ASTM D6133-00
(Test Method)Test Method for Acetone, p-Chlorobenzotrifluoride, Methyl Acetate or t-Butyl Acetate Content of Solvent-Reducible and Water-Reducible Paints, Coatings, Resins, and Raw Materials by Direct Injection Into a Gas Chromatograph
Test Method for Acetone, <i>p</i>-Chlorobenzotrifluoride, Methyl Acetate or <i>t</i>-Butyl Acetate Content of Solvent-Reducible and Water-Reducible Paints, Coatings, Resins, and Raw Materials by Direct Injection Into a Gas Chromatograph
SCOPE
1.1 This test method is for the determination of the total-concentration of acetone, p-chlorobenzotrifluoride, methyl acetate, or t-butyl acetate, or combination of any of the four, in solvent-reducible and water-reducible paints, coatings, resins, and raw materials. Because unknown compounds that coelute with the anallyte being measured or with the internal standard, will lead to erroneous results, this test method should only be used for materials of known composition so that the possibility of interferences can be eliminated. The established working range of this test method is from 1 % to 100 % acetone by weight.
1.2 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.
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Designation: D 6133 – 00
Standard Test Method for
Acetone, p-Chlorobenzotrifluoride, Methyl Acetate or t-Butyl
Acetate Content of Solvent-Reducible and Water-Reducible
Paints, Coatings, Resins, and Raw Materials by Direct
Injection Into a Gas Chromatograph
This standard is issued under the fixed designation D 6133; 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.
1. Scope 4. Significance and Use
1.1 This test method is for the determination of the total- 4.1 With the need to calculate volatile organic content
concentration of acetone, p-chlorobenzotrifluoride, methyl ac- (VOC) of paints, and with acetone, p-chlorobenzotrifluoride,
etate, or t-butyl acetate, or combination of any of the four, in methyl acetate and t-butyl acetate considered as exempt
solvent-reducible and water-reducible paints, coatings, resins, volatille compounds, it is necessary to know the content of
and raw materials. Because unknown compounds that coelute these analytes. This gas chromatographic test method provides
with the anallyte being measured or with the internal standard, a relatively simple and direct way to determine their content.
will lead to erroneous results, this test method should only be However, because the dectors used in this test method are not
used for materials of known composition so that the possibility selective, and because some coatings are very complex mix-
of interferences can be eliminated. The established working tures, compounds may be present in the sample that coelute
range of this test method is from 1 % to 100 % acetone by with the analyte, giving a result that is erroneously high. Or a
weight. component may elute with the internal standard, giving a result
1.2 This standard does not purport to address all of the that is erroneously low. It is therefore important to know the
safety concerns, if any, associated with its use. It is the composition of the sample to ensure that there are no interfer-
responsibility of the user of this standard to establish appro- ences, under the analysis conditions used.
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use.
5.1 Gas Chromatograph—Any instrument with temperature
2. Referenced Documents
programming capability may be used. It should be equipped
2.1 ASTM Standards: with either a thermal conductivity, flame ionization or photo-
D 3271 Practice for Direct Injection of Solvent-Reducible ionization detector (see Table 1).
Paints into a Gas Chromatograph for Solvent Analysis 5.2 Column—Any column that provides baseline separation
D 3272 Practice for Vacuum Distillation of Solvents from of the analyte of interest (acetone, p-chlorobenzotrifluoride,
Solvent-Reducible Paints for Analysis methyl acetate or t-butyl acetate), the internal standard, and any
E 180 Practice for Determining the Precision of ASTM volatile present in the samples may be used. It should be
Methods for Analysis and Testing of Industrial and Spe- understood that column performance may be influenced by
cialty Chemicals manufacturing conditions, such as type of deactivation and
chemical bonding/crosslinking used. One or more of the
3. Summary of Test Method
following column types may be used. In terms of durability and
3.1 A suitable aliquot of whole paint is internally standard- over all efficiency, a bonded phase poly (5 % phenyl 95 %
ized, diluted with an appropriate solvent, and then injected into
dimethylsiloxane) type of column should be considered first.
a gas chromatographic column that separates the chosen (Any reference to specific product brands does not indicate an
analytes from other volatile components. The analyte content is
endorsement for that particular brand of column).
determined from area calculations of the materials producing 5.2.1 Capillary, 25 to 60 m, 0.25 mm-inside diameter, 0.25
peaks on the chromatogram.
to 1.0-μm film thickness, fused silica bonded phase poly (5 %
phenyl 95 % dimethylsiloxane (DB-5, HP-5, Rtx-5, Ultra-2,
BP-5, CP-Sil 8 CB, etc.)).
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
D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved May 10, 2000. Published September 2000. Originally
published as D 6133 – 97. Last previous edition D 6133 – 97. At the time of the writing of this test method, t-butyl acetate was not yet
Annual Book of ASTM Standards, Vol 06.01. approved as an exempt solvent, but was under review by te USEPA and was
Annual Book of ASTM Standards, Vol 15.05. expected to be approved. Therefore, it has been included in this test method.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6133
TABLE 1 Suggested Instrument Conditions
7.8 Water—nanopure.
Detector Flame Ionization Detection (FID) 7.9 Chromatography Gases:
Hydrogen Flow 30 mL/min
Helium of 99.9995 % purity or higher.
Air Flow 400 mL/min
Hydrogen of 99.9995 % minimum purity (see Note 1).
Make-up (Helium) 30 mL/min
Carrier Gas (Hydrogen) 40 cm/s Air, “dry” quality, free of hydrocarbons.
Detector Temperature 250°C
A
Injection Port Temperature 200°C NOTE 1—The preferred choice of carrier gas is hydrogen, but helium or
B
Split Ratio 50:1
nitrogen may also be used. Chromatographic analysis time will increase
Initial Oven Temperature 40°C
and there may be a possible reduction in resolution.
Initial Temperature Hold Time 5 min
Program Rate 1 4°C/min 7.10 Liquid Charging Devices—micro syringes of 10 or 25
Program Time 1 5 min
μL capacity.
Final Temperature 1 60°C
7.11 Analytical Balance—four places (0.0001 g).
Program Rate 2 20°C/min
Program Time 2 8 min 7.12 Sealable Vials—7-mL screw cap.
Final Temperature 2 220°C
7.13 Medicine Droppers.
Final Temperature Hold Time 2 min
7.14 Autosampler Vials.
Total Run Time 20 min
Injection Volume 1.0 μL
7.15 Pipete—5-mL glass or autopipete.
A
The injection port temperature can be decreased to permit the analysis of
thermally unstable samples; however, each case must be individually investigated. 8. Hazards
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.
5.2.2 Capillary, 25 to 60 m, 0.25-mm inside diameter, 0.25
9. Preparation of Apparatus
to 1.0-μm film thickness, fused silica FFAP (polyethylene
9.1 Install the column in the chromatograph following the
glycol nitrophthalic acid ester phase).
manufacturer’s directions and establish the operating condi-
5.2.3 Capillary, 25 to 60 m, 0.25-mm inside diameter, 0.25
tions required to give the desired separation (see Table 1).
to 1.4-μm film thickness, fused silica bonded phase poly (6 %
Allow sufficient time for the instrument to reach equilibrium as
cyanophenylpropyl 94 % dimethylsiloxane) (DB-624, SPB-
indicated by a stable base line.
624, Rtx-624, etc.).
5.3 Recorder—A recording potentiometer with a full-scale
10. Calibration
deflection of 1 to 10 mV, full-scale response time of2sor less
10.1 Using the information in Table 1 (as a guide), select the
and sufficient sensitivity and stability to meet the requirements
conditions of temperature and carrier gas flow that give the
of 5.1. The use of a reporting electronic integrator or computer
necessary resolution of the desired analytes from interferences
based data system is preferred.
in the samples.
10.2 Determination of Relative Response Factors—
6. Column Peak Interferences
Cyclohexanol, or another suitable compound, is used as an
6.1 The following compounds are known to co-elute or
internal standard. The internal standard used should be a
otherwise interfere with the analysis on a DB-5 type column:
compound that is not in the sample matrix, and does not
(a) Acetone—isopropanol, propylene oxide, acetonitrile, and
co-elute with any other component of the sample. Most
(b) Cyclohexanol—sec-amyl acetate.
analyses can be done utilizing cyclohexanol for the internal
6.2 The following compound is known to co-elute or
standard providing it is soluble in the diluent solvent. The
otherwise interfere with the analysis on an
...
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