ASTM D7266-13(2018)e1

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.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.  
1.7 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

• Status: Historical
• Publication Date: 31-Dec-2017
• ICS: 71.080.10 - Aliphatic 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
´1
Designation: D7266 − 13 (Reapproved 2018)
Standard Test Method for
Analysis of Cyclohexane by Gas Chromatography (External
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.
ε NOTE—Section 8 was editorially corrected in January 2018.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of the purity
D3437 Practice for Sampling and Handling Liquid Cyclic
of cyclohexane by gas chromatography. Calibration of the gas
Products
chromatography system is done by the external standard
D4307 Practice for Preparation of Liquid Blends for Use as
calibration technique.
Analytical Standards
1.2 This test method has been found applicable to the
D4790 Terminology of Aromatic Hydrocarbons and Related
measurement of impurities such as those found in Table 1,
Chemicals
which are impurities that may be found in cyclohexane. The
D6809 Guide for Quality Control and Quality Assurance
impurities can be analyzed over a range of 3 to 200 mg/kg by
Procedures for Aromatic Hydrocarbons and Related Ma-
this method, but may be applicable to a wider range.
terials
E29 Practice for Using Significant Digits in Test Data to
1.3 The limit of detection is 1 mg/kg.
Determine Conformance with Specifications
1.4 In determining the conformance of the test results using
E355 Practice for Gas Chromatography Terms and Relation-
this test method to applicable specifications, results shall be
ships
rounded off in accordance with the rounding-off method of
E691 Practice for Conducting an Interlaboratory Study to
Practice E29.
Determine the Precision of a Test Method
E1510 Practice for Installing Fused Silica Open Tubular
1.5 The values stated in SI units are to be regarded as
Capillary Columns in Gas Chromatographs
standard. No other units of measurement are included in this
standard. 2.2 Other Document:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.6 This standard does not purport to address all of the
1910.1200
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety, health, and environmental practices and deter-
3.1 See Terminology D4790 for definitions of terms used in
mine the applicability of regulatory limitations prior to use.
this test method.
For specific hazard statements, see Section 8.
1.7 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
4.1 Cyclohexane is analyzed using a gas chromatograph
ization established in the Decision on Principles for the
(GC) equipped with a flame ionization detector (FID). A
Development of International Standards, Guides and Recom-
precisely repeatable volume of the sample to be analyzed is
mendations issued by the World Trade Organization Technical
injected onto the gas chromatograph. The peak areas of the
Barriers to Trade (TBT) Committee.
impurities are measured and converted to concentrations via an
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 [e-mail]. 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.
Current edition approved Jan. 1, 2018. Published January 2018. Originally Available from U.S. Government Printing Office Superintendent of Documents,
ε1
approved in 2007. Last previous edition approved in 2013 as D7266 – 13 . DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D7266-13R18E01. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D7266 − 13 (2018)
TABLE 1 Impurities Known or Suggested to be Present in TABLE 2 Instrumental Parameters
Commercial Cyclohexane
Detector flame ionization
Injection Port capillary splitter
C
Column A:
(1) n-butane
Tubing fused silica
(2) isobutene
C Stationary phase bonded and crosslinked
100 % dimethylpolysiloxane
(3) n-pentane
Film thickness, µm 0.5
(4) isopentane
Length, m 100
(5) cyclopentane
Diameter, mm 0.25
C
Temperatures:
(6) n-hexane
Injector, °C 230
(7) 2-methylpentane
Detector, °C 250
(8) 3-methylpentane
Oven, °C 32 hold for 12 min
(9) methylcyclopentane
Ramp 1 = 8°C/min to 64°C,
(10) benzene
hold for 10 min
(11) cyclohexene
Ramp 2 = 10°C/min to
(12) 2,2-dimethylbutane
200°C, hold for 5 min
(13) 2,3-dimethylbutane
Carrier gas Hydrogen
C
Flow rate, mls/min 3
(14) 3,3-dimethylpentane
Split ratio 100:1
(15) 2,2-dimethylpentane
Sample size, µl 1.0
(16) 2,3-dimethylpentane
(17) 2,4-dimethylpentane
(18) 1,1-dimethylcyclopentane
(19) trans-1,3-dimethylcyclopentane
(20) trans-1,2-dimethylcyclopentane
6.2 Columns—The choice of column is based on resolution
(21) cis-1,2-dimethylcyclopentane
requirements. Any column may be used that is capable of
(22) 2,2-dimethylcyclopentane
(23) 2,4-dimethylcyclopentane resolving all significant impurities from cyclohexane. The
(24) cis-1,3-dimethylcyclopentane
column described in Table 2 has been used successfully.
(25) ethylcyclopentane
(26) methylcyclohexane
6.3 Recorder—Electronic integration is required.
(27) 3-ethylpentane
6.4 Injector—The specimen must be precisely and repeat-
(28) 3-methylhexane
(29) 2-methylhexane
ably injected into the gas chromatograph. An automatic sample
(30) n-heptane
injection device is highly recommended. Manual injection can
(31) toluene
C be employed if the precision stated in Tables 3–7 can be
(32) iso-octane
reliably and consistently satisfied.
(33) p-xylene
C
7. Reagents and Materials
(34) isopropylcylohexane
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
external standard methodology. Purity by GC (the cyclohexane
where such specifications are available. Other grades may be
content) is calculated by subtracting the sum of the impurities
used, provided it is first ascertained that the reagent is of
from 100.00. Individual impurities are reported in mg/kg. The
sufficiently high purity to permit its use without lessening the
cyclohexane purity is reported in weight percent.
accuracy of the determination.
5. Significance and Use
7.2 Gases—Helium, hydrogen, nitrogen, or other as carrier.
5.1 This test method is suitable for setting specifications on
Carrier, makeup, and detector gases (except air) 99.999 %
the materials referenced in Table 1 and for use as an internal minimum purity. Oxygen in carrier gas less than 1 ppm, less
quality control tool where cyclohexane is produced or is used
than 0.5 ppm is preferred. Purify carrier, makeup, and detector
in a manufacturing process. It may also be used in development gases to remove oxygen, water, and hydrocarbons. Purify air to
or research work involving cyclohexane.
remove hydrocarbons and water, and the air used for an FID
should contain less than 0.1 ppm total hydrocarbons.
5.2 This test method is useful in determining the purity of
cyclohexane with normal impurities present. If extremely high
8. Hazards
boiling or unusual impurities are present in the cyclohexane,
8.1 Consult current OSHA regulations, suppliers’ Safety
this test method would not necessarily detect them and the
Data Sheets, and local regulations for all materials listed in this
purity calculation would be erroneous.
test method.
6. Apparatus
6.1 Gas Chromatograph—Any instrument having a flame
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
ionization detector that can be operated at the conditions given
listed by the American Chemical Society, see Analar Standards for Laboratory
in Table 2. The system should have sufficien
...

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 ´1
Designation: D7266 − 13 D7266 − 13 (Reapproved 2018)
Standard Test Method for
Analysis of Cyclohexane by Gas Chromatography (External
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.
ε NOTE—The number of samples in Section 15.1 was corrected editorially in April 2013.Section 8 was editorially cor-
rected 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 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.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 78.
1.7 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
2.1 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:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D4790 for definitions of terms used in this test method.
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons 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 Feb. 1, 2013Jan. 1, 2018. Published March 2013January 2018. Originally approved in 2007. Last previous edition approved in 20072013 as
ε1
D7266 – 0713 . DOI: 10.1520/D7266-13E01.10.1520/D7266-13R18E01.
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’sstandard’s Document Summary page on the ASTM website.
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
D7266 − 13 (2018)
TABLE 1 Impurities Known or Suggested to be Present in
Commercial Cyclohexane
C
(1) n-butane
(2) isobutene
C
(3) n-pentane
(4) isopentane
(5) cyclopentane
C
(6) n-hexane
(7) 2-methylpentane
(8) 3-methylpentane
(9) methylcyclopentane
(10) benzene
(11) cyclohexene
(12) 2,2-dimethylbutane
(13) 2,3-dimethylbutane
C
(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
(32) iso-octane
(33) p-xylene
C
(34) isopropylcylohexane
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
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 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.
6. Apparatus
6.1 Gas Chromatograph—Any instrument having a flame ionization detector that can be operated at the conditions given in
Table 2. The system should have sufficient sensitivity to obtain a minimum peak height response for 1 mg/kg benzene of twice
the height of the signal background noise.
6.2 Columns—The choice of column is based on resolution requirements. Any column may be used that is capable of resolving
all significant impurities from cyclohexane. The column described in Table 2 has been used successfully.
6.3 Recorder—Electronic integration is required.
´1
D7266 − 13 (2018)
TABLE 2 Instrumental Parameters
Detector flame ionization
Injection Port capillary splitter
Column A:
Tubing fused silica
Stationary phase bonded and crosslinked
100 % dimethylpolysiloxane†
Stationary phase bonded and crosslinked
100 % dimethylpolysiloxane
Film thickness, μm 0.5
Length, m 100
Diameter, mm 0.25
Temperatures:
Injector, °C 230
Detector, °C 250
Oven, °C 32 hold for 12 min
Ramp 1 = 8°C/min to 64°C,
hold for 10 min
Ramp 2 = 10°C/min to
200°C, hold for 5 min
Carrier gas Hydrogen
Flow rate, mls/min 3
Split ratio 100:1
Sample size, μl 1.0
† Corrected editorially.
6.4 Injector—The specimen must be precisely and repeatably injected into the gas chromatograph. An automatic sample
injection device is highly recommended. Manual injection can be employed if the precision stated in Tables 3–7 can be reliably
and consistently satisfied.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
7.2 Gases—Helium, hydrogen, nitrogen, or other as carrier. Carrier, makeup, and detector gases (except air) 99.999 % minimum
purity. Oxygen in carrier gas less than 1 ppm, less than 0.5 ppm is preferred. Purify carrier, makeup, and detector gases to remove
oxygen, water, and hydrocarbons. Purify air to remove hydrocarbons and water, and the air used for an FID should contain less
than 0.1 ppm total hydrocarbons.
8. Hazards
8.1 Consult current OSHA regulations, suppliers’ Material Safety Data Sheets, and local regulations for all materials
...