ASTM D4239-11
(Test Method)Standard Test Methods for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion Methods
Standard Test Methods for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion Methods
SIGNIFICANCE AND USE
Sulfur is part of the ultimate analysis of coal and coke.
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.
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.
1.2 When automated equipment is used the procedure 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.
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Designation:D4239–11
Standard Test Method for
Sulfur in the Analysis Sample of Coal and Coke Using High-
1
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.
1. Scope E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the determination of sulfur in
3
2.2 ISO Standard:
samples of coal or coke by high-temperature tube furnace
ISO 11722 Solid Mineral Fuels-Hard Coal – Determination
combustion.
of Moisture in the general analysis test sample by drying
1.2 When automated equipment is used the procedure can
in nitrogen
be classified as an instrumental method.
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
3.1 Combustion Method with Infrared Absorption
standard.
Detection—A weighed test portion of sample is burned in a
1.4 This standard does not purport to address all of the
tube furnace at a minimum operating temperature of 1350°C in
safety concerns, if any, associated with its use. It is the
a stream of oxygen. During combustion at temperatures above
responsibility of the user of this standard to establish appro-
1350 ºC, the sulfur and sulfur compounds contained in the
priate safety and health practices and determine the applica-
sample are decomposed and oxidized almost exclusively to
bility of regulatory limitations prior to use.
gaseous sulfur dioxide, SO . Moisture and particulates are
2
2. Referenced Documents removed from the gas by filters. The gas stream is passed
2
through a cell in which sulfur dioxide is measured by an
2.1 ASTM Standards:
infrared (IR) absorption detector. Sulfur dioxide absorbs IR
D346 Practice for Collection and Preparation of Coke
energy at a precise wavelength within the IR spectrum. Energy
Samples for Laboratory Analysis
isabsorbedasthegaspassesthroughthecellbodyinwhichthe
D2013 Practice for Preparing Coal Samples for Analysis
IRenergyisbeingtransmitted:thus,atthedetector,lessenergy
D3173 Test Method for Moisture in theAnalysis Sample of
is received.All other IR energy is eliminated from reaching the
Coal and Coke
detector by a precise wavelength filter. Thus, the absorption of
D3176 Practice for Ultimate Analysis of Coal and Coke
IR energy can be attributed only to sulfur dioxide whose
D3180 Practice for Calculating Coal and Coke Analyses
concentration is proportional to the change in energy at the
from As-Determined to Different Bases
detector. One cell is used as both a reference and a measure-
D7448 Practice for Establishing the Competence of Labo-
ment chamber. Total sulfur as sulfur dioxide is detected on a
ratories Using ASTM Procedures in the Sampling and
continuous basis.
Analysis of Coal and Coke
D7582 Test Methods for Proximate Analysis of Coal and
4. Significance and Use
Coke by Macro Thermogravimetric Analysis
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
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
coal preparation and cleaning, evaluation of potential sulfur
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
emissions from coal and coke combustion or conversion
Analysis.
processes,andevaluationofcoalandcokequalityinrelationto
Current edition approved April 1, 2011. Published April 2011. Originally
´1
approved in 1983. Last previous edition approved in 2010 as D4239 – 10 . DOI: contract specifications, as well as for scientific purposes.
10.1520/D4239-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4239–11
4.3 The competency of laboratories with respect to use of 7. Reagents
this standard can be established through reference to Practice
7.1 Purity of Reagents—Use reagent grade chemicals in all
D7448.
tests. Unless otherwise indicated, it is intended that
...
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.
´1
Designation:D4239–10 Designation: D4239 – 11
Standard Test Method for
Sulfur in the Analysis Sample of Coal and Coke Using High-
1
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.
1
´ NOTE—The title of Table 1 was editorially corrected in August 2010.
1. Scope
1.1 Thistestmethodcoversthedeterminationofsulfurinsamplesofcoalorcokebyhigh-temperaturetubefurnacecombustion.
1.2 When automated equipment is used the procedure 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
D3173 Test Method for Moisture in the Analysis Sample of Coal and Coke
D3176 Practice for Ultimate Analysis of Coal and Coke
D3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases
D7448 PracticeforEstablishingtheCompetenceofLaboratoriesUsingASTMProceduresintheSamplingandAnalysisofCoal
and Coke
D7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis Test Methods for
Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 ISO Standard:
ISO11722 SolidMineralFuels-HardCoal–DeterminationofMoistureinthegeneralanalysistestsamplebydryinginnitrogen
3. Summary of Test Method
3.1 Combustion Method with Infrared Absorption Detection—A weighed test portion of sample is burned in a tube furnace at
a minimum operating temperature of 1350°C in a stream of oxygen. During combustion at temperatures above 1350 ºC, the sulfur
and sulfur compounds contained in the sample are decomposed and oxidized almost exclusively to gaseous sulfur dioxide, SO .
2
Moisture and particulates are removed from the gas by filters. The gas stream is passed through a cell in which sulfur dioxide is
measuredbyaninfrared(IR)absorptiondetector.SulfurdioxideabsorbsIRenergyataprecisewavelengthwithintheIRspectrum.
Energy is absorbed as the gas passes through the cell body in which the IR energy is being transmitted: thus, at the detector, less
energy is received.All other IR energy is eliminated from reaching the detector by a precise wavelength filter.Thus, the absorption
of IR energy can be attributed only to sulfur dioxide whose concentration is proportional to the change in energy at the detector.
One cell is used as both a reference and a measurement chamber. Total sulfur as sulfur dioxide is detected on a continuous basis.
1
This test method is under the jurisdiction ofASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.
Current edition approved May 1, 2010. Published July 2010. Originally approved in 1983. Last previous edition approved in 2008 as D4239–08. DOI: 10.1520/D4239-10.
´1
Current edition approved April 1, 2011. Published April 2011. Originally approved in 1983. Last previous edition approved in 2010 as D4239 – 10 . DOI:
10.1520/D4239-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4239 – 11
4. Significance and Use
4.1 Sulfur is part of the ultimate analy
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