ASTM D5917-02
(Test Method)Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and External Calibration
Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and External Calibration
SIGNIFICANCE AND USE
Determining the type and amount of hydrocarbon impurities remaining from the manufacture of toluene, mixed xylenes, and p-xylenes used as chemical intermediates and solvents is often required. This test method is suitable for setting specifications and for use as an internal quality control tool where these products are produced or are used. Typical impurities are: alkanes containing 1 to 10 carbons atoms, benzene, toluene, ethylbenzene (EB), xylenes, and aromatic hydrocarbons containing nine carbon atoms.
5.1.1 Refer to Test Method D 2306 for determining the C8 aromatic hydrocarbon distribution in mixed xylenes.
Purity is commonly reported by subtracting the determined expected impurities from 100.00. However, a gas chromatographic analysis cannot determine absolute purity if unknown or undetected components are contained within the material being examined.
This test method is similar to Test Method D 2360, however, interlaboratory testing has indicated a bias may exist between the two methods. Therefore the user is cautioned that the two methods may not give comparable results.
SCOPE
1.1 This test method covers the determination of the total nonaromatic hydrocarbons and trace monocyclic aromatic hydrocarbons in toluene, mixed xylenes, and p-xylenes by gas chromatography. The purity of toluene, mixed xylenes, or p-xylenes can also be calculated. Calibration of the gas chromatographic system is done by the external standard calibration technique. A similar test method, using the internal standard calibration technique, is Test Method D 2360.
1.2 Total aliphatic hydrocarbons containing 1 through 10 carbon atoms (methane through decanes) can be detected by this test method at concentrations ranging from 0.001 to 2.500 weight %.
1.2.1 A small amount of benzene in mixed xylenes or p-xylenes may not be distinguished from the nonaromatics and the concentrations are determined as a composite (see 6.1).
1.3 Monocyclic aromatic hydrocarbon impurities containing 6 through 10 carbon atoms (benzene through C 10 aromatics) can be detected by this test method at individual concentrations ranging from 0.001 to 1.000 weight %.
1.4 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value 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.
1.5 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. For specific hazard statement, see Section 9.
General Information
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Standards Content (Sample)
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Designation: D 5917 – 02
Standard Test Method for
Trace Impurities in Monocyclic Aromatic Hydrocarbons by
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Gas Chromatography and External Calibration
This standard is issued under the fixed designation D5917; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* D2306 Test Method for C Hydrocarbon Analysis by Gas
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2
Chromatography
1.1 This test method covers the determination of the total
D2360 Test Method for Trace Impurities in Monocyclic
nonaromatic hydrocarbons and trace monocyclic aromatic
2
Aromatic Hydrocarbons by Gas Chromatography
hydrocarbons in toluene, mixed xylenes, and p-xylenes by gas
D3437 Practice for Sampling and Handling Liquid Cyclic
chromatography. The purity of toluene, mixed xylenes, or
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Products
p-xylenes can also be calculated. Calibration of the gas
D4052 Test Method for Density and Relative Density of
chromatographic system is done by the external standard
3
Liquids by Digital Density Meter
calibration technique.Asimilar test method, using the internal
D4307 PracticeforPreparationofLiquidBlendsforUseas
standard calibration technique, is Test Method D2360.
3
Analytical Standards
1.2 Total aliphatic hydrocarbons containing 1 through 10
D4534 Test Method for Benzene Content of Cyclic Prod-
carbon atoms (methane through decanes) can be detected by
2
ucts by Gas Chromatography
this test method at concentrations ranging from 0.001 to 2.500
D4790 Terminology of Aromatic Hydrocarbons and Re-
weight %.
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lated Chemicals
1.2.1 A small amount of benzene in mixed xylenes or
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D5136 Specification for High Purity p-Xylene
p-xylenesmaynotbedistinguishedfromthenonaromaticsand
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D5211 Specification for Xylenes for p-Xylene Feedstock
the concentrations are determined as a composite (see 6.1).
E29 Practice for Using Significant Digits in Test Data to
1.3 Monocyclicaromatichydrocarbonimpuritiescontaining
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Determine Conformance with Specifications
6 through 10 carbon atoms (benzene through C aromatics)
10
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E260 Practice for Packed Column Gas Chromatography
canbedetectedbythistestmethodatindividualconcentrations
E355 Practice for Gas Chromatography Terms and Rela-
ranging from 0.001 to 1.000 weight %.
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tionships
1.4 The following applies to all specified limits in this test
E691 Practice for Conducting an Interlaboratory Study to
method: for purposes of determining conformance with this
4
Determine the Precision of a Test Method
test method, an observed value or a calculated value shall be
E1510 Practice for Installing Fused Silica Open Tubular
rounded off “to the nearest unit” in the last right-hand digit
5
Capillary Columns in Gas Chromatographs
used in expressing the specification limit, in accordance with
2.2 Other Document:
the rounding-off method of PracticeE29.
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1.5 This standard does not purport to address all of the
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1910.1200
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 SeeTerminologyD4790fordefinitionsoftermsusedin
bility of regulatory limitations prior to use. For specific hazard
this test method.
statement, see Section 9.
4. Summary of Test Method
2. Referenced Documents
4.1 A repeatable volume of the specimen to be analyzed is
2.1 ASTM Standards:
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precisely injected into a gas chromatograph equipped with a
D841 Specification for Nitration Grade Toluene
flameionizationdetector(FID).Thepeakareaofeachimpurity
is measured. Concentration of each impurity is determined
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This test method is under the jurisdiction of ASTM Committee D16 on
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Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Annual Book of ASTM Standards, Vol 05.02.
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Subcommittee D16.04 on Instrumental Analysis. Annual Book of ASTM Standards, Vol 14.02.
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Current edition approved Oct. 10, 2002. Published December 2002. Originally Annual Book of ASTM Standards, Vol 03.06.
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published as D5917–96. Last previous edition D5917–99. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
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Annual Book of ASTM Standards, Vol 06.04. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5917–02
TABLE 1 Method Parameters
from the linear calibration curve of peak area versus concen-
tration. Purity by gas chromatography (GC) is calculat
...
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