ASTM D4294-08

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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.
An American National Standard
Designation: D 4294 – 08
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 (´) 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, biodiesel (see Note 2), and similar petroleum products.
NOTE 1—Oxygenated fuels with ethanol or methanol contents exceeding the limits given in Table 1 can be dealt with using this test method, but the
precision and bias statements do not apply (see Appendix X2).
NOTE 2—For samples with high oxygen contents (>3 wt %) sample dilution as described in 1.3 or matrix matching must be performed to assure
accurate results.
1.2 Interlaboratory studies on precision revealed the scope to be 17 mg/kg to 4.6 mass %. An estimate of this test method’s
pooled limit of quantitation (PLOQ) is 17.0 mg/kg as calculated by the procedures in Practice D 6259. 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.An estimate of the limit of detection is three times the
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reproducibility standard deviation, and an estimate of the limit of quantitation is ten times the reproducibility standard deviation.
1.3 Samples containing more than 4.6 mass % sulfur can 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 16 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 5.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards
(see Section 5) or by the presence of other heteroatoms.
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
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2.1 ASTM Standards:
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D 6259 Practice for Determination of a Pooled Limit of Quantitation
D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D 7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
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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 D02.03 on
Elemental Analysis.
Current edition approved March 1, 2008. Published April 2008. Originally approved in 1983. Last previous edition approved in 2003 as D 4294–03.
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Analytical Chemistry, Vol 55, 1983, pp. 2210-2218.
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