ASTM D1552-01

Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)

SCOPE
1.1 This test method covers three 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 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 procedure uses IR detection following pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.
1.3 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.

General Information

• Status: Historical
• Publication Date: 09-Nov-2001
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D1552-00 - Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
• Effective Date: 10-Nov-2001
• Replaced By: ASTM D1552-03 - Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
• Effective Date: 10-Mar-2003
• Referred By: ASTM D396-21 - Standard Specification for Fuel Oils
• Effective Date: 10-Nov-2001
• Referred By: ASTM D7666-12(2019) - Standard Specification for Triglyceride Burner Fuel
• Effective Date: 10-Nov-2001
• Referred By: ASTM D6443-14(2019)e1 - Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure)
• Effective Date: 10-Nov-2001
• Referred By: ASTM E1220-21 - Standard Practice for Visible Penetrant Testing Using Solvent-Removable Process
• Effective Date: 10-Nov-2001
• Referred By: ASTM E1418-21 - Standard Practice for Visible Penetrant Testing Using the Water-Washable Process
• Effective Date: 10-Nov-2001
• Referred By: ASTM D4868-17 - Standard Test Method for Estimation of Net and Gross Heat of Combustion of Hydrocarbon Burner and Diesel Fuels
• Effective Date: 10-Nov-2001
• Referred By: ASTM E1209-18 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Water-Washable Process
• Effective Date: 10-Nov-2001
• Referred By: ASTM D5185-18 - Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 10-Nov-2001
• Referred By: ASTM D4951-14(2019) - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Nov-2001
• Referred By: ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
• Effective Date: 10-Nov-2001
• Referred By: ASTM D7691-23 - Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 10-Nov-2001
• Referred By: ASTM E1210-21 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Hydrophilic Post-Emulsification Process
• Effective Date: 10-Nov-2001
• Referred By: ASTM E1208-21 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Lipophilic Post-Emulsification Process
• Effective Date: 10-Nov-2001

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 1552 – 01
Standard Test Method for
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Sulfur in Petroleum Products (High-Temperature Method)
This standard is issued under the fixed designation D 1552; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope * factor is employed to obtain accurate results. The combustion
products are passed into an absorber containing an acid
1.1 This test method covers three procedures for the deter-
solution of potassium iodide and starch indicator. A faint blue
mination of total sulfur in petroleum products including
color is developed in the absorber solution by the addition of
lubricating oils containing additives, and in additive concen-
standard potassium iodate solution. As combustion proceeds,
trates. This test method is applicable to samples boiling above
bleaching the blue color, more iodate is added. The amount of
177°C (350°F) and containing not less than 0.06 mass % sulfur.
standard iodate consumed during the combustion is a measure
Two of the three procedures use iodate detection; one employ-
of the sulfur content of the sample.
ing an induction furnace for pyrolysis, the other a resistance
3.2 IR Detection System—The sample is weighed into a
furnace. The third procedure uses IR detection following
special ceramic boat which is then placed into a combustion
pyrolysis in a resistance furnace.
furnace at 1371°C (2500°F) in an oxygen atmosphere. Most
1.2 Petroleum coke containing up to 8 mass % sulfur can be
sulfur present is combusted to SO which is then measured
2
analyzed.
with an infrared detector after moisture and dust are removed
1.3 This standard does not purport to address all of the
by traps. A microprocessor calculates the mass percent sulfur
safety concerns, if any, associated with its use. It is the
from the sample weight, the integrated detector signal and a
responsibility of the user of this standard to establish appro-
predetermined calibration factor. Both the sample identification
priate safety and health practices and determine the applica-
number and mass percent sulfur are then printed out. The
bility of regulatory limitations prior to use.
calibration factor is determined using standards approximating
2. Referenced Documents the material to be analyzed.
2.1 ASTM Standards:
4. Significance and Use
2
D 1193 Specification for Reagent Water
4.1 This test method provides a means of monitoring the
D 1266 Test Method for Sulfur in Petroleum Products
3
sulfur level of various petroleum products and additives. This
(Lamp Method)
knowledge can be used to predict performance, handling, or
D 4057 Practice for Manual Sampling of Petroleum and
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processing properties. In some cases the presence of sulfur
Petroleum Products
compounds is beneficial to the product and monitoring the
D 6299 Practice for Applying Statistical Quality Assurance
depletion of sulfur can provide useful information. In other
Techniques to Evaluate Analytical Measurement System
5
cases the presence of sulfur compounds is detrimental to the
Performance
processing or use of the product.
3. Summary of Test Method
5. Interferences
3.1 Iodate Detection System—The sample is burned in a
5.1 For the iodate systems, chlorine in concentrations less
stream of oxygen at a sufficiently high temperature to convert
than 1 mass % does not interfere. The IR system can tolerate
about 97 % of the sulfur to sulfur dioxide. A standardization
somewhat higher concentrations. Nitrogen when present in
excess of 0.1 mass % may interfere with the iodate systems; the
1
extent of such interference may be dependent on the type of
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
nitrogen compound as well as the combustion conditions.
D02.03 on Elemental Analysis.
Nitrogen does not interfere with the IR system. The alkali and
Current edition approved Nov. 10, 2001. Published November 2001. Originally
alkaline earth metals, as well as zinc, phosphorus, and lead, do
published as D 1552 – 58 T. Last previous edition D 1552 – 00.
2
Annual Book of ASTM Standards, Vol 11.01. not interfere with either system.
3
Annual Book of ASTM Standards, Vol 05.01.
4
Annual Book of ASTM Standards, Vol 05.02.
5
Annual Book of ASTM Standards, Vol 05.04.
*A Summary of Changes section appears at the end of this standard.
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