ASTM D2622-05
(Test Method)Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
SCOPE
le-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosine, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, M-85 and M-100.
1.2 Interlaboratory studies on precision covered a variety of materials with sulfur concentrations ranging from approximately 3 mg/kg to 5.3 mass %. For a subset of these samples, with sulfur concentrations below 60 mg/kg, the repeatability standard deviation (S r) was 1.5 mg/kg. An estimate of the limit of detection is 3 Sr, and an estimate of the limit of quantitation is 10 S r. However, because instrumentation covered by this test method can vary in sensitivity, the applicability of the test method at sulfur concentrations below approximately 20 mg/kg must be determined on an individual basis.
1.3 Samples containing more than 5.0 mass % sulfur can be diluted to bring the sulfur concentration of the diluted material within the scope of this test method.
1.4 Volatile samples (such as high vapor pressure gasolines or light hydrocarbons) may not meet the stated precision because of selective loss of light materials during the analysis.
1.5 A fundamental assumption in this test method is that the standard and sample matrix are well matched. Matrix mismatch can be caused by C/H ratio differences between samples and standards (see ) or by the presence of other heteroatoms (see ).
1.6 The values stated in either SI units or angstrom units are to be regarded as standard.
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:D2622–05
Standard Test Method for
Sulfur in Petroleum Products by Wavelength Dispersive
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X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D 2622; 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* 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the determination of total sulfur
responsibility of the user of this standard to establish appro-
in petroleum and petroleum products that are single-phase and
priate safety and health practices and determine the applica-
either liquid at ambient conditions, liquefiable with moderate
bility of regulatory limitations prior to use.
heat, or soluble in hydrocarbon solvents. These materials can
include diesel fuel, jet fuel, kerosine, other distillate oil,
2. Referenced Documents
naphtha, residual oil, lubricating base oil, hydraulic oil, crude
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2.1 ASTM Standards:
oil, unleaded gasoline, M-85 and M-100.
D 4057 Practice for Manual Sampling of Petroleum and
1.2 Interlaboratory studies on precision covered a variety of
Petroleum Products
materials with sulfur concentrations ranging from approxi-
D 4177 Practice for Automatic Sampling of Petroleum and
mately 3 mg/kg to 5.3 mass %. For a subset of these samples,
Petroleum Products
with sulfur concentrations below 60 mg/kg, the repeatability
D 4294 Test Method for Sulfur in Petroleum and Petroleum
standard deviation (S ) was 1.5 mg/kg.An estimate of the limit
r
Products by Energy-Dispersive X-Ray Fluorescence Spec-
of detection is 3 3 S , and an estimate of the limit of
r
2 troscopy
quantitation is 10 3 S . However, because instrumentation
r
D 4927 Test Methods for Elemental Analysis of Lubricant
covered by this test method can vary in sensitivity, the
and Additive Components—Barium, Calcium, Phospho-
applicability of the test method at sulfur concentrations below
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
approximately 20 mg/kg must be determined on an individual
Fluorescence Spectroscopy
basis.
E29 Practice for Using Significant Digits in Test Data to
1.3 Samples containing more than 5.0 mass % sulfur can be
Determine Conformance with Specifications
diluted to bring the sulfur concentration of the diluted material
within the scope of this test method.
3. Summary of Test Method
1.4 Volatile samples (such as high vapor pressure gasolines
3.1 The sample is placed in the X-ray beam, and the peak
or light hydrocarbons) may not meet the stated precision
intensity of the sulfur Ka line at 5.373 Å is measured. The
because of selective loss of light materials during the analysis.
background intensity, measured at a recommended wavelength
1.5 Afundamental assumption in this test method is that the
of5.190Å(5.437ÅforaRhtargettube)issubtractedfromthe
standard and sample matrix are well matched. Matrix mis-
peakintensity.Theresultantnetcountingrateisthencompared
match can be caused by C/H ratio differences between samples
to a previously prepared calibration curve or equation to obtain
and standards (see Tables 1 and 2) or by the presence of other
theconcentrationofsulfurinmass%.(Warning—Exposureto
heteroatoms (see Table 3).
excessive quantities of X-radiation is injurious to health. The
1.6 The values stated in either SI units or angstrom units are
operator needs to take appropriate actions to avoid exposing
to be regarded as standard.
any part of their body, not only to primary X-rays, but also to
secondary or scattered radiation that might be present. The
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This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
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D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2005. Published November 2005. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1967. Last previous edition approved in 2003 as D 2622-03. Standards volume information, refer to the standard’s Document Summary page on
2
Analytical Chemistry, Vol 55, 1983, pp. 2210–2218. the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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D2622–05
TABLE 1 Comparison of NIST and ASTM Int
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