ASTM D3797-00

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, -xylene by gas chromatography. Impurities determined include nonaromatic hydrocarbons, benzene, toluene, - and -xylenes, cumene, styrene, and ethylbenzene.  
1.2 This test method is applicable for impurities at concentrations from 0.001 to 2.000% and for -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 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 7.

General Information

• Status: Historical
• Publication Date: 09-Jun-2000
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.01 - Benzene, Toluene, Xylenes, Cyclohexane and Their Derivatives

Relations

• Replaced By: ASTM D3797-03 - Standard Test Method for Analysis of <i>o</i>-Xylene by Gas Chromatography
• Effective Date: 10-Feb-2003

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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.
Designation: D 3797 – 00
Standard Test Method for
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 2.2 Other Documents:
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1.1 This test method covers the analysis of normally occur-
1910.1200
ring impurities in, and the purity of, o-xylene by gas chroma-
tography. Impurities determined include nonaromatic hydro-
3. Terminology
carbons, benzene, toluene, p- and m-xylenes, cumene, styrene,
3.1 Definitions:
and ethylbenzene.
3.1.1 For definition of terms used in this test method see
1.2 This test method is applicable for impurities at concen-
Terminology D 4790.
trations from 0.001 to 2.000 % and for o-xylene purities of
98 % or higher.
4. Summary of Test Method
1.3 The following applies to all specified limits in this
4.1 A known amount of internal standard is added to the
standard: for purposes of determining conformance with this
sample. A gas chromatograph equipped with a flame ionization
standard, an observed value or a calculated value shall be
detector and a polar-fused silica capillary column is used for
rounded off “to the nearest unit” in the last right-hand digit
the analysis. The impurities are measured relative to the
used in expressing the specification limit, in accordance with
internal standard. To calculate o-Xylene purity subtract the
the rounding-off method of Practice E 29.
impurities found from 100.00 %.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 This test method is suitable for setting specifications on
priate safety and health practices and determine the applica-
o-xylene and for use as an internal quality control tool where
bility of regulatory limitations prior to use. For a specific
o-xylene is used in a manufacturing process. It may be used in
hazard statement, see Section 8.
development or research work involving o-xylene.
5.2 Purity is commonly reported by subtracting the deter-
2. Referenced Documents
mined expected impurities from 100 %. Absolute purity cannot
2.1 ASTM Standards:
be determined if unknown impurities are present.
D 3437 Practice for Sampling and Handling Liquid Cyclic
Products
6. Apparatus
D 4307 Practice for Preparation of Liquid Blends for Use as
3 6.1 Gas Chromatography—Any gas chromatograph having
Analytical Standards
a flame ionization detector and a splitter injector suitable for
D 4790 Terminology of Aromatic Hydrocarbons and Re-
use with a fused-silica capillary column may be used, provided
lated Chemicals
the system has sufficient sensitivity to obtain a minimum peak
E 29 Practice for Using Significant Digits in Test Data to
height response of 0.1 mV for 0.010 % internal standard when
Determine Conformance with Specifications
operated at the stated conditions. Background noise at these
E 355 Practice for Gas Chromatography Terms and Rela-
conditions is not to exceed 3 μV.
tionships
6.2 Chromatographic Column, fused silica capillary, 60-m
E 1510 Practice for Installing Fused Silica Open Tubular
long, 0.32-mm inside diameter, internally coated to a 0.5-μm
Capillary Columns in Gas Chromatographs
thickness with a bonded (cross-linked) polyethylene glycol.
Other columns may be used after it has been established that
This test method is under the jurisdiction of ASTM Committee D16 on
such column is capable of separating all major impurities and
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
the internal standard from the o-xylene under operating con-
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their
ditions appropriate for the column.
Derivatives.
Current edition approved June 10, 2000. Published August 2000. Originally
published as D 3797 – 79. Last previous edition D 3797 – 96.
Annual Book of ASTM Standards, Vol 06.04.
3 5
Annual Book of ASTM Standards, Vol 05.02. Available from Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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 3797
6.3 Recorder, electronic integration with tangent capabili- 10.4 Calculate response factors as follows:
ties (required).
C
i
R 5 (1)
6.4 Microsyringes, 10-μL, and 50-μL. i
A A
i b
~C ! 2
S D
6.5 Volumetric Flask, 50-mL. s
A A
si sb
where:
7. Reagents and Materials
R = response factor for impurity relative to internal
i
7.1 Carrier Gas, hydrogen or helium, chromatographic
standard,
grade.
A = area of impurity peak in calibration blend,
i
7.2 Compressed Air, oil free.
A = area of impurity in the stock o-xylene,
b
7.3 Hydrogen, chromatographic grade.
C = concentration of internal standard, weight %,
s
7.4 Nitrogen, chromatographic grade.
A = area of internal standard peak in calibration blend,
si
7.5 Pure compounds for calibration shall include n-nonane
A = area of internal standard peak in stock o-xylene, and
sb
(Note 1), toluene, styrene, ethylbenzene, p-xylene, m-xylene,
C = concentration of impurity, weight, %.
i
o-xylene, isopropylbenzene, isooctane, (Note 2), n-octane
10.5 Calculate response factors to the nearest 0.001.
(Note 2), n-undecane (Note 2), of a purity not less than 99 %.
If the purity of the calibration compounds is less than 99 %, the
11. Procedure
concentration and identification of impurities must be known
so that the composition of the final weighed blends can be 11.1 Install the chromatograph column and establish stable
adjusted for presence of the impurities. instrument operation at the operating conditions shown in
Table 1. Refer to instructions provided by the manufacturer of
NOTE 1—n-nonane rep
...