ASTM D7266-13
(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. Calibration of the gas chromatography system is done by the external standard calibration technique.
1.2 This test method has been found 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.TABLE 1 Impurities Known or Suggested to be Present in Commercial Cyclohexane
C4
(1) n-butane
(2) isobutene
C5
(3) n-pentane
(4) isopentane
(5) cyclopentane
C6
(6) n-hexane
(7) 2-methylpentane
(8) 3-methylpentane
(9) methylcyclopentane
(10) benzene
(11) cyclohexene
(12) 2,2-dimethylbutane
(13) 2,3-dimethylbutane
C7
(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
C8
(32) iso-octane
(33) p-xylene
C9
(34) isopropylcylohexane
1.3 The limit of detection is 1 mg/kg.
1.4 In 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.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.
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Designation: D7266 − 13
StandardTest 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* Analytical Standards
D4790 Terminology ofAromatic Hydrocarbons and Related
1.1 This test method covers the determination of the purity
Chemicals
of cyclohexane by gas chromatography. Calibration of the gas
D6809 Guide for Quality Control and Quality Assurance
chromatography system is done by the external standard
Procedures for Aromatic Hydrocarbons and Related Ma-
calibration technique.
terials
1.2 This test method has been found applicable to the
E29 Practice for Using Significant Digits in Test Data to
measurement of impurities such as those found in Table 1,
Determine Conformance with Specifications
which are impurities that may be found in cyclohexane. The
E355 Practice for Gas Chromatography Terms and Relation-
impurities can be analyzed over a range of 3 to 200 mg/kg by
ships
this method, but may be applicable to a wider range.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.3 The limit of detection is 1 mg/kg.
E1510 Practice for Installing Fused Silica Open Tubular
1.4 In determining the conformance of the test results using
Capillary Columns in Gas Chromatographs
this test method to applicable specifications, results shall be
2.2 Other Document:
rounded off in accordance with the rounding-off method of
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
Practice E29.
3
1910.1200
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 See Terminology D4790 for definitions of terms used in
1.6 This standard does not purport to address all of the
this test method.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Cyclohexane is analyzed using a gas chromatograph
bility of regulatory limitations prior to use. For specific hazard
(GC) equipped with a flame ionization detector (FID). A
statements, see Section 7.
precisely repeatable volume of the sample to be analyzed is
2. Referenced Documents
injected onto the gas chromatograph. The peak areas of the
2 impurities are measured and converted to concentrations via an
2.1 ASTM Standards:
external standard methodology. Purity by GC (the cyclohexane
D3437 Practice for Sampling and Handling Liquid Cyclic
content) is calculated by subtracting the sum of the impurities
Products
from 100.00. Individual impurities are reported in mg/kg. The
D4307 Practice for Preparation of Liquid Blends for Use as
cyclohexane purity is reported in weight percent.
5. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
5.1 This test method is suitable for setting specifications on
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and Their
the materials referenced in Table 1 and for use as an internal
Derivatives.
Current edition approved Feb. 1, 2013. Published March 2013. Originally quality control tool where cyclohexane is produced or is used
ε1
approved in 2007. Last previous edition approved in 2007 as D7266 – 07 . DOI:
10.1520/D7266-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. 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 − 13
TABLE 1 Impurities Known or Suggested to be Present in TABLE 2 Instrumental Parameters
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
...
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 − 07 D7266 − 13
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—Table 2 was corrected editorially in July 2008.
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 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 53 to 180200 mg/kg by this method,
but may be applicable to a wider range.
1.3 The limit of detection is 1 mg/kg.
1.4 In 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.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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:
D3437 Practice for Sampling and Handling Liquid Cyclic Products
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 Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E355 Practice for Gas Chromatography Terms and Relationships
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,CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D4790 for definitions of terms used in this test method.
4. Summary of Test Method
4.1 Cyclohexane is analyzed using a gas chromatograph (GC) equipped with a flame ionization detector (FID). A precisely
repeatable volume of the sample to be analyzed is injected onto the gas chromatograph. The peak areas of the impurities are
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons 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, 2007Feb. 1, 2013. Published January 2007March 2013. Originally approved in 2007. Last previous edition approved in 2007 as D7266
ε1
– 07 . DOI: 10.1520/D7266-07E01.10.1520/D7266-13.
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.
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.
*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 − 13
measured and converted to concentrations via an external standard methodology. Purity by GC (the cyclohexane content) is
calculated by subtracting the sum of the impurities from 100.00. Individual impurities are reported in mg/kg. The cyclohexane
purity is reported in weight percent.
5. 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 m
...
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