencil test cresylic acid content (of alkaline cresylate solutions), chemical film hardness of organic coatings, test, D 3363 (06.01) analysis, 0 3439 (06.03) 901 DUP050296462 Index of ASTM Standards, Section 6 Petroleum/petroleum products--distillates Petroleum/petroleum products--distillates water in petroleum products/bituminous materials, by distillation, test, D95 (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) Pfund wet film thickness gage wet film thickness of organic coatings, D1212 (06.01) pH Sa Acidity, alkalinity, pH (headings) apparent pH of electrocoat baths, test, D 4584 (06.01) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) pH of chemically cleaned/etched concrete surfaces, D4262 (06.01) Phenol analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) and cresylic acid, sampling and handling, practice, D3852 (06.03) apparent free phenols, in synthetic phenolic resins/solutibns (used in paints/related coatings), test, D1312 (06.02) aromatic hydrocarbons/related chemicals, terminology, D4790 (06.03) color of cresylic acids ("C" series standards), test, D3627 (06.03) phenol content of (refined) isopropylbenzene (cumene), test, D 3160 (06.03) phenol content (of tar add 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, D'1631 (06.03) Phenolic resins Sa Resins (headings) apparent free phenols, in synthetic phenolic resins/solutions ' (used in paints/related coatings), test, D1312 (06.02) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) methylol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) volatile content in phenolic resins, test, D 4639 (06.02) Phosphorus add content zinc hydroxy phosphite, test, D 4450 (06.02) Photographic processing photographic documentation of coarings/lining defects and Mures, D 4121 (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 (06.03) 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 (063)3) Phthalic anhydride--refined refined phthalic anhydride-1308, spec., D 2403 (06.03) Phthalic anhydride content alkyd resins/resin solutions in absence of dibasic acids, test, D 563(063)2) alkyl resins/resin solutions containing dibasic acids, by gravimetric test, D1306 (063)2) -- Phthalocyanine bine ' chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) Phthalocyanine green chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) Phthalocyanine (phthaio) bine chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) copper phthalocyanine blue pigment, spec., D 963 (06.02) Phthalocyanine (phthaio) green phthalocyanine green pigment, spec., D 3021 (06.02) Physical constants calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Physical strength/resistance (nonchemical) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) Pictorial surface preparation standards Sa Surface preparation (headings) standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) Pigment analysis See Pigments (general properties) Pigment bleeding test bleeding characteristics, of dry pigments, test, D 279 (06.02) Pigment content antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (063)2) moisture content of pigments, D1208 (06.02) nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06311) paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) pigment content of solvent-reducible paints, test, D 2371 (063)1) 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 solventreducible paints, test, D 2352 (06.02) ...... ' titanium dioxide content of pigments (recovered, from- whdle" 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, D3723 (06.01) water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Pigment dispersion (paint) Sa Pigments (general properties) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) coarse particles in pigments/pastes/paints, test, D185 (06.01,063)2) evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) fineness of grind, printing ink, test, D1316 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D 2621 (06.01) 902 | | :i; f 8 jj ' DU P0502 96463 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 (063)1) 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., D962(06.02) Pigments--aluminum silicate aluminum silicate (hydrous/anhydrous) pigment, analysis, test, 0718(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 D715 (06.02) Pigments--basic carbonate white lead basic carbonate white lead pigment, spec., D 81 (063)2) white lead- chemical analysis, test, D1301 (06.02) Pigments--basic lead silicochromate basic lead silicochromate pigment, spec., D1648 (063)2) 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--bone black bone black pigment, spec., D 210 (06.02) solvent extractable material in black pigments, test, D305 (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., D1199 (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, D 126 (06.02) Pigments--chrome yellow and orange chrome yellow/orange pigment, spec., D 211 (063)2) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Pigments--chromium oxide green chrome oxide green pigment, spec., D 263 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (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., D8S (06.02) Pigments--gold bronze powder chemical analysis of cuprous oxide/copper pigments, test, 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, D3872 (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, D50 (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, D50 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) Pigments--iron oxide yellow analysis, D 50 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) Pigments--lampblack lampblack pigment, spec., D 209 (06.02) solvent extractable material in black pigments, test, D 305 (063)2) 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, D717 (06.02) magnesium silicate pigment (talc), spec., D 605 (06.02) Pigments--mercuric oxide analysis, D 284 (063)2) mercuric oxide for use in antifouling paints, spec., D911 (06.02) Pigments--mica grit content of mica pigment, test, D 716 (063)2) 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 analysis, D 50 (06.02) ochre pigment, spec., D 85 (06.02) Pigments--para red para red/toiuidine red pigments, testing, D 970 (06.02) pure para red toner pigment, spec., D 475 (063)2) Pigments--phthalocyanine bine chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) DUP050296464 Index of ASTM Standards, Section 6 Pigments--phthalocyanine blue copper phthalocyanine blue pigment, spec., D963 (063)2) Pigments--phthalocyanine green chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (063)2) 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, D49 (06.02) red lead pigment, spec., D 83 (06.02) Pigments--sienna, burnt and raw analysis, D 50 (06.02) raw/bumt sienna pigments, spec., D 765 (06.02) Pigments--silica diatomaceous silica pigment, analysis, test, D 719 (06.02) Pigments--silica, diatomaceous diatomaceous silica pigment, spec., D 604 (06.02) Pigments--strontium chromate chemical analysis of strontium chromate pigment, test, D1845 (06.02) strontium chromate pigment, spec., D1649 (06.02) Pigments--titanium dioxide chemical/gravimetric analysis ofwhite/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 whole paint), by atomic absorption spectroscopy, test, D 4563 (06.01) titanium dioxide pigments, spec., D 476 (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/bumt 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 (06.02) chemical analysis of white pigments, selection of test methods, guide, D 34 (06.02) partide size distribution, by hydrometer of common white extender pigments, test, D 3360 (06.02) ratio of anatase to rutile in titanium dioxide (TiO^) 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, D2351 (06.02) sulfur dioxide in white pigment separated from solventredudble 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, 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 (06.02) Pigments--zinc dust analysis, DS21 (06.02) zinc dust pigment, spec., D 520 (06.02) Pigments--zinc hydroxy phosphite analysis, D 4450 (06.02) zinc hydroxy phosphite pigment, spec., D 4462 (06.02) Pigments--zinc oxide analysis of white zinc pigments, test, D 3280 (063)2) 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/ailcyd), spec., D 4302 (06.01) bleeding characteristics, of dry pigments, test, D 279 (06.02) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) coarse particles in pigments/pastes/paints, test, D185 (06.01,06312) 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, D 1210 (06.01) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (06312) lightfastness of pigments (in artists' paints), test, D 4303 (06.01) oil absorption, by Gardner-Coleman method, test, D1483 (06.02) oil absorption, by spatula rub-out, test, D 281 (06.02) partide size- fineness of grind- printing inks, iSt, D 1316 (06.01) relative tinting strength of chromatic paintsMest, D 4838 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) reporting particle size characteristics of pigments, practice, D1366 (06.02) specific gravity, test, D153 (06.02) tinting strength/color of colored pigments, by mechanical / muller, test, D 387 (06.02) tinting strength/color of colored pigments, by'miniature sandmili, test, A D3022(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 (063)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 ofsettling (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) partide size distribution, by hydrometer of common white extender pigments, test, D 3360 (06.02) Pinene sampling and testing turpentine, method, D 233 (06.03) Pinene--alpha and beta wood, gum, and sulfate turpentine, by gas chromatography, test, D 3009 (06.03) Pine tars/pine tar oils sampling and testing pine oil, method, D 802 (06.03) 904 DUP050296465 i 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, 0 4787 (06.01) 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, G42 (06.01) disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) impact resistance of pipeline coatings, by falling weight test, G14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Plasticizer grade alcohol C4-Cl3 alcohol, chemical/physical analysis (selection/use of test procedures), E 852 (06.03) Plasticizers plasticizer migration from: vinyl fabrics to lacquers, method, D 2199 (06.01) Plastics (general) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) evaluation of (clear/pigmented) coatings for rigid/semirigid plastic substrates, practice, 0 3002 (06.01) methylol group determination (qualitative) in phenolic resins, test, 04706(06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, 01013 (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, 0 4707 (06.01) Plastic sheet method capillary moisture in concrete, by plastic sheet method, test, 04263 (06.01) Plastics (thermoplastic) bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, 0 4796 (06.01) evaluation of color for thermoplastic traffic marking materials, test, 04960 (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, D1209 (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, D 4789 (06.03) Point impact impact resistance of pipeline coatings, by Ming weight test, G14 (06.01) Polarographic methods nitrobenzene in aniline, test, 0 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, 0 2456 (06.02) isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) Polyhexafluoropylene (FEP) substrate preparation of free films of organic coatings, practice, 0 4708(06.01) Polyhydric alcohol identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) Polymer content polymer content of styrene monomer, test, 0 2121 (06.03) qualitative identification of polymers in 'emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, 0 3168 (06.01) Polymeric powders/powder coatings selection/use of test procedures, practice, 0 3451 (06.01) Polymerization cellulose nitrate, test, 01716 (06.02) sampling and testing turpentine, method, 0 233 (06.03) unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) __ ' Polymerization inhibitors p-tcrt-butylcateehoi (TBC) in styrene monomer, test, 0 2120 (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, 0411 (06.02) qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, 0 3168 (06.01) silicone polymers- silicon content, by atomic absorption spectrophotometry, test, 0 3733 (06.02) solubility range, test, D 3132 (06.02) Polyol acetates identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) Polyurethane raw materials See Urethanes--polyurethane raw materials (headings) 905 DUP050296466 Index of ASTM Standards, Section 6 PolyOdnyl acetate) coating systems PoSy(vinyt acetate) coating systems water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) Poly(vinyl butyral) resins Sa Resins (headings) poly(vinyl butyral)- chemical analysis, test, D1396 (06.02) Polyvinyl chlorideXPVC) plastics--resins poly(vinyl chloride) resins, selecting test procedures, guide, D 4368 (06.02) residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) Ponderosa pine wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Porcelain enamel products directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectoraetry, test, E 97 (06.01) Porosity--coating porosity of paint films (to indicate coating penetration), test, D32S8 (06.01) Portable adhesion testers pull-off strength of coatings, using portable adhesion testers, test, D4S41 (06.01) Potash blue See Iron blue Potassium permanganate reduction See Permanganate time Potentiometric method acid number of rosin, test, D 465 (06.03) maleic acid content of maleic anhydride, by potentiometric titration, test, D 2930 (06.03) saponification number of rosin, test, D 464 (06.03) Powdered chemicals directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectoraetry, test, E 97 (06.01) Power generating facilities design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D4618 (06.01) dry film thickness of protective coating systems, by destructive means, test, D4138 (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) Precantionary labeling labeling art materials for chronic health hazards, practice, 04236(06.01) Precision conducting interlaboratory study to determine precision of test method, practice, E 691 (06.03) Precision--instrumentation directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Preformed tape (for traffic marking) pigment content of paint/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-, D 871 (06.02) primary hydroxyl content of cellulose esters, test, AD 817 (06.02) Primer formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D4146 (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, D 3322 (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 (06211) 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/v<?hicles, by inkometer, test, D 4361 (06.01) commercial hexanes, spec., D1836 (06.03) fineness ofgrind of printing inks, by NPIRJ method, test, D1316 (06.01) nonvolatile content of printing inks/resin solutions/vehicles, test, 04713 (06.01) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) relative tintingstrength 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 of lithographic printing inks/vehides in a laboratory mixer, test, D 4942 (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, D 4537 (06.01) Production method transfer efiidency under production conditions for spray application of automotive paints, by weight basis, practice, D 5066 (06.01) 2-Propanone See Acetone 906 Index of ASTM Standards, Section 6 Quality assurance Propiony] content acetyl and propionyl/butyral contents of cellulose mixed esters, test, A D 817 (06.02) K-Propyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, 0 3545 (06.03) -propyl acetate (96 % grade), spec., D 3130 (06.03) n-Propyl alcohol n-propyl alcohol (1-propanol), spec., D 3622 (06.03) Propylene glycol propylene glycol/dipropylene glycol, spec., 0 5164 (06.03) propylene glycol, spec., 0 2695 (06.03) Propylene glycol monomethyl ether acetate (PMA) propylene glycol monomethyl ether acetate, spec., D 4835 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Propylene glycol monomethyl ether (PM) propylene glycol monomethyl ether, spec., 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/Uning work for power generation facilities, terminology, D 4538 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D5144 (06.01) Protective equipment handling/sampling phenol and cresylic arid, practice, 0 3852(06.03) sampling and handling aniline, practice, 0 3436 (06.03) Protective linings design/fabrication of flue gas desulfurization system components (for protective lining application), spec., 0 4618 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, 04619 (0601) Prussian blue See Iron bine Pull testing Sa Adhesion (headings) adhesion of organic coatings to plastic substrates, by direct tensile testing, D5179 (0601) bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, 0 4796 (06.01) pull-off strength of coatings, using portable adhesion testers, test, 0 4541 (06.01) Pulp solubility in sodium hydroxide, test, 0 1696 (06.02) Pumice/pumice stone/pumacite pumice pigment, spec., D 867 (06.02) Purity acetaldehyde, spec., D 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 ofp-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., 0 4709 (06.03) ort/zo-xylene, by gas chromatography, test, 03797 (06.03) purity analysis ofisopropylbenzene (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, O 3329 (06X3) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, 0 4773 (06.03) purity ofstyrene, by freezing point method, test, 0 3799 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) sodium glycolate content of sodium carboxymethyicellulose, test, 01439 (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, 04790(06.03) hydroxyl content of cellulose acetate, by spectrophotometry, test, 0871 (06.02) hydroxyl content of pyridine-soluble cellulose esters, by spectrophotometry, test, A 0 817 (06.02) pyridine base content in cresylic acid, by direct titration, test, 04471(06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, 0 3437 (06.03) water content, by iodine reagent method, test, 0 1631 (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 (06.03) 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 (06.01) establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, 04537 (06.01) journeyman painters for application of coatings to concrete surfaces of safety-related areas in nuclear facilities, practice, 04227 (06.01) journeyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 4228 (06.01) sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., 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, 01394 (06.02) Quality assurance coatings for light-water cooled nuclear power plants, practice, 03843(06.01) 907 saps DUP050296468 Quality assurance Index of ASTM Standards, Section 6 use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Quality control color ofcresylic acids ("C" series standards), test, D3627 (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 coalings (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-aic 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, D3259(06.01) ultraviolet-cured coatings, cure time, practice, D 3732 (06.01) use of protective coating standards in nuclear 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 Otis (headings) Raw sienna Sa Pigments (headings) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D50 (06.02) raw/burnt sienna pigments, spec., D 765 (06.02) Reactor vessels See Nuclear reactor vessels (headings) Reagent resistance factory-applied coatings on wood products, practice, D 3023 (06.01) Reagents presence of and removing microbial (fungal/alga!) 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 ofexposure tests of paints, AD 1150 (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/brown pigments containing iron/maganese, test, D 50 (06.02) lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) para red/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., D83 (06.02) synthetic red iron oxide pigment, spec., D3721 (06.02) Reduction refined pyridine, by reducing substances, qualitative determination, test, D 2031 (06.03) 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, AD4214 (06.01) Refined benzene See Benzene (headings) Refined bleached lac See Bleached lac--dry Refined cresylic acid See Cresylic acid Refined naphtha derivatives See Naphtha and naphtha derivatives Refined phenol Sa Phenol refined phenol, spec., D 2439 (06.03) Refined phtbalic anhydride See Phtbalic anhydride Refined pyridine See Pyridine--refined Refined soybean oil See Soybean oil Refined tar acids See Tar acids--crude and refined Reflectance apd reflectivity '' chalking (of white/lightly tinted exterior paint films), practice, A D 4214 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metry, method, E 430 (06.01) - hiding power ofpaints, by reflectometry, test, A D 2805 (06.01) instrumental color difference, test, D 2244 (06.01) porosity of paint films (to indicate coating penetration), test, D3258 (06.01) reflection haze (of high gloss surfaces), test, O'4039 (06.01) ' relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) Reflectance and reflectivity--copy materials - directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) preparation of reference white reflectance standards, practice, E 259 (06.01) Reflection haze See Haze Reflective markers in traffic paint See Glass spheres (in traffic paint) Refractive index '. gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) sampling and testing dipentene, method, D 801 (06.03) sampling and testing pine oil, method, D 802 (06.03) sampling and testing turpentine, method, D 233 (06.03) Regular bleached lac See Bleached lac--dry Relative dry hiding power (of paints/coatings) See Hiding power--paints/coatings DUP050296469 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 film failure See Failure end point (headings) Residual glycol ether purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Residual odor See Odor Residue chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) sampling/testing flaked aluminum powders/pastes, methods, 3> 480 (06.03) Residue--evaporation naphthalene, test, D 2232 (06.03) sampling and testing turpentine, method, D 233 (06.03) Retins alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) amine resins--solvent tolerance, test, D1198 (06.02) amino resins, selecting test procedures, practice, D4277 (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, D 1310 (061)3) free formaldehyde content of amino resins, test, D1979 (06.02) poly(vinyl butyral)- chemical analysis, test, D1396 (06.02) poly(vinyl chloride) resins, selecting test procedures, guide, D 4368 (06.02) residual vinyl chloride monomer content ofpoly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) resin solution dilutability, test, D 5062 (06.03) softening point, by ring-and-ball apparatus, test, E 28 (06.03) solubility range, test, D 3132 (06.02) voiatile/nonvolatile content (of cellulosics/emulsions/resin solutions/sheilac/vanaishes), selecting test procedures, practice, D 4209 (06.02) volatile resin adds in tail oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) Resins--alkyd artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06D1) fatty adds content, test, D1398 (06.02) glycerol/etbylene 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 add content of alkyd/polyester resins, test, D 2690 (06.02) phthalic anhydride content (in absence of dibasic acids), test, 0563(06.02) phthalic anhydride content: (in presence of dibasic acids), by gravimetric test, D1306 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) rosin adds content, test, D1469 (06.02) silicone-modified-siiicon content, by atomic absorption spectrophorometry, test, D 3733 (06.02) specific gravity at 25/25C, 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, D 1847 (06.02) Resins--lac orange shellac/other indian lacs for electrical insulation, spec., D 784 (06.02) sampling/testing lac resins (orange sheliac/button lac/gamet lac/bleached lac), test, D 29 (06.02) 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), test, D1312 (06.02) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) methylol group determination (qualitative) in phenolic resins, test, D4706 (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 ofgelled vehicles, using microwave oven, practice, D5166 (06.02) Resin solution cloud point resin solution dilutability, test, D 5062 (06.03) Resin solutions color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02, 06.03) glycerol/ethylene giycol/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.acids, test,' D563 (06.02) resin solution dilutability, test, D 5062 (06.03) unsaponifiable matter content, test, D1397 (06.02) viscosity, test, D1725 (06.02) Resistance See Resistance--abrasion Sa Resistance--acid Resistance--alcohol Resistance--alkali Resistance--bacteria Resistance--blistering Resistance--blocking Resistance--chemical Resistance--chipping Resistance--cracking Resistance--deformation Resistance--foe! Resistance--heat Resistance--impact (pipeline coatings) Resistance--imprinting Resistance--mortar Resistance--oil Resistance--paint spatter 909 DUP050296470 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 963 (06.01) abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.0i) air blast abrasion tester, A D 658 (06.01) practical washability of organic coatings, test, D 4828 (06.01) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) Taber abraser, test, D 4060 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Resistance--acid acid/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) Resistance--alcohol wood furniture lacquers, test, D 2571 (06.01) Resistance--alkali clear/pigmented organic coatings, test, D1308 (06.01) dried varnish films, test, 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, D 4585 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) Resistance--blocking blocking resistance of trade sales paints, test, D4946 (06.01) organic coatings on wood substrates, test, D 2793 (06.01) pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Resistance--boiling water (H20) wood furniture lacquers, test, D 2571 (06.01) Resistance--chemical chemical resistance of pipeline coatings, test, G 20 (06.01) clear/pigmented organic coatings, test, D 1308 (06.01) coatings for light-water cooled nuclear power plants, D 3912 (06.01) Resistance--chipping paints and related coatings, A D 3170 (06.01) traffic paint, A D913 (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 (061)1) 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, D 2571 (06.01) Resistance--paint spatter paint spatter resistance to roller application; test, D 4707 (06.01) Resistance--penetration porosity of paint films (to indicate coating penetration), test, 0 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, 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, G13 (06.01) specific bendabiiity of pipeline coatings, test, G 10 (06.01) Resistance--pressure mottling pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Resistance--reagent factory-applied coatings on wood products, practice, D 3023 (06.01) Resistance--sag sag resistance of paints, using a multinotch applicator, test, -- D 4400 (06.01) Resistance--scrub scrub-to-failure of interior latex flat wail paints, test, . D 2486 (06.01) ----- wet abrasion resistance of interior paints to scrubbing, by weight loss, test, 174213 (06.01) Resistance--slip static friction of coating surfaces, test, D 4518 (06.01) Resistance--soil practical washability of organic coatings, test, D4828 (06.01) Resistance--solvent solvent/fuel resistance of traffic paint, test, D 2792 (06.01) Resistance--stain factory-applied coatings on wood products, practice, D3023 (06.01) practical washability of organic coatings, test, D 4828 (06.01) Resistance--temperature temperature-change (high-low) resistance of dear nitrocellulose lacquer films applied to wood, test, D 1211 (06.01) Resistance--water coatings using controlled condensation, practice, D 4585 (06.01) coatings, using water immersion, practice, D 870 (06.01) dried varnish films, test, D 1647 (06.01) testing water resistance of coatings at i 00 % relative humidity, practice, D 2247 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) 910 DUP050296471 Index of ASTM Standards, Section 6 Sampling--^hydrocarbons Resistance--wear See Wear testing (headings) Resistance--wet abrasion practical washabiiity of organic coatings, test, D4828 (06.01) Retort pine tars See Fine tars (kiln and retort) Retroreflection/retroreflectors sieve analysis of glass spheres (for retroreflective pavements markjngs/industrial uses), test, D1214 (06.02) Rheology printing inks/ink films/related materials, selecting test methods, guide, 0 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, A D3274 (06.01) Road service'testing Sa Traffic paint conducting road service tests on fluid traffic marking materials, practice, D 713 (06.01) evaluating degree of bleeding of traffic/pavement marking paint, test, A D 868 (06.01) evaluating degree ofchipping oftraffic paint, method, A 0913(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, D5150 (06.01) Roller coat testing industrial water-reducible coatings, guide, D4712 (06.01) Rosenmund-Kuhnhenn method iodine value of drying oils and their derivatives, test, D1541 (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 acid content of tall oil rosin, test, D1585 (06.03) sampling/grading rosin (delivered in commercial bagsI baxrels/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 (06.03) volatile resin acids 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, D 1131 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) tall oil, methods of testing, D 803 (06.03) Rosin content qualitative detection of rosin in varnishes, by LiebermanStoreh/Halphen-Hicks tests, D1542 (06.01, 06.02) Rosin esters rosin acids content, test, D 1469 (06.02) Rotational viscometer rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Rouge See Iron oxide red Roundness of glass spheres embedded in traffic paint, test for, 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 (06.02) Rupture/rupture strength impact resistance ofpipeline coatings, by failing 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 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) handling naphthalene, maleic/phthalic anhydride, practice, D 3438 (06.03) handling phenol and cresylic acid, practice, D 3852 (06.03) handling polymeric powders, practices, D 3451 (06.01) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Safflower oil safflower oil, spec., D1392 (06.03) Sag resistance paints, using ajnultinotcb applicator, test, D4400 (06.01) Sa!t water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Salt spray (fog) testing salt spray (fog) testing, method, B 117 (06.01) Sample preparation sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Sampling industrial chemicals, practice, E 300 (06.03) Sampling--aerospace fluids lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) Sampling--hydrocarbons cresylic acid and phenol, practice, D 3852 (06.03) naphthalene, maleic anhydride, and phthalic anhydride, practice, D 3438 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) 911 DUP050296472 Index of ASTM Standards, Section 6 Sampling--hydrocarbons sampiing/handling liquid cyclic products (at ambient temperature), practice, D3437 (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, D 1650 (06.02) sampling and testing turpentine, method, D 233 (06.03) sampting/grading rosin (delivered in commercial bags/ barrels/drums), test, D 509 (06.03) sampling liquid oils/fatty adds (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/varnish/related material), selecting test methods, D 268 (06.03) Sampling--petroleum products purity of hydrocarbons from freezing points, test, D 1016 (06.03) Sand abrasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) Sandstone preparatory surface cleaning ofarchitectural sandstone, practice, D 5107 (06.01) Saponification number/value Set Unsaponifiable 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, D 1650 (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 adds/polymerized fatty acids, test, D1962 (06.03) tall oil, methods of testing, D 803 (06.03) Saybolt viscometers See Viscometers--Saybolt Scaling See Flaking Scattering coefficient hiding power of paints, by reflectoraetry, test, A D 2805 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) Scrub resistance scrub-to-failure of interior latex flat wall 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 rec-Butyl alcohol Sediment clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) Sedimentation reporting particle size characteristics of pigments, practice, D1366 (06.02) Self-aligning adhesion tester pull-off strength of coatings, using portable adhesion testers, test, D4541 (06.01) Semi-gloss paints interior latex semigloss/gloss paints, selecting test methods, guide, D4540 (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, 03278(06.03) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01,06.03) Settlement evaluating degree ofsettling (pigment suspension/ease of remixing a shelf-aged sample) of paint; test, 0869 (06.01) traffic paint, in containers, by laboratory simulation, test, D1309 (06.01) Set-to-tonch-time See Drying time Shear testing--paints/related coatings/materials consistency of paints, using Stormer viscometer, test,, D 562 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (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, D 3928 (06.01) practical washability of organic coatings, test, D 4828 (06.01) - specular gloss of nonmetallic specimens, test, D 523 (06.01) Sheet materials (general) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) Sheet metal flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, D4145 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) - Shellac sampling and testing shellac varnish, D I650J06.02) shellac varnishes, spec., D 360 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (061)2) Shellac--electrical insulating orange shellac/other indian laes for electrical insulation, spec., 0 784(06.02) shellac (dry/powdered) used for electrical insulation, selecting test methods, D 411 (06.02). Shellac--orange orange shellac and (button lac/gamet lac), spec., D 237 (06.02) sampling and testing shellac varnish, D1650 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) - Shipping amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D.4948 (06.01) impact resistance of pipeline coatings, by failing weight test, G14 (06.01) Shortness ratio laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) 912 Index of ASTM Standards, Section 6 Solid phase materials--paints/related 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, D 1696 (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, D1696 (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(vinyI 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 nonpassivated galvanized steel panels for testing paint/varnish/lacquer/related products, test, D 2201 (06.01) 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 solution/dispersion containing dispersed solids, test, D 4948 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) artists' paints (oil/resin-oil/alkyd), spec., D 4302 (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, D 3718 (064)1) commercial hexanes, spec., D 1836 (06.02) conducting tests on paint/vamish/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 (064)1) interior semigloss wali/trim enamels, selection/use of test methods, practice, D 3425 (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 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, D1849 (064)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 (06.01) porosity of paint films (to indicate coating penetration), test, D 3258 (064)1) practical washability of oiganic coatings, test, D 4828 (06.01) preparing drawdowns of artists' paste paints, practice, 04941(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 cbating 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 solvent- reducible paints, test, D 2352 (06.02) testing solvent-bome 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, D 4764 (06.01) vacuum distillation (for vehicle separation in solvent-type paints), practice, D3272 (06.01) vehicle separation from solvent-reducible paints, by centrifuge,- practice, 0 2372 (06.01) - volatile matter content determination, test, D 2369 (06.01) volatile organic compounds (VOC) of solvent reducible paints in aerosol cans, test, D 5200 (06.01) T! 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., 0 358(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, 0 5087 (06.01) Solvent rub method MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, 0 4752 (06.01) Solvents field identification of coatings, test, D 5043 (06.01) hexyl acetate, spec., D 5137 (06.03) 914 DUP050296474 Index of ASTM 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, 01613 (06.03) amount of volatile organic compound (VOC) released from solventbome automotive coatings and available for removal in a VOC control device (abatement), test, 05087(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 (06.03) ethyl acetate (all grades), spec., D 4614 (06.03) heptane miscibility of lacquer solvents, test, D1476 (06.03) hexyl acetate, spec., 0 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 oiganic solvents), test, D1259 (06.02) nonvolatile matter content, test, D1353 (06.03) M-propy! acetate (96 % grade), spec., 03130 (06.03) odor (character!stic/residual), tek, 01296 (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 (insolvent-type paints), by gas chromatography, test, D 3271 (06.01) solvent extractable materkl in black pigments, test, D 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 (ofdriers/drying oils/naval stores and solvents), selecting test procedures, guide, D414G (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, D1722 (06.03) Solvent tolerance resin solution dilutabiiity, test, D 5062 (06.03) Southern pine wood used as panels in weathering tests of coatings, spec., D 358(061)1) 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, D 3627 (06.03) Spark testers discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Spattering paint spatter resistance to roller application, test, D 4707 (06.01) Spat test (for lead) detection of lead in paint/dried paint films, test, D3618 (06.01) Spatula rub-out test absorption of linseed oil in pigments, test, D 281 (06.02) Specifications--petroleum 2-methoxyethand, 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, 03505(06.03) drying oils, varnishes, alkyd resins, fatty adds, and related materials, at 25/25C, test, D1963 (06.03) pigments, tests, D153 (06.02) sampling and testing dipentene, method, D 801 (06.03) sampling and testing pine oil, method, D 802 (06.03) sampling and testing pine tars/pine-tar oils, method, 0 856 (06.03) sampling and testing turpentine, method, D 233 (06.03) Spedfic permeability moisture vapor transmission of oiganic 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)--paints/related coatings abrading concrete, practice, 0 4259 (06.01) add etching concrete, practice, 0 4260 (06.01) ... magnesium alloys, practice, 01732 (06.01)_ making and preparing concrete/masonry panels for testing paint finishes, mdhod, D1734 (06.01) paint and related coatings exposure tests, methods for preparation, 0 609 (06.01) pH of chemically cleaned/etched concrete surfaces, 04262(06.01) preparation of aluminum/aluminum-alloy surfaces (for painting), practice, 0 1730 (06.01) preparation of hot-dip aluminum surfaces (for painting), practice, 01731 (06.01) preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/vamish/lacquer/related products, test, 02201(06.01) preparation of methyl esters from fatty adds, for fatty add composition analysis, test, 0 3457 (06.03) preparation of paint brushes for evaluation, practice, 0 5068(06.01) preparation of paint roller covers for evaluation, 0 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, 0 3964 (0601) 915 DUP050296475 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, D4258 (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/related coatings sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Spectral data conducting tests on paint/vamish/iacquer/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) gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Spectrometry--mass color of cresylic acids ("C" series standards), test, 0 3627(06.03) Spectrophotometry--absorption carbon disulfide content of aromatic hydrocarbons, using spectrophotometry, test, D 2324 (06.03) iron content (of rosin), D 1064 (06.03) spectrophotometric diene value of dehydrated castor oii/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, 04834 (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, 02066(06.01) Spectrophotometry--goniophptometry gloss of high-gloss metallic/nonmetaliic surfaces, by goniophotometry, method, E 430 (06.01) Spectrophotometry--infrared cellulose nitrate in aikyd 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 (of traffic 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, D4563 (06.01) Spectroscopy--atomic absorption antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, 0 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, 0 5066(06.01) Spray method testing industrial water-reducible coatings, guide, D 4712 (06.01) Spreading rate hiding power of paints, by reflectometry, test, A D 2805 (06.01) Stability--paints/related coatings/materials accelerated testing of paints/vamishes/lacqueis/reiated products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) conducting tests on paint/varnish/Iacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) copper phthaiocyanine 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 soivent-reducible/water-redutible paint, test, 01849(06.01) Staining .. 1 .- effect of staining agents (on organic finishes in the automobile industry), practice, D1540 (06.01) practical washability of organic coatings, test, 0 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, 0 3023 (06.01) Standard color solutions See Color (headings) Static coefficient of friction See Coefficient of friction Statistical methods conducting interiaboratory study to determine precision of test'' method, practice, E 691 (06.03) Steam-distilled wood turpentine See Turpentine Steel bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, 04796 (06.01) Steel--panels paint and related coatings exposure tests, methods for preparation, 0 609 (06.01) 916 r Index of ASTM Standards, Section 6 Sulfate content--paints/related coatings preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/vamish/Lacquer/related products, test, D 2201 (06.01) Steel--substrates film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Steel--surfaces assessing the condition of aged coatings on steel surfaces, guide, I D 5065(06.01) coating contractor qualification (for nuclear-powered generation facilities), practice, D 4286 (06.01) degree of rusting oh painted steel surfaces, method, AD 610 (06.01) evaluating (interipr/exterior) coatings for protecting Steel surfaces at high-temperature service, test, A D 2485 (06.01) profile of abrasive blast-deaned steel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 4228 (06.01) Steel blue pigment See Iron blue Steel cubes bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D4796 (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, 02201 (06.01) Steel samples sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Step gages ' wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Sticking blocking resistance of trade sales paints, test, D4946 (06.01) Stiffness free films of paints and related coatings, test, D 2370 (06.01) Stone--marble/limestone/sandstone/granite preparatory surface cleaning of architectural sandstone, practice, D 5107 (06.01) Stonner method consistency of paints, using Stormer viscometer, test, 0562(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, D 332 (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 (06.01) Strip test detection of copper corrosion from petroleum products, by copper strip tarnish test, A D 130 (06.03) Stroke cure time stroke cure time of thermosetting phenol-formaldehyde resins, test, D4640 (06.02) Strontium chromate pigment Sa Pigments (general properties) chemical analysis of strontium chromate pigment, test, D1845 (06.02) strontium chromate pigment, spec., D1649 (06.02) Structural applications--paint field identification of coatings, test, D 5043 (06.01) Styrene analysis of styrene by capillary gas chromatography, test, 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, D2119 (06.03) polymer content of styrene monomer, test, D 2121 (06J)3) . p-fert-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, D 1016 (06.03) purity ofstyrene, by freezing point method, test, D 3799 (06.03) residual p-iert-butylcatechol (TBC) in styrene monomer, by addition of NaOH, test, D 4590 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) styrene monomer 996, spec., D 2827 (06.03) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) volume/weight of industrial aromatic hydrocarbons, method, D 1555 (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 substrata, 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 (06.01) 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, 04708(06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D5146 (06.01) Sulfate ash content pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) Sulfate content--paints/related coatings acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D 1135 (06.02) cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, D 871 (06.02) 917 DUP050296477 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) yellow/orange/green pigments containing lead chromate/ chromium oxide green, test, D126 (06.02) Sulfated ash content ashing cellulose, test, D3S16 (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, D871 (06.02) cellulosic materials, by X-ray fluorescence, test, D 2929 (06.02) sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcqulometry, test, D 3961 (06.03) zinc dust (metallic zinc powder), test, D 521 (06.02) Sulfur content--petroleum products mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec, D 235 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) Sulfur dioxide (S02) content qualitative, of industrial aromatic hydrocarbons, test, D 853 (06.03) sulfur dioxide in white pigment separated from solvent- reducible paints, test, D 2352 (06.02) Sunflower oil sunflower oil (once-refined, technical grade), spec., D 3169 (06.03) Sunlight/mouochromatic 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 viSuial evaluation, D 4449 (06.01) ' gloss of high-gloss metallic/nonmetallic surfaces, by goniophoto- metry, 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, D4417 (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 antifouling 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, 0 3259(06.01) Surface preparation--paints/related coatings Set Specimen preparation (for testing)--paints/related coatings preparation, of hot-dipped nonpassivated galvanized steel panels for testing paint/vamish/lacquer/related products, test, D 2201 (06.01) 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, D4227 (06.01) qualification ofjourneyman 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) Suspension fluids flash point (of feel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Sustained burning test 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, D4207 (06.03) Swelling clear/pigmented organic coatings, test, D 1308 (06.01) Swelling and cracking edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) Synthetic amyl alcohol amyl alcohol (synthetic), spec., D 319 (06.03) Synthetic black iron oxide (magnetite) See Iron oxide black Synthetic drying oils See Oils--drying Synthetic ethyihexanol ' See 2-Ethylhexanol Synthetic hematite (red) See Iron oxide red Synthetic phenolic resins See Resins--phenolic '> Synthetic pine oil See Oils--pine (uatural/synthetic) Synthetic primary amyl acetate '' See Primary amyl acetate _ ~~ Synthetic yellow won oxide See Iron oxide yellow T -- - - Tack apparent tack of printing inks/vehicles, by inkometer, test, D 4361 (06.01) Tag closed-cup tester flash point by Tag closed tester, test, D 56 (06.03) Tag open-cup tester flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Talc (pigment) See Magnesium silicate Tail oil/tall oil rosin tail oil, methods of testing,. D 803 (06.03) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D3008 (06.03) Tank cars/wagons/other shipping containers See Containers--tank cars/wagons Tanks cresylic acid and phenol, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handiing liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) 918 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, D3626 (06.03) TBC inhibitor p-fert-butylcatechol (TBC') in styrene monomer, test, D 2120 (06.03) residual p-tett-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, D 4797 (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 light-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 (oflatex paint films), test, D 3793 (06.01) minimum film formation temperature (MFFT) of emulsion vehicles, test, D 2354 (06.02) nonvolatile content oflatexes, test, D 4758 (06.02) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) solidification point of 4,4- isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) temperature of applied coatings on wood products during the caring cycle, by infrared radiation thermometers,, practice, D 3259 (06.01) Temperature tests--plastics operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Ten-degree xylene (10 xylol) See Xylene (ten-degree) Tension (tensile) properties/tests--paints/related coatings adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) paints/related coatings (free films), test, D 2370 (06.01) preparation of free films of organic coatings, practice, D4708(06.0I) Terminology--paints/related coatings/materials aromatic hydrocarbons/related chemicals, terminology, 0 4790(06.03) cellulose/cellulose derivatives, terminology, D1695 (06.02) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) paint/vamish/lacquer/related products, terminology, D16 (06.01, 06.02, 06.03) Terpene alcohols content sampling and testing pine oil, method, D 802 (06.03) Terpene solvents Sa Solvents (headings) sampling and testing dipentene, method, D 801 (06.03) Terra alba See Calcium sulfate content Term di sienna See Sienna (burnt and raw) Testing methods recording results on single-/multi-panel forms, method, A D1150 (06.01) Testing methods--paints/related coatings See Guides for testing paints/related coatings/materials Test samples sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Test specimens See Specimen preparation (for testing) (headings) 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 (06.01) Thermistor-type infrared radiation thermometers temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) Thermometers _ thermometer specifications for flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Thermoplastic traffic marking evaluation ofcolor for thermoplastic traffic marking materials, test, D.4960 (06.01) Thermoplastic traffic marking material chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D4451 (06.01) Thermosetting materials/properties--resins stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) Thermosetting phenol-formaldehyde See Phenolic resins Thickness--paints/related coatings/materials dry film thickness, of nonmagnetic coatings (paints/ vamish/lacquer) applied to a ferrous base, 01186 (06.01) dry film thickness of protective coating systems, by destructive means, test, D4138 (06.01) erosion testing of antifouling paints, using high velocity water,' test, D 4938 (06.01) producing films of uniform thickness of paint/varnish/related products on test panels, test, D 823 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D4939 (06.01) 919 "`73S3P3 . DUP050296479 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, D 1685 (06.03) Thiosulfate method chromium content of strontium chromate pigment, by thiosulfate method, test, D1845 (06.02) Thixotropy rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, 0 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, 04948(06.01) Tinting strength colored pigments (dry/pastes in oil), with a mechanical muller, test, D 387 (06.02) relative tinting strength of chromatic paints, test, 04838 (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, 0 332 (06;02) Titanium content white titanium pigments, chemical analysis, test, D1394 (06.02) Titanium dioxide slurries 1 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 (06D1) 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, 01394 (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 (06.03) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocarbons/related chemicals, terminology, 04790(06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, 0 4534 (06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) distillation, test, D 850 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) nitration grade toluene, spec., D 841 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06,03) satnpliog/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03), soluble cellulose nitrate, testing, methods, 0 301 (06.02) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D 2360 (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) xylene isomer analysis, by gas chromatography, test, 02306(06.03) Toluene insolubles content toluene-insoluble solid matter (sand/chips/dirt/baik) in rosin, test, D 269 (06.03) Toluidine red pure toluidine red toner, spec., 0 656 (06.02) Toluidine red pigment para red/toluidine red pigments, testing, D 970 (06.02) Toner (para/tofaidine red) para red/toluidine red pigments, testing, 0970 (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, 01394 (06.02) Toxicity/toxicology ~~ unreacted monomer content of latexes, by gas-liquid chromatography^ test, 0 4747 (06.02) Trace elements contents ' sulfur (trace quantities) in liquid aromatic hydrocarbons, by " oxidative microcoulometry, test, 3961 (06.03) Trace elements contents--chloride Sa Chloride content (headings) trace (tptal) chloride (oiganic/inorganic) in-liquid aromatic . hydrocarbons, test, 0 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 (06.01) Trace monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) 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 0868 (06.01) evaluating degree of chipping, A 0 913 (06.01) glass spheres in, test for roundness, D1155 (06.02) laboratory evaluation of degree of bleeding of traffic/pavement marking paint, test, 0 969 (06.01) 920 mm DUP050296480 Index of ASTM Standards, Section 6 Urethanes laboratory test for settling properties, during storage, 01309(06.01) methods of conducting road sendee tests on, D 713 (06.01) no-pick-up time (drying time), test, D 711 (06.01) pigment content of paint/traflic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) practices for testing, 0 2205 (06.01) sieve analysis ofglass spheres (for retroreflective pavements markings/industrial uses), test, 01214 (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, D 2743 (06.01) Transesterification identification of carboxylic acids in alkyd resins 0 2455 (06.02) Transfer efficiency (TE) 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, 05066(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, 0 5108 (06.01) Trichlorotriiluoroethane-extractable matter permanganate time of acetone/methanol, test, D1721 (06.03) unsaponifiable matter content, test, D1399 (06.03) Tricresy! 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, 049 (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) Turbidimetric method reporting particle size characteristics of pigments, practice, D1366 (06.02) Turbidity . resin solution dilutability, test, 0 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 solulion/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, 0 3806 (06.01) u Ultrafiltrates add/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) apparent pH of electracoat baths, test, D 4584 (06.01) electrical conductivity of electrocoat baths, test, D 4399 (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, 03256 (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/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) 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) 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., 0763 (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 cais/wagons/other shipping containers cresylic arid and phenol, practice, D 3852 (06.03) naphthalene, maleic/phthalic 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, D 4747 (06.02)-- unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) Unsaponifiable matter content alkyd resins and resin solutions, test, D1397 (06.02) rosin, test, 0 1065 (06.03) tall oil, methods of testing, 0 803 (06.03) tricresyl phosphate, test, 0 1399 (06.03) unsaponifiable matter in drying oils/fatty acids/polymerized fatty acids, test, 0 1965 (06.03) Unsatnration drying oils/derivatives total, by modified RosenmundKuhnhenn method, test, 0 1541 (06.03) drying oils/derivatives Wijs method, test, 01959 (06.03) Up and down method impact resistance of pipeline coatings, by falling weight test, G14 (06.01) Upper liquid layer amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, 04948(06.01) Urethanes isocyanate group content of urethane materials/prepolymeis, test, 02572(06.02) 921 DUP050296481 Index of ASTM Standards, Section 6 Urethanes unreacted toluene diisocyanates in urethane prepolymers/ coating solutions, by gas chromatography, test, 0 3432(06.02) Urethanes--coatings 2-ethoxyethyl acetate (99 % grade), spec., D 3728 (06.03) isocyanate group content of urethane materials/prepolymers, 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/iacquer/related products), test, D1613 (06.03) conducting tests on paint/vamish/iacquer/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/lacqueis/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, 0 822 (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) clear/pigmented organic coatings, test, 01308 (06.01) color of transparent liquids, by Gardner color scale, test, 0 1544 (06.01, 06.02, 06.03) discoloration (light stability), test, D 2620 (06.01) dried varnish films, test, D1647 (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) elasticity/toughness of varnishes, test, D 1642 (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, D 3278 (06.03) gas checking and draft test, D1643 (06.01) glacial acrylic acid (99.0 % grade), spec., D 4416 (06.03) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, 04287 (06.01) indentation hardness of organic coatings, by Knoop and Pfiind methods, test, 01474 (06.01) liquid paint driers, selection of test methods, D 564 (06.03) methyl -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, D 609 (06.01) paint/vamish/iacquer/related products, terminology, D 16 (06.01,06.02, 06.03) paint/vamish/iacquer/related products, test, A D1475 (06.01) preparation of free films of organic coatings, practice, 04708(06.01) preparing glass panels for testing, 0 3891 (06411) qualitative detection of rosin in varnishes, by IiebermanStorch/Halphen-Hicks tests, 01542 (06.01,06.02) rosin acids content, test, 01469 (06.02) sampling and testing shellac varnish, 01650 (06.02) selection and use of test procedures, 0 154 (06.01) specific gravity at 25/25C, test, 01963 (06.03) standard environments for conditioning/testing paint/ vamish/lacquer/related materials, spec., 03924 (06.01) steel surfaces, resistance to failure, by water immersion test, D 870 (06.01) testing water resistance ofcoatings at 100 % relative humidity, practice, 02247 (06.01) viscosity of paints/vamishes/lacquers, by Ford viscosity cup, test, 01200 (064)1) viscosity (of paints/vamishes/lacquers/related materials), by dip-type viscosity cups, test, 0 4212 (06.01) volatile content in phenolic resins, test, 0 4639 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D4209 (06.02) wet film thickness of organic coatings, 01212 (06.01) wet film thickness of organic coatings, by notched gages, practice, 0 4414 (06.01) Vegetable origin artists' paints (oil/resin-oil/alkyd), spec., 0 4302 (064)1) Vehicles nonvolatile content of printing inks/resin solutions/vehicles, test, D4713 (06.01) Vehicle separation--solvent-type paints amount of liquid separated as tipper layer from a viscous solution/dispersiOn containing dispersed solids, test, 04948(06.01) high-speed centrifuge, for pigment content, test, 0 2698 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, 0 2621 (06.01) pigment content of solvent-reducible paints, test, 0 2371 (064)1) vacuum distillation (for vehicle separation in solvent-type paints), practice, 0 3272 (06.01) vehicle separation from solvent-reducible paints,-by centrifuge, practice, 0 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, 0 2191 (06.03) acidity in vinyl acetate and acetaldehyde, test, 0 2086 (06.03) 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, 0 3680 (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, 04040 (06.01) BS0. DUP050296482 Index of ASTM Standards, Section 6 Volatile matter content Viscometers--Ford viscosity of paints/varaishes/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 Stormer/Saybolt Furol viscometers, test, 0856 (06.03) Viscometers--Stormer viscosity of pine tars/pine-tar oils, by Stormer/Saybolt Furol viscometers, test, D856 (06.03) Viscometers--Weissenberg Rheogonlometer viscosity of polymeric powders/powder coatings, test, 03451(06.01) Viscometers--Zahn coil coatings, testing, practice, D 3794 (06.01) Viscosity--paints/related coatings/materials cellulose acetate propionates/butyrate, test, A D817 (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/reiated 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, 01795 (06.02) raethylcellulose, test, O1347 (06.02) paints/varaishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) polymeric powders/powder coatings, by Weissenberg rheogoniometer, test, ID 3451 (06.01) resin solutions, test, D1725 (06.02) rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) rosin oil, test, 01131 (06.03) sodium glycolate content of sodium carboxymethylcellulose, 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, 0 803 (06.03) transparent liquids, by bubble-dome method, test, D1545 (06.01, 06.02,06.03) viscosity of cellulose derivatives, by ball-drop method, test, D1343 (06.02) viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) 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/vamishes/reiated products), by ICI cone/plate viscometer, test, D4287 (06.01) Viscous iiquids/materials flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) iiquid/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 maieic 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, 01686 (06.03) evaluating degree of bleeding of traffic/pavement marking paint, test, A D 868 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01) formability/adbesion of zinc-rich primer/chromate complex coatings (on steel), test, D4146 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, 04449 (06.01) gloss/sheen uniformity evaluation, test, 0 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, D3258 (06.01) relative tinting strength ofwhite pigments, by visual observation, test, D332 (06.02) solution color of4,4'-isopropylidenediphenol (dissolved in methanol), test, D4789 (06.83) 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, 05007 (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, Gil (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.ayailable for removal in a VOC control device (abatement), test, 0 5087 (06411) VOC calculation volatile organic content (VOC) of paints/related coatings, selecting test procedures, practice, 0 3960 (06.01) Volatile acids content sampling and testing pine tars/pine-tar oils, method, 0856(06.03) Volatile liquids low viscosity, rate of evaporation, test, 03539 (06.01) Volatile matter content calcium borosilicate, test, 0 4487 (06.02) cellulosics/emulsions/resin solutions/shellac/varnishes, selecting test procedures, practice, 0 4209 (06.02) driers/drying oils/naval stores and solvents, selecting test procedures, guide, 0 4140 (06.03) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, 0 280 (06.02) loss on heating of drying oils, test, 01960 (06.03) moisture content of pigments, 0 1208 (06.02) paint/raw paint material, practice, 0 2832 (06.01) paints (solvent-reducible), test, 0 2369 (06.01) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) 923 DUP0502 96483 Index of ASTM Standards, Section 6 Volatile matter content sampling/testing volatile solvents/chemical intermediates (for paints/lacquer/vamish/reJated material), selecting test methods, D 268 (06.03) volatile content in phenolic resins, test, 0 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/1,1,1 -trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D44S7(06.01) distillation range (between 30 and 350"C) of volatile organic liquids, test, D1078 (06.03) nonvolatile content in alanes/siloxanes/silane-sitoxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) nonvolatile content of resin solutions (in volatile organic solvents), test, D1259 (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, 0 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 350C) 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, 0 4942 (06.01) w WashabOity interior architectural coatings, test, D 3450 (063)1) practical washability of organic coatings, test, 0 4828 (06.01) Water water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 0 4942 (06.01) Water--high-purity/reagent-grade reagent water, spec., 0 1193 (06.03) Water--resistance See Resistance--water Water--sea water erosion testing of antifouling paints, using high velocity water, test, 04938(06.01) organotin release rates of antifouling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, 0 5108 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, O 4939 (06.01) Water absorption comparative corrosion preventive characteristics of materials used for joints/couplings/ftttings/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, D4938 (06.01) Watercolor paint Sa Artists' paints artists' watercolor paints, spec., 0 5067 (06.01) Water content--paints/related coatings/materials cresylic acid content (of alkaline cresylate solutions), chemical analysis, 0 3439 (06.03) fatty nitrogen compounds, test, 0 2072 (06.03) Karl Fischer reagent method, test, O 4017 (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), 04285 (06.01) phenol/related materials, by iodine reagent method, test, D1631 (06.03) water content of water-reducible paints, by direct injection into gas chromatograph, test, 0 3792 (06.01) water in liquid naval stores, test, 0 890 (06.03) water in volatile solvents, by Fischer reagent titration method, test, 0 1364(06.03) Water content--petroleum products water in petroleum products/bituminous materials, by distillation, test, 0 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-insoinble matter content apparent pH of water insoluble phenol-formaldehyde resin, test, 04613(063)2) hydrogen sulfide/sulfur dioxide (quantitative) of industrial' aromatic-hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D 1347 (06.02) Water miscibility Sa Miscibility water miscibility of water-soluble solvents, test, D1722 (06.03) Water of hydration calcium borosilicate, test, D 4487 (06.02) Water penetration water penetration into pipeline coatings, test, G 9 (06.01) Water pickup water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 0 4942 (06.01) Water-reducible coatings testing industrial water-reducible coatings, guide, 0 4712 (06.01) Water repellency wood products, qualitative test for, 0 2921 (06.01) Water resistance See Resistance--water Water-soluble-matter content conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, 0 4940 (06.01) moisture content of pigments, D1208 (06.02) painting inspectors (metal substrates), guide, D3276 (06.01) 924 D U P050296484 Index of ASTM Standards, Section 6 Wijs procedure--iodine value salt content of blue pigments, test, D1135 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet 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 of exterior 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, D5031 (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/vamshes/lacqudrs/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 of coatings, using water fog apparatus, practice, D1735 (06.01) Weathering--outdoor conducting exterior exposure tests of (exterior) paints on steel, test, D 1014 (06.01) conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D1006 (06.01). effects of outdoor weathering on pipeline coatings, test, G 11 (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) Weight 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, D 1555 (06.03) Weight--weight loss wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Weight--weight-per-gallon cup paint/vamish/lacquer/related products, test, A D1475 (06.01) Weight percent epoxide (WPEj epoxy content of epoxy resins, test, D 1652 (06.02) Weight solids calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Weissenberg rheogoniometer test viscosity of polymeric powders and powder coatings, practice, D 3451 (06.01) Welding/weids design/fabrication of flue gas desulfurization system components (for protective lining 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, D5007 (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/Lesded tine 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, I>3280 (06.02) antimony oxide content ofwhite pigment (separated from solvent-type paints), test, D2350 (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, 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 (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 (of low viscosity iiquid mixtures), by Wick test, D4207 (06.03) Wijs procedure--iodine value drying oils and their derivatives, test, D1959 (06.03) 925 aswww# DUP050296485 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, 04147 (06.01) Wolfe-potentiometrie method oleic acid content of tall oil rosin, test, D 1585 (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, 03259(66.01) wood used as panels in weathering tests of coatings, spec., 0358 (06.01) Wood and wood products--cellulose pulp metals (iron/copper/manganese/calcium) content ofcellulose pulp (from wood/cottonj, by atomic spectrophotometry, test, 0 4085 (06.02) pentosans content of cellulose, test, D 1787 (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, 02691(06.01) factory-primed, durability and compatibility, with finish coatings, test, D 2830 (06.01) humid-dry cycling (for coatings on wood/wood products), method, D 3459 (06.01) specifying properties of paint from the Squid state through the curing stage for factory applied coatings bn 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-are type) with/ without water for exposure of nonmetaliic 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/xyienes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color, test, D 848 (06.03) aromatic hydrocarbons/related chemicals, terminology, 0 4790(06.03) distillation, test, D 850 (06.03) flash/fire point of liquids, by Tag open-cup apparatus, test, D 1310 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D5060 (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) 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, 01555(06.03) xylene isonier analysis, by gas chromatography, test, D 2306 (06.03) xylenes for p-xyiene feedstock, spec., D 5211 (06.03) meta-Xylene apparent density of industrial aromatic hydrocarbons, test, D 2935(06.03) commercial density (of pure liquid chemicals), test, 03505(06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) ortho-Xylene apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) commercial density (of pure liquid chemicals), test, 0 3505(06.03) purity, by gas chromatography, test, D 3797 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) oxylene 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/inoiganic) in liquid-aromatic hydrocarbons, test, O 5194 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) xylenes for p-xylene feedstock, spec., D 5211 (06.03) Xylene (five-degree) xylene isomer analysis, by gas chromatography, test, 0 2306(06.03) - Xylene (mixed) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) --. ' commercial density (of pure liquid chemicals), test, 03505(003) volume/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 (06.03) Xylene (ten-degree) xylene isomer analysis, by gas chromatography, test; 02306(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., 0211 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, O 126 (06.02) 926 *w L DUP050296486 Index of ASTM Standards, Section 6 Yield value laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) z Zahn viscometers See Viscometers--Zahn Zeisel technique 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, 0 3876(06.02) Zinc liquid paint driers, selection of test methods, D 564 (06.03) Zinc chromate (yellow) analysis, D 444 (06.02) zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Zinc-coated (galvanized) surfaces preparation for painting, practice, D 2092 (06.01) Zinc content analysis of white zinc pigments, test, D 3280 (06.02) paint driers, by EDTA method, test, D 2613 (06.03) zinc dust (metallic zinc powder), test, D 521 (06.02) zinc yellow (zinc chromate yellow) pigment, test, D 444 (06.02) Zinc driers See Driers ZTO chromate Sa Oils--drying Zinc dust Sa Pigments (general properties) analysis, D 521 (06.02) zinc dust pigment, spec., D 520 (06.02) Zinc hydroxy phosphite analysis, D4450 (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 (inoiganic) 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, D 3969 (06.03) ZTO chromate See Zinc chromate (yellow) DUP050296487 1916 Race Street Philadelphia, PA 19103 Phone: (215) 299-5454 FAX: (215) 977-9679 European Office 27-29 Knowl Piece, Wiibury Way Hitchin, Herts SG4 OSX, England Phone: 0462-437933 FAX: 0462-433678 %m mmmmmP' mmcmwm THIS APPLICATION IS FOR SOCIETY MEMBERSHIP ONLY. 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