ASTM D6159-17

Standard Test Method for Determination of Hydrocarbon Impurities in Ethylene by Gas Chromatography

SIGNIFICANCE AND USE
4.1 High-purity ethylene is required as a feedstock for some manufacturing processes and the presence of trace amounts of certain hydrocarbon impurities can have deleterious effects. This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in development or research work.  
4.2 This test method does not detect such impurities as H2O, CO, CO2, and alcohols that may be present in the sample. Hydrocarbons higher than n-decane cannot be analyzed by this test method, if present in the sample. Test Method D2504 addresses the analysis of noncondensable gases and Test Method D2505 addresses the analysis of CO2. Guide D5234 describes all potential impurities present in ethylene. These standards should be consulted when determining the total concentration of impurities in ethylene.
SCOPE
1.1 This test method covers the determination of methane, ethane, propane, propene, acetylene, iso-butane, propadiene, butane, trans-2-butene, butene-1, isobutene, cis-2-butene, methyl acetylene and 1,3-butadiene in high-purity ethylene. The purity of the ethylene can be calculated by subtracting the total percentage of all impurities from 100.00 %. Since this test method does not determine all possible impurities such as CO, CO2, H2O, alcohols, nitrogen oxides, and carbonyl sulfide, as well as hydrocarbons higher than decane, additional tests may be necessary to fully characterize the ethylene sample.  
1.2 Data are reported in this test method as ppmV (parts per million by gaseous volume) and ppmMol (parts per million Mol). This test method was evaluated in an interlaboratory cooperative study in the concentration range of 4 ppmV to 340 ppmV (2 mg/kg to 204 mg/kg). The participants in the interlaboratory cooperative study reported the data in non-SI units. Wherever possible, SI units are included.  
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.

General Information

• Status: Historical
• Publication Date: 31-Dec-2016
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.02 - Ethylene

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: D6159 − 17
Standard Test Method for
Determination of Hydrocarbon Impurities in Ethylene by Gas
1
Chromatography
This standard is issued under the fixed designation D6159; 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. Scope* 3. Summary of Test Method
1.1 This test method covers the determination of methane, 3.1 A gaseous ethylene sample is analyzed as received. The
ethane, propane, propene, acetylene, iso-butane, propadiene, gaseous sample is injected into a capillary gas chromatograph.
butane, trans-2-butene, butene-1, isobutene, cis-2-butene, Sample may be introduced by direct valve injection or by split
methyl acetylene and 1,3-butadiene in high-purity ethylene. valve injection. The gas chromatograph is provided with a
The purity of the ethylene can be calculated by subtracting the 6-port sampling valve and two wide bore capillary columns
total percentage of all impurities from 100.00 %. Since this test connected in series. These columns are a dimethyl polysi-
method does not determine all possible impurities such as CO, loxane column and a porous layer open tubular column (PLOT)
CO , H O, alcohols, nitrogen oxides, and carbonyl sulfide, as Al O /KCl column. (See Note 1.) A flame ionization detector is
2 2 2 3
well as hydrocarbons higher than decane, additional tests may used for detection. The integrated detector signal (peak areas)
be necessary to fully characterize the ethylene sample. are corrected for detector response. The hydrocarbon impuri-
ties are determined and the total impurities are used to
1.2 Data are reported in this test method as ppmV (parts per
determine the ethylene content.
million by gaseous volume) and ppmMol (parts per million
Mol). This test method was evaluated in an interlaboratory
NOTE 1—This column is supplied by major column manufacturers.
cooperative study in the concentration range of 4 ppmV to
4. Significance and Use
340 ppmV (2 mg ⁄kg to 204 mg ⁄kg). The participants in the
interlaboratory cooperative study reported the data in non-SI
4.1 High-purity ethylene is required as a feedstock for some
units. Wherever possible, SI units are included.
manufacturing processes and the presence of trace amounts of
1.3 This standard does not purport to address all of the certain hydrocarbon impurities can have deleterious effects.
safety concerns, if any, associated with its use. It is the
This test method is suitable for setting specifications, for use as
responsibility of the user of this standard to establish appro- an internal quality control tool, and for use in development or
priate safety and health practices and determine the applica-
research work.
bility of regulatory limitations prior to use.
4.2 This test method does not detect such impurities as H O,
2
CO, CO , and alcohols that may be present in the sample.
2
2. Referenced Documents
Hydrocarbons higher than n-decane cannot be analyzed by this
2
2.1 ASTM Standards:
test method, if present in the sample. Test Method D2504
D2504 Test Method for Noncondensable Gases in C and
2 addresses the analysis of noncondensable gases and Test
Lighter Hydrocarbon Products by Gas Chromatography
Method D2505 addresses the analysis of CO . Guide D5234
2
D2505 Test Method for Ethylene, Other Hydrocarbons, and
describes all potential impurities present in ethylene. These
Carbon Dioxide in High-Purity Ethylene by Gas Chroma-
standards should be consulted when determining the total
tography
concentration of impurities in ethylene.
D5234 Guide for Analysis of Ethylene Product
5. Apparatus
5.1 Gas Chromatograph (GC), a gas chromatographic in-
1
This test method is under the jurisdiction of ASTM Committee D02 on
strument provided with a temperature programmable column
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.02 on Ethylene.
oven and a flame ionization detector (FID). Carrier gas is
Current edition approved Jan. 1, 2017. Published February 2017. Originally
regulated by pressure control.
approved in 1997. Last previous edition approved in 2012 as D6159 – 97 (2012).
DOI: 10.1520/D6159-17.
5.2 Detector—A flame ionization detector (FID) having a
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sensitivity of approximately 2.0 ppmV (1.2 mg ⁄kg) or less for
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
the compounds listed in 1.1. An FID was exclusively used in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the interlaboratory cooperative study.
*A Summary of
...

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.
Designation: D6159 − 97 (Reapproved 2012) D6159 − 17
Standard Test Method for
Determination of Hydrocarbon Impurities in Ethylene by Gas
1
Chromatography
This standard is issued under the fixed designation D6159; 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. Scope Scope*
1.1 This test method covers the determination of methane, ethane, propane, propene, acetylene, iso-butane, propadiene, butane,
trans-2-butene, butene-1, isobutene, cis-2-butene, methyl acetylene and 1,3-butadiene in high-purity ethylene. The purity of the
ethylene can be calculated by subtracting the total percentage of all impurities from 100.00 %. 100.00 %. Since this test method
does not determine all possible impurities such as CO, CO , H O, alcohols, nitrogen oxides, and carbonyl sulfide, as well as
2 2
hydrocarbons higher than decane, additional tests may be necessary to fully characterize the ethylene sample.
1.2 Data are reported in this test method as ppmV (parts per million by volume). gaseous volume) and ppmMol (parts per
million Mol). This test method was evaluated in an interlaboratory cooperative study in the concentration range of 44 ppmV to 340
ppmV340 ppmV (2 mg (2 ⁄kg to 204204 mg mg/kg). ⁄kg). The participants in the interlaboratory cooperative study reported the
data in non-SI units. Wherever possible, SI units are included.
1.3 This standard dosedoes 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D2504 Test Method for Noncondensable Gases in C and Lighter Hydrocarbon Products by Gas Chromatography
2
D2505 Test Method for Ethylene, Other Hydrocarbons, and Carbon Dioxide in High-Purity Ethylene by Gas Chromatography
D5234 Guide for Analysis of Ethylene Product
3. Summary of Test Method
3.1 A gaseous ethylene sample is analyzed as received. The gaseous sample is injected into a capillary gas chromatograph. A
split-injector may or may not be used.Sample may be introduced by direct valve injection or by split valve injection. The gas
chromatograph is provided with a 6–port6-port sampling valve and two wide bore capillary columns connected in series. These
columns are a dimethyl siliconepolysiloxane column and a (porousporous layer open tubular column (PLOT) Al O /KCl column.
2 3
(See Note 1.) A flame ionization detector is used for detection. The integrated detector signal (peak areas) are corrected for detector
response. The hydrocarbon impurities are determined and the total impurities are used to determine the ethylene content.
NOTE 1—This column is supplied by major column manufacturers.
4. Significance and Use
4.1 High-purity ethylene is required as a feedstock for some manufacturing processes and the presence of trace amounts of
certain hydrocarbon impurities can have deleterious effects. This test method is suitable for setting specifications, for use as an
internal quality control tool, and for use in development or research work.
4.2 This test method does not detect such impurities as H O, CO, CO , and alcohols that may be present in the sample.
2 2
Hydrocarbons higher than n-decane cannot be analyzed by this test method, if present in the sample. Test Method D2504 addresses
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.D0.02 on Ethylene.
Current edition approved Dec. 1, 2012Jan. 1, 2017. Published December 2012February 2017. Originally approved in 1997. Last previous edition approved in 20072012
as D6159–97(2007).D6159 – 97 (2012). DOI: 10.1520/D6159-97R12.10.1520/D6159-17.
2
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’s Document Summary page on the ASTM website.
*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
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