ASTM D7266-23
(Test Method)Standard Test Method for Analysis of Cyclohexane by Gas Chromatography (External Standard)
Standard Test Method for Analysis of Cyclohexane by Gas Chromatography (External Standard)
SIGNIFICANCE AND USE
5.1 This test method is suitable for setting specifications on the materials referenced in Table 1 and for use as an internal quality control tool where cyclohexane is produced or is used in a manufacturing process. It may also be used in development or research work involving cyclohexane.
5.2 This test method is useful in determining the purity of cyclohexane with normal impurities present. If extremely high boiling or unusual impurities are present in the cyclohexane, this test method would not necessarily detect them and the purity calculation would be erroneous.
SCOPE
1.1 This test method covers the determination of the purity of cyclohexane by gas chromatography.
1.2 This test method is applicable to the measurement of impurities in Table 1. This test method is applicable to samples with concentrations to 400 mg/kg, but may be applicable to a wider range. The limit of detection (LOD) is 1 mg/kg and the limit of quantitation (LOQ) is 3 mg/kg for benzene.
Note 1: The LOD and LOQ were calculated from the ILS data for benzene.
1.3 The following applies for the purposes of determining the conformance of the test results using this test 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 specific hazard statements, 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
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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.
Designation: D7266 − 23
Standard Test Method for
Analysis of Cyclohexane by Gas Chromatography (External
1
Standard)
This standard is issued under the fixed designation D7266; 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
2.1 ASTM Standards:
1.1 This test method covers the determination of the purity
of cyclohexane by gas chromatography. D3437 Practice for Sampling and Handling Liquid Cyclic
Products
1.2 This test method is applicable to the measurement of
D4307 Practice for Preparation of Liquid Blends for Use as
impurities in Table 1. This test method is applicable to samples
Analytical Standards
with concentrations to 400 mg/kg, but may be applicable to a
D4790 Terminology of Aromatic Hydrocarbons and Related
wider range. The limit of detection (LOD) is 1 mg/kg and the
Chemicals
limit of quantitation (LOQ) is 3 mg/kg for benzene.
D6809 Guide for Quality Control and Quality Assurance
NOTE 1—The LOD and LOQ were calculated from the ILS data for
Procedures for Aromatic Hydrocarbons and Related Ma-
benzene.
terials
1.3 The following applies for the purposes of determining E29 Practice for Using Significant Digits in Test Data to
the conformance of the test results using this test method to Determine Conformance with Specifications
applicable specifications, results shall be rounded off in accor- E355 Practice for Gas Chromatography Terms and Relation-
dance with the rounding-off method of Practice E29. ships
E691 Practice for Conducting an Interlaboratory Study to
1.4 The values stated in SI units are to be regarded as
Determine the Precision of a Test Method
standard. No other units of measurement are included in this
E1510 Practice for Installing Fused Silica Open Tubular
standard.
Capillary Columns in Gas Chromatographs
1.5 This standard does not purport to address all of the
2.2 Other Document:
safety concerns, if any, associated with its use. It is the
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
responsibility of the user of this standard to establish appro-
3
1910.1200
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3. Terminology
For specific hazard statements, see Section 8.
3.1 See Terminology D4790 for definitions of terms used in
1.6 This international standard was developed in accor-
this test method.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
4.1 Cyclohexane is analyzed using a gas chromatograph
mendations issued by the World Trade Organization Technical
(GC) equipped with a flame ionization detector (FID). A
Barriers to Trade (TBT) Committee.
precisely repeatable volume of the sample to be analyzed is
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 D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and Standards volume information, refer to the standard’s Document Summary page on
Their Derivatives. the ASTM website.
3
Current edition approved July 1, 2023. Published July 2023. Originally approved Available from U.S. Government Printing Office Superintendent of Documents,
ε1
in 2007. Last previous edition approved in 2018 as D7266 – 13 (2018) . DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D7266-23. 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
1
---------------------- Page: 1 ----------------------
D7266 − 23
TABLE 1 Impurities Known or Suggested to be Present in TABLE 2 Recommended Operating Conditions
Commercial Cyclohexane
Detector flame ionization
Injection Port capillary splitter
C
4
Column A:
(1) n-butane
Tubing fused silica
(2) isobutene
Stationary phase bonded and crosslinked
C
5
100 % dimethylpolysiloxane
(3) n-pentane
Film thickness, μm 0.5
(4) isopentane
Length, m 100
(5) cyclopentane
Diameter, mm 0.25
C
6
Temperatures:
(6) n-hexane
Injector, °C 230
(7) 2-methylpentane
Detector, °C 250
(8)
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D7266 − 13 (Reapproved 2018) D7266 − 23
Standard Test Method for
Analysis of Cyclohexane by Gas Chromatography (External
1
Standard)
This standard is issued under the fixed designation D7266; 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
ε NOTE—Section 8 was editorially corrected in January 2018.
1. Scope Scope*
1.1 This test method covers the determination of the purity of cyclohexane by gas chromatography. Calibration of the gas
chromatography system is done by the external standard calibration technique.
1.2 This test method has been found is applicable to the measurement of impurities such as those found in Table 1, which are
impurities that may be found in cyclohexane. The impurities can be analyzed over a range of 3 to 200 mg/kg by this method, but
may be applicable to a wider range. This test method is applicable to samples with concentrations to 400 mg/kg, but may be
applicable to a wider range. The limit of detection (LOD) is 1 mg/kg and the limit of quantitation (LOQ) is 3 mg/kg for benzene.
NOTE 1—The LOD and LOQ were calculated from the ILS data for benzene.
1.3 The limit of detection is 1 mg/kg.
1.3 In The following applies for the purposes of determining the conformance of the test results using this test 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 specific hazard statements, 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D3437 Practice for Sampling and Handling Liquid Cyclic Products
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and Their Derivatives.
Current edition approved Jan. 1, 2018July 1, 2023. Published January 2018July 2023. Originally approved in 2007. Last previous edition approved in 20132018 as D7266
ε1
– 13 (2018) . DOI: 10.1520/D7266-13R18E01.10.1520/D7266-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
1
---------------------- Page: 1 ----------------------
D7266 − 23
TABLE 1 Impurities Known or Suggested to be Present in
Commercial Cyclohexane
C
4
(1) n-butane
(2) isobutene
C
5
(3) n-pentane
(4) isopentane
(5) cyclopentane
C
6
(6) n-hexane
(7) 2-methylpentane
(8) 3-methylpentane
(9) methylcyclopentane
(10) benzene
(11) cyclohexene
(12) 2,2-dimethylbutane
(13) 2,3-dimethylbutane
C
7
(14) 3,3-dimethylpentane
(15) 2,2-dimethylpentane
(16) 2,3-dimethylpentane
(17) 2,4-dimethylpentane
(18) 1,1-dimethylcyclopentane
(19) trans-1,3-dimethylcyclopentane
(20) trans-1,2-dimethylcyclopentane
(21) cis-1,2-dimethylcyclopentane
(22) 2,2-dimethylcyclopentane
(23) 2,4-dimethylcyclopentane
(24) cis-1,3-dimethylcyclopentane
(25) ethylcyclopentane
(26) methylcyclohexane
(27) 3-ethylpentane
(28) 3-methylhexane
(29) 2-methylhexane
(30) n-heptane
(31) toluene
C
8
(32) iso-octane
(33) p-xylene
C
9
(34) isopropylcylohexane
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality As
...
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