ASTM D1552-23

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 − 16 (Reapproved 2021) D1552 − 23
Standard Test Method for
Sulfur in Petroleum Products by High Temperature
Combustion and Infrared (IR) Detection or Thermal
Conductivity 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 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 %(350 °F). Other sulfur concentrations outside of those listed in 1.1.1 and
24.2 %.1.1.2 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.
1.1.1 Procedure A, IR Detection:
1.1.1.1 This procedure is applicable to samples containing a mass fraction of sulfur between 0.22 % and 24.2 %.
1.1.1.2 Petroleum coke containing a mass fraction of sulfur between 2.53 % to 3.79 % sulfur may be analyzed.
1.1.2 Procedure B, TCD Detection:
1.1.2.1 This procedure is applicable to samples containing a mass fraction of sulfur between 0.071 % and 25.8 %.
1.1.2.2 Petroleum coke containing a mass fraction of sulfur between 0.19 % to 6.38 % sulfur may be analyzed.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
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 July 1, 2021May 1, 2023. Published July 2021May 2023. Originally approved in 1958. Last previous edition approved in 20162021 as
ɛ1
D1552 – 16 (2021). . DOI: 10.1520/D1552-16R21.10.1520/D1552-23.
*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
D1552 − 23
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.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic 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, Liquid Fuels, and
Lubricants
D6792 Practice for Quality Management Systems in Petroleum Products, Liquid Fuels, and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 The sample is weighed and placed into a 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 measured with a detector after moisture and dust are removed by traps. The instrument calculates the mass percent
sulfur from the sample mass, the integrated detector signal, and a predetermined calibration factor. The calibration factor is
determined using standards approximating the material to be analyzed.
3.1.1 Procedure A—After combustion of the sample and subsequent moisture/dust removal, SO is measured using infrared (IR)
detection.
3.1.2 Procedure B—After combustion of the sample and subsequent moisture/dust removal, SO is measured using thermal
conductivity detection. An apparatus utilizing TCD may require the sample gas to pass an oxygen scrubber and adsorption/
desorption traps to allow passing of contaminants prior to measuring SO .
4. 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.
5. Apparatus
5.1 Combustion Furnace:
5.1.1 Procedure A—Furnace capable of maintaining a constant temperature (between 1150 °C minimum and 1450 °C maximum)
sufficient to ensure quantitative recovery of sulfur as its corresponding gas SO .
5.1.2 Procedure B—Furnace capable of maintaining a temperature (1150 °C) sufficient to ensure quantitative recovery of sulfur
as its corresponding gas SO .
5.2 Combustion and Sulfur Detection System, comprised of automatic balance, gas flow controls, drying tubes, oxygen scrubber,
adsorption/desorption traps as required, combustion furnace, combustion boats or tin (Sn) containers as required and either an IR
(Procedure A) or TCD (Procedure B) SO detector.
5.3 Sieve, 60 mesh (250 μm).
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
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.
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reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Combustion Promoter—Magnesium oxide (MgO), tungsten trioxode (WO ), or aluminum oxide (Al O ). Alternatively,
3 2 3
COM-CAT, a dual promoter that is both a fixing agent and oxidizing agent, may be used.
6.3 Drying Agent, Magnesium perchlorate: anhydrone
(Mg(ClO ) ) or phosphorus pentoxide (P O ). (Warning—In addition to other precautions, handle magnesium perchlorate with
4 2 2 5
care. Avoid contacting it with acid and organic materials. Reactions with fuel may be violent.)
6.4 Oxygen (Extra Dry)—The oxygen shall be at least 99.5 % pure and show no detectable sulfur by blank determination.
(Warning—Oxygen vigorously accelerates combustion.)
6.5 Inert Gas—Helium or argon, high purity grade, 99.995 % minimum purity, as required by manufacturer’s recommendations.
6.6 Quality Control (QC) Sample(s), preferably are portions of one or more petroleum products that are stable and representative
of the samples of interest. These QC samples can be used to check the validity of the testing process and performance of the
instrument as described in Section 11.
7. Sampling
7.1 Take samples in accordance with the instructions in Practice D4057 or D4177.
8. Preparation of Apparatus
8.1 Assemble and adjust apparatus according to manufacturer’s instructions. Initialize instrument, check power supplies, set gas
pressure and flows, and set furnace temperature.
8.1.1 Condition the instrument with samples that are representative or typical of the sample types to be analyzed. During the
interlaboratory study, laboratories analyzed between one and five conditioning samples.
8.1.2 Calibrate the automatic balance according to manufacturer’s instructions.
9. Standardization
9.1 Determination of Standardization Factor:
9.1.1 Because effects such as sample volatility can also affect the relative recovery as SO of the sulfur originally present in the
sample, it is necessary to determine a standardization factor. Proceed as described in Sections 9 through 12, using an oil sample
of similar type to the unknown sample and of accurately known sulfur content.
9.1.2 Determine the calibration factor for the particular type of sample to be analyzed (lubricating oil, petroleum coke, residual
fuel) as recommended by the manufacturer.
9.2 Quality Control—Run a suitable analytical quality control sample several times daily. When the observed value lies between
acceptable limits on a quality control chart, proceed with sample determinations.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
The sole source of supply of COM-CAT known to the committee at this time is LECO Corporation, 3000 Lakeview Ave. St. Joseph, MI 49085 USA. If you are aware
of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
Residual fuel oil Standard Reference Materials may be obtained from the National Institute of Standards and Technology or other sources.
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10. Preparation of Coke
10.1 It is assumed that a representative sample has been received for analysis. If the sample of coke received is not dry, it is
recommended that the sample be dried prior to grinding.
10.2 Grind and sieve the sample received so as to pass a 60 mesh (250 μm) sieve.
10.3 Dry the sieved material to constant weight at 105 °C to 110 °C.
11. Analysis of Quality Control Samples
11.1 A QC sample shall be analyzed each day samples are analyzed to verify the testing procedure and instrument performance.
Additional QC samples may be analyzed. The QC samples shall be treated as outlined in Section 12, depending upon the type of
furnace set-up used by the lab.
11.2 When QC/Quality Assurance (QA) protocols are already established in the testing facility, these may be used to confirm the
reliability of the test result.
11.3 When there is no QC/QA protocol established in the testing facility, Appendix X1 can be used as the QC/QA system.
12. Procedures
12.1 Procedure A—Combustion with Infrared (IR) Detection:
12.1.1 Following instrument manufacturer recommendations, allow the system to warm up and the furnace to reach an operating
temperature between 1150 °C minimum and 1450 °C maximum.
12.1.2 Mix or swirl the test sample thoroughly to ensure homogeneity. Select the appropriate test specimen size as recommended
by the instrument manufacturer. As an example, for liquid samples, take up to 0.13 g for analysis and for solid samples, take up
to 0.4 g for analysis.
12.1.3 Determine and store the system blank value.
12.1.4 Weigh solid samples i
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