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ASTM D3257-22

(Test Method)

Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography

Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography

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 experience with gas chromatographic analyses of hydrocarbons may experience difficulty in performing the tests.
SCOPE
1.1 These test methods cover the determination of ethylbenzene and total eight-carbon (C8) and heavier aromatics in the concentration range from 0.1 to 30 % in mineral spirits having a distillation range from 149 to 210 °C (300 to 410 °F) as determined by Test Method D86. The procedures permit the identification and calculation of concentrations of aromatic components to 0.1 volume %.  
1.2 It is recognized by analytical chemists that a single column gas chromatography analysis of an unknown sample is risky. In such cases, multiple and different analytical techniques must be used for absolutely positive identification, for example, several different gas chromatography columns, gas chromatography/mass spectrometer, or gas chromatography/infrared, etc. In these test methods the material is known and is clearly defined.  
1.3 Oxygenated compounds, if present, may interfere and cause erroneous results. Such oxygenated compounds are not normally present in mineral spirits.  
1.4 Three test methods are covered as follows:  
1.4.1 Test Method A, measurement of ethylbenzene content, C8 plus higher aromatics (except ethylbenzene), and total aromatics by means of a single packed column gas chromatographic analysis.  
1.4.2 Test Method B, measurement of ethylbenzene content by means of a rapid packed column gas chromatographic analysis.  
1.4.3 Test Method C, measurement of ethylbenzene content, C8 plus higher aromatics (except ethylbenzene) and total aromatics by means of a capillary column gas chromatographic analysis.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.6 For purposes of determining conformance of an observed 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 E29.  
1.7 For hazard information and guidance, see the supplier’s Material Safety Data Sheet.  
1.8 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.  
1.9 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.

General Information

Status
Published
Publication Date
31-Dec-2021
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

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ASTM D3257-22 - Standard Test Methods for Aromatics in Mineral Spirits by Gas ChromatographyASTM D3257-22 - Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography
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ASTM D3257-22 - Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography
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Standards Content (Sample)

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.
Designation: D3257 − 22
Standard Test Methods for
1
Aromatics in Mineral Spirits by Gas Chromatography
This standard is issued under the fixed designation D3257; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 1.6 For purposes of determining conformance of an ob-
served or a calculated value using this test method to relevant
1.1 Thesetestmethodscoverthedeterminationofethylben-
specifications, test result(s) shall be rounded off “to the nearest
zene and total eight-carbon (C ) and heavier aromatics in the
8
unit” in the last right-hand digit used in expressing the
concentration range from 0.1 to 30% in mineral spirits having
specificationlimit,inaccordancewiththerounding-offmethod
a distillation range from 149 to 210°C (300 to 410°F) as
of Practice E29.
determined by Test Method D86. The procedures permit the
identification and calculation of concentrations of aromatic
1.7 For hazard information and guidance, see the supplier’s
components to 0.1 volume%.
Material Safety Data Sheet.
1.2 It is recognized by analytical chemists that a single
1.8 This standard does not purport to address all of the
column gas chromatography analysis of an unknown sample is
safety concerns, if any, associated with its use. It is the
risky. In such cases, multiple and different analytical tech-
responsibility of the user of this standard to establish appro-
niques must be used for absolutely positive identification, for
priate safety, health, and environmental practices and deter-
example, several different gas chromatography columns, gas
mine the applicability of regulatory limitations prior to use.
chromatography/mass spectrometer, or gas chromatography/
1.9 This international standard was developed in accor-
infrared,etc.Inthesetestmethodsthematerialisknownandis
dance with internationally recognized principles on standard-
clearly defined.
ization established in the Decision on Principles for the
1.3 Oxygenated compounds, if present, may interfere and
Development of International Standards, Guides and Recom-
cause erroneous results. Such oxygenated compounds are not
mendations issued by the World Trade Organization Technical
normally present in mineral spirits.
Barriers to Trade (TBT) Committee.
1.4 Three test methods are covered as follows:
1.4.1 Test Method A, measurement of ethylbenzene content, 2. Referenced Documents
C plus higher aromatics (except ethylbenzene), and total
8 2
2.1 ASTM Standards:
aromatics by means of a single packed column gas chromato-
D86Test Method for Distillation of Petroleum Products and
graphic analysis.
Liquid Fuels at Atmospheric Pressure
1.4.2 Test Method B, measurement of ethylbenzene content
E29Practice for Using Significant Digits in Test Data to
by means of a rapid packed column gas chromatographic
Determine Conformance with Specifications
analysis.
E180Practice for Determining the Precision of ASTM
1.4.3 Test Method C, measurement of ethylbenzene content,
Methods for Analysis and Testing of Industrial and Spe-
C plus higher aromatics (except ethylbenzene) and total
8 3
cialty Chemicals (Withdrawn 2009)
aromaticsbymeansofacapillarycolumngaschromatographic
E260Practice for Packed Column Gas Chromatography
analysis.
2.2 ASTM Adjuncts:
1.5 The values stated in SI units are to be regarded as the
4
D2PP Determination of Precision and Bias Data
standard. The values given in parentheses are for information
only.
1 2
These test methods are under the jurisdiction of ASTM Committee D01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Paint and Related Coatings, Materials, and Applications and are the direct contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
responsibility of Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Standards volume information, refer to the standard’s Document Summary page on
Intermediates. the ASTM website.
3
Current edition approved Jan. 1, 2022. Published January 2022. Originally The last approved version of this historical standard is referenced on
approved in 1973. Last previous edition approved in 2012 as D3257–06 (2012) www.astm.org.
4
which was withdrawn January 2021 and reinstated in January 2022. DOI: 10.1520/ Available from ASTM International Headquarters. Order Adjunct No.
D3257-22. ADJD6300.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C70
...

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SCOPE
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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.
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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).
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4.1 Benzene is classed as a toxic and carcinogenic material. A knowledge of the concentration of this compound may be an aid in evaluating the possible health hazards to persons handling and using hydrocarbon solvents, but this test method is not intended to evaluate such hazards.
SCOPE
1.1 This test method covers the determination by gas chromatography of benzene at levels from 0.01 to 1 volume % in hydrocarbon solvents.
Note 1: For benzene levels lower than 0.01 volume %, use Test Method D6229.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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