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ASTM D1613-02

(Test Method)

Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products

Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products

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 For purposes of determining conformance of an observed value or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
1.3 For specific hazard information and guidance consult supplier's Material Safety Data Sheet.
1.4 This standard does not purport to address the safety concerns, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
09-Jul-2002
ICS
87.060.30 - Solvents
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.35 - Solvents, Plasticizers, and Chemical Intermediates
Current Stage
Ref Project

Relations

Replaces
ASTM D1613-96(1999) - Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products
Effective Date
10-Jul-2002
Replaced By
ASTM D1613-03 - Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products
Effective Date
01-Oct-2003
Referred By
ASTM D4836-09(2023) - Standard Specification for Dipropylene Glycol Monomethyl Ether
Effective Date
10-Jul-2002
Referred By
ASTM D7713-18 - Standard Specification for Aqueous Engine Coolant Grade Glycol (53 % by Volume Nominal)
Effective Date
10-Jul-2002
Referred By
ASTM E202-18 - Standard Test Methods for Analysis of Ethylene Glycols and Propylene Glycols
Effective Date
10-Jul-2002
Referred By
ASTM D2916-09(2023) - Standard Specification for Isophorone
Effective Date
10-Jul-2002
Referred By
ASTM D7388-23 - Standard Specification for Engine Coolant Grade 1,3-Propanediol (PDO)
Effective Date
10-Jul-2002
Referred By
ASTM D3128-07(2021) - Standard Specification for 2-Methoxyethanol
Effective Date
10-Jul-2002
Referred By
ASTM D5008-22 - Standard Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol By Gas Chromatography
Effective Date
10-Jul-2002
Referred By
ASTM D330-07(2021) - Standard Specification for 2-Butoxyethanol
Effective Date
10-Jul-2002
Referred By
ASTM D331-11(2019) - Standard Specification for 2-Ethoxyethanol<sup>,</sup>
Effective Date
10-Jul-2002
Referred By
ASTM D3893-03(2023) - Standard Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by Gas Chromatography
Effective Date
10-Jul-2002
Referred By
ASTM D4360-11(2019) - Standard Specification for Methyl <emph type="bdit">n</emph>-Amyl Ketone
Effective Date
10-Jul-2002
Referred By
ASTM D3131-07(2021) - Standard Specification for Isopropyl Acetate (99 % Grade)
Effective Date
10-Jul-2002
Referred By
ASTM D1718-09(2023) - Standard Specification for Isobutyl Acetate (95 % Grade)
Effective Date
10-Jul-2002

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ASTM D1613-02 - Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related ProductsASTM D1613-02 - Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products
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ASTM D1613-02 - Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products
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Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1613 – 02
Standard Test Method for
Acidity in Volatile Solvents and Chemical Intermediates
1
Used in Paint, Varnish, Lacquer, and Related Products
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 standard has been approved for use by agencies of the Department of Defense.
1. Scope * 3. Summary of Test Method
1.1 This test method covers the determination of total 3.1 The specimen is mixed with either an equal volume of
acidity as acetic acid, in concentrations below 0.05 %, in water or an equal volume of alcohol, and titrated with aqueous
organic compounds and hydrocarbon mixtures used in paint, sodium hydroxide solution to the phenolphthalein end point.
varnish, and lacquer solvents and diluents. It is known to be
4. Significance and Use
applicable to such mixtures as low molecular weight saturated
and unsaturated alcohols, ketones, ethers, esters, hydrocarbon 4.1 This test method is useful for determining low levels of
acidity, below 0.05 %, in organic compounds and hydrocarbon
diluents, naphtha, and other light distillate petroleum fractions.
1.2 For purposes of determining conformance of an ob- mixtures. The total acidity is calculated as acetic acid or
milligrams of sodium hydroxide per gram of sample.
served value or a calculated value using this test method to
relevant specifications, test result(s) shall be rounded off “to 4.2 Acidity may be present as a result of contamination,
decomposition during storage or distribution, or manufacture.
the nearest unit” in the last right-hand digit used in expressing
the specification limit, in accordance with the rounding-off This test method may be used in assessing compliance with a
specification.
method of Practice E 29.
1.3 For specific hazard information and guidance consult
5. Apparatus
supplier’s Material Safety Data Sheet.
5.1 Buret, 10-mL, graduated in 0.05-mL subdivisions.
1.4 This standard does not purport to address the safety
5.2 Erlenmeyer Flask, 250-mL capacity.
concerns, if any, associated with its use. It is the responsibility
of whoever uses this standard to consult and establish appro-
6. Purity of Reagents
priate safety and health practices and determine the applica-
6.1 Reagent grade chemicals shall be used in all tests.
bility of regulatory limitations prior to use.
Unless otherwise indicated, it is intended that all reagents shall
2. Referenced Documents
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
2.1 ASTM Standards:
6
2
specifications are available. Other grades may be used pro-
D 770 Specification for Isopropyl Alcohol
3
vided it is first ascertained that the reagent is of sufficiently
D 1193 Specification for Reagent Water
high purity to permit its use without lessening the accuracy of
E 200 Practice for Preparation, Standardization, and Stor-
the determination.
age of Standard and Reagent Solutions for Chemical
4
6.2 Unless otherwise indicated, references to water shall be
Analysis
understood to mean reagent water conforming to Type IV of
E 29 Practice for Using Significant Digits in Test Data to
5
Specification D 1193.
Determine Conformance with Specifications
7. Reagents
7.1 Alcohols, refined, ethyl or isopropyl.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
NOTE 1—Isopropyl alcohol (99 % grade) conforming to Specification
and Related Coatings, Materials, and Applications and is the direct responsibility of
D 770, or 190 proof ethyl alcohol conforming to formula No. 3A of the
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved July 10, 2002. Published September 2002. Originally
published as D 1613 – 64 T. Last previous edition D 1613 – 96 (1999).
6
Reagent Chemicals, American Chemical Society Specifications, American
2
Annual Book of ASTM Standards, Vol 06.04.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
Annual Book of ASTM Standards, Vol 11.01.
listed by the American Chemical Society, see Analar Standards for Laboratory
4
Annual Book of ASTM Standards, Vol 15.05.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5
Annual Book of ASTM Standards, Vol 14.02.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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Standard Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products

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ASTM D804-12(2022)(Terminology)
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1.1 Although the pine chemical industry has been a continuing producer of chemical products for many centuries, the nature of the industry, its products, and its terminology have changed. In particular, the original practice of recovering pine chemical through the processing of the exudate from pine trees has been supplemented by their extraction by solvent products of the wood pulping industry. For many years the industry was known as the Naval Stores industry but that term has gradually been replaced by the more descriptive and meaningful term, Pine Chemicals Industry. Thus, this terminology contains some old terms now mostly of historic value, together with the terms of the modern pine chemical industry.2  
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ASTM D6438-05(2022)(Test Method)
Standard Test Method for Acetone, Methyl Acetate, and Parachlorobenzotrifluoride Content of Paints, and Coatings by Solid Phase Microextraction-Gas Chromatography

SIGNIFICANCE AND USE
5.1 In order to calculate the volatile organic content (VOC) of paints containing EPA exempt solvents, it is necessary to know the acetone, methyl acetate, or parachlorobenzotrifluoride content. This gas chromatographic test method provides a simple and direct way for measuring these solvents. Each analyte is measured with respect to a unique internal standard. For acetone, the internal standard used is acetone-d6, for methyl acetate it is methyl acetate-d3, and for PCBTF it is metachlorobenzotrifluoride (MCBTF). These unique analyte/internal standard pairs behave very nearly as single solvents with respect to evaporation rate and adsorption rate onto a coated silica fiber (SPME) but are separable on a gas chromatograph (GC) capillary column. The only critical analytical technique required for successfully performing this test method is the ability of an analyst to weigh a paint sample and internal standard, corresponding to the analyte of interest, into a septum capped vial. After weighing, solvent evaporation has no effect on the final value of the determination. Since whole paint is not injected into the gas chromatograph, the analytical system is never compromised.
SCOPE
1.1 This test method is for the determination of acetone, methyl acetate, or parachlorobenzotrifluoride (PCBTF), or combination of any of the three, in paints and coatings, by solid phase microextraction (SPME) headspace sampling, and subsequent injection into a gas chromatograph. It has been evaluated for cellulose nitrate, acrylic, and urethane solvent-borne systems. The established working range of this test method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %; parachlorobenzotrifluoride, 10 to 17 %. There is no reason to believe that it will not work outside these ranges. A minor modification of this test method would make it suitable for the analysis of the same analytes in water-borne coatings (see Note 1).
Note 1: Water-borne paints are internally standardized and diluted with water followed by addition of solid sodium chloride.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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