ASTM D2622-98
(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
1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquifiable 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 The interlaboratory study 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 (Sr) was 1.5 mg/kg. An estimate of the limit of detection is 3 X Sr , and an estimate of the limit of quantitation 2 is 10 X Sr. 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 Tables 1 and 2) or by the presence of other heteroatoms (see Table 3).
1.6 The values stated in either SI units or angstrom units are to be regarded separately as standard.
1.7 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 Note 1.
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Designation:D2622–98
Standard Test Method for
Sulfur in Petroleum Products by Wavelength Dispersive
1
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 (ϵ) 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 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 Note 1.
in petroleum and petroleum products that are single-phase and
either liquid at ambient conditions, liquifiable with moderate
2. Referenced Documents
heat, or soluble in hydrocarbon solvents. These materials can
2.1 ASTM Standards:
include diesel fuel, jet fuel, kerosine, other distillate oil,
D 4057 Practice for Manual Sampling of Petroleum and
naphtha, residual oil, lubricating base oil, hydraulic oil, crude
3
Petroleum Products
oil, unleaded gasoline, M-85 and M-100.
D 4177 Practice for Automatic Sampling of Petroleum and
1.2 The interlaboratory study on precision covered a variety
3
Petroleum Products
of materials with sulfur concentrations ranging from approxi-
D 4294 Test Method for Sulfur in Petroleum Products by
mately 3 mg/kg to 5.3 mass %. For a subset of these samples,
3
Energy-Dispersive X-Ray Fluorescence Spectroscopy
with sulfur concentrations below 60 mg/kg, the repeatability
D 4927 Test Methods for Elemental Analysis of Lubricant
standard deviation (S ) was 1.5 mg/kg.An estimate of the limit
r
and Additive Components—Barium, Calcium, Phospho-
of detection is 3 3 S , and an estimate of the limit of
r
2 rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
quantitation is 10 3 S . However, because instrumentation
r
3
Fluorescence Spectroscopy
covered by this test method can vary in sensitivity, the
E29 Standard Practice for Using Significant Digits in Test
applicability of the test method at sulfur concentrations below
4
Data to Determine Conformance with Specifications
approximately 20 mg/kg must be determined on an individual
basis.
3. Summary of Test Method
1.3 Samples containing more than 5.0 mass % sulfur can be
3.1 The sample is placed in the X-ray beam, and the peak
diluted to bring the sulfur concentration of the diluted material
intensity of the sulfur Kα line at 5.373 Å is measured. The
within the scope of this test method.
background intensity, measured at a recommended wavelength
1.4 Volatile samples (such as high vapor pressure gasolines
of5.190Å(5.437ÅforaRhtargettube)issubtractedfromthe
or light hydrocarbons) may not meet the stated precision
peakintensity.Theresultantnetcountingrateisthencompared
because of selective loss of light materials during the analysis.
to a previously prepared calibration curve or equation to obtain
1.5 Afundamental assumption in this test method is that the
the concentration of sulfur in mass %.
standard and sample matrix are well matched. Matrix mis-
match can be caused by C/H ratio differences between samples
NOTE 1—Warning: Exposure to excessive quantities of X-radiation is
and standards (see Tables 1 and 2) or by the presence of other injurioustohealth.Theoperatorneedstotakeappropriateactionstoavoid
exposing any part of their body, not only to primary X-rays, but also to
heteroatoms (see Table 3).
secondary or scattered radiation that might be present. The X-ray
1.6 The values stated in either SI units or angstrom units are
spectrometer should be operated in accordance with the regulations
to be regarded separately as standard.
governing the use of ionizing radiation.
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 This test method provides rapid and precise measure-
ment of total sulfur in petroleum and petroleum products with
a minimum of sample preparation.Atypical analysis time is 1
1
This test method is under the jurisdiction of ASTM Committee D-2 on
to 2 min per sample.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03.B on Spectrometric Methods.
Current edition approved Apr. 10, 1998. Published September 1998. Originally
3
published as D 2622–67. Last previous edition D 2622–94. Annual Book of ASTM Standards, Vol 05.02.
2 4
Analytical Chemistry, Vol 55, 1983, pp. 2210–2218. Annual Index of ASTM Standards, Vol 14.02.
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