ASTM D4239-08
(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
p>Determination of sulfur is, by definition, part of the ultimate analysis of coal.
Results of the sulfur analysis are used to serve a number of interests: evaluation of coal preparation, evaluation of potential sulfur emissions from coal combustion or conversion processes, and evaluation of the coal quality in relation to contract specifications, as well as other scientific purposes.
The instrumental analysis provides a reliable, rapid method for determining the concentration of sulfur in a lot of coal or coke and are especially applicable when results must be obtained rapidly for the successful completion of industrial, beneficiation, trade, or other evaluations.
SCOPE
1.1 These test methods cover two alternative procedures using high-temperature tube furnace combustion methods for the rapid determination of sulfur in samples of coal and coke.
1.2 These test methods appear in the following order:
Sections Method A—High-Temperature Combustion Method with Acid Base Titration Detection Procedures6-9 Method B—High-Temperature Combustion Method with Infrared Absorption Detection Procedures10-12
Note 1—High Temperature Combustion Method with Iodimetric Detection procedures, formally Method B in the 2000 version of this standard is still a viable method that may be used.
1.2.1 When automated equipment is used to perform any of the two methods of this test method, the procedures can be classified as instrumental methods. There are several manufacturers that offer to the coal industry equipment with instrumental analysis capabilities for the determination of the sulfur content of coal and coke samples.
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. See 7.7 and 11.2.
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Designation:D4239–08
Standard Test Methods for
Sulfur in the Analysis Sample of Coal and Coke Using High-
1
Temperature Tube Furnace Combustion Methods
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 D2013 Practice for Preparing Coal Samples for Analysis
3
D2361 Test Method for Chlorine in Coal
1.1 These test methods cover two alternative procedures
D3173 Test Method for Moisture in theAnalysis Sample of
using high-temperature tube furnace combustion methods for
Coal and Coke
the rapid determination of sulfur in samples of coal and coke.
D3176 Practice for Ultimate Analysis of Coal and Coke
1.2 These test methods appear in the following order:
D3180 Practice for Calculating Coal and Coke Analyses
Sections
from As-Determined to Different Bases
Method A—High-Temperature Combustion
D4208 Test Method for Total Chlorine in Coal by the
Method withAcid Base Titration Detec-
Oxygen Bomb Combustion/Ion Selective Electrode
tion Procedures 6-9
Method
Method B—High-Temperature Combustion
Method with InfraredAbsorption Detec-
D4621 Guide for Quality Management in an Organization
tion Procedures 10-12
That Samples or Tests Coal and Coke
NOTE 1—High Temperature Combustion Method with Iodimetric De-
D5142 TestMethodsforProximateAnalysisoftheAnalysis
tectionprocedures,formallyMethodBinthe2000versionofthisstandard
Sample of Coal and Coke by Instrumental Procedures
is still a viable method that may be used.
3. Summary of Test Methods
1.2.1 When automated equipment is used to perform any of
the two methods of this test method, the procedures can be
3.1 Method A—High-Temperature Combustion Method with
classified as instrumental methods. There are several manufac-
Acid-Base Titration Detection Procedures—Aweighed sample
turers that offer to the coal industry equipment with instrumen-
isburnedinatubefurnaceataminimumoperatingtemperature
tal analysis capabilities for the determination of the sulfur
of1350°Cinastreamofoxygen.Duringcombustion,allsulfur
content of coal and coke samples.
contained in the sample is oxidized to gaseous oxides of sulfur
1.3 This standard does not purport to address all of the
(sulfur dioxide, SO , and sulfur trioxide, SO ) and the chlorine
2 3
safety concerns, if any, associated with its use. It is the
in the sample is released as Cl . These products are then
2
responsibility of the user of this standard to establish appro-
absorbed into a solution of hydrogen peroxide (H O ) where
2 2
priate safety and health practices and determine the applica-
they dissolve forming dilute solutions of sulfuric (H SO ) and
2 4
bility of regulatory limitations prior to use. See 7.7 and 11.2.
hydrochloric (HCl) acids. The quantities of both acids pro-
duced are directly dependent upon the amounts of sulfur and
2. Referenced Documents
chlorine present in the original coal sample. Once the amounts
2
2.1 ASTM Standards:
of each acid present have been determined, the percentage of
D346 Practice for Collection and Preparation of Coke
sulfur contained in the coal may be calculated.
Samples for Laboratory Analysis
3.1.1 This method is written to include commercially avail-
D1193 Specification for Reagent Water
able sulfur analyzers that must be calibrated with appropriate
certified reference materials to establish recovery factors or a
calibration curve based on the range of sulfur in the coal or
1 coke samples being analyzed.
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
NOTE 2—ElementsordinarilypresentincoaldonotinterfereinMethod
Analysis.
A(3.1), with the exception of chlorine; results must be corrected for
Current edition approved Feb. 1, 2008. Published March 2008. Originally
chlorine content of the samples (9.1).
approved in 1983. Last previous edition approved in 2005 as D4239 – 05. DOI:
10.1520/D4239-08.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. on www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1
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D4239–08
3.2 Method B—High-Temperature Combustion
...
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:D4239–05 Designation:D4239–08
Standard Test Methods for
Sulfur in the Analysis Sample of Coal and Coke Using High-
1
Temperature Tube Furnace Combustion Methods
This standard is issued under the fixed designation D 4239; 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
1.1 These test methods cover two alternative procedures using high-temperature tube furnace combustion methods for the rapid
determination of sulfur in samples of coal and coke.
1.2 These test methods appear in the following order:
Sections
Method A—High-Temperature Combustion
Method withAcid Base Titration Detec-
tion Procedures 6-9
Method B—High-Temperature Combustion
Method with InfraredAbsorption Detec-
tion Procedures 10-12
NOTE 1—High Temperature Combustion Method with Iodimetric Detection procedures, formally Method B in the 2000 version of this standard is still
a viable method that may be used.
1.2.1 Whenautomatedequipmentisusedtoperformanyofthetwomethodsofthistestmethod,theprocedurescanbeclassified
as instrumental methods. There are several manufacturers that offer to the coal industry equipment with instrumental analysis
capabilities for the determination of the sulfur content of coal and coke samples.
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. See 7.7 and 11.2.
2. Referenced Documents
2
2.1 ASTM Standards:
D 346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D 1193 Specification for Reagent Water
D 2013Method of Practice for Preparing Coal Samples for Analysis
D 2361 Test Method for Chlorine in Coal
D 3173 Test Method for Moisture in the Analysis Sample of Coal and Coke
D 3176 Practice for Ultimate Analysis of Coal and Coke
D 3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases
D 4208 Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
D 4621 Guide for Quality Management in an Organization thatThat Samples or Tests Coal and Coke
D 5142 Test Methods for the Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Procedures
3. Summary of Test Methods
3.1 Method A—High-Temperature Combustion Method with Acid-Base Titration Detection Procedures—Aweighed sample is
burned in a tube furnace at a minimum operating temperature of 1350°C in a stream of oxygen. During combustion, all sulfur
contained in the sample is oxidized to gaseous oxides of sulfur (sulfur dioxide, SO , and sulfur trioxide, SO ) and the chlorine
2 3
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 Oct. 1, 2005. Published October 2005. Originally approved in 1983. Last previous as D4239–83. Last previous edition approved in 2004 as
D4239–04a.
Current edition approved Feb. 1, 2008. Published March 2008. Originally approved in 1983. Last previous edition approved in 2005 as D 4239 – 05.
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.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4239–08
in the sample is released as Cl .These products are then absorbed into a solution of hydrogen peroxide (H O ) where they dissolve
2 2 2
forming dilute solutions of sulfuric (H SO ) and hydrochloric (HCl) acids. The quantities of both acids produced are directly
2 4
dependentupontheamountsofsulfurandchlorinepresentintheoriginalcoalsample.Oncetheamountsofeachacidpresenthave
been determined, the percentage of sulfur contained in the coal may be calculated.
3.1.1 Thismethodiswrittentoincludecommerciallyavailablesulfuranalyzersthatmustbecalibratedwithappropriatecertified
referencematerialst
...
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