ASTM D2622-10

Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
This test method provides rapid and precise measurement of total sulfur in petroleum and petroleum products with a minimum of sample preparation. A typical analysis time is 1 to 2 minutes per sample.
The quality of many petroleum products is related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuels.
This test method provides a means of determining whether the sulfur content of petroleum or a petroleum product meets specification or regulatory limits.
When this test method is applied to petroleum materials with matrices significantly different from the white oil calibration materials specified in this test method, the cautions and recommendations in Section 5 should be observed when interpreting results.
Note 2—The equipment specified for Test Method D2622 tends to be more expensive than that required for alternative test methods, such as Test Method D4294. Consult the Index to ASTM Standards for alternative test methods.
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, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosene, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasohol and biodiesel.
1.2 The range of this test method is between the PLOQ value (calculated by procedures consistent with Practice D6259) of 3 mg/kg total sulfur and the highest level sample in the round robin, 4.6 wt. % total sulfur.
Note 1—Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at sulfur concentrations below 3 mg/kg may be determined on an individual basis for WDXRF instruments capable of measuring lower levels, but precision in this test method does not apply.
1.2.1 The values of the limit of quantitation (LOQ) and method precision for a specific laboratory’s instrument depends on instrument source power (low or high power), sample type, and the practices established by the laboratory to perform the method.
1.3 Samples containing more than 4.6 mass % sulfur should be diluted to bring the sulfur concentration of the diluted material within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 14 than non-diluted samples.
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 matrices are well matched, or that the matrix differences are accounted for (see 12.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other interfering heteroatoms or species (see Table 1).
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.

General Information

• Status: Historical
• Publication Date: 14-Feb-2010
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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: D2622 − 10
StandardTest Method for
Sulfur in Petroleum Products by Wavelength Dispersive
1
X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D2622; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* match can be caused by C/H ratio differences between samples
and standards or by the presence of other interfering heteroa-
1.1 This test method covers the determination of total sulfur
toms or species (see Table 1).
in petroleum and petroleum products that are single-phase and
either liquid at ambient conditions, liquefiable with moderate 1.6 The values stated in SI units are to be regarded as
heat, or soluble in hydrocarbon solvents. These materials can standard. No other units of measurement are included in this
include diesel fuel, jet fuel, kerosene, other distillate oil, standard.
naphtha, residual oil, lubricating base oil, hydraulic oil, crude
1.7 This standard does not purport to address all of the
oil, unleaded gasoline, gasohol and biodiesel.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
1.2 The range of this test method is between the PLOQ
priate safety and health practices and determine the applica-
value (calculated by procedures consistent with Practice
bility of regulatory limitations prior to use.
D6259) of 3 mg/kg total sulfur and the highest level sample in
the round robin, 4.6 wt. % total sulfur.
2. Referenced Documents
NOTE 1—Instrumentation covered by this test method can vary in
2
2.1 ASTM Standards:
sensitivity. The applicability of the test method at sulfur concentrations
D4057 Practice for Manual Sampling of Petroleum and
below 3 mg/kg may be determined on an individual basis for WDXRF
instruments capable of measuring lower levels, but precision in this test
Petroleum Products
method does not apply.
D4177 Practice for Automatic Sampling of Petroleum and
1.2.1 The values of the limit of quantitation (LOQ) and Petroleum Products
methodprecisionforaspecificlaboratory’sinstrumentdepends D4294 Test Method for Sulfur in Petroleum and Petroleum
on instrument source power (low or high power), sample type, Products by Energy Dispersive X-ray Fluorescence Spec-
and the practices established by the laboratory to perform the
trometry
method. D4927 Test Methods for Elemental Analysis of Lubricant
and Additive Components—Barium, Calcium,
1.3 Samples containing more than 4.6 mass % sulfur should
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
be diluted to bring the sulfur concentration of the diluted
X-Ray Fluorescence Spectroscopy
material within the scope of this test method. Samples that are
D6259 Practice for Determination of a Pooled Limit of
dilutedcanhavehighererrorsthanindicatedinSection14than
Quantitation
non-diluted samples.
D6299 Practice for Applying Statistical Quality Assurance
1.4 Volatile samples (such as high vapor pressure gasolines
and Control Charting Techniques to Evaluate Analytical
or light hydrocarbons) may not meet the stated precision
Measurement System Performance
because of selective loss of light materials during the analysis.
D7343 Practice for Optimization, Sample Handling,
1.5 Afundamental assumption in this test method is that the Calibration, and Validation of X-ray Fluorescence Spec-
trometry Methods for Elemental Analysis of Petroleum
standard and sample matrices are well matched, or that the
matrix differences are accounted for (see 12.2). Matrix mis- Products and Lubricants
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 15, 2010. Published March 2010. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1967. Last previous edition approved in 2008 as D2622–08. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2622-10. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D2622 − 10
TABLE 1 Concentrati
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This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D2622–08 Designation:D2622–10
Standard Test Method for
Sulfur in Petroleum Products by Wavelength Dispersive
1
X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D2622; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. 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, liquefiable with moderate heat, or soluble in hydrocarbon solvents.These materials can include
diesel fuel, jet fuel, kerosene, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded
gasoline, gasohol and biodiesel.
1.2 The range of this test method is between the PLOQ value (calculated by procedures consistent with Practice D6259) of 3
mg/kg total sulfur and the highest level sample in the round robin, 4.6 wt. % total sulfur.
NOTE 1—Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at sulfur concentrations below 3
mg/kg may be determined on an individual basis for WDXRF instruments capable of measuring lower levels, but precision in this test method does not
apply.
1.2.1 The values of the limit of quantitation (LOQ) and method precision for a specific laboratory’s instrument depends on
instrument source power (low or high power), sample type, and the practices established by the laboratory to perform the method.
1.3 Samples containing more than 4.6 mass % sulfur should be diluted to bring the sulfur concentration of the diluted material
within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 14 than non-diluted
samples.
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 Afundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix
differences are accounted for (see 12.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards
or by the presence of other interfering heteroatoms or species (see Table 1).
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4294 Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
D4927 Test Methods for ElementalAnalysis of Lubricant andAdditive ComponentsBarium, Calcium, Phosphorus, Sulfur, and
Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
D6259 Practice for Determination of a Pooled Limit of Quantitation
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
1
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved March 1, 2008.Feb. 15, 2010. Published March 2008.2010. Originally approved in 1967. Last previous edition approved in 20072008 as
D2622–07.D2622–08. DOI: 10.1520/D2622-108.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standar
...