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

SIGNIFICANCE AND USE
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 measurement of sulfur in the production and final product of gasoline and diesel is required for both regulatory purposes and to ensure maximum life expectancy of catalytic converters used in the automotive industry.
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 and fuels with oxygenates boiling in the range from 26 to 274°C (80 to 525°F).
Note 1: Preliminary data has shown that this test method is also applicable to the determination of sulfur in denatured fuel ethanol (Specification D4806), automotive spark ignition engine fuel (Specification D4814), Ed75–Ed85 (Specification D5798) or gasoline-oxygenate fuel blends with greater than 10% ethanol. However, the precision for these materials has not been determined. Subcommittee D02.03 is undertaking activities to obtain precision statements for these materials.  
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 standard. No other units of measurement are included in this standard. 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 – 9.

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Publication Date
30-Apr-2014
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D3120 − 08 (Reapproved 2014)
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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope D1298Test Method for Density, Relative Density, or API
Gravity of Crude Petroleum and Liquid Petroleum Prod-
1.1 This test method covers the determination of sulfur
ucts by Hydrometer Method
concentration in the range from 3.0 to 1000mg⁄kg in light
D4052Test Method for Density, Relative Density, and API
liquid hydrocarbons and fuels with oxygenates boiling in the
Gravity of Liquids by Digital Density Meter
range from 26 to 274°C (80 to 525°F).
D4057Practice for Manual Sampling of Petroleum and
NOTE 1—Preliminary data has shown that this test method is also
Petroleum Products
applicable to the determination of sulfur in denatured fuel ethanol
D4177Practice for Automatic Sampling of Petroleum and
(Specification D4806), automotive spark ignition engine fuel (Specifica-
Petroleum Products
tion D4814), Ed75–Ed85 (Specification D5798) or gasoline-oxygenate
D4806Specification for Denatured Fuel Ethanol for Blend-
fuel blends with greater than 10% ethanol. However, the precision for
these materials has not been determined. Subcommittee D02.03 is
ing with Gasolines for Use asAutomotive Spark-Ignition
undertaking activities to obtain precision statements for these materials.
Engine Fuel
1.2 Other materials falling within the distillation range D4814Specification for Automotive Spark-Ignition Engine
specified in 1.1, but having sulfur concentrations above 1000 Fuel
mg/kg,maybetestedusingappropriatedilutionstobringthem D5798Specification for Ethanol Fuel Blends for Flexible-
withinthespecifiedlimit.Inaddition,sampletypesthatmaybe Fuel Automotive Spark-Ignition Engines
outside the specified distillation range, such as diesels and D6299Practice for Applying Statistical Quality Assurance
biodiesels, may be analyzed by this test method. and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 2.2 OSHA Regulations:
standard. The preferred units are milligrams per kilogram OSHA Regulations29 CFR, paragraphs 1910.1000 and
3
(mg/kg). 1910.1200
1.4 This standard does not purport to address all of the
3. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1 A liquid sample is introduced into a pyrolysis tube
priate safety and health practices and determine the applica-
maintained at a temperature between 900 to 1200°C, having a
bility of regulatory limitations prior to use.For specific hazard
flowing stream of gas containing 50 to 80% oxygen and 20 to
statements, see Sections7–9.
50% inert gas (for example, argon, helium, and so forth).
Oxidativepyrolysisconvertsthesulfurtosulfurdioxide,which
2. Referenced Documents
then flows into a titration cell where it reacts with triiodide ion
2
2.1 ASTM Standards:
present in the electrolyte. The triiodide ion consumed is
D1193Specification for Reagent Water
coulometricallyreplacedandthetotalcurrent(I×t)requiredto
replace it is a measure of the sulfur present in the sample.
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.2 The reaction occurring in the titration cell as sulfur
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis. dioxide enters is:
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
2 2 1
I 1SO 1H O→SO 13I 12H (1)
in 1972. Last previous edition approved in 2008 as D3120–08. DOI: 10.1520/ 3 2 2 3
D3120-08R14.
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
the ASTM website. Documents, 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 − 08 (2014)
The triiodide ion consumed
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D3120 − 08 D3120 − 08 (Reapproved 2014)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*Scope
1.1 This test method covers the determination of sulfur concentration in the range from 3.0 to 10001000 mg mg/kg ⁄kg in light
liquid hydrocarbons and fuels with oxygenates boiling in the range from 26 to 274°C (80 to 525°F).
NOTE 1—Preliminary data has shown that this test method is also applicable to the determination of sulfur in denatured fuel ethanol (Specification
D4806), automotive spark ignition engine fuel (Specification D4814), Ed75–Ed85 (Specification D5798) or gasoline-oxygenate fuel blends with greater
than 10% ethanol. However, the precision for these materials has not been determined. Subcommittee D02.03 is undertaking activities to obtain precision
statements for these materials.
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 standard. No other units of measurement are included in this standard.
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 – 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products by
Hydrometer Method
D4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4806 Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine Fuel
D4814 Specification for Automotive Spark-Ignition Engine Fuel
D5798 Specification for Ethanol Fuel Blends for Flexible-Fuel Automotive Spark-Ignition Engines
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
2.2 OSHA Regulations:
3
OSHA Regulations 29 CFR, paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 A liquid sample is introduced into a pyrolysis tube maintained at a temperature between 900-1200°C, 900 to 1200°C, having
a flowing stream of gas containing 50-80% 50 to 80% oxygen and 20-50% 20 to 50% inert gas (for example, argon, helium, etc.)
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved Dec. 15, 2008May 1, 2014. Published February 2009July 2014. Originally approved in 1972. Last previous edition approved in 20062008 as
ε1
D3120D3120 – 08.–06 . DOI: 10.1520/D3120-08.10.1520/D3120-08R14.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office, Superintendent of Documents, 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 − 08 (2014)
and so forth
...

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