ASTM D1552-00

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

• Replaced By: ASTM D1552-01 - Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
• 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 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 D240-19 - Standard Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter
• Effective Date: 10-Nov-2001
• Referred By: ASTM D3338/D3338M-20a - Standard Test Method for Estimation of Net Heat of Combustion of Aviation Fuels
• Effective Date: 10-Nov-2001
• Referred By: ASTM D6376-10(2017)e1 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy
• Effective Date: 10-Nov-2001
• Referred By: ASTM D3238-22a - Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the n-d-M Method
• Effective Date: 10-Nov-2001
• Referred By: ASTM D6448-16(2022) - Standard Specification for Industrial Burner Fuels from Used Lubricating Oils
• Effective Date: 10-Nov-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1552 – 00 An American National Standard
Standard Test Method for
1
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 solution of potassium iodide and starch indicator. A faint blue
color is developed in the absorber solution by the addition of
1.1 This test method covers three procedures for the deter-
standard potassium iodate solution. As combustion proceeds,
mination of total sulfur in petroleum products including
bleaching the blue color, more iodate is added. The amount of
lubricating oils containing additives, and in additive concen-
standard iodate consumed during the combustion is a measure
trates. This test method is applicable to samples boiling above
of the sulfur content of the sample.
177°C (350°F) and containing not less than 0.06 mass % sulfur.
3.2 IR Detection System—The sample is weighed into a
Two of the three procedures use iodate detection; one employ-
special ceramic boat which is then placed into a combustion
ing an induction furnace for pyrolysis, the other a resistance
furnace at 1371°C (2500°F) in an oxygen atmosphere. Most
furnace. The third procedure uses IR detection following
sulfur present is combusted to SO which is then measured
pyrolysis in a resistance furnace. 2
with an infrared detector after moisture and dust are removed
1.2 Petroleum coke containing up to 8 mass % sulfur can be
by traps. A microprocessor calculates the mass percent sulfur
analyzed.
from the sample weight, the integrated detector signal and a
1.3 This standard does not purport to address all of the
predetermined calibration factor. Both the sample identification
safety concerns, if any, associated with its use. It is the
number and mass percent sulfur are then printed out. The
responsibility of the user of this standard to establish appro-
calibration factor is determined using standards approximating
priate safety and health practices and determine the applica-
the material to be analyzed.
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents
4.1 This test method provides a means of monitoring the
2.1 ASTM Standards:
2
sulfur level of various petroleum products and additives. This
D 1193 Specification for Reagent Water
knowledge can be used to predict performance, handling, or
D 1266 Test Method for Sulfur in Petroleum Products
3
processing properties. In some cases the presence of sulfur
(Lamp Method)
compounds is beneficial to the product and monitoring the
D 4057 Practice for Manual Sampling of Petroleum and
4
depletion of sulfur can provide useful information. In other
Petroleum Products
cases the presence of sulfur compounds is detrimental to the
D 6299 Practice for Applying Statistical Quality Assurance
processing or use of the product.
Techniques to Evaluate Analytical Measurement System
5
Performance
5. Interferences
3. Summary of Test Method 5.1 For the iodate systems, chlorine in concentrations less
than 1 mass % does not interfere. The IR system can tolerate
3.1 Iodate Detection System—The sample is burned in a
somewhat higher concentrations. Nitrogen when present in
stream of oxygen at a sufficiently high temperature to convert
excess of 0.1 mass % may interfere with the iodate systems; the
about 97 % of the sulfur to sulfur dioxide. A standardization
extent of such interference may be dependent on the type of
factor is employed to obtain accurate results. The combustion
nitrogen compound as well as the combustion conditions.
products are passed into an absorber containing an acid
Nitrogen does not interfere with the IR system. The alkali and
alkaline earth metals, as well as zinc, phosphorus, and lead, do
1
This test method is under the jurisdiction of ASTM Committee D02 on
not interfere with either system.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
6. Apparatus
Current edition approved Nov. 10, 2000. Published December 2000. Originally
published as D 1552 – 58 T. Last previous edition D 1552 – 95.
6.1 Combustion and Iodate Detection System
2
Annual Book of ASTM Standards, Vol 11.01.
6.1.1 Furnaces—Two major types are available, the pri-
3
Annual Book of ASTM Standards, Vol 05.01.
4
mary difference being the manner in which the necessary high
Annual Book of ASTM Standards, Vol 05.02.
5
Annual Book of ASTM Standards, Vol 05.04.
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