ASTM D1552-15
(Test Method)Standard Test Method for Sulfur in Petroleum Products by High Temperature Combustion and IR Detection
Standard Test Method for Sulfur in Petroleum Products by High Temperature Combustion and IR Detection
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 a procedure 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 furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.
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 − 15
StandardTest Method for
Sulfur in Petroleum Products by High Temperature
1
Combustion and IR Detection
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* D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.1 This test method covers a procedure for the determina-
Measurement System Performance
tion of total sulfur in petroleum products including lubricating
D6792 Practice for Quality System in Petroleum Products
oilscontainingadditives,andinadditiveconcentrates.Thistest
and Lubricants Testing Laboratories
method is applicable to samples boiling above 177 °C (350 °F)
and containing a mass fraction of sulfur not less than 0.06 %.
3. Summary of Test Method
This procedure uses IR detection following pyrolysis in a
3.1 The sample is weighed into a special ceramic boat
resistance furnace.
which is then placed into a combustion furnace at 1350 °C
1.2 Petroleum coke containing up to 8 mass % sulfur can be
(2460 °F) in an oxygen atmosphere. Most sulfur present is
analyzed.
combusted to SO which is then measured with an infrared
2
detector after moisture and dust are removed by traps. A
NOTE 1—The D1552–08 (2014) version of this standard contained two
other procedures using iodate titrations. Since these procedures are no microprocessor calculates the mass percent sulfur from the
longer being used in the industry laboratories based on a survey of
sample weight, the integrated detector signal and a predeter-
D02.SC 3 laboratories conducted in September 2014, they are being
mined calibration factor. The calibration factor is determined
deleted. For earlier information on the deleted procedures, D1552–08
using standards approximating the material to be analyzed.
(2014) may be perused.
4. Significance and Use
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
4.1 This test method provides a means of monitoring the
only.
sulfur level of various petroleum products and additives. This
1.4 This standard does not purport to address all of the knowledge can be used to predict performance, handling, or
safety concerns, if any, associated with its use. It is the
processing properties. In some cases the presence of sulfur
responsibility of the user of this standard to establish appro- compounds is beneficial to the product and monitoring the
priate safety and health practices and determine the applica-
depletion of sulfur can provide useful information. In other
bility of regulatory limitations prior to use. cases the presence of sulfur compounds is detrimental to the
processing or use of the product.
2. Referenced Documents
5. Apparatus
2
2.1 ASTM Standards:
5.1 Resistance Type Furnace, capable of maintaining a
D1266 Test Method for Sulfur in Petroleum Products (Lamp
temperature of at least 1350 °C (2460 °F).
Method)
D4057 Practice for Manual Sampling of Petroleum and
5.2 Absorber, as described in Test Method D1266.
Petroleum Products
5.3 Combustion and IR Detection System, comprised of
automatic balance, oxygen flow controls, drying tubes, com-
1 bustion furnace, infrared detector and microprocessor. The
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
furnace shall be capable of maintaining a nominal operating
Subcommittee D02.03 on Elemental Analysis.
temperature of 1350 °C (2460 °F).
Current edition approved April 1, 2015. Published May 2015. Originally
ε1
approved in 1958. Last previous edition approved in 2014 as D1552 – 08 (2014) .
5.4 Sieve, 60 mesh (250 µm).
DOI: 10.1520/D1552-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Reagents and Materials
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. used in all tests. Unless otherwise indicated, it is intended that
*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 − 15
all reagents shall conform to the specifications of the Commit- using an oil sample of similar
...
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.
´1
Designation: D1552 − 08 (Reapproved 2014) D1552 − 15
Standard Test Method for
Sulfur in Petroleum Products (High-Temperature Method)by
1
High Temperature Combustion and IR Detection
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
ε NOTE—Footnotes were updated editorially in September 2014.
1. Scope Scope*
1.1 This test method covers three proceduresa procedure 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)177 °C (350 °F) and containing a mass fraction of sulfur not less than 0.06 mass % sulfur. Two of the three procedures use
iodate detection; one employing an induction furnace for pyrolysis, the other a resistance furnace. The third 0.06 %. This procedure
uses IR detection following pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.
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:
D1193 Specification for Reagent Water
D1266 Test Method for Sulfur in Petroleum Products (Lamp Method)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 Iodate Detection System—The sample is burned in a stream of oxygen at a sufficiently high temperature to convert about
97 % of the sulfur to sulfur dioxide. A standardization factor is employed to obtain accurate results. The combustion products are
passed into an absorber containing an acid solution of potassium iodide and starch indicator. A faint blue color is developed in the
absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more
iodate is added. The amount of standard iodate consumed during the combustion is a measure of the sulfur content of the sample.
3.1 IR Detection System—The sample is weighed into a special ceramic boat which is then placed into a combustion furnace
at 1371°C (2500°F)1350 °C (2460 °F) in an oxygen atmosphere. Most sulfur present is combusted to SO which is then measured
2
with an infrared detector after moisture and dust are removed by traps. A microprocessor calculates the mass percent sulfur from
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 June 15, 2014April 1, 2015. Published July 2014May 2015. Originally approved in 1958. Last previous edition approved in 20082014 as
ε1
D1552D1552 – 08 (2014) –08. DOI: 10.1520/D1552-08R14E01.10.1520/D1552-15.
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
1
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