ASTM D4294-03
(Test Method)Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectrometry
Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectrometry
SIGNIFICANCE AND USE
This test method provides rapid and precise measurement of total sulfur in petroleum products with a minimum of sample preparation. A typical analysis time is 2 to 4 min 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 compliance with specifications or limits set by regulations for sulfur content of petroleum products.
If this test method is applied to petroleum matrices with significantly different composition than the white oil calibration materials specified in this test method, the cautions and recommendations in Section 5 should be observed when interpreting the results.
Compared to other test methods for sulfur determination, Test Method D 4294 has high throughput, minimal sample preparation, good precision, and is capable of determining sulfur over a wide range of concentrations. The equipment specified is in most cases less costly than that required for alternative methods. Consult the ASTM website2 or ASTM Subject Index3 for names of alternative test methods.
SCOPE
1.1 This test method covers the measurement of sulfur in hydrocarbons, such as diesel, naphtha, kerosine, residuals, lubricating base oils, hydraulic oils, jet fuels, crude oils, gasoline (all unleaded), and other distillates. In addition, sulfur in other products, such as M-85 and M-100, may be analyzed using this technique. The applicable concentration range is 0.0150 to 5.00 mass % sulfur.
1.2 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mass % sulfur.
1.3 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 warning statements, see Section 7.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D4294–03
Standard Test Method for
Sulfur in Petroleum and Petroleum Products by Energy-
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Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D 4294; 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* from previously prepared calibration standards that bracket the
sample concentration range of interest to obtain the sulfur
1.1 This test method covers the measurement of sulfur in
concentration in mass %.
hydrocarbons, such as diesel, naphtha, kerosine, residuals,
lubricating base oils, hydraulic oils, jet fuels, crude oils,
4. Significance and Use
gasoline (all unleaded), and other distillates. In addition, sulfur
4.1 This test method provides rapid and precise measure-
in other products, such as M-85 and M-100, may be analyzed
ment of total sulfur in petroleum products with a minimum of
using this technique. The applicable concentration range is
sample preparation. A typical analysis time is 2 to 4 min per
0.0150 to 5.00 mass % sulfur.
sample.
1.2 The values stated in SI units are to be regarded as the
4.2 The quality of many petroleum products is related to the
standard. The preferred concentration units are mass % sulfur.
amount of sulfur present. Knowledge of sulfur concentration is
1.3 This standard does not purport to address all of the
necessary for processing purposes. There are also regulations
safety concerns, if any, associated with its use. It is the
promulgated in federal, state, and local agencies that restrict
responsibility of the user of this standard to establish appro-
the amount of sulfur present in some fuels.
priate safety and health practices and determine the applica-
4.3 This test method provides a means of compliance with
bility of regulatory limitations prior to use. For specific
specifications or limits set by regulations for sulfur content of
warning statements, see Section 7.
petroleum products.
2. Referenced Documents 4.4 If this test method is applied to petroleum matrices with
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significantly different composition than the white oil calibra-
2.1 ASTM Standards:
tion materials specified in this test method, the cautions and
D 3120 Test Method for Trace Quantities of Sulfur in Light
recommendations in Section 5 should be observed when
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
interpreting the results.
lometry
4.5 Compared to other test methods for sulfur determina-
D 4057 Practice for Manual Sampling of Petroleum and
tion,TestMethodD 4294hashighthroughput,minimalsample
Petroleum Products
preparation, good precision, and is capable of determining
D 4177 Practice for Automatic Sampling of Petroleum and
sulfur over a wide range of concentrations. The equipment
Petroleum Products
specified is in most cases less costly than that required for
E 29 Practice for Using Significant Digits in Test Data to
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alternative methods. Consult the ASTM website or ASTM
Determine Conformance with Specifications
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Subject Index for names of alternative test methods.
3. Summary of Test Method
5. Interferences
3.1 The sample is placed in the beam emitted from an X-ray
5.1 Spectral interferences result when some sample compo-
source. The resultant excited characteristic X radiation is
nent element or elements emit X-rays that the detector cannot
measured, and the accumulated count is compared with counts
resolve from sulfur X-ray emission. As a result, the lines
produce spectral peaks that overlap with each other. Spectral
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interferences may arise from samples containing water, lead
This test method is under the jurisdiction of Committee D02 on Petroleum
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
alkyls, silicon, phosphorus, calcium, potassium, and halides if
Elemental Analysis.
present at concentrations greater than one tenth of the mea-
Current edition approved Nov. 1, 2003. Published December 2003. Originally
sured concentration of sulfur, or more than a few hundred
approved in 1983. Last previous edition approved in 2002 as D 4294-02.
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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
Standards volume information, refer to the standard’s Document Summary page on
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the ASTM website. Annual Book of ASTM Standards, Vol 00.01.
*A Summary of Changes section appears at the end of this standard.
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