ASTM D3120-03a

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3120–03a
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.
4
1. Scope* Petroleum Products
D6299 Practice forApplying Statistical QualityAssurance
1.1 This test method covers the determination of sulfur
Techniques to Evaluate Analytical Measurement System
concentration in the range from 3.0 to 1000 mg/kg in light
5
Performance
liquid hydrocarbons boiling in the range from 26 to 274°C (80
2.2 OSHA Regulations:
to 525°F).
OSHA Regulations 29 CFR, paragraphs 1910.1000 and
1.2 Other materials falling within the distillation range
6
1910.1200
specified in 1.1, but having sulfur concentrations above 1000
mg/kg,maybetestedusingappropriatedilutionstobringthem
3. Summary of Test Method
withinthespecifiedlimit.Inaddition,sampletypesthatmaybe
3.1 A liquid sample is introduced into a pyrolysis tube
outside the specified distillation range, such as diesels and
maintained at a temperature between 900-1200°C, having a
biodiesels, may be analyzed by this test method.
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
inertgas(forexample,argon,helium,etc.)Oxidativepyrolysis
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 7-9.
I 1SO 1H O→SO 13I 12H (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 12e (2)
D1193 Specification for Reagent Water
3
D1298 TestMethodforDensity,RelativeDensity(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.
D4052 Test Method for Density and Relative Density of
4
4. Significance and Use
Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and
4.1 This test method is used to determine the concentration
4
Petroleum Products
ofsulfurinlightliquidhydrocarbons,gasoline,anddieselsand
D4177 Practice for Automatic Sampling of Petroleum and
their additives, where such concentrations of sulfur can be
detrimental to their production, performance, and use. The
measurement of sulfur in the production and final product of
gasolineanddieselisrequiredforbothregulatorypurposesand
1
This test method is under the jurisdiction of ASTM Committee D02 on
to ensure maximum life expectancy of catalytic converters
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
D02.03 on Elemental Analysis. used in the automotive industry.
Current edition approved Sept. 10, 2003. Published September 2003. Originally
approved in 1972. Last previous edition approved in 2003 as D3120–03.
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.
1

---------------------- Page: 1 ----------------------
D3120–03a
5. Interferences 6.7 Dryer Tube—The oxidation of samples produces water
vapor which, if allowed to condense between the exit of the
5.1 This test method is applicable in the presence of total
...