ASTM D6667-10
(Test Method)Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence
Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence
SIGNIFICANCE AND USE
The sulfur content of LPG, used for fuel purposes, contributes to SOx emissions and can lead to corrosion in engine and exhaust systems. Some process catalysts used in petroleum and chemical refining can be poisoned by sulfur bearing materials in the feed stocks. This test method can be used to determine sulfur in process feeds, to measure sulfur in finished products, and can also be used for compliance determinations when acceptable to a regulatory authority.
SCOPE
1.1 This test method covers the determination of total volatile sulfur in gaseous hydrocarbons and liquefied petroleum (LP) gases. It is applicable to analysis of natural, processed, and final product materials containing sulfur in the range of 1 to 100 mg/kg (Note 1).
Note 1—An estimate of pooled limit of quantification (PLOQ), information regarding sample stability and other general information derived from the inter-laboratory study on precision can be referenced in the ASTM research report.
1.2 This test method may not detect sulfur compounds that do not vaporize under the conditions of the test.
1.3 This test method is applicable for total volatile sulfur determination in LP gases containing less than 0.35 % (mass/mass) halogen(s).
1.4 The values stated in SI units are to be regarded as 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 and health practices and determine the applicability of regulatory limitations prior to use. See 3.1 and Sections 6 and 7 for specific warning statements.
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Designation:D6667 −10
StandardTest Method for
Determination of Total Volatile Sulfur in Gaseous
Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet
1
Fluorescence
This standard is issued under the fixed designation D6667; 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* D3700 Practice for Obtaining LPG Samples Using a Float-
ing Piston Cylinder
1.1 This test method covers the determination of total
D5287 Practice for Automatic Sampling of Gaseous Fuels
volatile sulfur in gaseous hydrocarbons and liquefied petro-
D6299 Practice for Applying Statistical Quality Assurance
leum (LP) gases. It is applicable to analysis of natural,
and Control Charting Techniques to Evaluate Analytical
processed, and final product materials containing sulfur in the
Measurement System Performance
range of 1 to 100 mg/kg (Note 1).
F307 Practice for Sampling Pressurized Gas for Gas Analy-
NOTE 1—An estimate of pooled limit of quantification (PLOQ),
sis
information regarding sample stability and other general information
4
2.2 Gas Processor Association (GPA) Standards:
derived from the inter-laboratory study on precision can be referenced in
2
GPA 2166 Obtaining Natural Gas Samples for Analysis by
the ASTM research report.
Gas Chromatography
1.2 This test method may not detect sulfur compounds that
GPA 2174 Obtaining Liquid Hydrocarbon Samples for
do not vaporize under the conditions of the test.
Analysis by Gas Chromatography
1.3 This test method is applicable for total volatile sulfur
3. Summary of Test Method
determination in LP gases containing less than 0.35 % (mass/
mass) halogen(s).
3.1 Aheatedsamplevalveisusedtoinjectgaseoussamples.
Liquefied petroleum gas (LPG) samples are injected by a
1.4 The values stated in SI units are to be regarded as
sample valve connected to a heated expansion chamber. The
standard.
gaseous sample then enters a high temperature combustion
1.5 This standard does not purport to address all of the
tube where sulfur is oxidized to sulfur dioxide (SO)inan
2
safety concerns, if any, associated with its use. It is the
oxygen rich atmosphere. Water produced during the sample
responsibility of the user of this standard to establish appro-
combustion is removed and the sample combustion gases are
priate safety and health practices and determine the applica-
next exposed to ultraviolet (UV) light. The SO absorbs the
2
bility of regulatory limitations prior to use. See 3.1 and
energy from the UV light and is converted to an excited sulfur
Sections 6 and 7 for specific warning statements.
*
dioxide (SO ). Fluorescence emitted from the excited SO as
2 2
*
2. Referenced Documents it returns to a stable state SO is detected by a photomultiplier
2
3 tube,theresultingsignalisameasureofthesulfurcontainedin
2.1 ASTM Standards:
the sample. (Warning—Exposure to excessive quantities of
D1070 Test Methods for Relative Density of Gaseous Fuels
ultraviolet light is injurious to health. The operator shall avoid
D1265 Practice for Sampling Liquefied Petroleum (LP)
exposing their person, especially their eyes, not only to direct
Gases, Manual Method
UV light but also to secondary or scattered radiation that is
present.)
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
4. Significance and Use
D02.03 on Elemental Analysis.
Current edition approved Oct. 1, 2010. Published November 2010. Originally 4.1 The sulfur content of LPG, used for fuel purposes,
approved in 2001. Last previous edition approved in 2010 as D6667–04(2010).
contributes to SOx emissions and can lead to corrosion in
DOI: 10.1520/D6667-10.
engine and exhaust systems. Some process catalysts used in
2
Supporting data have been filed at ASTM International Headquarters and may
petroleum and chemical refining can be poisoned by sulfur
be obtained by requesting Research Report RR:D02-1506.
3
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
4
Standards volume information, refer to the standard’s Document Summary page on Available from Gas ProcessorsAssociation (GPA), 6526 E. 60th St.,Tulsa, OK
the ASTM website. 74145.
*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
---------------------- Page: 1 ----------------------
D6667−10
FIG. 1Example of a Typical Direct Inject Quartz Pyrolysis Tube
bearing materials in the feed stoc
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6667–04 (Reapproved 2010) Designation: D6667 – 10
Standard Test Method for
Determination of Total Volatile Sulfur in Gaseous
Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet
1
Fluorescence
This standard is issued under the fixed designation D6667; 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 covers the determination of total volatile sulfur in gaseous hydrocarbons and liquefied petroleum (LP)
gases. It is applicable to analysis of natural, processed, and final product materials containing sulfur in the range of 1 to 100 mg/kg
(Note 1).
NOTE 1—An estimate of pooled limit of quantification (PLOQ), information regarding sample stability and other general information derived from the
2
inter-laboratory study on precision can be referenced in the ASTM research report.
1.2 This test method may not detect sulfur compounds that do not vaporize under the conditions of the test.
1.3 This test method is applicable for total volatile sulfur determination in LP gases containing less than 0.35 % (mass/mass)
halogen(s).
1.4 The values stated in SI units are to be regarded as 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 and health practices and determine the applicability of regulatory
limitations prior to use. See 3.1 and Sections 6 and 7 for specific warning statements.
2. Referenced Documents
3
2.1 ASTM Standards:
D1070 Test Methods for Relative Density of Gaseous Fuels
D1265 Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
D5287 Practice for Automatic Sampling of Gaseous Fuels
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
F307 Practice for Sampling Pressurized Gas for Gas Analysis
4
2.2 Gas Processor Association (GPA) Standards:
GPA 2166 Obtaining Natural Gas Samples for Analysis by Gas Chromatography
GPA 2174 Obtaining Liquid Hydrocarbon Samples for Analysis by Gas Chromatography
3. Summary of Test Method
3.1 Aheated sample valve is used to inject gaseous samples. Liquefied petroleum gas (LPG) samples are injected by a sample
valve connected to a heated expansion chamber.The gaseous sample then enters a high temperature combustion tube where sulfur
is oxidized to sulfur dioxide (SO ) in an oxygen rich atmosphere. Water produced during the sample combustion is removed and
2
the sample combustion gases are next exposed to ultraviolet (UV) light. The SO absorbs the energy from the UV light and is
2
* *
converted to an excited sulfur dioxide (SO ). Fluorescence emitted from the excited SO as it returns to a stable state SO is
2 2 2
detected by a photomultiplier tube, the resulting signal is a measure of the sulfur contained in the sample. (Warning—Exposure
to excessive quantities of ultraviolet light is injurious to health. The operator shall avoid exposing their person, especially their
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
CurrenteditionapprovedMayOct.1,2010.PublishedMayNovember2010.Originallyapprovedin2001.Lastpreviouseditionapprovedin20042010asD6667–04(2010).
DOI: 10.1520/D6667-10.
2
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1506.
3
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
4
Available from Gas Processors Association (GPA), 6526 E. 60th St., Tulsa, OK 74145.
*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
---------------------- Page: 1 ----------------------
D6667 – 10
eyes, not only to direct UV light but also to secondary or scattered radiation that is present.)
4. Significance and Use
4.1
...
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