ASTM D1552-16
(Test Method)Standard Test Method for Sulfur in Petroleum Products by High Temperature Combustion and Infrared (IR) Detection or Thermal Conducitivity Detection (TCD)
Standard Test Method for Sulfur in Petroleum Products by High Temperature Combustion and Infrared (IR) Detection or Thermal Conducitivity Detection (TCD)
SIGNIFICANCE AND USE
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product.
SCOPE
1.1 This test method covers procedures for the determination of total sulfur in petroleum products including lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177 °C (350 °F) and containing a mass fraction of sulfur between 0.22 % and 24.2 %. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply. These procedures use IR detection or TCD following combustion in a furnace.
1.2 Petroleum coke containing a mass fraction of sulfur between 2.53 % to 3.79 % sulfur may be analyzed. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.
Note 1: The D1552–08 (2014) version of this standard contained two other procedures using iodate titrations. Since these procedures are no longer being used in the industry laboratories based on a survey of D02.SC 3 laboratories conducted in September 2014, they are being deleted. For earlier information on the deleted procedures, D1552–08 (2014) may be perused.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
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Designation: D1552 − 16
Standard Test Method for
Sulfur in Petroleum Products by High Temperature
Combustion and Infrared (IR) Detection or Thermal
1
Conducitivity Detection (TCD)
This standard is issued under the fixed designation D1552; 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* D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers procedures for the determina-
D4177 Practice for Automatic Sampling of Petroleum and
tion of total sulfur in petroleum products including lubricating
Petroleum Products
oilscontainingadditives,andinadditiveconcentrates.Thistest
D6299 Practice for Applying Statistical Quality Assurance
method is applicable to samples boiling above 177 °C (350 °F)
and Control Charting Techniques to Evaluate Analytical
and containing a mass fraction of sulfur between 0.22 % and
Measurement System Performance
24.2 %. Other sulfur concentrations may be analyzed, but the
D6300 Practice for Determination of Precision and Bias
precision stated may or may not apply. These procedures use
Data for Use in Test Methods for Petroleum Products and
IR detection or TCD following combustion in a furnace.
Lubricants
1.2 Petroleum coke containing a mass fraction of sulfur
D6792 Practice for Quality System in Petroleum Products
between2.53 %to3.79 %sulfurmaybeanalyzed.Othersulfur
and Lubricants Testing Laboratories
concentrations may be analyzed, but the precision stated may
or may not apply. 3. Summary of Test Method
NOTE 1—The D1552–08 (2014) version of this standard contained two 3.1 The sample is weighed and placed into a furnace having
other procedures using iodate titrations. Since these procedures are no
an oxygen atmosphere sufficient to combust the entire sample
longer being used in the industry laboratories based on a survey of
and a temperature between 1150 °C and 1450 °C for Procedure
D02.SC 3 laboratories conducted in September 2014, they are being
A or 1150 °C for Procedure B. Most sulfur present is com-
deleted. For earlier information on the deleted procedures, D1552–08
busted to SO , which is then measured with a detector after
(2014) may be perused.
2
moisture and dust are removed by traps. The instrument
1.3 The values stated in SI units are to be regarded as the
calculates the mass percent sulfur from the sample mass, the
standard. The values given in parentheses are for information
integrated detector signal, and a predetermined calibration
only.
factor. The calibration factor is determined using standards
1.4 This standard does not purport to address all of the
approximating the material to be analyzed.
safety concerns, if any, associated with its use. It is the
3.1.1 Procedure A—After combustion of the sample and
responsibility of the user of this standard to establish appro-
subsequent moisture/dust removal, SO is measured using
2
priate safety and health practices and determine the applica-
infrared (IR) detection.
bility of regulatory limitations prior to use.
3.1.2 Procedure B—After combustion of the sample and
subsequent moisture/dust removal, SO is measured using
2
2. Referenced Documents
thermal conductivity detection. An apparatus utilizing TCD
2
2.1 ASTM Standards:
may require the sample gas to pass an oxygen scrubber and
adsorption/desorption traps to allow passing of contaminants
1
prior to measuring SO .
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
4. Significance and Use
Current edition approved July 1, 2016. Published August 2016. Originally
4.1 This test method provides a means of monitoring the
approved in 1958. Last previous edition approved in 2015 as D1552 – 15. DOI:
10.1520/D1552-16.
sulfur level of various petroleum products and additives. This
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
knowledge can be used to predict performance, handling, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
processing properties. In some cases the presence of sulfur
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. compounds is beneficial to the product and monitoring the
*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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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: D1552 − 15 D1552 − 16
Standard Test Method for
Sulfur in Petroleum Products by High Temperature
Combustion and IR DetectionInfrared (IR) Detection or
1
Thermal Conducitivity Detection (TCD)
This standard is issued under the fixed designation D1552; 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*
1.1 This test method covers a procedure procedures for the determination of total sulfur in petroleum products including
lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177 °C
(350 °F) and containing a mass fraction of sulfur not less than 0.06 %. This procedure uses IR detection following pyrolysis in a
resistance between 0.22 % and 24.2 %. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.
These procedures use IR detection or TCD following combustion in a furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.a mass fraction of sulfur between 2.53 % to 3.79 % sulfur
may be analyzed. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.
NOTE 1—The D1552–08 (2014) version of this standard contained two other procedures using iodate titrations. Since these procedures are no longer
being used in the industry laboratories based on a survey of D02.SC 3 laboratories conducted in September 2014, they are being deleted. For earlier
information on the deleted procedures, D1552–08 (2014) may be perused.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1266D4057 Test Method for Sulfur in Petroleum Products (Lamp Method)Practice for Manual Sampling of Petroleum and
Petroleum Products
D4057D4177 Practice for ManualAutomatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 The sample is weighed into a special ceramic boat which is then and placed into a combustion furnace at 1350 °C (2460 °F)
in an oxygen atmosphere. furnace having an oxygen atmosphere sufficient to combust the entire sample and a temperature between
1150 °C and 1450 °C for Procedure A or 1150 °C for Procedure B. Most sulfur present is combusted to SO , which is then
2
measured with an infrared a detector after moisture and dust are removed by traps. A microprocessorThe instrument calculates the
mass percent sulfur from the sample weight,mass, the integrated detector signal, and a predetermined calibration factor. The
calibration factor is determined using standards approximating the material to be analyzed.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved April 1, 2015July 1, 2016. Published May 2015August 2016. Originally approved in 1958. Last previous edition approved in 20142015 as
ε1
D1552 – 08 (2014)D1552 – 15. . DOI: 10.1520/D1552-15.10.1520/D1552-16.
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.
*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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D1552
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