ASTM D3797-03
(Test Method)Standard Test Method for Analysis of o-Xylene by Gas Chromatography
Standard Test Method for Analysis of <i>o</i>-Xylene by Gas Chromatography
SCOPE
1.1 This test method covers the analysis of normally occurring impurities in, and the purity of, o-xylene by gas chromatography. Impurities determined include nonaromatic hydrocarbons, benzene, toluene, p- and m-xylenes, cumene, styrene, and ethylbenzene.
1.2 This test method is applicable for impurities at concentrations from 0.001 to 2.000 % and for o-xylene purities of 98 % or higher.
1.3 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, 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.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8.
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Designation: D 3797 – 03
Standard Test Method for
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Analysis of o-Xylene by Gas Chromatography
This standard is issued under the fixed designation D 3797; 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 E 1510 Practice for Installing Fused Silica Open Tubular
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Capillary Columns in Gas Chromatographs
1.1 This test method covers the analysis of normally occur-
2.2 Other Documents:
ring impurities in, and the purity of, o-xylene by gas chroma-
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
tography. Impurities determined include nonaromatic hydro-
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1910.1200
carbons, benzene, toluene, p- and m-xylenes, cumene, styrene,
and ethylbenzene.
3. Terminology
1.2 This test method is applicable for impurities at concen-
3.1 Definitions:
trations from 0.001 to 2.000 % and for o-xylene purities of
3.1.1 For definition of terms used in this test method see
98 % or higher.
Terminology D 4790.
1.3 The following applies to all specified limits in this
standard: for purposes of determining conformance with this
4. Summary of Test Method
standard, an observed value or a calculated value shall be
4.1 A known amount of internal standard is added to the
rounded off “to the nearest unit” in the last right-hand digit
sample. A gas chromatograph equipped with a flame ionization
used in expressing the specification limit, in accordance with
detector and a polar-fused silica capillary column is used for
the rounding-off method of Practice E 29.
the analysis. The impurities are measured relative to the
1.4 This standard does not purport to address all of the
internal standard. To calculate o-Xylene purity subtract the
safety concerns, if any, associated with its use. It is the
impurities found from 100.00 %.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. For a specific
5.1 This test method is suitable for setting specifications on
hazard statement, see Section 8.
o-xylene and for use as an internal quality control tool where
o-xylene is used in a manufacturing process. It may be used in
2. Referenced Documents
development or research work involving o-xylene.
2.1 ASTM Standards:
5.2 Purity is commonly reported by subtracting the deter-
D 3437 Practice for Sampling and Handling Liquid Cyclic
mined expected impurities from 100 %. Absolute purity cannot
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Products
be determined if unknown impurities are present.
D 4307 Practice for Preparation of Liquid Blends for Use as
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Analytical Standards
6. Apparatus
D 4790 Terminology of Aromatic Hydrocarbons and Re-
6.1 Gas Chromatography—Any gas chromatograph having
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lated Chemicals
a flame ionization detector and a splitter injector suitable for
E 29 Practice for Using Significant Digits in Test Data to
use with a fused-silica capillary column may be used, provided
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Determine Conformance with Specifications
the system has sufficient sensitivity to obtain a minimum peak
E 355 Practice for Gas Chromatography Terms and Rela-
4 height response of 0.1 mV for 0.010 % internal standard when
tionships
operated at the stated conditions. Background noise at these
conditions is not to exceed 3 μV.
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6.2 Chromatographic Column, fused silica capillary, 60-m
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
long, 0.32-mm inside diameter, internally coated to a 0.5-μm
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their
thickness with a bonded (cross-linked) polyethylene glycol.
Derivatives.
Other columns may be used after it has been established that
Current edition approved Feb. 10, 2003. Published April 2003. Originally
approved in 1979. Last previous edition approved in 2000 as D 3797 – 00.
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Annual Book of ASTM Standards, Vol 06.04.
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Annual Book of ASTM Standards, Vol 05.02. Available from U.S. Government Printing Office Superintendent of Documents,
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Annual Book of ASTM Standards, Vol 14.02. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3797–03
such column is capable of separating all major impurities and 10.2 Analyze the o-xylene used in preparing the calibration
the internal standard from the o-xylene under operating con- blend as described in 11.2 and 11.3. Calculate the purity of the
ditions appropriate for the column. stock o-xyl
...
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