ASTM D7360-16

Standard Test Method for Analysis of Benzene by Gas Chromatography with External Calibration (Withdrawn 2023)

SIGNIFICANCE AND USE
5.1 This test method is suitable for determining the concentrations of known impurities in finished benzene and for use as an integral quality control tool where benzene is either produced or used in a manufacturing procedure. It is generally applied to impurities such as nonaromatics containing nine carbons or less, toluene, C8 aromatics, and 1,4-dioxane.  
5.2 Absolute purity cannot be determined if undetected impurities are present.
SCOPE
1.1 This test method covers the determination of normally occurring trace impurities in, and the purity of, finished benzene by gas chromatography with external calibration. A similar test method, using the internal standard technique of calibration is Test Method D4492.  
1.2 This test method is applicable for nonaromatic hydrocarbon impurities at levels from 5 to 2000 mg/kg and for benzene purities of 99.80 weight % or higher.  
1.3 This test method is applicable for aromatic impurities from 5 to 2000 mg/kg in benzene.  
1.4 This test method has been found applicable to heteroatomic species such as 1,4-dioxane, from 10 to 2000 mg/kg in benzene.  
1.5 The limit of detection for aromatic impurities is 0.9 mg/kg, 2.7 mg/kg for 1,4-dioxane and 1.1 mg/kg for methyl cyclohexane.  
1.6 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.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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 9.
WITHDRAWN RATIONALE
This Test Method covered the determination of normally occurring trace impurities in, and the purity of, finished benzene by gas chromatography with external calibration.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, this test method was withdrawn in August 2023 and replaced by Test Method D7504 on trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number.1

General Information

• Status: Withdrawn
• Publication Date: 31-Oct-2016
• 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

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: D7360 − 16
Standard Test Method for
Analysis of Benzene by Gas Chromatography with External
1
Calibration
This standard is issued under the fixed designation D7360; 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* 2. Referenced Documents
2
1.1 This test method covers the determination of normally 2.1 ASTM Standards:
occurring trace impurities in, and the purity of, finished D3437 Practice for Sampling and Handling Liquid Cyclic
benzene by gas chromatography with external calibration. A Products
similar test method, using the internal standard technique of D3798 Test Method for Analysis of p-Xylene by Gas Chro-
3
calibration is Test Method D4492. matography (Withdrawn 2009)
D4307 Practice for Preparation of Liquid Blends for Use as
1.2 This test method is applicable for nonaromatic hydro-
Analytical Standards
carbon impurities at levels from 5 to 2000 mg/kg and for
D4492 Test Method for Analysis of Benzene by Gas Chro-
benzene purities of 99.80 weight % or higher.
matography
1.3 This test method is applicable for aromatic impurities D4790 Terminology of Aromatic Hydrocarbons and Related
from 5 to 2000 mg/kg in benzene.
Chemicals
D6809 Guide for Quality Control and Quality Assurance
1.4 This test method has been found applicable to hetero-
Procedures for Aromatic Hydrocarbons and Related Ma-
atomic species such as 1,4-dioxane, from 10 to 2000 mg/kg in
terials
benzene.
E29 Practice for Using Significant Digits in Test Data to
1.5 The limit of detection for aromatic impurities is 0.9
Determine Conformance with Specifications
mg/kg, 2.7 mg/kg for 1,4-dioxane and 1.1 mg/kg for methyl
E177 Practice for Use of the Terms Precision and Bias in
cyclohexane.
ASTM Test Methods
E260 Practice for Packed Column Gas Chromatography
1.6 In determining the conformance of the test results using
E355 Practice for Gas Chromatography Terms and Relation-
this method to applicable specifications, results shall be
ships
rounded off in accordance with the rounding-off method of
E1510 Practice for Installing Fused Silica Open Tubular
Practice E29.
Capillary Columns in Gas Chromatographs
1.7 The values stated in SI units are to be regarded as 4
2.2 Other Document:
standard. No other units of measurement are included in this
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
standard.
1910.1200
1.8 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1 See Terminology D4790 for definition of terms used in
priate safety and health practices and determine the applica-
this test method.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 9.
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
1
This test method is under the jurisdiction of ASTM Committee D16 on Standards volume information, refer to the standard’s Document Summary page on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of the ASTM website.
3
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and Their The last approved version of this historical standard is referenced on
Derivatives. www.astm.org.
4
Current edition approved Nov. 1, 2016. Published January 2017. Originally Available from U.S. Government Printing Office Superintendent of Documents,
approved in 2011. Last previous edition approved in 2011 as D7360 – 11. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D7360-16. www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7360 − 16
FIG. 1 Typical Chromatogram
TABLE 1 Typical Instrumental Parameters
Detector flame ionization
4. Summary of Test Method
Column: fused silica
Length 50 m
4.1 A repeatable volume of the specimen to be analyzed is
Inside diameter 0.32 mm
precisely injected into a gas chromatograph equipped with a
Stationary phase crosslinked polyethylene
glycol
flame ionization detector (FID) and a capillary column.
Film thickness 0.25 µm
4.2 The peak area of each impurity is measured. The Temperatures:
Injector 200°C
concentration of each impurity is determined using response
Detector 250°C
factor or the linear calibration curve of peak area versus
Column 70°C isothermal
concentra
...