ASTM D1552-03
(Test Method)Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
SIGNIFICANCE AND USE
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 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.
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An American National Standard
Designation:D1552–03
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* about 97 % of the sulfur to sulfur dioxide. A standardization
factor is employed to obtain accurate results. The combustion
1.1 This test method covers three procedures for the deter-
products are passed into an absorber containing an acid
mination of total sulfur in petroleum products including
solution of potassium iodide and starch indicator. A faint blue
lubricating oils containing additives, and in additive concen-
color is developed in the absorber solution by the addition of
trates. This test method is applicable to samples boiling above
standard potassium iodate solution. As combustion proceeds,
177°C(350°F)andcontainingnotlessthan0.06mass %sulfur.
bleaching the blue color, more iodate is added. The amount of
Two of the three procedures use iodate detection; one employ-
standard iodate consumed during the combustion is a measure
ing an induction furnace for pyrolysis, the other a resistance
of the sulfur content of the sample.
furnace. The third procedure uses IR detection following
3.2 IR Detection System—The sample is weighed into a
pyrolysis in a resistance furnace.
special ceramic boat which is then placed into a combustion
1.2 Petroleum coke containing up to 8 mass % sulfur can be
furnace at 1371°C (2500°F) in an oxygen atmosphere. Most
analyzed.
sulfur present is combusted to SO which is then measured
2
1.3 This standard does not purport to address all of the
with an infrared detector after moisture and dust are removed
safety concerns, if any, associated with its use. It is the
by traps. A microprocessor calculates the mass percent sulfur
responsibility of the user of this standard to establish appro-
from the sample weight, the integrated detector signal and a
priate safety and health practices and determine the applica-
predeterminedcalibrationfactor.Boththesampleidentification
bility of regulatory limitations prior to use.
number and mass percent sulfur are then printed out. The
2. Referenced Documents
calibration factor is determined using standards approximating
the material to be analyzed.
2.1 ASTM Standards:
2
D 1193 Specification for Reagent Water
4. Significance and Use
D 1266 Test Method for Sulfur in Petroleum Products
3
4.1 This test method provides a means of monitoring the
(Lamp Method)
sulfur level of various petroleum products and additives. This
D 4057 Practice for Manual Sampling of Petroleum and
4
knowledge can be used to predict performance, handling, or
Petroleum Products
processing properties. In some cases the presence of sulfur
D 6299 Practice for Applying Statistical Quality Assurance
compounds is beneficial to the product and monitoring the
Techniques to Evaluate Analytical Measurement System
5 depletion of sulfur can provide useful information. In other
Performance
cases the presence of sulfur compounds is detrimental to the
3. Summary of Test Method processing or use of the product.
3.1 Iodate Detection System—The sample is burned in a
5. Interferences
stream of oxygen at a sufficiently high temperature to convert
5.1 For the iodate systems, chlorine in concentrations less
than 1 mass % does not interfere. The IR system can tolerate
1
This test method is under the jurisdiction of ASTM Committee D02 on
somewhat higher concentrations. Nitrogen when present in
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
excessof0.1mass %mayinterferewiththeiodatesystems;the
D02.03 on Elemental Analysis.
extent of such interference may be dependent on the type of
Current edition approved March 10, 2003. Published April 2003. Originally
approved in 1958. Last previous edition approved in 2001 as D 1552–01.
nitrogen compound as well as the combustion conditions.
2
Annual Book of ASTM Standards, Vol 11.01.
Nitrogen does not interfere with the IR system. The alkali and
3
Annual Book of ASTM Standards, Vol 05.01.
4 alkaline earth metals, as well as zinc, phosphorus, and lead, do
Annual Book of ASTM Standards, Vol 05.02.
5
not interfere with either system.
Annual Book of ASTM Standards, Vol 05.03.
*A Summary of Changes section appears at the end of this standard.
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