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ASTM D3257-97

(Test Method)

Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography

Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography

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 210oC (300 to 410oF) 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 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 and health practices and determine the applicability of regulatory limitations prior to use.
1.6 For hazard information and guidance, see the supplier's Material Safety Data Sheet.

General Information

Status
Historical
Publication Date
09-Jun-2001
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

Replaced By
ASTM D3257-01 - Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography
Effective Date
10-Jun-2001
Referred By
ASTM D235-22 - Standard Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)
Effective Date
10-Jun-2001
Referred By
ASTM D268-22 - Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
Effective Date
10-Jun-2001
Referred By
ASTM D3735-22 - Standard Specification for VM&P Naphthas
Effective Date
10-Jun-2001

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ASTM D3257-97 - Standard Test Methods for Aromatics in Mineral Spirits by Gas ChromatographyASTM D3257-97 - Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography
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ASTM D3257-97 - Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3257 – 97
Standard Test Methods for
1
Aromatics in Mineral Spirits by Gas Chromatography
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 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 bility of regulatory limitations prior to use.
1.6 For hazard information and guidance, see the supplier’s
1.1 These test methods cover the determination of ethylben-
Material Safety Data Sheet.
zene and total eight-carbon (C ) and heavier aromatics in the
8
concentration range from 0.1 to 30 % in mineral spirits having
2. Referenced Documents
a distillation range from 149 to 210°C (300 to 410°F) as
2.1 ASTM Standards:
determined by Test Method D 86. The procedures permit the
2
D 86 Test Method for Distillation of Petroleum Products
identification and calculation of concentrations of aromatic
E 180 Practice for Determining the Precision of ASTM
components to 0.1 volume %.
3
Methods for Analysis and Testing of Industrial Chemicals
1.2 It is recognized by analytical chemists that a single
4
E 260 Practice for Packed Column Gas Chromatography
column gas chromatography analysis of an unknown sample is
risky. In such cases, multiple and different analytical tech-
3. Summary of Test Methods
niques must be used for absolutely positive identification, for
3.1 The material, with an internal standard, is introduced
example, several different gas chromatography columns, gas
into a gas chromatographic column containing a strongly polar
chromatography/mass spectrometer, or gas chromatography/
liquid phase. The polar phase has very little affinity for
infrared, etc. In these test methods the material is known and is
saturated and olefinic hydrocarbons while exhibiting a pro-
clearly defined.
nounced retention of aromatics. This selectivity, which is
1.3 Oxygenated compounds, if present, may interfere and
illustrated in Fig. 1, results in the elution of all saturated and
cause erroneous results. Such oxygenated compounds are not
olefinic hydrocarbons in the products described above prior to
normally present in mineral spirits.
the elution of toluene. Either a thermal conductivity or flame
1.4 Three test methods are covered as follows:
ionization detector may be used. Calibration is obtained in Test
1.4.1 Test Method A, measurement of ethylbenzene content,
Method A and C from a synthetic blend of the most important
C plus higher aromatics (except ethylbenzene), and total
8
aromatic compounds. Internal standards are used in all three
aromatics by means of a single packed column gas chromato-
test methods. Typical chromatograms are shown in Fig. 2 and
graphic analysis.
Fig. 3.
1.4.2 Test Method B, measurement of ethylbenzene content
by means of a rapid packed column gas chromatographic
NOTE 1—Refer to Practice E 260 for additional information on gas
analysis. chromatography techniques.
1.4.3 Test Method C, measurement of ethylbenzene content,
4. Significance and Use
C plus higher aromatics (except ethylbenzene) and total
8
4.1 These test methods were developed to measure the types
aromatics by means of a capillary column gas chromatographic
and amounts of aromatics in mineral spirits to determine
analysis.
compliance with air pollution regulations that restrict the
1.5 This standard does not purport to address all of the
aromatic content of solvents. They have been demonstrated to
safety concerns, if any, associated with its use. It is the
be workable and to produce accurate results. However, due to
responsibility of the user of this standard to establish appro-
the sensitivity of the tests to operating variables, some labora-
priate safety and health practices and determine the applica-
tories having limited experience with gas chromatographic
1
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and are the direct responsibility
2
of Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Annual Book of ASTM Standards, Vol 05.01.
3
Current edition approved June 10, 1997. Published September 1997. Originally Annual Book of ASTM Standards, Vol 15.05.
e1 4
published as D 3257 – 73. Last previous edition D 3257 – 93 . Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 3257
FIG. 1 Typical Resolution of Test Blend Using Packed Column
FIG. 2 Typical Packed Column Chromatogram of Mineral Spirits
...

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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).
Note 1: Water-borne paints are internally standardized and diluted with water followed by addition of solid sodium chloride.  
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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.  
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