ASTM D4239-13e1
(Test Method)Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion
Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion
SIGNIFICANCE AND USE
4.1 Sulfur is part of the ultimate analysis of coal and coke.
4.2 Results of the sulfur analysis are used for evaluation of coal preparation and cleaning, evaluation of potential sulfur emissions from coal and coke combustion or conversion processes, and evaluation of coal and coke quality in relation to contract specifications, as well as for scientific purposes.
4.3 The competency of laboratories with respect to use of this standard can be established through reference to Practice D7448.
SCOPE
1.1 This test method covers the determination of sulfur in samples of coal or coke by high-temperature tube furnace combustion.
1.1.1 Two analysis methods are described.
1.2 When automated equipment is used, either method can be classified as an instrumental method.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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
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Standards Content (Sample)
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Designation: D4239 − 13
StandardTest Method for
Sulfur in the Analysis Sample of Coal and Coke Using High-
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Temperature Tube Furnace Combustion
This standard is issued under the fixed designation D4239; 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.
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ε NOTE—Footnote 6 was corrected editorially in November 2013.
1. Scope D7582 Test Methods for Proximate Analysis of Coal and
Coke by Macro Thermogravimetric Analysis
1.1 This test method covers the determination of sulfur in
E691 Practice for Conducting an Interlaboratory Study to
samples of coal or coke by high-temperature tube furnace
Determine the Precision of a Test Method
combustion.
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2.2 ISO Standard:
1.1.1 Two analysis methods are described.
ISO 11722 Solid Mineral Fuels-Hard Coal – Determination
1.2 When automated equipment is used, either method can
of Moisture in the general analysis test sample by drying
be classified as an instrumental method.
in nitrogen
1.3 The values stated in SI units are to be regarded as
3. Summary of Test Method
standard. No other units of measurement are included in this
standard.
3.1 Combustion Method A (1350°C)—A weighed test por-
tion of sample is burned in a tube furnace at a minimum
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the combustion tube operating temperature of 1350°C in a stream
of oxygen. During combustion at temperatures above 1350 ºC,
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- the sulfur and sulfur compounds contained in the sample are
decomposed and oxidized almost exclusively to gaseous sulfur
bility of regulatory limitations prior to use.
dioxide, SO . Moisture and particulates are removed from the
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2. Referenced Documents
gas by filters. The gas stream is passed through a cell in which
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sulfur dioxide is measured by an infrared (IR) absorption
2.1 ASTM Standards:
detector. Sulfur dioxide absorbs IR energy at a precise wave-
D346 Practice for Collection and Preparation of Coke
length within the IR spectrum. Energy is absorbed as the gas
Samples for Laboratory Analysis
passes through the cell body in which the IR energy is being
D2013 Practice for Preparing Coal Samples for Analysis
transmitted: thus, at the detector, less energy is received. All
D3173 Test Method for Moisture in the Analysis Sample of
other IR energy is eliminated from reaching the detector by a
Coal and Coke
precisewavelengthfilter.Thus,theabsorptionofIRenergycan
D3176 Practice for Ultimate Analysis of Coal and Coke
be attributed only to sulfur dioxide whose concentration is
D3180 Practice for Calculating Coal and Coke Analyses
proportional to the change in energy at the detector. One cell is
from As-Determined to Different Bases
used as both a reference and a measurement chamber. Total
D7448 Practice for Establishing the Competence of Labora-
sulfur as sulfur dioxide is detected on a continuous basis.
tories Using ASTM Procedures in the Sampling and
3.1.1 One procedure for Method A uses coal or coke
Analysis of Coal and Coke
reference materials to calibrate the sulfur analyzer. A second
procedure for Method A uses a pure substance, BBOT, to
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This test method is under the jurisdiction of ASTM Committee D05 on Coal
calibrate the sulfur analyzer.
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
3.2 Combustion Method B (1150°C)—A weighed test por-
Current edition approved Oct. 1, 2013. Published October 2013. Originally
tion of sample is burned in a quartz combustion tube in a
approved in 1983. Last previous edition approved in 2012 as D4239 – 12. DOI:
10.1520/D4239-13.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from International Organization for Standardization (ISO), 1, ch. de
Standards volume information, refer to the standard’s Document Summary page on la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://
the ASTM website. www.iso.ch.
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D4239 − 13
stream of oxygen with an equal or excess weight of tungsten 5.2 Analyze a separate portion of the analysis sample for
trioxide (WO ). Sulfur is oxidized during the reaction of the moisture content
...
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