ASTM D7011-10a

Standard Test Method for Determination of Trace Thiophene in Refined Benzene by Gas Chromatography and Sulfur Selective Detection

SIGNIFICANCE AND USE
Accurate gas chromatographic determination of trace levels of thiophene in benzene involves special analytical problems because of the difficulties of trace level analysis. These problems arise from the low concentration levels that need to be measured, the type of column and detector needed for analysis, and the potential interference from the benzene matrix.
This test method was found applicable for determining thiophene in refined benzene conforming to the specifications described in Specifications D2359, D4734, and D5871 and may be applicable toward other grades of benzene if the user has taken the necessary precautions as described in the text.
This test method was developed as an alternative technique to Test Methods D1685 and D4735.
SCOPE
1.1 This test method covers the determination of thiophene in refined benzene using gas chromatography and sulfur selective detection. The test method is applicable to the determination of thiophene at levels of 0.02 to 2.18 mg thiophene per kg in benzene (mg/kg) on the AED, 0.03 to 1.87 mg/kg on the PFPD, and 0.03 to 2.11 mg/kg on the SCD. The range of the test method may be extended by modifying the sample injection volume, split ratios, calibration range, or sample dilution with thiophene-free solvent.
1.2 In determining the conformance 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.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 specific hazard statements, see Section 7.

General Information

• Status: Historical
• Publication Date: 31-May-2010
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D7011 −10a
StandardTest Method for
Determination of Trace Thiophene in Refined Benzene by
1
Gas Chromatography and Sulfur Selective Detection
This standard is issued under the fixed designation D7011; 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.
1. Scope D3437 Practice for Sampling and Handling Liquid Cyclic
Products
1.1 This test method covers the determination of thiophene
D4734 Specification for Refined Benzene-545
in refined benzene using gas chromatography and sulfur
D4735 Test Method for Determination of Trace Thiophene
selective detection. The test method is applicable to the
in Refined Benzene by Gas Chromatography
determination of thiophene at levels of 0.02 to 2.18 mg
D5871 Specification for Benzene for Cyclohexane Feed-
thiophene per kg in benzene (mg/kg) on theAED, 0.03 to 1.87
stock
mg/kg on the PFPD, and 0.03 to 2.11 mg/kg on the SCD. The
D6809 Guide for Quality Control and Quality Assurance
range of the test method may be extended by modifying the
Procedures for Aromatic Hydrocarbons and Related Ma-
sample injection volume, split ratios, calibration range, or
terials
sample dilution with thiophene-free solvent.
E29 Practice for Using Significant Digits in Test Data to
1.2 In determining the conformance of the test results using
Determine Conformance with Specifications
this method to applicable specifications, results shall be
E177 Practice for Use of the Terms Precision and Bias in
rounded off in accordance with the rounding-off method of
ASTM Test Methods
Practice E29.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this E1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
standard.
2.2 Other Document:
1.4 This standard does not purport to address all of the
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
safety concerns, if any, associated with its use. It is the
4
1910.1200
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3. Summary of Test Method
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 7. 3.1 The thiophene concentration in refined benzene is de-
termined at the sub-mg/kg to low mg/kg level using conven-
2. Referenced Documents
tional gas chromatography with a sulfur selective detector. A
2
reproducible volume of sample is injected. Quantitative results
2.1 ASTM Standards:
are obtained by the use of the external standard calibration
D1193 Specification for Reagent Water
technique.
D1685 Test Method for Traces of Thiophene in Benzene by
3
Spectrophotometry (Withdrawn 2009)
3.2 The method allows the use of a sulfur chemilumines-
D2359 Specification for Refined Benzene-535
cence detector, atomic emission detector, pulsed flame photo-
metric detector, or any other sulfur selective detector provided
that its performance meets requirements as set forth in 5.4.As
1
This test method is under the jurisdiction of ASTM Committee D16 on
sulfur compounds elute from the gas chromatographic column,
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
they are detected and quantified. While the benzene molecule
Subcommittee D16.04 on Instrumental Analysis.
Current edition approved Dec. 1, 2010. Published December 2010. Originally does not contain any sulfur atoms, the possibility of matrix
approved in 2004. Last previous edition approved in 2010 as D7011 – 10. DOI:
quenching and interference is a concern, especially for thio-
10.1520/D7011-10A.
phene determination at levels less than about 0.5 mg/kg. The
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4
the ASTM website. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
3
The last approved version of this historical standard is referenced on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.astm.org. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D7011−10a
column and conditions specified in Table 1 yield acceptable 5.4 Detector—A sulfur selective detector is used and shall
results with minimal matrix quenching and interference.
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D7011–10 Designation: D7011 – 10a
Standard Test Method for
Determination of Trace Thiophene in Refined Benzene by
1
Gas Chromatography and Sulfur Selective Detection
This standard is issued under the fixed designation D7011; 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.
1. Scope
1.1 This test method covers the determination of thiophene in refined benzene using gas chromatography and sulfur selective
detection.The test method is applicable to the determination of thiophene at levels of 0.02 to 2.18 mg thiophene per kg in benzene
(mg/kg) on the AED, 0.03 to 1.87 mg/kg on the PFPD, and 0.03 to 2.11 mg/kg on the SCD. The range of the test method may
be extended by modifying the sample injection volume, split ratios, calibration range, or sample dilution with thiophene-free
solvent.
1.2 In determining the conformance 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.
1.3The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 specific hazard statements, see Section 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1685 Test Method for Traces of Thiophene in Benzene by Spectrophotometry
D2359 Specification for Refined Benzene-535
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D4734 Specification for Refined Benzene-545
D4735 Test Method for Determination of Trace Thiophene in Refined Benzene by Gas Chromatography
D5871 Specification for Benzene for Cyclohexane Feedstock
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
2.2 Other Document:
3
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 The thiophene concentration in refined benzene is determined at the sub-mg/kg to low mg/kg level using conventional gas
chromatography with a sulfur selective detector.Areproducible volume of sample is injected. Quantitative results are obtained by
the use of the external standard calibration technique.
3.2 The method allows the use of a sulfur chemiluminescence detector, atomic emission detector, pulsed flame photometric
detector, or any other sulfur selective detector provided that its performance meets requirements as set forth in 5.4. As sulfur
1
This test method is under the jurisdiction ofASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.04 on Instrumental Analysis.
Current edition approved JuneDec. 1, 2010. Published JuneDecember 2010. Originally approved in 2004. Last previous edition approved in 20042010 as D7011 - 104.
DOI: 10.1520/D7011-10A.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D7011 – 10a
compounds elute from the gas chromatographic column, they are detected and quantified. While the benzene molecule does not
contain any sulfur atoms,
...