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 , 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, but the precision statements for these types of materials have not yet been determined.
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).
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. For specific hazard statements, see Sections 7 and 8.

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09-Mar-2003
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ASTM D3120-03 - 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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 3120 – 03
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 D 3120; 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 (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.
4
1. Scope * Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and
1.1 This test method covers the determination of sulfur
4
Petroleum Products
concentration in the range from 3.0 to 1000 mg/kg in light
D 6299 Practice for Applying Statistical Quality Assurance
liquid hydrocarbons boiling in the range from 26 to 274°C (80
Techniques to Evaluate Analytical Measurement System
to 525°F).
5
Performance
1.2 Other materials falling within the distillation range
2.2 OSHA Regulations:
specified in 1.1, but having sulfur concentrations above 1000
OSHA Regulations 29 CFR, paragraphs 1910.1000 and
mg/kg, may be tested using appropriate dilutions to bring them
6
1910.1200
within the specified limit. In addition, sample types that may be
outside the specified distillation range, such as diesels and
3. Summary of Test Method
biodiesels, may be analyzed by this test method, but the
3.1 A liquid sample is introduced into a pyrolysis tube
precision statements for these types of materials have not yet
maintained at a temperature between 900-1200°C, having a
been determined.
flowing stream of gas containing 50-80% oxygen and 20-50%
1.3 The values stated in SI units are to be regarded as the
inert gas (for example, argon, helium, etc.) Oxidative pyrolysis
standard. The values given in parentheses are provided for
converts the sulfur to sulfur dioxide, which then flows into a
information only. The preferred units are milligrams per
titration cell where it reacts with triiodide ion present in the
kilogram (mg/kg).
electrolyte. The triiodide ion consumed is coulometrically
1.4 This standard does not purport to address all of the
replaced and the total current (I 3 t) required to replace it is a
safety concerns, if any, associated with its use. It is the
measure of the sulfur present in the sample.
responsibility of the user of this standard to establish appro-
3.2 The reaction occurring in the titration cell as sulfur
priate safety and health practices and determine the applica-
dioxide enters is:
bility of regulatory limitations prior to use. For specific hazard
2 2 1
statements, see Sections 7 and 8.
I 1 SO 1 H O → SO 1 3I 1 2H (1)
3 2 2 3
The triiodide ion consumed in the above reaction is gener-
2. Referenced Documents
ated coulometrically thus:
2.1 ASTM Standards:
2 2 2
2
3I → I 1 2e (2)
D 1193 Specification for Reagent Water
3
D 1298 Test Method for Density, Relative Density (Specific
3.3 These microequivalents of triiodide ion (iodine) are
Gravity), or API Gravity of Crude Petroleum and Liquid
equal to the number of microequivalents of titratable SO ion
2
3
Petroleum Products by Hydrometer Method
entering the titration cell.
D 4052 Test Method for Density and Relative Density of
4
4. Significance and Use
Liquids by Digital Density Meter
D 4057 Practice for Manual Sampling of Petroleum and
4.1 This test method is used to determine the concentration
of sulfur in light liquid hydrocarbons, gasoline, and diesels and
their additives, where such concentrations of sulfur can be
detrimental to their production, performance, and use. The
1
This test method is under the jurisdiction of ASTM Committee D02 on
measurement of sulfur in the production and final product of
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved March 10, 2003. Published May 2003. Originally
e1
approved in 1972. Last previous edition approved in 2002 as D 3120–96 (2002) .
2 5
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 05.03.
3 6
Annual Book of ASTM Standards, Vol 05.01. Available from U.S. Government Printing Office, Superintendent of Docu-
4
Annual Book of ASTM Standards, Vol 05.02. 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.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
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