ASTM D5060-12(2021)e1
(Test Method)Standard Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography
Standard Test Method for Determining Impurities in High-Purity Ethylbenzene by Gas Chromatography
SIGNIFICANCE AND USE
4.1 The test is suitable for setting specifications on ethylbenzene and for use as an internal quality control tool where ethylbenzene is used in manufacturing processes. It may be used in development or research work involving ethylbenzene.
4.2 Purity is commonly reported by subtracting the determined expected impurities from 100 %. Absolute purity cannot be determined if unknown impurities are present.
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, p-xylene may not be detected.
1.3 In determining the performance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8.
1.6 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.
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Designation: D5060 − 12 (Reapproved 2021)
Standard Test Method for
Determining Impurities in High-Purity Ethylbenzene by Gas
Chromatography
This standard is issued under the fixed designation D5060; 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.
ε NOTE—Editorial changes were made throughout in January 2021.
1. Scope 2. Referenced Documents
1.1 This test method describes the analysis of normally 2.1 ASTM Standards:
occurring impurities in, and the purity of, ethylbenzene by gas D3437 Practice for Sampling and Handling Liquid Cyclic
chromatography. Impurities determined include nonaromatic Products
hydrocarbons, benzene, toluene, xylenes, cumene, and dieth- D4307 Practice for Preparation of Liquid Blends for Use as
ylbenzene isomers. Analytical Standards
D6809 Guide for Quality Control and Quality Assurance
1.2 This test method is applicable for impurities at concen-
Procedures for Aromatic Hydrocarbons and Related Ma-
trations from 0.001 to 1.000 % and for ethylbenzene purities of
terials
99 % or higher. At this level, p-xylene may not be detected.
E29 Practice for Using Significant Digits in Test Data to
1.3 In determining the performance of the test results using
Determine Conformance with Specifications
this method to applicable specifications, results shall be
E355 Practice for Gas Chromatography Terms and Relation-
rounded off in accordance with the rounding-off method of
ships
Practice E29.
E1510 Practice for Installing Fused Silica Open Tubular
1.4 The values stated in SI units are to be regarded as Capillary Columns in Gas Chromatographs
2.2 Other Documents:
standard. No other units of measurement are included in this
standard. OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1910.1200
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Summary of Test Method
responsibility of the user of this standard to establish appro-
3.1 A known amount of internal standard is added to the
priate safety, health, and environmental practices and deter-
sample.Agas chromatograph equipped with a flame ionization
mine the applicability of regulatory limitations prior to use.
detector and a polar fused silica capillary column is used for
For a specific hazard statement, see Section 8.
the analysis. The impurities are measured relative to the
1.6 This international standard was developed in accor-
internal standard. Ethylbenzene purity is calculated by sub-
dance with internationally recognized principles on standard-
tracting the impurities found from 100.00 %.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4. Significance and Use
mendations issued by the World Trade Organization Technical
4.1 The test is suitable for setting specifications on ethyl-
Barriers to Trade (TBT) Committee.
benzene and for use as an internal quality control tool where
1 2
This test method is under the jurisdiction of ASTM Committee D16 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
bility of Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10Aromatic Standards volume information, refer to the standard’s Document Summary page on
Hydrocarbons. the ASTM website.
Current edition approved Jan. 1, 2021. Published February 2021. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1990. Last previous edition approved in 2012 as D5060 – 12. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D5060-12R21E01. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5060 − 12 (2021)
ethylbenzene is used in manufacturing processes. It may be 8. Hazards
used in development or research work involving ethylbenzene.
8.1 Consult current OSHA regulations, supplier’s Safety
Data Sheets, and local regulations for all materials used in this
4.2 Purity is commonly reported by subtracting the deter-
mined expected impurities from 100 %.Absolute purity cannot test method.
be determined if unknown impurities are present.
9. Sampling
5. Interferences
9.1 Guidelines for taking samples from bulk are given in
Practice D3437.
5.1 A key operational parameter for this method is the
separation of p-xylene from ethylbenzene. Care should be
10. Calibration
taken during calibration to ensure the separation of these two
10.1 Prepare a calibration standard of ethylbenzene with
components. If p-xylene is not separated from ethylbenzene
impurities (listed in 7.5) at concentrations representative of
during the calibration of the instrument, modify the column
those expected in the samples to be analyzed as described in
flow rate slightly until separation is achieved.
Practice D4307.
6. Apparatus
10.2 Fill a 50-mL volumetric flask partially with the cali-
bration standard. With a microsyringe, add 30 µL of the
6.1 Gas Chromatograph (GC), any GC built for capillary
internalstandardn-undecane,andmakeuptothemarkwiththe
column chromatography and equipped with a flame ionization
calibration standard. Mix well. Using a density of 0.740 for
detector (FID). The system shall have sufficient sensitivity,
n-undecane and 0.867 for the calibration standard, this calibra-
linearity, and range to obtain a minimum peak height response
tion blend will contain 0.0512 mass % internal standard.
for 0.0010 mass % impurity of twice the height of the signal
background noise, while not exceeding the full scale of either 10.3 Fill a 50-mL volumetric flask to the mark with ethyl-
the detector or the electronic integration for the major compo- benzene.With a microsyringe add 30 µL(or proper size) of the
nents. It shall have a split injection system that will not internal standard n-undecane. Mix well. The resulting stock
discriminate over the boiling range of the samples analyzed. ethylbenzene solution will contain 0.0512 mass % internal
standard.
6.2 Chromatographic Column, fused silica capillary, 60 m
10.4 Analyze the calibration blend (10.2) as described in
long, 0.32-mm inside diameter, internally coated to a 0.5-µm
thickness with a bonded (crosslinked) polyethylene glycol. 11.3.
Other columns may be used after it has been established that
10.5 Analyze the stock ethylbenzene solution (10.3)as
such column is capable of separating all major impurities and
described in 11.3.
the internal standard from the ethylbenzene under operating
10.6 Calculate response factors as follows:
conditions appropriate for the column.
C
i
6.3 Chromato
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