ASTM D5060-95(2000)

Standard Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography

SCOPE
1.1 This test method describes the analysis of normally occurring impurities in, and the purity of, ethylbenzene by gas chromatography. Impurities determined include nonaromatic hydrocarbons, benzene, toluene, xylenes, cumene, and diethylbenzene isomers.  
1.2 This test method is applicable for impurities at concentrations from 0.001 to 1.000% and for ethylbenzene purities of 99% or higher. At this level, -xylene may not be detected.
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: D16.07 - Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons

Relations

• Replaced By: ASTM D5060-95(2000)e1 - Standard Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography
• Effective Date: 15-May-1995
• Referred By: ASTM D3193-19 - Standard Specification for Ethylbenzene
• Effective Date: 10-Jun-2000
• Referred By: ASTM D7504-23 - Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number
• Effective Date: 10-Jun-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5060 – 95 (Reapproved 2000)
Standard Test Method for
Determining Impurities in High-Purity Ethylbenzene by Gas
Chromatography
This standard is issued under the fixed designation D 5060; 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 describes the analysis of normally
1910.1200
occurring impurities in, and the purity of, ethylbenzene by gas
chromatography. Impurities determined include nonaromatic
3. Summary of Test Method
hydrocarbons, benzene, toluene, xylenes, cumene, and dieth-
3.1 A known amount of internal standard is added to the
ylbenzene isomers.
sample. A gas chromatograph equipped with a flame ionization
1.2 This test method is applicable for impurities at concen-
detector and a polar fused silica capillary column is used for
trations from 0.001 to 1.000 % and for ethylbenzene purities of
the analysis. The impurities are measured relative to the
99 % or higher. At this level, p-xylene may not be detected.
internal standard. Ethylbenzene purity is calculated by sub-
1.3 The following applies to all specified limits in this
tracting the impurities found from 100.00 %.
standard: for purposes of determining conformance with this
standard, an observed value or a calculated value shall be
4. Significance and Use
rounded off “to the nearest unit” in the last right-hand digit
4.1 The test is suitable for setting specifications on ethyl-
used in expressing the specification limit, in accordance with
benzene and for use as an internal quality control tool where
the rounding-off method of Practice E 29.
ethylbenzene is used in manufacturing processes. It may be
1.4 This standard does not purport to address all of the
used in development or research work involving ethylbenzene.
safety concerns, if any, associated with its use. It is the
4.2 Purity is commonly reported by subtracting the deter-
responsibility of the user of this standard to establish appro-
mined expected impurities from 100 %. Absolute purity cannot
priate safety and health practices and determine the applica-
be determined if unknown impurities are present.
bility of regulatory limitations prior to use. For a specific
hazard statement, see Section 7.
5. Apparatus
5.1 Gas Chromatograph—Any gas chromatograph having a
2. Referenced Documents
flame ionization detector and a splitter injector suitable for use
2.1 ASTM Standards:
with a fused-silica capillary column may be used, provided the
D 3437 Practice for Sampling and Handling Liquid Cyclic
system has sufficient sensitivity to obtain a minimum peak
Products
height response of 0.1 mV for 0.010 % internal standard when
D 4307 Practice for Preparation of Liquid Blends for Use as
operated at the stated conditions. Background noise at these
Analytical Standards
conditions is not to exceed 3 μV.
E 29 Practice for Using Significant Digits in Test Data to
5.2 Chromatographic Column, fused silica capillary, 60 m
Determine Conformance with Specifications
long, 0.32-mm inside diameter, internally coated to a 0.5-μm
E 355 Practice for Gas Chromatography Terms and Rela-
thickness with a bonded (crosslinked) polyethylene glycol.
tionships
Other columns may be used after it has been established that
E 1510 Practice for Installing Fused Silica Open Tubular
4 such column is capable of separating all major impurities and
Capillary Columns in Gas Chromatographs
the internal standard from the ethylbenzene under operating
conditions appropriate for the column.
5.3 Recorder, 1-mV,1sor less full scale response or
This test method is under the jurisdiction of ASTM Committee D16 on
electronic integration with tangent capabilities (recom-
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.07 on Styrene, Ethylbenzene, and C and C Aromatic mended).
9 10
Hydrocarbons.
5.4 Microsyringe, 10-μL.
Current edition approved May 15, 1995. Published July 1995. Originally
published as D 5090 – 90. Last previous edition D 5090 – 90.
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 2O402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5060 – 95 (2000)
5.5 Microsyringe, 50-μL. 10. Procedure
5.6 Volumetric Flask, 50-mL.
10.1 Install the chromatographic column and establish
stable instrument operation at the operating conditions shown
6. Reagents and Materials
in Table 1. Refer to instructions provided by the manufacturer
of the gas chromatograph and Practices E 355 and E 1510.
6.1 Carrier Gas, hydrogen or helium, chromatographic
10.2 Fill a 50-mL volumetric flask to the mark with test
grade.
specimen. With a microsyringe, add 30 μL of the standard. Mix
6.2 Compressed Air, oil-free.
well. Using a density of 0.740 for n-undecane and 0.867 for
6.3 Hydrogen, chromatographic grade.
ethylbenzene, this solution will contain 0.0512 weight %
6.4 Nitrogen, chromatographic grade.
internal standard.
6.5 Pure Compounds for Calibration—n-Nonane, benzene,
10.3 Inject 0.6 μL of solution into the gas chromatograph
toluene, ethylbenzene, and o-xylene. The purity of the ethyl-
and obtain the chromatogram. A typical chromatogram is
benzene should be 99.8 % or better. The ethylbenzene must be
shown
...