Standard Test Method for Trace Quantities of Sulfur in Light Liquid Petroleum Hydrocarbons by Oxidative Microcoulometry

SCOPE
1.1 This test method covers the determination of sulfur concentration in the range from 3.0 to 1000 mg/kg in light liquid hydrocarbons boiling in the range from 26 to 274°C (80 to 525°F).
1.2 Other materials falling within the distillation range specified in 1.1, but having sulfur concentrations above 1000 mg/kg, may be tested using appropriate dilutions to bring them within the specified limit. In addition, sample types that may be outside the specified distillation range, such as diesels and biodiesels, may be analyzed by this test method.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only. The preferred units are milligrams per kilogram (mg/kg).
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. For specific hazard statements, see Sections 7-9.

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ASTM D3120-06 - Standard Test Method for Trace Quantities of Sulfur in Light Liquid Petroleum Hydrocarbons by Oxidative Microcoulometry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
An American National Standard
Designation:D3120–06
Standard Test Method for
Trace Quantities of Sulfur in Light Liquid Petroleum
1
Hydrocarbons by Oxidative Microcoulometry
This standard is issued under the fixed designation D3120; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of sulfur
D6299 Practice forApplying Statistical QualityAssurance
concentration in the range from 3.0 to 1000 mg/kg in light
Techniques to Evaluate Analytical Measurement System
liquid hydrocarbons boiling in the range from 26 to 274°C (80
Performance
to 525°F).
2.2 OSHA Regulations:
1.2 Other materials falling within the distillation range
OSHA Regulations 29 CFR, paragraphs 1910.1000 and
specified in 1.1, but having sulfur concentrations above 1000
3
1910.1200
mg/kg,maybetestedusingappropriatedilutionstobringthem
withinthespecifiedlimit.Inaddition,sampletypesthatmaybe
3. Summary of Test Method
outside the specified distillation range, such as diesels and
3.1 A liquid sample is introduced into a pyrolysis tube
biodiesels, may be analyzed by this test method.
maintained at a temperature between 900-1200°C, having a
1.3 The values stated in SI units are to be regarded as the
flowing stream of gas containing 50-80% oxygen and 20-50%
standard. The values given in parentheses are provided for
inertgas(forexample,argon,helium,etc.)Oxidativepyrolysis
information only. The preferred units are milligrams per
converts the sulfur to sulfur dioxide, which then flows into a
kilogram (mg/kg).
titration cell where it reacts with triiodide ion present in the
1.4 This standard does not purport to address all of the
electrolyte. The triiodide ion consumed is coulometrically
safety concerns, if any, associated with its use. It is the
replaced and the total current (I 3 t) required to replace it is a
responsibility of the user of this standard to establish appro-
measure of the sulfur present in the sample.
priate safety and health practices and determine the applica-
3.2 The reaction occurring in the titration cell as sulfur
bility of regulatory limitations prior to use. For specific hazard
dioxide enters is:
statements, see Sections 7-9.
2 2 1
I 1SO 1H O→SO 13I 12H (1)
3 2 2 3
2. Referenced Documents
The triiodide ion consumed in the above reaction is gener-
2
2.1 ASTM Standards:
ated coulometrically thus:
D1193 Specification for Reagent Water
2 2 2
3I →I 12e (2)
D1298 TestMethodforDensity,RelativeDensity(Specific
3
Gravity), or API Gravity of Crude Petroleum and Liquid
3.3 These microequivalents of triiodide ion (iodine) are
Petroleum Products by Hydrometer Method
equal to the number of microequivalents of titratable SO ion
2
D4052 Test Method for Density and Relative Density of
entering the titration cell.
Liquids by Digital Density Meter
4. Significance and Use
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
4.1 This test method is used to determine the concentration
ofsulfurinlightliquidhydrocarbons,gasoline,anddieselsand
their additives, where such concentrations of sulfur can be
1
This test method is under the jurisdiction of ASTM Committee D02 on
detrimental to their production, performance, and use. The
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
D02.03 on Elemental Analysis.
measurement of sulfur in the production and final product of
Current edition approved Dec. 1, 2006. Published January 2007. Originally
gasolineanddieselisrequiredforbothregulatorypurposesand
approved in 1972. Last previous edition approved in 2003 as D3120–03a.
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from U.S. Government Printing Office, Superintendent of Docu-
the ASTM website. ments, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*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

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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.
D3120–06
NOTE 1—Take care not to use excessive stirring and possibly da
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