ASTM D4239-04
(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
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:
SectionsMethod A—High-Temperature Combustion Method with Acid Base Titration Detection Procedures6-9Method 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 7.8 and 11.2.
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Designation: D 4239 – 04
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.
Note—Table 2 was reinstated and Table 3 was editorially revised. Editorial changes were made throughout and the year date was changed on May 17, 2004.
1. Scope D 346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis
1.1 These test methods cover two alternative procedures
D 1193 Specification for Reagent Water
using high-temperature tube furnace combustion methods for
2
D 2013 Method of Preparing Coal Samples for Analysis
the rapid determination of sulfur in samples of coal and coke.
D 2361 Test Method for Chlorine in Coal
1.2 These test methods appear in the following order:
D 3173 Test Method for Moisture in the Analysis Sample of
Sections
Coal and Coke
Method A—High-Temperature Combustion
D 3176 Practice for Ultimate Analysis of Coal and Coke
Method with Acid Base Titration Detec-
D 3180 Practice for Calculating Coal and Coke Analyses
tion Procedures 6-9
from As-Determined to Different Bases
Method B—High-Temperature Combustion
Method with Infrared Absorption Detec-
D 4208 Test Method for Total Chlorine in Coal by the
tion Procedures 10–12
Oxygen Bomb Combustion/Ion Selective Electrode
NOTE 1—High Temperature Combustion Method with Iodimetric De-
Method
tection procedures, formally Method B in the 2000 version of this standard
D 4621 Guide for Quality Management in an Organization
is still a viable method that may be used.
that Samples or Tests Coal and Coke
1.2.1 When automated equipment is used to perform any of
D 5142 Test Methods for the Proximate Analysis of the
the two methods of this test method, the procedures can be
Analysis Sample of Coal and Coke by Instrumental
classified as instrumental methods. There are several manufac-
Procedures
turers that offer to the coal industry equipment with instrumen-
3. Summary of Test Methods
tal analysis capabilities for the determination of the sulfur
content of coal and coke samples.
3.1 Method A—High-Temperature Combustion Method with
1.3 This standard does not purport to address all of the
Acid-Base Titration Detection Procedures—A weighed sample
safety concerns, if any, associated with its use. It is the
is burned in a tube furnace at a minimum operating temperature
responsibility of the user of this standard to establish appro-
of 1350°C in a stream of oxygen. During combustion, all sulfur
priate safety and health practices and determine the applica-
contained in the sample is oxidized to gaseous oxides of sulfur
bility of regulatory limitations prior to use. See 7.8 and 11.2.
(sulfur dioxide, SO , and sulfur trioxide, SO ) and the chlorine
2 3
in the sample is released as Cl . These products are then
2
2. Referenced Documents
absorbed into a solution of hydrogen peroxide (H O ) where
2 2
2
they dissolve forming dilute solutions of sulfuric (H SO ) and
2 4
2.1 ASTM Standards:
hydrochloric (HCl) acids. The quantities of both acids pro-
duced are directly dependent upon the amounts of sulfur and
1 chlorine present in the original coal sample. Once the amounts
This test method is under the jurisdiction of ASTM Committee D05 on Coal
of each acid present have been determined, the percentage of
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
sulfur contained in the coal may be calculated.
Current edition approved May 17, 2004. Published May 2004. Originally
3.1.1 This method is written to include commercially avail-
approved in 1983. Last previous as D 4239 – 83. Last previous edition approved in
able sulfur analyzers that must be calibrated with appropriate
2002 as D 4239 – 02a.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or certified reference materials to establish recovery factors or a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
calibration curve based on the range of sulfur in the coal or
Standards volume information, refer to the standard’s Document Summary page on
coke samples being analyzed.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4239–04
NOTE 2—Elements ordinarily present in coal do not interfere in Method
5.4 Certified Reference Materials, or other commercially
A (3.1), with the exception of chlorine; result
...
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