ASTM D7266-13e1
(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.
General Information
Relations
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
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—The number of samples in Section 15.1 was corrected editorially in April 2013.
1. Scope* D4307 Practice for Preparation of Liquid Blends for Use as
Analytical Standards
1.1 This test method covers the determination of the purity
D4790 Terminology ofAromatic Hydrocarbons and Related
of cyclohexane by gas chromatography. Calibration of the gas
Chemicals
chromatography system is done by the external standard
D6809 Guide for Quality Control and Quality Assurance
calibration technique.
Procedures for Aromatic Hydrocarbons and Related Ma-
1.2 This test method has been found applicable to the
terials
measurement of impurities such as those found in Table 1,
E29 Practice for Using Significant Digits in Test Data to
which are impurities that may be found in cyclohexane. The
Determine Conformance with Specifications
impurities can be analyzed over a range of 3 to 200 mg/kg by
E355 Practice for Gas ChromatographyTerms and Relation-
this method, but may be applicable to a wider range.
ships
E691 Practice for Conducting an Interlaboratory Study to
1.3 The limit of detection is 1 mg/kg.
Determine the Precision of a Test Method
1.4 In determining the conformance of the test results using
E1510 Practice for Installing Fused Silica Open Tubular
this test method to applicable specifications, results shall be
Capillary Columns in Gas Chromatographs
rounded off in accordance with the rounding-off method of
2.2 Other Document:
Practice E29.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
3
1.5 The values stated in SI units are to be regarded as
1910.1200
standard. No other units of measurement are included in this
standard. 3. Terminology
1.6 This standard does not purport to address all of the
3.1 See Terminology D4790 for definitions of terms used in
safety concerns, if any, associated with its use. It is the
this test method.
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
4.1 Cyclohexane is analyzed using a gas chromatograph
statements, see Section 7.
(GC) equipped with a flame ionization detector (FID). A
precisely repeatable volume of the sample to be analyzed is
2. Referenced Documents
injected onto the gas chromatograph. The peak areas of the
2
2.1 ASTM Standards:
impurities are measured and converted to concentrations via an
D3437 Practice for Sampling and Handling Liquid Cyclic
external standard methodology. Purity by GC (the cyclohexane
Products
content) is calculated by subtracting the sum of the impurities
from 100.00. Individual impurities are reported in mg/kg. The
1 cyclohexane purity is reported in weight percent.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
5. Significance and Use
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and Their
Derivatives.
5.1 This test method is suitable for setting specifications on
Current edition approved Feb. 1, 2013. Published March 2013. Originally
ε1
the materials referenced in Table 1 and for use as an internal
approved in 2007. Last previous edition approved in 2007 as D7266 – 07 . DOI:
10.1520/D7266-13E01.
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 ----------------------
´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
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.