ASTM D5504-20
(Test Method)Standard Test Method for Determination of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatography and Chemiluminescence
Standard Test Method for Determination of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatography and Chemiluminescence
SIGNIFICANCE AND USE
5.1 Many sources of natural and petroleum gases contain sulfur compounds that are odorous, corrosive, and poisonous to catalysts used in gaseous fuel processing.
5.2 Low ppm amounts of sulfur odorants are added to natural gas and LP gases for safety purposes. Some odorants are unstable and react to form compounds having lower odor thresholds. Quantitative analysis of these odorized gases ensures that odorant injection equipment is performing to specification.
5.3 Although not intended for application to gases other than natural gas and related fuels, this test method has been successfully applied to fuel type gases, including refinery, landfill, cogeneration, and sewage digester gas. Refinery, landfill, sewage digester, and other related fuel type gases inherently contain volatile sulfur compounds that are subject to federal, state, or local control. The methane fraction of these fuel type gases is occasionally sold to distributors of natural gas. For these reasons, both regulatory agencies and production and distribution facilities may require the accurate determination of sulfur to satisfy regulatory, production, or distribution requirements. Fuel gases are also used in energy production or are converted to new products using catalysts that are poisoned by excessive sulfur in the feed gas. Industry frequently requires measurement of sulfur in these fuel type gases to protect their catalyst investments.
5.4 Analytical Methods—Gas chromatography (GC) is commonly used in the determination of fixed gas and organic composition of natural gas (Test Method D1945). Other standard ASTM methods for the analysis of sulfur in fuel gases include Test Methods D1072 and D4468 for total sulfur and Test Methods D4010 and D4884 for hydrogen sulfide.
SCOPE
1.1 This test method is primarily for the determination of speciated volatile sulfur-containing compounds in high methane content gaseous fuels such as natural gas. It has been successfully applied to other types of gaseous samples, including air, digester, landfill, and refinery fuel gas. The detection range for sulfur compounds, reported as picograms sulfur, is 0.01 to 1000. This is equivalent to 0.01 to 1000 mg/m3, based upon the analysis of a 1 cc sample.
1.2 The range of this test method may be extended to higher concentration by dilution or by selection of a smaller sample loop.
Note 1: Dilution will reduce method precision.
1.3 This test method does not purport to identify all sulfur species in a sample. Only compounds that are eluted through the selected column under the chromatographic conditions chosen are determined. The detector response to sulfur is equimolar for all sulfur compounds within the scope (1.1) of this test method. Thus, unidentified compounds are determined with equal precision to that of identified substances. Total sulfur content is determined from the total of individually quantified components.
1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.
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.
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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.
Designation: D5504 − 20
Standard Test Method for
Determination of Sulfur Compounds in Natural Gas and
Gaseous Fuels by Gas Chromatography and
1
Chemiluminescence
This standard is issued under the fixed designation D5504; 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 Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method is primarily for the determination of
Barriers to Trade (TBT) Committee.
speciated volatile sulfur-containing compounds in high meth-
ane content gaseous fuels such as natural gas. It has been
2. Referenced Documents
successfully applied to other types of gaseous samples, includ-
2
2.1 ASTM Standards:
ing air, digester, landfill, and refinery fuel gas. The detection
D1072 Test Method for Total Sulfur in Fuel Gases by
range for sulfur compounds, reported as picograms sulfur, is
3
Combustion and Barium Chloride Titration
0.01 to 1000. This is equivalent to 0.01 to 1000 mg/m , based
D1945 Test Method for Analysis of Natural Gas by Gas
upon the analysis of a 1 cc sample.
Chromatography
1.2 The range of this test method may be extended to higher
D3609 Practice for Calibration Techniques Using Perme-
concentration by dilution or by selection of a smaller sample
ation Tubes
loop.
D4010 Specification for Waterless Hand Cleaner (With-
3
drawn 2000)
NOTE 1— Dilution will reduce method precision.
D4150 Terminology Relating to Gaseous Fuels
1.3 This test method does not purport to identify all sulfur
D4468 Test Method for Total Sulfur in Gaseous Fuels by
species in a sample. Only compounds that are eluted through
Hydrogenolysis and Rateometric Colorimetry
the selected column under the chromatographic conditions
D4884 Test Method for Strength of Sewn or Bonded Seams
chosen are determined. The detector response to sulfur is
of Geotextiles
equimolar for all sulfur compounds within the scope (1.1) of
E177 Practice for Use of the Terms Precision and Bias in
this test method. Thus, unidentified compounds are determined
ASTM Test Methods
with equal precision to that of identified substances. Total
E594 Practice for Testing Flame Ionization Detectors Used
sulfur content is determined from the total of individually
in Gas or Supercritical Fluid Chromatography
quantified components.
E691 Practice for Conducting an Interlaboratory Study to
1.4 Units—The values stated in SI units are to be regarded
Determine the Precision of a Test Method
as standard. The values given in parentheses after SI units are
provided for information only and are not considered standard.
3. Terminology
1.5 This standard does not purport to address all of the
3.1 For definitions of general terms used in D03 Gaseous
safety concerns, if any, associated with its use. It is the
Fuels standards, refer to Terminology D4150.
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.1 The analysis of gaseous sulfur compounds is challeng-
1.6 This international standard was developed in accor-
ing due to the reactivity of these substances. They are difficult
dance with internationally recognized principles on standard-
to sample and analyze. Ideally, analysis is performed on-site to
ization established in the Decision on Principles for the
eliminate sample deterioration as a factor in analysis. Sampling
1 2
This test method is under the jurisdiction of ASTM Committee D03 on Gaseous For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuels and is the direct responsibility of Subcommittee D03.06.01 on Analysis of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Major Constituents by Gas Chromatography. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2020. Published December 2020. Originally the ASTM website.
3
approved in 1994. Last previous edition approved in 2012 as D5504 – 12. DOI: The last approved version of this historical standard is referenced on
10.1520/D5504-20. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5504 − 20
must be performed using non-reactive containers, such as tion of sulf
...
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: D5504 − 12 D5504 − 20
Standard Test Method for
Determination of Sulfur Compounds in Natural Gas and
Gaseous Fuels by Gas Chromatography and
1
Chemiluminescence
This standard is issued under the fixed designation D5504; 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
1.1 This test method is primarily for the determination of speciated volatile sulfur-containing compounds in high methane content
gaseous fuels such as natural gas. It has been successfully applied to other types of gaseous samples, including air, digester, landfill,
and refinery fuel gas. The detection range for sulfur compounds, reported as picograms sulfur, is ten (10) to one million (1 000
3
000). 0.01 to 1000. This is equivalent to 0.01 to 1 000 1000 mg/m , based upon the analysis of a 1 cc sample.
1.2 The range of this test method may be extended to higher concentration by dilution or by selection of a smaller sample loop.
NOTE 1— Dilution will reduce method precision.
1.3 This test method does not purport to identify all sulfur species in a sample. Only compounds that are eluted through the
selected column under the chromatographic conditions chosen are determined. The detector response to sulfur is equimolar for all
sulfur compounds within the scope (1.1) of this test method. Thus, unidentified compounds are determined with equal precision
to that of identified substances. Total sulfur content is determined from the total of individually quantified components.
1.4 Units—The values stated in SI units are to be regarded as standard. The values stated in inch-pound given in parentheses after
SI units are provided for information only.only and are not considered 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.
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
2.1 ASTM Standards:
D1072 Test Method for Total Sulfur in Fuel Gases by Combustion and Barium Chloride Titration
1
This test method is under the jurisdiction of ASTM Committee D03 on Gaseous Fuels and is the direct responsibility of Subcommittee D03.05 on Determination of
Special Constituents of Gaseous Fuels.
Current edition approved June 1, 2012Nov. 1, 2020. Published November 2012December 2020. Originally approved in 1994. Last previous edition approved in 20082012
as D5504 – 08.D5504 – 12. DOI: 10.1520/D5504-12.10.1520/D5504-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5504 − 20
D1945 Test Method for Analysis of Natural Gas by Gas Chromatography
D3609 Practice for Calibration Techniques Using Permeation Tubes
3
D4010 Specification for Waterless Hand Cleaner (Withdrawn 2000)
D4150 Terminology Relating to Gaseous Fuels
D4468 Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and Rateometric Colorimetry
D4884 Test Method for Strength of Sewn or Bonded Seams of Geotextiles
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 For definitions of general terms used in D03 Gaseous Fuels standards, refer to Terminology D4150.
4. Summary of Test Method
4.1 The analysis of gaseous sulfur compounds is challenging due to the reactivity of these substances. They are difficult to sample
and analyze. Ideally, ana
...
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