ASTM D5713-14(2018)e1

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

SIGNIFICANCE AND USE
5.1 This test method is useful for benzene purity on the basis of impurities normally present in benzene and may be used for final product inspections and process control.  
5.2 This test method will detect the following impurities: toluene, methylcyclopentane, n-hexane, 2-methylhexane, cyclohexane, cyclopentane, 2-methylpentane, 2,3-dimethylpentane, 3-methylhexane, n-heptane, methylcyclohexane, ethylcyclopentane, 2,4-dimethylhexane, trimethylpentane, and others where specific impurity standards are available. Absolute purity cannot be accurately determined if unknown impurities are present.
SCOPE
1.1 This test method covers the determination of specific impurities in, and the purity of benzene for cyclohexane feedstock by gas chromatography.  
1.2 This test method has been found applicable to benzene in the range from 99 to 100 % purity and to impurities at concentrations of 2 to 10 000 mg/kg.  
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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 7.2 and Section 8.  
1.6 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-May-2018
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5713 − 14 (Reapproved 2018)
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. 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—Editorial corrections made in Footnote 1 and 8.1 in June 2018.
1. Scope D3437 Practice for Sampling and Handling Liquid Cyclic
Products
1.1 This test method covers the determination of specific
D4790 Terminology of Aromatic Hydrocarbons and Related
impurities in, and the purity of benzene for cyclohexane
Chemicals
feedstock by gas chromatography.
D6809 Guide for Quality Control and Quality Assurance
1.2 This test method has been found applicable to benzene
Procedures for Aromatic Hydrocarbons and Related Ma-
in the range from 99 to 100 % purity and to impurities at
terials
concentrations of 2 to 10 000 mg/kg.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1.3 In determining the conformance of the test results using
this method to applicable specifications, results shall be E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relation-
rounded off in accordance with the rounding-off method of
Practice E29. ships
E1510 Practice for Installing Fused Silica Open Tubular
1.4 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
2.2 Other Document:
standard.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.5 This standard does not purport to address all of the 3
1910.1200
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3.1 Definitions:
mine the applicability of regulatory limitations prior to use.
3.1.1 See Terminology D4790 for definition of terms used in
For specific hazard statements, see 7.2 and Section 8.
this test method.
1.6 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4.1 In this test method, the chromatogram peak area for each
Development of International Standards, Guides and Recom-
impurity is compared to the peak area of the internal standard
mendations issued by the World Trade Organization Technical
(n-octane or other suitable known) added to the sample. From
Barriers to Trade (TBT) Committee.
the response factor of toluene relative to that of the internal
standard, and using a response factor of 1.00 for nonaromatic
2. Referenced Documents
impurities and the amount of internal standard added, the
2.1 ASTM Standards: concentrations of the impurities are calculated. The benzene
content is obtained by subtracting the total amount of all
impurities from 100.00.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
5. Significance and Use
bility of Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane and
5.1 This test method is useful for benzene purity on the
Their Derivatives.
Current edition approved June 1, 2018. Published June 2018. Originally
basis of impurities normally present in benzene and may be
approved in 1995. Last previous edition approved in 2014 as D5713 – 14. DOI:
used for final product inspections and process control.
10.1520/D5713-14R18E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from U.S. Government Printing Office Superintendent of Documents,
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5713 − 14 (2018)
TABLE 2 Summary of Precision Data
5.2 This test method will detect the following impurities:
toluene, methylcyclopentane, n-hexane, 2-methylhexane, Average
Intermediate
Component Concentration Reproducibility
cyclohexane, cyclopentane, 2-methylpentane, 2,3-
Precision
mg/kg
dimethylpentane, 3-methylhexane, n-heptane,
Benzene (weight %) 99.96 0.006 0.022
methylcyclohexane, ethylcyclopentane, 2,4-dimethylhexane,
99.97 0.007 0.020
trimethylpentane, and others where specific impurity standards 99.96 0.008 0.025
are available. Absolute purity cannot be accurately determined
Methylcyclopentane 104 8.3 27.9
if unknown impurities are present.
43 12.2 19.4
54 2.5 15.1
6. Apparatus
Toluene 64 5.1 22.0
63 3.0 16.6
6.1 Gas Chromatograph—Any gas chromatograph having a
28 1.8 9.1
temperature programmable oven, flame ionization detector and
Methylcyclohexane 132 7.4 34.8
a splitter injector suitable for use with a fused silica capillary
43 1.4 5.4
column may be used, provided the system has sufficient
79 3.2 17.0
sensitivity that will give a minimum peak height of 3 times the
Methylcyclohexane + 196 7.9 54.9
background noise for 2 mg/kg of an impurity.
Toluene 106 12.9 33.6
106 4.4 20.4
6.2 Column—Fused silica capillary columns have been
found to be satisfactory. An example is 50 m of 0.20-mm inside
n-Hexane 4 2.2 3.7
diameter fused silica capillary internally coated to a film
3 1.5 2.2
2 1.8 2.5
thickness of 0.50 µm with polydimethylsiloxane (see Table 1
for suggested instrument parameters). Other columns may be
n-Heptane 6 2.7 11.1
used after it has been established that such a column is capable
16 1.5 5.6
15 4.0 23.4
of separating all major impurities (for example, compounds
listed in 5.2) and the internal standard from the benzene under
Ethylcyclopentane 7 1.8 3.7
operating conditions appropriate for the column. The column
6 1.9 11.0
11 1.5 6.1
must give satisfactory resolution (distance from the valley
between the peaks is not greater than 50 % of the peak heights
Total Other Impurities 99 22.5 163.0
of the impurity) of cyclohexane from benzene as well as other
107 44.6 190.6
185 55.5 233.0
impurity peaks. A poorly resolved peak, such as cyclohexane,
will often require a tangent skim from the neighboring peak.
6.3 Electronic Integration, with tangent skim capabilities is
7. Reagents and Materials
recommended.
7.1 Purity of Reagents—Reagent grade chemicals shall be
6.4 Vial.
used in all tests. Unless otherwise indicated it is intended that
6.5 Microsyringes, assorted volumes.
all reagents shall conform to the specifications of the Commit-
tee on Analytical reagents of the American Chemical Society,
6.6 Injector, the specimen must be precisely and repeatedly
where such specifications are available. Other grades may be
injected into the gas chromatograph. An automatic sample
used, provided it is first ascertained that the reagent is of
injection device is highly recommended. Manual injection can
sufficiently high purity to permit its use without lessening the
be employed if the precision stated in Table 2 can be reliably
accuracy of the determination.
and consistently satisfied.
7.2 Carrier Gas—a carrier gas (99.999 % minimum purity)
appropriate to the type of detector used should be employed.
(Warning—If hydrogen is used as the carrier gas, take special
safety precautions to ensure that the system is free of leaks and
TABLE 1 Recommended Operating Conditions
that the effluent is properly vented or burned.)
Carrier gas hydrogen
Linear velocity at 40°C, cm/s 40
7.3 Hydrogen, for the flame ionization detector (FID) mini-
Detector flam
...

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
Designation: D5713 − 14 D5713 − 14 (Reapproved 2018)
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. 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—Editorial corrections made in Footnote 1 and 8.1 in June 2018.
1. Scope*Scope
1.1 This test method covers the determination of specific impurities in, and the purity of benzene for cyclohexane feedstock by
gas chromatography.
1.2 This test method has been found applicable to benzene in the range from 99 to 100 % purity and to impurities at
concentrations of 2 to 10 000 mg/kg.
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded
off in accordance with the rounding-off method of Practice E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 7.2 and Section 8.
1.6 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
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
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
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 Definitions:
3.1.1 See Terminology D4790 for definition 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. 15, 2014June 1, 2018. Published March 2014June 2018. Originally approved in 1995. Last previous edition approved in 20092014 as
D5713 – 09.D5713 – 14. DOI: 10.1520/D5713-14.10.1520/D5713-14R18E01.
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
D5713 − 14 (2018)
4. Summary of Test Method
4.1 In this test method, the chromatogram peak area for each impurity is compared to the peak area of the internal standard
(n-octane or other suitable known) added to the sample. From the response factor of toluene relative to that of the internal standard,
and using a response factor of 1.00 for nonaromatic impurities and the amount of internal standard added, the concentrations of
the impurities are calculated. The benzene content is obtained by subtracting the total amount of all impurities from 100.00.
5. Significance and Use
5.1 This test method is useful for benzene purity on the basis of impurities normally present in benzene and may be used for
final product inspections and process control.
5.2 This test method will detect the following impurities: toluene, methylcyclopentane, n-hexane, 2-methylhexane,
cyclohexane, cyclopentane, 2-methylpentane, 2,3-dimethylpentane, 3-methylhexane, n-heptane, methylcyclohexane,
ethylcyclopentane, 2,4-dimethylhexane, trimethylpentane, and others where specific impurity standards are available. Absolute
purity cannot be accurately determined if unknown impurities are present.
6. Apparatus
6.1 Gas Chromatograph—Any gas chromatograph having a temperature programmable oven, flame ionization detector and a
splitter injector suitable for use with a fused silica capillary column may be used, provided the system has sufficient sensitivity that
will give a minimum peak height of 3 times the background noise for 2 mg/kg of an impurity.
6.2 Column—Fused silica capillary columns have been found to be satisfactory. An example is 50 m of 0.20-mm inside diameter
fused silica capillary internally coated to a film thickness of 0.50 μm with polydimethylsiloxane (see Table 1 for suggested
instrument parameters). Other columns may be used after it has been established that such a column is capable of separating all
major impurities (for example, compounds listed in 5.2) and the internal standard from the benzene under operating conditions
appropriate for the column. The column must give satisfactory resolution (distance from the valley between the peaks is not greater
than 50 % of the peak heights of the impurity) of cyclohexane from benzene as well as other impurity peaks. A poorly resolved
peak, such as cyclohexane, will often require a tangent skim from the neighboring peak.
6.3 Electronic Integration, with tangent skim capabilities is recommended.
6.4 Vial.
6.5 Microsyringes, assorted volumes.
6.6 Injector, the specimen must be precisely and repeatedly injected into the gas chromatograph. An automatic sample injection
device is highly recommended. Manual injection can be employed if the precision stated in Table 2 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.
TABLE 1 Recommended Operating Conditions
Carrier gas hydrogen
Linear velocity at 40°C, cm/s 40
Detector flame ionization
Detector temperature, °C 250°C
Injection port temperature, °C 250°C
Split ratio 40:1
Split flow, mL/min 60
Column 50 m by 0.20 mm ID by 0.5 μm
bonded polydimethylsiloxane
capillary column
Initial column temperature, °C 40
Initial time, min 17
Programming rate 10°C/min
Final temperature, °C 250°C
Final time, min 10
Sample size, μL 1.2
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BHD, Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
´1
D5713 − 14 (2018)
TABLE 2 Summary of Precision Data
Average
Intermediate
Component Concentration Reproducibility
Precision
mg/kg
Benzene (weight %) 99.96 0.006 0.022
99.97 0.007 0.020
99.96 0.008 0.025
Methylcyclopentane 104 8.3 27.9
43 12.2 19.4
54 2.5 15.1
Toluene 64 5.1 22.0
63 3.0 16.6
28 1.8 9.1
Methylcyclohexane 132 7.4 34.8
43 1.4 5.4
79 3.2 17.0
Methylcyclohexane + 196 7.9 54.9
Toluene 106 12.9 33.6
106 4.4 20.4
n-Hexane 4 2.2 3.7
3 1.5 2.2
2 1.8 2.5
n-Heptane 6 2.7 11.1
16 1.5 5.6
15 4.0 23.4
Ethylcyclopentane 7 1.8 3.7
6 1.9 11.0
11 1.5 6.1
Total Other Impurities 99 22.5 163.0
...