ASTM D5713-00

Standard Test Method for Analysis of High Purity Benzene for Cyclohexane Feedstock by Capillary Gas Chromatography

SCOPE
1.1 This test method covers the determination of specific impurities in, and the purity of benzene for cyclohexane feedstock by gas chromatography. It is applicable to benzene in the range from 99 to 100% purity and to impurities at concentrations of 2 to 10000 mg/kg.  
1.2 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.  
1.3 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 a specific hazard statement, see Section 7 and Note 1.

General Information

• Status: Historical
• Publication Date: 09-Jun-2000
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.01 - Benzene, Toluene, Xylenes, Cyclohexane and Their Derivatives

Relations

• Replaced By: ASTM D5713-05 - Standard Test Method for Analysis of High Purity Benzene for Cyclohexane Feedstock by Capillary Gas Chromatography
• Effective Date: 01-Jul-2005
• Referred By: ASTM D5871-19 - Standard Specification for Benzene for Cyclohexane Feedstock
• Effective Date: 10-Jun-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5713–00
Standard Test Method for
Analysis of High Purity Benzene for Cyclohexane Feedstock
by Capillary Gas Chromatography
This standard is issued under the fixed designation D5713; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1910.1200
1.1 This test method covers the determination of specific
impurities in, and the purity of benzene for cyclohexane
3. Terminology
feedstockbygaschromatography.Itisapplicabletobenzenein
3.1 Definitions:
the range from 99 to 100% purity and to impurities at
3.1.1 For definition of terms used in this test method see
concentrations of 2 to 10000 mg/kg.
Terminology D4790.
1.2 The following applies to all specified limits in this test
method: for purposes of determining conformance with this
4. Summary of Test Method
test method, an observed value or a calculated value shall be
4.1 Inthistestmethod,thechromatogrampeakareaforeach
rounded off “to the nearest unit” in the last right-hand digit
impurity is compared to the peak area of the internal standard
used in expressing the specification limit, in accordance with
(n-octane or other suitable known) added to the sample. From
the rounding-off method of PracticeE29.
the response factor of toluene relative to that of the internal
1.3 This standard does not purport to address all of the
standard, and using a response factor of 1.00 for nonaromatic
safety concerns, if any, associated with its use. It is the
impurities and the amount of internal standard added, the
responsibility of the user of this standard to establish appro-
concentrations of the impurities are calculated. The benzene
priate safety and health practices and determine the applica-
content is obtained by subtracting the total amount of all
bility of regulatory limitations prior to use. For a specific
impurities from 100.00.
hazard statement, see Section 8 and Note 1.
5. Significance and Use
2. Referenced Documents
5.1 Thistestmethodisdesignedtoobtainbenzenepurityon
2.1 ASTM Standards:
thebasisofimpuritiesnormallypresentinbenzeneandmaybe
D3437 Practice for Sampling and Handling Cyclic Prod-
2 used for final product inspections and process control.
ucts
5.2 This test method will detect the following impurities:
D4790 Terminology of Aromatic Hydrocarbons and Re-
2 toluene, methylcyclopentane, n-hexane, 2-methylhexane, cy-
lated Chemicals
clohexane, cyclopentane, 2-methylpentane, 2,3-
E29 Practice for Using Significant Digits in Test Data to
3 dimethylpentane,3-methylhexane, n-heptane,methylcyclohex-
Determine Conformance with Specifications
ane, ethylcyclopentane, 2,4-dimethylhexane, trimethylpentane,
E260 Practice for Packed Column Gas Chromatography
and others where specific impurity standards are available.
E355 Practices for Gas Chromatography Terms and Rela-
Absolute purity cannot be accurately determined if unknown
tionships
impurities are present.
E1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
6. Apparatus
2.2 Other Document:
6.1 Gas Chromatograph—Anygaschromatographhavinga
temperatureprogrammableoven,flameionizationdetectorand
a splitter injector suitable for use with a fused silica capillary
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbon and Related Chemicals and is the direct responsibility of
column may be used, provided the system has sufficient
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their
sensitivity that will give a minimum peak height of 3 times the
Derivatives.
Current edition approved June 10, 2000. Published August 2000. Originally
published as D5713–95. Last previous edition D5713–96.
2 4
Annual Book of ASTM Standards, Vol 06.04. Available from the Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5713–00
TABLE 2 Intermediate Precision and Reproducibility
background noise for 2 mg/kg of an impurity when operated at
recommended conditions. Average
Intermediate
Component Concentration ppm Reproducibility
6.2 Column—Fused silica capillary columns have been
Precision
Weight %
foundtobesatisfactory.Anexampleis50mof0.20-mminside
Benzene 99.96 0.006 0.022
diameter fused silica capillary internally coated to a film
99.97 0.007 0.020
thickness of 0.50 µm with cross-linked methyl silicone (see
99.96 0.008 0.025
Table1forparameters).Othercolumnsmaybeusedafterithas
Methylcyclopentane 104 8.3 27.9
beenestablishedthatsuchacolumniscapableofseparatingall
43 12.2 19.4
major impurities (for example, compounds listed in 5.2) and
54 2.5 15.1
the internal standard from the benzene under operating condi-
Toluene 64 5.1 22.0
tions appropriate for the column. The column must give
63 3.0 16.6
satisfactory resolution (distance from the valley between the 28 1.8 9.1
peaks is not greater than 50% of the peak heights of the
Methylcyclohexane 132 7.4 34.8
impurity) of cyclohexane from benzene as well as other
43 1.4 5.4
impurity peaks. A poorly resolved peak, such as cyclohexane, 79 3.2 17.0
will often require a tangent skim from the neighboring peak.
Methylcyclohexane + 196 7.9 54.9
6.3 Electronic Integration, with tangent skim capabilities is
Toluene 106 12.9 33.6
recommended. 106 4.4 20.4
6.4 Vial.
n-Hexane 4 2.2 3.7
6.5 Microsyringes, assorted volumes.
3 1.5 2.2
2 1.8 2.5
7. Reagents and Materials
n-Heptane 6 2.7 11.1
7.1 Carrier Gas—acarriergas(minimumpurityof99.95%
16 1.5 5.6
mol) appropriate to the type of detector used should be
15 4.0 23.4
employed.
Ethylcyclopentane 7 1.8 3.7
6 1.9 11.0
NOTE 1—Precaution: If hydrogen is used as the carrier gas, take
11 1.5 6.1
specialsafetyprecautions
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