ASTM D7266-07

Standard Test Method for Analysis of Cyclohexane by Gas Chromatography (External Standard)

SIGNIFICANCE AND USE
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.
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 5 to 180 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 E 29.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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

• Status: Historical
• Publication Date: 31-Dec-2006
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.01 - Benzene, Toluene, Xylenes, Cyclohexane and Their Derivatives

Relations

• Replaced By: ASTM D7266-07e1 - Standard Test Method for Analysis of Cyclohexane by Gas Chromatography (External Standard)
• Effective Date: 01-Jan-2007
• Referred By: ASTM D5309-22 - Standard Specification for Cyclohexane 999
• Effective Date: 01-Jan-2007

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D7266–07
Standard Test Method for
Analysis of Cyclohexane by Gas Chromatography (External
Standard)
This standard is issued under the fixed designation D 7266; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Procedures for Aromatic Hydrocarbons and Related Ma-
terials
1.1 This test method covers the determination of the purity
E29 Practice for Using Significant Digits in Test Data to
of cyclohexane by gas chromatography. Calibration of the gas
Determine Conformance with Specifications
chromatography system is done by the external standard
E 355 Practice for Gas Chromatography Terms and Rela-
calibration technique.
tionships
1.2 This test method has been found applicable to the
E 1510 Practice for Installing Fused Silica Open Tubular
measurement of impurities such as those found in Table 1,
Capillary Columns in Gas Chromatographs
which are impurities that may be found in cyclohexane. The
2.2 Other Document:
impurities can be analyzed over a range of 5 to 180 mg/kg by
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
this method, but may be applicable to a wider range.
1910.1200
1.3 The limit of detection is 1 mg/kg.
1.4 In determining the conformance of the test results using
3. Terminology
this test method to applicable specifications, results shall be
3.1 SeeTerminologyD 4790fordefinitionsoftermsusedin
rounded off in accordance with the rounding-off method of
this test method.
PracticeE29.
1.5 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 Cyclohexane is analyzed using a gas chromatograph
standard.
(GC) equipped with a flame ionization detector (FID). A
1.6 This standard does not purport to address all of the
precisely repeatable volume of the sample to be analyzed is
safety concerns, if any, associated with its use. It is the
injected onto the gas chromatograph. The peak areas of the
responsibility of the user of this standard to establish appro-
impurities are measured and converted to concentrations via an
priate safety and health practices and determine the applica-
external standard methodology. Purity by GC (the cyclohexane
bility of regulatory limitations prior to use. For specific hazard
content) is calculated by subtracting the sum of the impurities
statements, see Section 7.
from 100.00. Individual impurities are reported in mg/kg. The
2. Referenced Documents cyclohexane purity is reported in weight percent.
2.1 ASTM Standards:
5. Significance and Use
D 3437 Practice for Sampling and Handling Liquid Cyclic
5.1 This test method is suitable for setting specifications on
Products
the materials referenced in Table 1 and for use as an internal
D 4307 PracticeforPreparationofLiquidBlendsforUseas
quality control tool where cyclohexane is produced or is used
Analytical Standards
inamanufacturingprocess.Itmayalsobeusedindevelopment
D 4790 Terminology of Aromatic Hydrocarbons and Re-
or research work involving cyclohexane.
lated Chemicals
5.2 This test method is useful in determining the purity of
D 6809 Guide for Quality Control and Quality Assurance
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
This test method is under the jurisdiction of ASTM Committee D16 on
purity calculation would be erroneous.
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, 2007. Published January 2007.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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.
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D7266–07
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
Stationary phase bonded and crosslinked 100% dimethylpolysilicane
C
A
Film thickness, µm 0.5
(3) n-pentane
A
Length, m 100
(4) isopentane
A
Diameter, mm 0.25
(5) cyclopentane
Temperatures:
C
Injector, °C 230
(6) n-hexane
A
Detector, °C 250
(7) 2-methylpentane
A
Oven, °C 32 hold for 12 min
(8) 3-methylpentane
A
(9) methylcyclopentane Ramp1=8°C/minto 64°C, hold for 10 min
A
Ramp 2 = 10°C/min to 200°C, hold for 5 min
(10) benzene
A
Carrier gas Hydrogen
(11) cyclohexene
A
Flow rate, mls/min 3
(12) 2,2-dimethylbutane
A
Split ratio 100:1
(13) 2,3-dimethylbutane
Sample size, µl 1.0
C
(14) 3,3-dimethylpentane
A
(15) 2,2-dimethylpentane
A
(16) 2,3-dimethylpentane
TABLE 3 Summary of Precision Data (mg/kg)
A
(17) 2,4-dimethylpentane
A
(18) 1,1-dimethylcyclopentane
Expected
Impurity Average Repeatability
A
(19) trans-1,3-dimethylcyclopentane
Value
A
(20) trans-1,2-dimethylcyclopentane
Isopentane 21.1 21.1 2.0
(21) cis-1,2-dimethylcyclopentane
n-pentane 24.7 25.8 3.0
(22) 2,2-dimethylcyclopentane
2,2-dimethylbutane 9.9 9.9 1.0
(23) 2,4-dimethylcyclopentane
cyclopentane 11.5 11.4 0.8
A
(24) cis-1,3-dimethylcyclopentane
A 2,3-diemthylbutane 10.0 10.2 1.0
(25) ethylcyclopentane
A 2-methylpentane 17.3 18.1 2.2
(26) methylcyclohexane
A 3-methylpentane 23.9 24.8 2.0
(27) 3-ethylpentane
A n-hexane 46.7 48.4 5.2
(28) 3-methylhexane
A 2,2-dimethylpentane 4.9 5.2 0.8
(29) 2-methylhexane
A methycylopentane 36.1 36.8 2.1
(30) n-heptane
2,4-dimethylpentane 49.7 51.7 5.1
A
(31) toluene
benzene 12.1 12.4 1.3
C
A 2,3-dimethylpentane 57.3 58.3 4.2
(32) iso-octane
A 1,1-dimethylcyclopentane 23.5 23.0 1.2
(33) p-xylene
cyclohexene 29.4 29.6 1.3
C
A 3-methylhexane 9.9 10.5 0.9
(34) isopropylcylohexane
cis-1,3-dimethylcyclopentane 22.6 23.6 1.6
A
These components were used to prepare the standard used in the repeatabil-
trans-1,3-dimethylcyclopentane 10.8 11.1 0.8
ity program.
3-ethylpentane 29.9 31.0 2.5
trans-1,2-dimethylcyclopentane 41.2 40.4 2.3
isooctane 10.0 10.5 1.1
n-heptane 37.1 38.4 3.7
6. Apparatus
methylcyclohexane 178.5 181.0 10.0
ethylcyclopentane 19.0 19.6 1.7
6.1 Gas Chromatograph—Any instrument having a flame
toluene 19.9 20.9 1.9
ionization detector that can be operated at the conditions given
para-xylene 19.9 20.9 2.0
in Table 2. The system should have sufficient sensitivity to
isopropylcyclohexane 19.6 20.4 1.8
obtain a minimum peak height response for 1 mg/kg benzene
of twice the height of the signal background noise.
6.2 C
...