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ASTM D3246-11

(Test Method)

Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry

Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry

SIGNIFICANCE AND USE
Trace quantities of sulfur compounds in hydrocarbon products can be harmful to many catalytic chemical processes in which these products are used. Maximum permissible levels of total sulfur are normally included in specifications for such hydrocarbons. It is recommended that this test method be used to provide a basis for agreement between two laboratories when the determination of sulfur in hydrocarbon gases is important.
On liquefied petroleum gas, total volatile sulfur is measured on an injected gas sample. For such material a liquid sample must be used to measure total sulfur.
SCOPE
1.1 This test method covers determination of sulfur in the range from 1.5 to 100 mg/kg (ppm by mass) by weight in hydrocarbon products that are gaseous at normal room temperature and pressure.
Note 1— The test method has been tested cooperatively only on high-purity ethylene gas. Precision data have not been developed for other products.
1.2 The values stated in Si units are to be regarded as the standard. The values given n parentheses are for information only
1.3This 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.

General Information

Status
Historical
Publication Date
31-May-2011
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D3246-05 - Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
Effective Date
01-Jun-2011
Replaced By
ASTM D3246-14 - Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
Effective Date
01-May-2014
Referred By
ASTM D5274-00(2019) - Standard Guide for Analysis of 1,3–Butadiene Product
Effective Date
01-Jun-2011
Referred By
ASTM D5234-92(2017) - Standard Guide for Analysis of Ethylene Product
Effective Date
01-Jun-2011
Referred By
ASTM D5273-18 - Standard Guide for Analysis of Propylene Concentrates
Effective Date
01-Jun-2011
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-Jun-2011
Referred By
ASTM D7166-23 - Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels
Effective Date
01-Jun-2011
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Jun-2011

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ASTM D3246-11 - Standard Test Method for Sulfur in Petroleum Gas by Oxidative MicrocoulometryASTM D3246-11 - Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
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ASTM D3246-11 - Standard Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
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Standards Content (Sample)

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: D3246 − 11
StandardTest Method for
1
Sulfur in Petroleum Gas by Oxidative Microcoulometry
This standard is issued under the fixed designation D3246; 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.
1. Scope* 2.2 Other Standards:
CompressedGasAssociationBookletsG-4andG-4-1onthe
1.1 This test method covers determination of sulfur in the
3
Use of Oxygen
range from 1.5 to 100 mg/kg (ppm by mass) by weight in
hydrocarbon products that are gaseous at normal room tem-
3. Summary of Test Method
perature and pressure.
3.1 Asample is injected into a combustion tube maintained
NOTE 1—The test method has been tested cooperatively only on
at about 800°C having a flowing stream of gas containing
high-purityethylenegas.Precisiondatahavenotbeendevelopedforother
about 80% oxygen and 20% inert gas (for example, nitrogen,
products.
argon, etc.). Oxidative pyrolysis converts the sulfur to sulfur
1.2 The values stated in SI units are to be regarded as
dioxide which then flows into a titration cell where it reacts
standard. No other units of measurement are included in this
with triiodide ion present in the electrolyte. The triiodide thus
standard.
consumed, is coulometrically replaced and the total current
1.3 This standard does not purport to address all of the
required to replace it is a measure of the sulfur present in the
safety concerns, if any, associated with its use. It is the
sample injected.
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.
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:
D1265Practice for Sampling Liquefied Petroleum (LP)
2 2 2
3I →I 12e (2)
3
Gases, Manual Method
3.3 Thesemicroequivalentsoftriiodide(iodine)areequalto
D1193Specification for Reagent Water
the number of microequivalents of titratable sample ion enter-
D3120Test Method for Trace Quantities of Sulfur in Light
ing the titration cell.
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
lometry
3.4 A liquid blend containing a known amount of sulfur is
D6299Practice for Applying Statistical Quality Assurance
used for calibration.
and Control Charting Techniques to Evaluate Analytical
4. Significance and Use
Measurement System Performance
F307Practice for Sampling Pressurized Gas for GasAnaly-
4.1 Trace quantities of sulfur compounds in hydrocarbon
sis
products can be harmful to many catalytic chemical processes
inwhichtheseproductsareused.Maximumpermissiblelevels
1
of total sulfur are normally included in specifications for such
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
hydrocarbons. It is recommended that this test method be used
D02.03 on Elemental Analysis.
to provide a basis for agreement between two laboratories
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved
when the determination of sulfur in hydrocarbon gases is
in 1973. Last previous edition approved in 2005 as D3246–05. DOI: 10.1520/
D3246-11. important.
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 Compressed Gas Association, 1235 Jefferson Davis Hwy.,
the ASTM website. Arlington, VA 22202.
*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 ----------------------
D3246 − 11
4.2 On liquefied petroleum gas, total volatile sulfur is means. (Warning—Excessive speed will decouple the stirring
measuredonaninjectedgassample.Forsuchmaterialaliquid bar,causingittoriseinthecellanddamagetheelectrodes.The
sample must be used to measure total sulfur. creation of a slight vortex is adequate.)
6.4 Microcoulometer, having variable attenuation gain con-
5. Interferences
trol, and capable of measuring the potential of the sensing-
5.1 This test method is applicable in the presence of total
reference electrode pair, and comparing this potential with a
halideconcentrationsofupto10timesthesulfurlevelandtotal
biaspotential,amplifyingthepotentialdifference,andapplying
nitrogen content
...

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1.3 The values stated in inch-pound units or in SI units and which are not in parentheses are to be regarded as the standard. The values given in parentheses are for information only.  
Note 2: Oil tubes and apparatus used in this test method have traditionally been marked in inches, (the tube is required to be etched with 1/8 in. divisions.) The Saybolt Color Numbers are aligned with inch, 1/2 in., 1/4 in., and 1/8 in. changes in the depth of oil. These fractional inch changes do not readily correspond to SI equivalents and in view of the preponderance of apparatus already in use and marked in inches, the inch/pound unit is regarded as the standard. However the test method does use SI units of length when the length is not directly related to divisions on the oil tube and Saybolt Color Numbers. The test method uses SI units for temperature.  
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5.1 Predicting the viscosity of a blend of components is a common problem. Both the Wright Blending Method and the ASTM Blending Method, described in this practice, may be used to solve this problem.  
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5.5 The calculations described in this practice have been computerized as a spreadsheet and are available as an adjunct.3
SCOPE
1.1 This practice covers the procedures for calculating the estimated kinematic viscosity of a blend of two or more petroleum products, such as lubricating oil base stocks, fuel components, residual fuel oil with kerosene, crude oils, and related products, from their kinematic viscosities and blend fractions.  
1.2 This practice allows for the estimation of the fraction of each of two petroleum products needed to prepare a blend meeting a specific viscosity.  
1.3 This practice may not be applicable to other types of products, or to materials which exhibit strong non-Newtonian properties, such as viscosity index improvers, additive packages, and products containing particulates.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 Logarithms may be either common logarithms or natural logarithms, as long as the same are used consistently. This practice uses common logarithms. If natural logarithms are used, the inverse function, exp(×), must be used in place of the base 10 exponential function, 10×, used herein.  
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ASTM D4952-23(Test Method)
Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)

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5.1 Sulfur present as mercaptans or as hydrogen sulfide in distillate fuels and solvents can attack many metallic and non-metallic materials in fuel and other distribution systems. A negative result in the doctor test ensures that the concentration of these compounds is insufficient to cause such problems in normal use.
SCOPE
1.1 This test method covers and is intended primarily for the detection of mercaptans in motor fuel, kerosine, and similar petroleum products. This method may also provide information on hydrogen sulfide and elemental sulfur that may be present in these sample types.  
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5.1 The boiling range distribution of petroleum fractions provides an insight into the composition of feedstocks and products related to petroleum refining processes. The gas chromatographic simulation of this determination can be used to replace conventional distillation methods for control of refining operations. This test method can be used for product specification testing with the mutual agreement of interested parties.  
5.2 Boiling range distributions obtained by this test method are essentially equivalent to those obtained by true boiling point (TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillations such as those obtained with Test Method D86 or D1160.  
5.3 Procedure B was tested with biodiesel mixtures and reports the Boiling Point Distribution of FAME esters of vegetable and animal origin mixed with ultra low sulfur diesel.
SCOPE
1.1 This test method covers the determination of the boiling range distribution of petroleum products. The test method is applicable to petroleum products and fractions having a final boiling point of 538 °C (1000 °F) or lower at atmospheric pressure as measured by this test method. This test method is limited to samples having a boiling range greater than 55.5 °C (100 °F), and having a vapor pressure sufficiently low to permit sampling at ambient temperature.
Note 1: Since a boiling range is the difference between two temperatures, only the constant of 1.8 °F/°C is used in the conversion of the temperature range from one system of units to another.  
1.1.1 Procedure A (Sections 6 – 14)—Allows a larger selection of columns and analysis conditions such as packed and capillary columns as well as a Thermal Conductivity Detector in addition to the Flame Ionization Detector. Analysis times range from 14 min to 60 min.  
1.1.2 Procedure B (Sections 15 – 23)—Is restricted to only 3 capillary columns and requires no sample dilution. In addition, Procedure B is used not only for the sample types described in Procedure A but also for the analysis of samples containing biodiesel mixtures B5, B10, and B20. The analysis time, when using Procedure B (Accelerated D2887), is reduced to about 8 min.  
1.2 This test method is not to be used for the analysis of gasoline samples or gasoline components. These types of samples must be analyzed by Test Method D7096.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

  • Standard
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    English language
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  • Standard
    35 pages
    English language
    sale 15% off