ASTM D7090-04(2018)
(Test Method)Standard Test Method for Purity of Isophorone by Capillary Gas Chromatography
Standard Test Method for Purity of Isophorone by Capillary Gas Chromatography
SIGNIFICANCE AND USE
4.1 This test method determines the purity of isophorone, as well as the concentration of various potential impurities, several of which are critical in the application of these solvents.
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 E29.
1.4 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, health, and environmental practices and to determine the applicability of regulatory limitations prior to use.
1.5 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.
General Information
Relations
Standards Content (Sample)
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: D7090 − 04 (Reapproved 2018)
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 Fischer Reagent Titration Method)
E29 Practice for Using Significant Digits in Test Data to
1.1 This test method covers the determination of the purity
Determine Conformance with Specifications
of isophorone. This method also determines the impurities of
E300 Practice for Sampling Industrial Chemicals
the material in concentration level less than 0.5 mass %, which
may include mesityl oxide (MSO), mesityl oxide-isomer,
3. Summary of Test Method
mesitylene, trimethyl cyclohexenone (TMCH), phorone,
3.1 A representative specimen is introduced into a gas
phorone-isomer, xylitone, and tetralone.
chromatograph with a bonded polyethylene glycol capillary
1.2 Water cannot be determined by this test method and
column using temperature programming and a flame ionization
shall be measured by other appropriate ASTM procedure. The
detector. The concentrations of the sample components are
result is used to normalize the chromatographic data deter-
calculated from the integrated component peaks using internal
mined by this test method.
standardization technique with response factors. Water is
1.3 For purposes of determining conformance of an ob-
measured in accordance with Test Method D1364 and the
served or a calculated value using this test method to relevant
result is used to normalize the values obtained by gas chroma-
specifications, test result(s) shall be rounded off “to the nearest
tography.
unit” in the last right-hand digit used in expressing the
specification limit, in accordance with the rounding-off method
4. Significance and Use
of Practice E29.
4.1 This test method determines the purity of isophorone, as
1.4 This standard does not purport to address all of the
well as the concentration of various potential impurities,
safety concerns, if any, associated with its use. It is the
severalofwhicharecriticalintheapplicationofthesesolvents.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and to
5. Apparatus
determine the applicability of regulatory limitations prior to
5.1 Chromatograph—Any gas chromatograph utilizing a
use.
capillary column and has the following characteristics (see
1.5 This international standard was developed in accor-
Table 1 for typical GC parameters):
dance with internationally recognized principles on standard-
5.1.1 Detector—A flame ionization detector (FID) capable
ization established in the Decision on Principles for the
of continuous operation at a temperature equivalent to the
Development of International Standards, Guides and Recom-
maximum column temperature employed. The detector shall
mendations issued by the World Trade Organization Technical
havesufficientsensitivitytodetect0.001mass %ofimpurityin
Barriers to Trade (TBT) Committee.
the specimen at a peak height 3 times the noise level.
5.1.2 Column—fused silica capillary column with bonded
2. Referenced Documents
polyethylene (see Table 1 for details).
2.1 ASTM Standards:
5.1.3 Column Temperature Programming—The chromato-
D1364 Test Method for Water in Volatile Solvents (Karl
graph shall be capable of reproducible linear temperature
programming.
5.1.4 Sample Inlet System—The sample inlet system shall
This test method is under the jurisdiction of ASTM Committee D01 on Paint
be capable of split injection, typically at a 100:1 split ratio.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
NOTE 1—An autoinjector is recommended. Manual injection with a
Current edition approved Nov. 1, 2018. Published November 2018. Originally
syringe is acceptable, however the observed precision may not apply.
approved in 2004. Last previous edition approved in 2010 as D7090 – 04 (2010).
DOI: 10.1520/D7090-04R18.
5.1.5 Integrator—Means shall be provided for determining
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the area of the observed chromatographic peaks. This can be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
done by means of an electronic integrator or a computer based
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. chromatography data system. The integrator/computer system
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7090 − 04 (2018)
TABLE 1 Typical GC Parameters
6.3 Carrier Gases—Helium or hydrogen (minimum
Parameters Values 99.95 % purity). (Warning—Helium and hydrogen are com-
Column 30m×0.32mmfused silica capillary column pressed gases under high pressure. Hydrogen is highly flam-
with 0.5 micron bonded phase polyethylene
mable.)
glycol
Column Temperature 50°C for 5 min., programmed to 210°C at 10°C/
7. Sampling
min. Hold for 10 min.
Injector Temperature 230°C
7.1 Take samples of the material to be tested using proce-
Sample size 1 µL
Split ratio 100:1 dures described in Practice E300.
Detector Flame Ionization
Detector Temperature 250°C
8. Conditioning of Capillary Column
Carrier Gas (Helium) 30 cm/s
Hydrogen Gas 30 mL/min.
8.1 Condition the gas chromatographic capillary column
Air 300 mL/min.
following the column supplier recommendation.
9. Calibration and Standardization
9.1 Prepare a calibration mixture containing approximately
0.1 mass % of each of the components of interest and the
shall have standard chromatographic software for determining
decane internal standard in pure isophorone. The total weight
the retention times and quantification of eluting peaks.
of the calibration mixture solution should be 100 g. If pure
5.1.6 Flow Controller—The chromatograph shall be
isophorone is not available, then isophorone containing rela-
equipped with a constant flow device capable of maintaining
tively low concentration of the components of interest can be
the carrier gas at a constant flow rate throughout the tempera-
used, and the composition of the calibration mixture corrected
ture program.
for components already present. Typical components suitable
5.1.7 Microsyringe—A microsyringe of appropriate capac-
for the calibration mixture are: MSO, MSO-isomer,
ity is required for injection of the specimen into the chromato-
mesitylene, TMCH, phorone, phorone isomer, xylitone, and
graph. Typically,a5µL syringe is used.
tetralone (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
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