ASTM D7039-07
(Test Method)Standard Test Method for Sulfur in Gasoline and Diesel Fuel by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
Standard Test Method for Sulfur in Gasoline and Diesel Fuel by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
SIGNIFICANCE AND USE
This test method provides for the precise measurement of the total sulfur content of gasolines and diesels with minimal sample preparation and analyst involvement. The typical time for each analysis is two to three minutes.
Knowledge of the sulfur content of diesel fuels, gasolines, and refinery process streams used to blend gasolines is important for process control as well as the prediction and control of operational problems such as unit corrosion and catalyst poisoning, and in the blending of products to commodity specifications.
Various federal, state, and local agencies regulate the sulfur content of some petroleum products, including gasoline and diesel fuel. Unbiased and precise determination of sulfur in these products is critical to compliance with regulatory standards.
SCOPE
1.1 This test method covers the determination of total sulfur by monochromatic, wavelength-dispersive X-ray fluorescence (MWDXRF) spectrometry in single-phase gasolines, diesel fuels, and refinery process streams used to blend gasoline and diesel, at concentrations from 2 mg/kg to 500 mg/kg. The precision of this test method was determined by an interlaboratory study using representative samples of the liquids described in 1.1 and 1.2. The pooled limit of quantitation (PLOQ) was estimated to be 4 mg/kg.Note 1
Volatile samples such as high-vapor-pressure gasolines or light hydrocarbons might not meet the stated precision because of the evaporation of light components during the analysis.
1.2 Gasoline samples containing oxygenates may be analyzed with this test method provided the matrix of the calibration standards is either matched to the sample matrices or the matrix correction described in Annex A1 is applied to the results. The conditions for matrix matching and matrix correction are provided in the Interferences section (Section 5).
1.3 Gasolines and diesels with sulfur contents above 500 mg/kg can be analyzed after dilution with appropriate solvent (see 5.2). The precision and bias of sulfur determinations on diluted samples has not been determined and may not be the same as shown for neat samples (Section 15).
1.4 When the elemental composition of the samples differ significantly from the calibration standards used to prepare the calibration curve, the cautions and recommendation in Section 5 should be carefully observed.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. For specific hazard information, see 3.1.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7039 − 07
StandardTest Method for
Sulfur in Gasoline and Diesel Fuel by Monochromatic
1
Wavelength Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D7039; 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.
1. Scope* priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
1.1 This test method covers the determination of total sulfur
information, see 3.1.
by monochromatic, wavelength-dispersive X-ray fluorescence
(MWDXRF) spectrometry in single-phase gasolines, diesel
2. Referenced Documents
fuels, and refinery process streams used to blend gasoline and
2
2.1 ASTM Standards:
diesel, at concentrations from 2 mg/kg to 500 mg/kg. The
D4057 Practice for Manual Sampling of Petroleum and
precision of this test method was determined by an interlabo-
Petroleum Products
ratory study using representative samples of the liquids de-
D4177 Practice for Automatic Sampling of Petroleum and
scribedin1.1and1.2.Thepooledlimitofquantitation(PLOQ)
Petroleum Products
was estimated to be 4 mg/kg.
D6299 Practice for Applying Statistical Quality Assurance
NOTE 1—Volatile samples such as high-vapor-pressure gasolines or
and Control Charting Techniques to Evaluate Analytical
light hydrocarbons might not meet the stated precision because of the
Measurement System Performance
evaporation of light components during the analysis.
D6300 Practice for Determination of Precision and Bias
1.2 Gasoline samples containing oxygenates may be ana-
Data for Use in Test Methods for Petroleum Products and
lyzed with this test method provided the matrix of the
Lubricants
calibration standards is either matched to the sample matrices 3
2.2 EPA Documents:
orthematrixcorrectiondescribedinAnnexA1isappliedtothe
40 CFR 80.584 Code of Federal Regulations; Title 40; Part
results. The conditions for matrix matching and matrix correc-
80; U.S. Environmental Agency, July 1, 2005
tion are provided in the Interferences section (Section 5).
3. Summary of Test Method
1.3 Gasolines and diesels with sulfur contents above 500
mg/kg can be analyzed after dilution with appropriate solvent
3.1 A monochromatic X-ray beam with a wavelength suit-
(see 5.2). The precision and bias of sulfur determinations on able to excite the K-shell electrons of sulfur is focused onto a
diluted samples has not been determined and may not be the
test specimen contained in a sample cell (see Fig. 1). The
same as shown for neat samples (Section 15). fluorescent Kα radiation at 0.5373 nm (5.373 Å) emitted by
sulfur is collected by a fixed monochromator (analyzer). The
1.4 When the elemental composition of the samples differ
intensity (counts per second) of the sulfur X rays is measured
significantly from the calibration standards used to prepare the
using a suitable detector and converted to the concentration of
calibration curve, the cautions and recommendation in Section
sulfur (mg/kg) in a test specimen using a calibration equation.
5 should be carefully observed.
Excitation by monochromatic X rays reduces background,
1.5 The values stated in SI units are to be regarded as the
simplifies matrix correction, and increases the signal/
standard. The values given in parentheses are for information
backgroundratiocomparedtopolychromaticexcitationusedin
only. 4
conventional WDXRF techniques. (Warning—Exposure to
1.6 This standard does not purport to address all of the
excessive quantities of X-ray radiation is injurious to health.
safety concerns, if any, associated with its use. It is the
The operator needs to take appropriate actions to avoid
responsibility of the user of this standard to establish appro-
2
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
1
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.
3
D02.03 on Elemental Analysis. Available from U.S. Government Printing Office, 732 N. Capitol Street, NW,
Current edition approved May 1, 2007. Published June 2007. Originally Washington, DC 20401.
4
approved in 2004. Last previous edition approved in 2004 as D7039–04. DOI: Bertin, E. P., Principles and Practices of X-ray Spectrometric Analysis ,
10.1520/D7039-07. Plenum Press, New York, 1975, pp. 115-118.
*A Summary of Changes section appears at the end of this standard
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