ASTM D7039-04

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An American National Standard
Designation:D7039–04
Standard Test Method for
Sulfur in Gasoline and Diesel Fuel by Monochromatic
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Wavelength Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D 7039; 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.
1. Scope 2. Referenced Documents
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2.1 ASTM Standards:
1.1 This test method covers the determination of total sulfur
by monochromatic, wavelength-dispersive X-ray fluorescence D 4057 Practice for Manual Sampling of Petroleum and
(MWDXRF) spectrometry in single-phase gasolines, diesel Petroleum Products
fuels, and refinery process streams used to blend gasoline and D 4177 Practice for Automatic Sampling of Petroleum and
diesel, at concentrations from 2 mg/kg to 500 mg/kg. The Petroleum Products
precision of this test method was determined by an interlabo- D 6299 Practice for Applying Statistical Quality Assurance
ratory study using representative samples of the liquids de- Techniques to Evaluate Analytical Measurement System
scribedin1.1and1.2.Thepooledlimitofquantitation(PLOQ) Performance
was estimated to be 4 mg/kg. D 6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products and
NOTE 1—Volatile samples such as high-vapor-pressure gasolines or
Lubricants
light hydrocarbons might not meet the stated precision because of the
evaporation of light components during the analysis.
3. Summary of Test Method
1.2 Gasoline samples containing oxygenates may be ana-
3.1 A monochromatic X-ray beam with a wavelength suit-
lyzed with this test method provided the matrix of the
able to excite the K-shell electrons of sulfur is focused onto a
calibration standards is either matched to the sample matrices
test specimen contained in a sample cell (see Fig. 1). The
orthematrixcorrectiondescribedinAnnexA1isappliedtothe
fluorescent Ka radiation at 0.5373 nm (5.373 Å) emitted by
results. The conditions for matrix matching and matrix correc-
sulfur is collected by a fixed monochromator (analyzer). The
tion are provided in the Interferences section (Section 5).
intensity (counts per second) of the sulfur X rays is measured
1.3 Gasolines and diesels with sulfur contents above 500
using a suitable detector and converted to the concentration of
mg/kg can be analyzed after dilution with appropriate solvent
sulfur (mg/kg) in a test specimen using a calibration equation.
(see 5.2). The precision and bias of sulfur determinations on
Excitation by monochromatic X rays reduces background,
diluted samples has not been determined and may not be the
simplifies matrix correction, and increases the signal/
same as shown for neat samples (Section 15).
backgroundratiocomparedtopolychromaticexcitationusedin
1.4 When the elemental composition of the samples differ
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conventional WDXRF techniques. (Warning—Exposure to
significantly from the calibration standards used to prepare the
excessive quantities of X-ray radiation is injurious to health.
calibration curve, the cautions and recommendation in Section
The operator needs to take appropriate actions to avoid
5 should be carefully observed.
exposing any part of his/her body, not only to primary X rays,
1.5 The values stated in SI units are to be regarded as the
but also to secondary or scattered radiation that might be
standard. The values given in parentheses are for information
present. The X-ray spectrometer should be operated in accor-
only.
dance with the regulations governing the use of ionizing
1.6 This standard does not purport to address all of the
radiation.)
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 This test method provides for the precise measurement
bility of regulatory limitations prior to use. For specific hazard
ofthetotalsulfurcontentofgasolinesanddieselswithminimal
information, see 3.1.
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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
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This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the ASTM website.
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D02.03 on Elemental Analysis. Bertin, E. P., Principles and Practices of X-ray Spectrometric Analysis, Plenum
Current edition approved May 1, 2004. Published June 2004. Press, New York, 1975, pp. 115-1
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