ASTM D7090-04

Standard Test Method for Purity of Isophorone by Capillary Gas Chromatography

SCOPE
1.1 This test method covers the determination of the purity of isophorone. This method also determines the impurities of the material in concentration level less than 0.5 mass %, which may include mesityl oxide (MSO), mesityl oxide-isomer, mesitylene, trimethyl cyclohexenone (TMCH), phorone, phorone-isomer, xylitone, and tetralone.
1.2 Water cannot be determined by this test method and shall be measured by other appropriate ASTM procedure. The result is used to normalize the chromatographic data determined by this test method.
1.3 For purposes of determining conformance of an observed or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding - off method of Practice E 29.
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 to determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Oct-2004
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

Relations

• Replaced By: ASTM D7090-04(2010) - Standard Test Method for Purity of Isophorone by Capillary Gas Chromatography
• Effective Date: 01-Dec-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D7090–04
Standard Test Method for
Purity of Isophorone by Capillary Gas Chromatography
This standard is issued under the fixed designation D7090; 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 column using temperature programming and a flame ionization
detector. The concentrations of the sample components are
1.1 This test method covers the determination of the purity
calculated from the integrated component peaks using internal
of isophorone. This method also determines the impurities of
standardization technique with response factors. Water is
the material in concentration level less than 0.5 mass %, which
measured in accordance with Test Method D1364 and the
may include mesityl oxide (MSO), mesityl oxide-isomer,
result is used to normalize the values obtained by gas chroma-
mesitylene, trimethyl cyclohexenone (TMCH), phorone,
tography.
phorone-isomer, xylitone, and tetralone.
1.2 Water cannot be determined by this test method and
4. Significance and Use
shall be measured by other appropriate ASTM procedure. The
4.1 This test method determines the purity of isophorone, as
result is used to normalize the chromatographic data deter-
well as the concentration of various potential impurities,
mined by this test method.
severalofwhicharecriticalintheapplicationofthesesolvents.
1.3 For purposes of determining conformance of an ob-
served or a calculated value using this test method to relevant
5. Apparatus
specifications, test result(s) shall be rounded off “to the nearest
5.1 Chromatograph—Any gas chromatograph utilizing a
unit” in the last right-hand digit used in expressing the
capillary column and has the following characteristics (see
specification limit, in accordance with the rounding - off
Table 1 for typical GC parameters):
method of Practice E29.
5.1.1 Detector—A flame ionization detector (FID) capable
1.4 This standard does not purport to address all of the
of continuous operation at a temperature equivalent to the
safety concerns, if any, associated with its use. It is the
maximum column temperature employed. The detector shall
responsibility of the user of this standard to establish appro-
havesufficientsensitivitytodetect0.001mass%ofimpurityin
priate safety and health practices and to determine the
the specimen at a peak height 3 times the noise level.
applicability of regulatory limitations prior to use.
5.1.2 Column—fused silica capillary column with bonded
2. Referenced Documents polyethylene (see Table 1 for details).
2 5.1.3 Column Temperature Programming—the chromato-
2.1 ASTM Standards:
graph shall be capable of reproducible linear temperature
D1364 Test Method for Water in Volatile Solvents (Karl
programming.
Fischer Reagent Titration Method)
5.1.4 SampleInletSystem—the sample inlet system shall be
E29 Practice for Using Significant Digits in Test Data to
capable of split injection, typically at a 100:1 split ratio.
Determine Conformance with Specifications
E300 Practice for Sampling Industrial Chemicals
NOTE 1—An autoinjector is recommended. Manual injection with a
syringe is acceptable, however the observed precision may not apply.
3. Summary of Test Method
5.1.5 Integrator—means shall be provided for determining
3.1 A representative specimen is introduced into a gas
the area of the observed chromatographic peaks. This can be
chromatograph with a bonded polyethylene glycol capillary
done by means of an electronic integrator or a computer based
chromatography data system. The integrator/computer system
shall have standard chromatographic software for determining
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of the retention times and quantification of eluting peaks.
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
5.1.6 Flow Controller—the chromatograph shall be
Current edition approved Nov. 1, 2004. Published November 2004. DOI:
equipped with a constant flow device capable of maintaining
10.1520/D7090-04.
the carrier gas at a constant flow rate throughout the tempera-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
ture program.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D7090–04
TABLE 1 Typical GC Parameters
8. Conditioning of Capillary Column
Parameters Values
8.1 Condition the gas chromatographic capillary column
Column 30mx0.32mmfused silica capillary column
following the column supplier recommendation.
with 0.5 micron bonded phase polyethylene
glycol
Column Temperature 50° C for 5 min., programmed to 210° C at 10°
9. Calibration and Standardization
C/min. Hold for 10 min.
Injector Temperature 230° C
9.1 Prepare a calibration mixture containing approximately
Sample size 1 µL
0.1 mass % of each of the components of interest and the
Split ratio 100:1
decane internal standard in pure isophorone. The total weight
Detector Flame Ionization
Detector Temperature 250° C
of the calibration mixture solution should be 100 g. If pure
Carrier Gas (Helium) 30 cm/s
isophorone is not available, then isophorone containing rela-
Hydrogen Gas 30 mL/min.
Air 300 mL/min. tively low concentration of the components of interest can be
used, and the composition of the calibration mixture corrected
for components already present. Typical components suitable
5.1.7 Microsyringe—a microsyringe of appropriate capacity
for the calibration mixture are: MSO, MSO-isomer, mesity-
is required for injection of the specimen into the chromato-
lene, TMCH, phorone, phorone isomer, xylitone, and tetralone
graph. Typically,a5µL syringe is used.
(see 6.2).
6. Reagents and Materials 9.2 Record the actual weight of each added component, the
internal standard, and the total weight of the calibration
6.1 Purity of Reagents—Reagent grade chemicals shall be
mixture.
used in the preparation of the calibration mixture.
9.3 Determine the detector response factor of the various
6.2 Calibration Mixture Components:
components of interest, by injecting 1 µL of the calibration
6.2.1 Isophorone—solvent used in the preparation of the
mixture into a GC using the typical chromatographic param-
calibration mixture, and shall be free of the components of
eters given in Table 1, and using the equation:
...