ASTM D5504-98

Standard Test Method for Determination of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatography and Chemiluminescence

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 (1 000 000). This is equivalent to 0.01 to 1 000 mg/m3, based upon the analysis of a 1 cc sample.
1.2 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.
1.3 The values stated in SI units are standard. The values stated in inch-pound units are for information only.
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.

General Information

• Status: Historical
• Publication Date: 09-Nov-2001
• ICS: 75.160.01 - Fuels in general
• ICS: 75.160.30 - Gaseous fuels
• Technical Committee: D03 - Gaseous Fuels

Relations

• Replaced By: ASTM D5504-01 - Standard Test Method for Determination of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatography and Chemiluminescence
• Effective Date: 10-Nov-2001

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D 5504–98
Standard Test Method for
Determination of Sulfur Compounds in Natural Gas and
Gaseous Fuels by Gas Chromatography and
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Chemiluminescence
This standard is issued under the fixed designation D 5504; 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 (ε) indicates an editorial change since the last revision or reapproval.
1. Scope D4626 Practice for Calculation of Gas Chromatographic
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Response Factors
1.1 This test method provides for the determination of
E594 Practice forTesting Flame Ionization Detectors Used
individual volatile sulfur-containing compounds in gaseous
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in Gas Chromatography
fuels including natural gas. The detection range for sulfur
compounds, reported as picograms sulfur, is ten (10) to one
3. Terminology
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million (1000000). This is equivalent to 0.01 to 1000 mg/m ,
3 3.1 Abbreviations:
based upon the analysis of a 1-cm sample.
3.2 A common abbreviation of hydrocarbon compounds is
1.2 The test method does not purport to identify all indi-
to designate the number of carbon atoms in the compound. A
vidual sulfur species. The detector response to sulfur is
prefix is used to indicate the carbon chain form, while a
equimolar for all sulfur compounds within the scope (1.1) of
subscript suffix denotes the number of carbon atoms (for
this test method; thus unknown individual compounds are
example, normal decane = n-C ; iso-tetradecane = I-C ).
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determined with equal precision to that of known compounds.
3.3 Sulfur compounds are commonly referred to by their
Total sulfur content of samples can be estimated from the total
initials (chemical or formula), for example, dimethyl sulfide =
of the individual compounds determined.
DMS; carbonyl sulfide = COS.
1.3 The values stated in SI units are to be regarded as
standard. The values stated in inch-pound units are for infor-
4. Summary of Test Method
mation only.
4.1 The analysis of gaseous sulfur compounds is difficult
1.4 This standard does not purport to address all of the
because of the reactive nature of these materials. They pose
safety concerns, if any, associated with its use. It is the
problems both in sampling and analysis. Analysis is ideally
responsibility of the user of this standard to establish appro-
performed on-site to eliminate potential sample deterioration.
priate safety and health practices and determine the applica-
Sampling must be done using containers proven to be nonre-
bility of regulatory limitations prior to use.
active,suchasTedlarbags.Laboratoryequipmentmustalsobe
2. Referenced Documents inert and well conditioned to ensure reliable results. Frequent
calibrationusingstablestandardsisrequiredinsulfuranalysis.
2.1 ASTM Standards:
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2 4.2 A1-cm sampleofthefuelgastobeanalyzedisinjected
D1072 Test Method for Total Sulfur in Fuel Gases
2 into a gas chromatograph where it is passed through a 60-m,
D1145 Method of Sampling Natural Gas
megabore, thick film, methyl silicone liquid phase, open
D1945 Test Method for Analysis of Natural Gas by Gas
2 tubular partitioning column, and separated into its individual
Chromatography
constituents.
D2725 Test Method for Hydrogen Sulfide in Natural Gas
2 4.3 Sulfur Chemiluminescence Detection—As sulfur com-
(Methylene Blue Method)
pounds elute from the gas chromatographic column, they are
D3031 Test Method for Total Sulfur in Natural Gas by
2 combusted. These combustion products are collected and
Hydrogeneration
transferredtoasulfurchemiluminescencedetector(SCD).This
D4468 Test Method for Total Sulfur in Gaseous Fuels by
2 detection technique provides a highly sensitive, selective, and
Hydrogenolysis and Rateometric Colorimetry
linear response to volatile sulfur compounds and may be used
simultaneously while the usual fixed gas and hydrocarbon
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ThistestmethodisunderthejurisdictionofASTMCommitteeD-3onGaseous
determinations are being made.
Fuels and is the direct responsibility of Subcommittee D03.05 on Determination of
Special Constituents of Gaseous Fuels.
Current edition approved May 10, 1998. Published March 1999. Originally
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published as D 5504–94. Last previous edition D5504–94. Annual Book of ASTM Standards, Vol 05.02.
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Annual Book of ASTM Standards, Vol 05.05. Annual Book of ASTM Standards, Vol 14.01.
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D 5504–98
4.4 Other Detectors—This test method is written for the 6.1.4.1 FID—The detector must meet or exceed the typical
sulfur chemiluminescent detector. Other methods are available specifications given in Table 1 of Practice E594 while oper-
using the lead a
...