ASTM D6438-05(2015)

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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-May-2015
• ICS: 87.060.30 - Solvents
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6438 −05 (Reapproved 2015)
Standard Test Method for
Acetone, Methyl Acetate, and Parachlorobenzotrifluoride
Content of Paints, and Coatings by Solid Phase
1
Microextraction-Gas Chromatography
This standard is issued under the fixed designation D6438; 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 Methyl Acetate or t-Butyl Acetate Content of Solvent-
borne and Waterborne Paints, Coatings, Resins, and Raw
1.1 This test method is for the determination of acetone,
Materials by Direct Injection Into a Gas Chromatograph
methyl acetate, or parachlorobenzotrifluoride (PCBTF), or
E180 Practice for Determining the Precision of ASTM
combinationofanyofthethree,inpaintsandcoatings,bysolid
Methods for Analysis and Testing of Industrial and Spe-
phase microextraction (SPME) headspace sampling, and sub-
3
cialty Chemicals (Withdrawn 2009)
sequent injection into a gas chromatograph. It has been
evaluated for cellulose nitrate, acrylic, and urethane solvent-
3. Terminology
borne systems. The established working range of this test
method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %; 3.1 Abbreviations:
parachlorobenzotrifluoride, 10 to 17 %. There is no reason to
3.1.1 PCBTF—parachlorobenzotrifluoride
believe that it will not work outside these ranges. A minor (4-chlorobenzotrifluoride)
modification of this test method would make it suitable for the
3.1.2 MCBTF—metachlorobenzotrifluoride
analysisofthesameanalytesinwater-bornecoatings(seeNote
(3-chlorobenzotrifluoride)
1).
3.1.3 SPME—solid phase microextraction
NOTE 1—Water-borne paints are internally standardized and diluted
3.1.4 VOC—volatile organic compound
with water followed by addition of solid sodium chloride.
3.1.5 PEG/DVB—polyethylene glycol/divinylbenzene
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3.1.6 FID—flame ionization detector
standard.
3.1.7 MS—mass selective or mass spectral
1.3 This standard does not purport to address all of the
3.1.8 SIM—selected ion monitoring
safety concerns, if any, associated with its use. It is the
3.1.9 GC—gas chromatograph
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1.10 Sr—repeatability standard deviations
bility of regulatory limitations prior to use.
3.1.11 SR—reproducibility standard deviations
3.1.12 r—repeatability, 95 % confidence limit
2. Referenced Documents
3.1.13 R—reproducibility, 95 % confidence limit
2
2.1 ASTM Standards:
D3925 Practice for Sampling Liquid Paints and Related
4. Summary of Test Method
Pigmented Coatings
4.1 A suitable aliquot of whole solvent-borne paint is
D6133 Test Method for Acetone, p-Chlorobenzotrifluoride,
internally standardized and diluted with dioctyl phthalate. The
headspace of this solution is sampled with an SPME fiber,
1
which is then thermally desorbed in the injection port of a gas
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
chromatograph onto a suitable capillary column. Either a flame
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
ionization or mass specific detector may be used to measure
Current edition approved June 1, 2015. Published June 2015. Originally
peak areas of analytes and internal standards.
approved in 1999. Last previous edition approved in 2010 as D6438 – 05 (2010).
DOI: 10.1520/D6438-05R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6438−05 (2015)
TABLE 1 FID Instrument Conditions TABLE 2 MS Instrument Conditions
Detector: Flame ionization Detector: Electron ionization or mass selective
Column: 60m×0.25mm100%polyethylene glycol, 0.5-µm Detection Mode: Selected ion monitoring (SIM) of ions m/e 58, 64,
film thickness 74, 77, and 180
Carrier Gas: Helium Dwell Time: 100 milliseconds or less
Flow Rage: 1.0 mL per minute (20 cm per second) Solvent Delay: 0.0 min
Split Ratio: 200 to 1 Column: 25m×0.20mm5% phenyl/95 % methyl
A
Fiber desorption time: 5 to 6 s polydimethylsiloxane
Temperature, ° C Carrier
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6438 − 05 (Reapproved 2010) D6438 − 05 (Reapproved 2015)
Standard Test Method for
Acetone, Methyl Acetate, and Parachlorobenzotrifluoride
Content of Paints, and Coatings by Solid Phase
1
Microextraction-Gas Chromatography
This standard is issued under the fixed designation D6438; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings
D6133 Test Method for Acetone, p-Chlorobenzotrifluoride, Methyl Acetate or t-Butyl Acetate Content of Solventborne and
Waterborne Paints, Coatings, Resins, and Raw Materials by Direct Injection Into a Gas Chromatograph
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
3. Terminology
3.1 Abbreviations:
3.1.1 PCBTF—parachlorobenzotrifluoride,parachlorobenzotrifluoride
(4-chlorobenzotrifluoride)
3.1.2 MCBTF—metachlorobenzotrifluoride
(3-chlorobenzotrifluoride)
3.1.3 SPME—solid phase microextraction
3.1.4 VOC—volatile organic compound
3.1.5 PEG/DVB—polyethylene glycol/divinylbenzene
3.1.6 FID—flame ionization detector
3.1.7 MS—mass selective or mass spectral
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Dec. 1, 2010June 1, 2015. Published December 2010June 2015. Originally approved in 1999. Last previous edition approved in 20052010 as
D6438 – 99 (2005).D6438 – 05 (2010). DOI: 10.1520/D6438-05R10.10.1520/D6438-05R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6438 − 05 (2015)
3.1.8 SIM—selected ion monitoring
3.1.9 GC—gas chromatograph
3.1.10 Sr—repeatability standard deviations
3.1.11 SR—reproducibility standard deviations
3.1.12 r—repeatability, 95 % confidence limit
3.1.13 R—reproducibility, 95 % confidence limit
4. Summary of Test Method
4.1 A suitable aliquot of whole solvent-borne paint is internally standardized and diluted with dioctyl phthalate. The headspace
of this solution is sampled with an SPME fiber, which is then thermally desorbed in the injection port of a gas chromatograph onto
a suitable capillary column. Either a flame ionization or mass specific detector may be used to measure peak areas of analytes and
internal standards.
5. Significance and Use
5.1 In order to calculate the volatile organic content (VOC) of paints containing EPA exempt solvents, it is
...