ASTM D6438-05
(Test Method)Standard Test Method for Acetone, Methyl Acetate, and Parachlorobenzotrifluoride Content of Paints, and Coatings by Solid Phase Microextraction-Gas Chromatography
Standard Test Method for Acetone, Methyl Acetate, and Parachlorobenzotrifluoride Content of Paints, and Coatings by Solid Phase Microextraction-Gas Chromatography
SIGNIFICANCE AND USE
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
Relations
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
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 and Waterborne Paints, Coatings, Resins, and Raw Mate-
rials by Direct Injection Into a Gas Chromatograph
1.1 This test method is for the determination of acetone,
E180 Practice for Determining the Precision of ASTM
methyl acetate, or parachlorobenzotrifluoride (PCBTF), or
Methods for Analysis and Testing of Industrial and Spe-
combinationofanyofthethree,inpaintsandcoatings,bysolid
3
cialty Chemicals
phase microextraction (SPME) headspace sampling, and sub-
sequent injection into a gas chromatograph. It has been
3. Terminology
evaluated for cellulose nitrate, acrylic, and urethane solvent-
3.1 Abbreviations:
borne systems. The established working range of this test
3.1.1 PCBTF—parachlorobenzotrifluoride,
method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %;
(4-chlorobenzotrifluoride)
parachlorobenzotrifluoride, 10 to 17 %. There is no reason to
3.1.2 MCBTF—metachlorobenzotrifluoride
believe that it will not work outside these ranges. A minor
(3-chlorobenzotrifluoride)
modification of this test method would make it suitable for the
3.1.3 SPME—solid phase microextraction
analysisofthesameanalytesinwater-bornecoatings(seeNote
3.1.4 VOC—volatile organic compound
1).
3.1.5 PEG/DVB—polyethylene glycol/divinylbenzene
NOTE 1—Water-borne paints are internally standardized and diluted
3.1.6 FID—flame ionization detector
with water followed by addition of solid sodium chloride.
3.1.7 MS—mass selective or mass spectral
1.2 The values stated in SI units are to be regarded as
3.1.8 SIM—selected ion monitoring
standard. No other units of measurement are included in this
3.1.9 GC—gas chromatograph
standard.
3.1.10 Sr—repeatability standard deviations
1.3 This standard does not purport to address all of the
3.1.11 SR—reproducibility standard deviations
safety concerns, if any, associated with its use. It is the
3.1.12 r—repeatability, 95 % confidence limit
responsibility of the user of this standard to establish appro-
3.1.13 R—reproducibility, 95 % confidence limit
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 A suitable aliquot of whole solvent-borne paint is
2. Referenced Documents
internally standardized and diluted with dioctyl phthalate. The
2
2.1 ASTM Standards:
headspace of this solution is sampled with an SPME fiber,
D3925 Practice for Sampling Liquid Paints and Related
which is then thermally desorbed in the injection port of a gas
Pigmented Coatings
chromatograph onto a suitable capillary column. Either a flame
D6133 Test Method for Acetone, p-Chlorobenzotrifluoride,
ionization or mass specific detector may be used to measure
MethylAcetateor t-ButylAcetateContentofSolventborne
peak areas of analytes and internal standards.
5. Significance and Use
5.1 In order to calculate the volatile organic content (VOC)
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
of paints containing EPA exempt solvents, it is necessary to
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
know the acetone, methyl acetate, or parachlorobenzotrifluo-
Current edition approved July 1, 2005. Published July 2005. Originally approved
ride content. This gas chromatographic test method provides a
in 1999. Last previous edition approved in 1999 as D6438 – 99. DOI: 10.1520/
simple and direct way for measuring these solvents. Each
D6438-05.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. 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
TABLE 1 FID Instrument Conditions TABLE 2 MS Instrument Conditions
Detector: Flame ionization Detector: Electron ionization or mass selective
Column: 60 m 3 0.25 mm 100 % polyethylene glycol, 0.5-µm Detection Mode: Selected ion monitoring (SIM) of ions m/e 58, 64,
film thic
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.