ASTM D3054-98

Standard Test Methods for Analysis of Cyclohexane by Gas Chromatography (Withdrawn 2007)

SCOPE
1.1 These test methods cover the determination of the hydrocarbon impurities typically found in cyclohexane and the purity of cyclohexane by difference by gas chromatography. The absolute purity of cyclohexane cannot be determined, since trace quantities of unknowns may be present. Typical impurities in high purity cyclohexane are listed in Table 1.  
1.2 These test methods are applicable to impurity concentrations in the range of 0.0001 to 0.1000 wt% and for cyclohexane purities of 98% or higher when using the internal standard procedure.  
1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off to the nearest unit in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.  
1.4 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 Note 2 and Section 7.
WITHDRAWN RATIONALE
These test methods cover the determination of the hydrocarbon impurities typically found in cyclohexane and the purity of cyclohexane by difference by gas chromatography. These test methods are applicable to impurity concentrations in the range of 0.0001 to 0.1000 wt% and for cyclohexane purities of 98 % or higher when using the internal standard procedure.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, these test methods were withdrawn in February 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 09-Aug-1998
• Withdrawal Date: 06-Feb-2007
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
Designation:D3054–98
Standard Test Methods for
Analysis of Cyclohexane by Gas Chromatography
This standard is issued under the fixed designation D 3054; 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.
TABLE 1 Impurities Known or Suggested to be Present in
1. Scope
Commercial Cyclohexane
1.1 These test methods cover the determination of the
C
hydrocarbon impurities typically found in cyclohexane and the
(1) n-butane
purity of cyclohexane by difference by gas chromatography.
(2) isobutane
C
Typical impurities in high purity cyclohexane are listed in
(3) n-pentane
Table 1.
(4) isopentane
1.2 These test methods are applicable to impurity concen- (5) cyclopentane
C
trations in the range of 0.0001 to 0.1000 wt% and for
A
(6) n-hexane
cyclohexane purities of 98 % or higher when using the internal
(7) 2-methylpentane
standard procedure.
(8) 3-methylpentane
A
(9) methylcyclopentane
1.3 The following applies to all specified limits in this test
A
(10) benzene
method: for purposes of determining conformance with this
(11) 2,2-dimethylbutane
test method, an observed value or a calculated value shall be (12) 2,3-dimethylbutane
C
rounded off to the nearest unit in the last right-hand digit used
(13) 3,3-dimethylpentane
in expressing the specification limit, in accordance with the
(14) 2,3-dimethylpentane
rounding-off method of PracticeE29. (15) 1,1-dimethylcyclopentane
(16) 1,t3-dimethylcyclopentane
1.4 This standard does not purport to address all of the
(17) 1,t2-dimethylcyclopentane
safety concerns, if any, associated with its use. It is the
(18) 1,c2-dimethylcyclopentane
(19) 2,2-dimethylpentane
responsibility of the user of this standard to establish appro-
(20) 2,4-dimethylpentane
priate safety and health practices and determine the applica-
(21) 1,c3-dimethylcyclopentane
bility of regulatory limitations prior to use. For specific hazard
(22) ethylcyclopentane
A
statements, see Note 2 and Section 7. (23) methylcyclohexane
(24) 3-ethylpentane
(25) 3-methylhexane
2. Referenced Documents
(26) 2-methylhexane
2.1 ASTM Standards: (27) n-heptane
A
D 3437 Practice for Sampling and Handling Liquid Cyclic
These components were used to prepare the standards used in the round
robin program.
Products
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
OSHA Regulations, 29 CFR, Paragraphs 1910.1000 and
E 260 Practice for Packed Column Gas Chromatography
1910.1200
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
3. Summary of Test Methods
E 1510 Practice for Installing Fused Silica Open Tubular
3.1 Test Method A: Internal Standard Procedure—This
Capillary Columns in Gas Chromatographs
procedure is used when the impurities are at 0.00010 to 0.1000
2.2 Other Document:
wt% levels. A known amount of internal standard is added to
the sample. A portion of the sample is injected into the
These test methods are under the jurisdiction of ASTM Committee D16 on
chromatograph and the levels of impurities are calculated
Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of
relative to the amount of internal standard added. The amount
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their
Derivatives.
Current edition approved Feb. 21, 2002. Published October 1998. Originally
published as D 3054 – 93. Last previous edition D 3054 – 95.
2 4
Annual Book of ASTM Standards, Vol 06.04. Available from Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20004.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D3054–98
of measured impurities, including benzene, is subtracted from column used must be capable of resolving all significant
100.00 to establish the purity of the cyclohexane samples. impurities from cyclohexane. The internal standard peak must
3.2 Test Method B: Straight Normalization Procedure—A be individually resolved without interference from cyclohex-
portion of the sample is injected into the chromatograph using ane or any other impurities. A typical chromatogram with the
a microlitre syringe at the specified conditions of the test identified impurities is found in Fig. 1.
method. The area of all the peaks and main component are 5.2.1 Cross-Linked Methyl Silicone Fused Silica Capillary
electronically integrated. These areas are normalized to Column, 60 m by 0.50 µm film thickness by 0.32 mm inside
100.00 %. diameter.
5.3 Integrator or Data Handling System— Electronic or
4. Significance and Use
equivalent equipment for obtaining peak areas. This device
4.1 These test methods are suitable for establishing contract
must integrate areas at a rate of 15 readings per second so that
specifications on cyclohexane and for use in internal quality
very narrow peaks resulting from fused silica capillary col-
control where cyclohexane is either produced or used in a
umns can be accurately measured.
manufacturing process.They may also be used in development
5.4 Microsyringes, capacities 1.0 or 10 µL, and 50 µL.
or research work. Purity is commonly reported by subtracting
5.5 Volumetric Flasks, 100-mL capacity.
the determined impurities from 100.00. However, a gas chro-
matographic analysis can not determine absolute purity if
6. Reagents and Materials
unknown components are contained within the material being
6.1 2,2-Dimethylbutane, 99.0 % minimum purity (internal
examined.
standard).
NOTE 1—In case of dispute, the internal standard procedure will be the
6.2 Helium.
correct procedure to use.
6.3 Hydrogen and Air, for FID detector.
5. Apparatus
7. Hazards
5.1 Gas Chromatograph (GC) (for a Fused Silica
7.1 Consult current OSHA regulations, suppliers’ Material
Column)—Amulti-ramp temperature, programmable GC built
Safety Data Sheets (MSDS), and local regulations for all
for capillary column chromatography. It must have a flame
materials used in this test method.
ionization detector and a split injection system that will not
discriminate over the boiling range of the samples analyzed.
8. Sampling
5.1.1 Gas Chromatograph—Any chromatograph having a
flame ionization detector that can be operated at the conditions 8.1 Take samples in accordance with Practice D 3437.
given in Table 2. The system should have sufficient sensitivity
to obtain a minimum peak height response for a 0.0001 wt%
9. Procedures
impurity twice the height of the signal background noise.
9.1 Test Method A:
5.2 Chromatographic Column—The recommended column
9.1.1 Internal Standard Procedure—Install the chromato-
is a methyl silicone-fused silica capillary column. Any other
graphic column and establish stable instrument operation at the
proper operating conditions shown in Table 2. The selected
TABLE 2 Typical Instrument Conditions for Cyclohexane
columnandconditionsmustsatisfytheresolutionrequirements
Analysis (See Chromatogram Fig. 1)
as stated in 5.2. Make reference to instructions provided by the
Instrument:
Range 3 manufacturerofthechromatograph,andtoPracticesE 260and
Attenuation 1
E 1510.
Inlet, °C 200
9.1.2 Place 50 to 60 mL of the cyclohexane sample to be
Detector,° C 275
Sample size, µL 1.2 analyzedintoa100-mLvolumetricflask.Accuratelyadd,using
Column:
a micropipet or microsyringe, 25 µLof the internal standard to
Carrier gas helium
the flask and then fill to the calibration mark with additional
Linear velocity, cm/sec 20.0
Sp
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