ASTM D6133-02(2021)

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:D6133 −02 (Reapproved 2021)
Standard 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
This standard is issued under the fixed designation D6133; 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 D3271 Practice for Direct Injection of Solvent-Reducible
Paints Into a Gas Chromatograph for Solvent Analysis
1.1 This test method is for the determination of the total-
(Withdrawn 2019)
concentration of acetone, p-chlorobenzotrifluoride, methyl
D3272 Practice for Vacuum Distillation of Solvents From
acetate, or t-butyl acetate, or combination of any of the four, in
Solvent-Reducible Paints For Analysis (Withdrawn
solvent-reducible and water-reducible paints, coatings, resins,
2008)
and raw materials. Because unknown compounds that co-elute
D6438 Test Method for Acetone, Methyl Acetate, and
with the analyte being measured or with the internal standard,
Parachlorobenzotrifluoride Content of Paints, and Coat-
will lead to erroneous results, this test method should only be
ings by Solid Phase Microextraction-Gas Chromatogra-
used for materials of known composition so that the possibility
phy
of interferences can be eliminated. The established working
E177 Practice for Use of the Terms Precision and Bias in
range of this test method is from 1 % to 100 % for each analyte
ASTM Test Methods
by weight.
E691 Practice for Conducting an Interlaboratory Study to
1.2 The values stated in SI units are to be regarded as
Determine the Precision of a Test Method
standard. No other units of measurement are included in this
standard.
3. Summary of Test Method
1.3 This standard does not purport to address all of the
3.1 A suitable aliquot of whole paint is internally
safety concerns, if any, associated with its use. It is the
standardized, diluted with an appropriate solvent, and then
responsibility of the user of this standard to establish appro-
injected into a gas chromatographic column that separates the
priate safety, health, and environmental practices and deter-
chosen analytes from other volatile components. The analyte
mine the applicability of regulatory limitations prior to use.
content is determined from area calculations of the materials
1.4 This international standard was developed in accor-
producing peaks on the chromatogram.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 4. Significance and Use
Development of International Standards, Guides and Recom-
4.1 With the need to calculate volatile organic content
mendations issued by the World Trade Organization Technical
(VOC) of paints, and with acetone, p-chlorobenzotrifluoride,
Barriers to Trade (TBT) Committee. 4
methyl acetate and t-butyl acetate considered as exempt
volatile compounds, it is necessary to know the content of
2. Referenced Documents
these analytes. This gas chromatographic test method provides
2.1 ASTM Standards:
a relatively simple and direct way to determine their content.
However, because the detectors used in this test method are not
selective, and because some coatings are very complex
This test method is under the jurisdiction of ASTM Committee D01 on Paint
mixtures,compoundsmaybepresentinthesamplethatcoelute
and Related Coatings, Materials, andApplications and is the direct responsibility of
with the analyte, giving a result that is erroneously high. Or a
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Feb. 1, 2021. Published March 2021. Originally
approved in 1997. Last previous edition approved in 2014 as D6133 – 02 (2014).
DOI: 10.1520/D6133-02R21. The last approved version of this historical standard is referenced on
For referenced ASTM standards, visit the ASTM website, www.astm.org, or www.astm.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM At the time of the revision of this test method, t-butyl acetate was not yet
Standards volume information, refer to the standard’s Document Summary page on approved as an exempt solvent, but was under review by the USEPA and was
the ASTM website. expected to be approved. Therefore, it has been included in this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6133−02 (2021)
component may elute with the internal standard, giving a result of 5.1. The use of a reporting electronic integrator or computer
that is erroneously low. It is therefore important to know the based data system is preferred.
composition of the sample to ensure that there are no
interferences, under the analysis conditions used. Test Method 6. Column Peak Interferences
D6438employsmass-spectraldetectionofanalytesandmaybe
6.1 The following compounds are known to co-elute or
used as an alternative method.
otherwise interfere with the analysis on a DB-5 type column:
(a) Acetone—isopropanol, propylene oxide, acetonitrile,
5. Apparatus
and
5.1 Gas Chromatograph—Any instrument with temperature
(b) Cyclohexanol—sec-amyl acetate.
programming capability may be used. It should be equipped
6.2 The following compound is known to co-elute or
with a flame ionization detector (see Table 1).
otherwise interfere with the analysis on an FFAP type column:
5.2 Column—Any column that provides baseline separation
(a) Cyclohexanol—butyl cellosolve.
of the analyte of interest (acetone, p-chlorobenzotrifluoride,
methylacetateor t-butylacetate),theinternalstandard,andany
6.3 The analyst must verify that, under the analysis condi-
volatile present in the samples may be used. It should be
tions being used, none of the components of the sample
understood that column performance may be influenced by
interfere with the analyte being quantitated or with the internal
manufacturing conditions, such as type of deactivation and
standard being used.
chemical bonding/crosslinking used. One or more of the
followingcolumntypesmaybeused.Intermsofdurabilityand
7. Reagents and Materials
over all efficiency, a bonded phase poly (5 % phenyl 95 %
7.1 Purity of Reagents—Use reagent grade chemicals in all
dimethylsiloxane) type of column should be considered first.
tests, unless otherwise specified. Other grades may be used,
(Any reference to specific product brands does not indicate an
provided it is first ascertained that the reagent is sufficiently
endorsement for that particular brand of column).
high purity to permit its use without lessening the accuracy of
5.2.1 Capillary, 25 to 60 m, 0.25 mm-inside diameter, 0.25
the determination.
to 1.0-µm film thickness, fused silica bonded phase poly (5 %
phenyl 95 % dimethylsiloxane (DB-5, HP-5, Rtx-5, Ultra-2,
7.2 Tetrahydrofuran (THF)—high performance liquid chro-
BP-5, CP-Sil 8 CB, etc.)).
matography (HPLC) grade, uninhibited.
5.2.2 Capillary, 25 to 60 m, 0.25-mm inside diameter, 0.25
7.3 Cyclohexanol—98+ %.
to 1.0-µm film thickness, fused silica FFAP (polyethylene
glycol nitrophthalic acid ester phase).
7.4 Acetone—HPLC grade.
5.2.3 Capillary, 25 to 60 m, 0.25-mm inside diameter, 0.25
7.5 p-Chlorobenzotrifluoride—98+ %.
to 1.4-µm film thickness, fused silica bonded phase poly (6 %
cyanopropyl/phenyl, 94 % dimethylsiloxane) (DB-624, SPB-
7.6 Methyl Acetate—99+ %.
624, Rtx-624, etc.).
7.7 t-Butyl Acetate—99+ %.
5.3 Recorder—A recording potentiometer with a full-scale
7.8 Water—nanopure.
deflection of 1 to 10 mV, full-scale response time of2sor less
and sufficient sensitivity and stability to meet the requirements
7.9 Chromatography Gases: Helium of 99.9995 % purity or
higher.
TABLE 1 Suggested Instrument Conditions
Hydrogen of 99.9995 % minimum purity (see Note 1).
Detector Flame Ionization Detection (FID)
Air, “dry” quality, free of hydrocarbons.
Hydrogen Flow 30 mL/min
NOTE 1—The preferred choice of carrier gas is hydrogen, but helium or
Air Flow 400 mL/min
Make-up (Helium) 30 mL/min nitrogen may also be used. Chromatographic analysis time will increase
Carrier Gas (Hydrogen) 40 cm/s and there may be a possible reduction in resolution.
Detector Temperature 250°C
A
Injection Port Temperature 200°C 7.10 Liquid Charging Devices—micro syringes of 10 or 25
B
Split Ratio 50:1
µL capacity.
Initial Oven Temperature 40°C
Initial Temperature Hold Time 5 min
7.11 Analytical Balance—four places (0.0001 g).
Program Rate 1 4°C/min
Program Time 1 5 min
7.12 Sealable Vials—7-mL screw cap.
Final Temperature 1 60°C
Program Rate 2 20°C/min
7.13 Medicine Droppers.
Program Time 2 8 min
Final Temperature 2 220°C
7.14 Autosampler Vials.
Final Temperature Hold Time 2 min
Total Run Time 20 min
7.15 Pipete—5-mL glass or autopipete.
Injection Volume 1.0 µL
A
The injection port temperature can be decreased to permit the analysis of
8. Hazards
thermally unstable samples; however, each case must be individually investigated.
B
The split ratio may be adjusted according to the theoretical level of solvent
8.1 Check the supplier’s Material Safety Data Sheet
composition.
(MSDS) on all chemicals before use.
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