ASTM D2622-03

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.

General Information

• Status: Historical
• Publication Date: 09-Sep-2003
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D2622-98 - Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 10-Sep-2003
• Replaced By: ASTM D2622-05 - Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7468-22 - Standard Test Method for Cummins ISM Test
• Effective Date: 10-Sep-2003
• Referred By: ASTM D6681-23 - Standard Test Method for Evaluation of Engine Oils in a High Speed, Single-Cylinder Diesel Engine—Caterpillar 1P Test Procedure
• Effective Date: 10-Sep-2003
• Referred By: ASTM D8074-22 - Standard Test Method for Evaluation of Diesel Engine Oils in DD13 Diesel Engine
• Effective Date: 10-Sep-2003
• Referred By: ASTM D7484-23 - Standard Test Method for Evaluation of Automotive Engine Oils for Valve-Train Wear Performance in Cummins ISB Medium-Duty Diesel Engine
• Effective Date: 10-Sep-2003
• Referred By: ASTM D240-19 - Standard Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter
• Effective Date: 10-Sep-2003
• Referred By: ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
• Effective Date: 10-Sep-2003
• Referred By: ASTM D8147-17(2023) - Standard Specification for Special-Purpose Test Fuels for Aviation Compression-Ignition Engines
• Effective Date: 10-Sep-2003
• Referred By: ASTM D4057-22 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 10-Sep-2003
• Referred By: ASTM D6615-22 - Standard Specification for Jet B Wide-Cut Aviation Turbine Fuel
• Effective Date: 10-Sep-2003
• Referred By: ASTM D6227-18(2023) - Standard Specification for Unleaded Aviation Gasoline Containing a Non-hydrocarbon Component
• Effective Date: 10-Sep-2003
• Referred By: ASTM D6448-16(2022) - Standard Specification for Industrial Burner Fuels from Used Lubricating Oils
• Effective Date: 10-Sep-2003
• Referred By: ASTM D8256-23 - Standard Test Method for Evaluation of Automotive Engine Oils for Inhibition of Deposit Formation in the Sequence VH Spark-Ignition Engine Fueled with Gasoline and Operated Under Low-Temperature, Light-Duty Conditions
• Effective Date: 10-Sep-2003
• Referred By: ASTM D7547-23 - Standard Specification for Hydrocarbon Unleaded Aviation Gasoline
• Effective Date: 10-Sep-2003

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
An American National Standard
Designation:D2622–03
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 (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.
TABLE 1 Comparison of NIST and ASTM Interlaboratory Study
1. Scope*
(RR) Results
1.1 This test method covers the determination of total sulfur
NIST SRM Sulfur, Sulfur, C/H mass Apparent Relative Significant
in petroleum and petroleum products that are single-phase and
mass %, mass %, ratio Bias, % Bias, %
either liquid at ambient conditions, liquefiable with moderate
NIST ASTM RR Sulfur
Average
heat, or soluble in hydrocarbon solvents. These materials can
1616a 0.0146 0.0148 5.205 0.0002 1.37 No
include diesel fuel, jet fuel, kerosine, other distillate oil,
1617a 0.1731 0.1776 5.205 0.0045 2.60 Yes
naphtha, residual oil, lubricating base oil, hydraulic oil, crude
2724a 0.0430 0.0417 5.986 -0.0013 -3.02 Yes
oil, unleaded gasoline, M-85 and M-100.
1623c 0.3806 0.3661 7.504 -0.0145 -3.81 Yes
2717 3.0220 2.948 8.229 -0.0736 -2.44 Yes
1.2 Interlaboratory studies on precision covered a variety of
1621e 0.948 0.8973 8.553 -0.0507 -5.35 Yes
materials with sulfur concentrations ranging from approxi-
1624c 0.3918 6.511
mately 3 mg/kg to 5.3 mass %. For a subset of these samples,
2723 0.0299 5.937
with sulfur concentrations below 60 mg/kg, the repeatability
standard deviation (S ) was 1.5 mg/kg.An estimate of the limit
r
of detection is 3 3 S , and an estimate of the limit of
r
priate safety and health practices and determine the applica-
2
quantitation is 10 3 S . However, because instrumentation
r
bility of regulatory limitations prior to use.
covered by this test method can vary in sensitivity, the
applicability of the test method at sulfur concentrations below 2. Referenced Documents
approximately 20 mg/kg must be determined on an individual
2.1 ASTM Standards:
basis.
D 4057 Practice for Manual Sampling of Petroleum and
1.3 Samples containing more than 5.0 mass % sulfur can be 3
Petroleum Products
diluted to bring the sulfur concentration of the diluted material
D 4177 Practice for Automatic Sampling of Petroleum and
within the scope of this test method. 3
Petroleum Products
1.4 Volatile samples (such as high vapor pressure gasolines
D 4294 Test Method for Sulfur in Petroleum Products by
or light hydrocarbons) may not meet the stated precision 3
Energy-Dispersive X-Ray Fluorescence Spectroscopy
because of selective loss of light materials during the analysis.
D 4927 Test Methods for Elemental Analysis of Lubricant
1.5 Afundamental assumption in this test method is that the
and Additive Components—Barium, Calcium, Phospho-
standard and sample matrix are well matched. Matrix mis-
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
match can be caused by C/H ratio differences between samples 3
Fluorescence Spectroscopy
and standards (see Tables 1 and 2) or by the presence of other
E 29 Standard Practice for Using Significant Digits in Test
heteroatoms (see Table 3). 4
Data to Determine Conformance with Specifications
1.6 The values stated in either SI units or angstrom units are
to be regarded as standard. 3. Summary of Test Method
1.7 This standard does not purport to address all of the
3.1 The sample is placed in the X-ray beam, and the peak
safety concerns, if any, associated with its use. It is the
intensity of the sulfur Ka line at 5.373 Å is measured. The
responsibility of the user of this standard to establish appro-
background intensity, measured at a recommended wavelength
of5.190Å(5.437ÅforaRhtargettube)issubtractedfromthe
peakintensity.Theresultantnetcountingrateisthencompared
1
This test method is under the jurisdiction of ASTM Committee D02 on
to a previously prepared calibration curve or equation to obtain
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Sept. 10, 2003. Published October 2003. Originally
3
approved in 1967. Last previous edition approved in 1998 as D 2622–98. 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.
*A Summary of Changes section appears at the end of this standard.
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