ASTM D4239-02
(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 three 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 Iodimetric Titration Detection Procedures10-13Method C—High-Temperature Combustion Method with Infrared Absorption Detection Procedures14-16
1.2.1 When automated equipment is used to perform any of the three 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 15.2.
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Designation: D 4239 – 02
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.
1. Scope D 4208 Test Method for Total Chlorine in Coal by the
Oxygen Bomb Combustion/Ion Selective Electrode
1.1 These test methods cover three alternative procedures
2
Method
using high-temperature tube furnace combustion methods for
D 4621 Guide for Quality Management in an Organization
the rapid determination of sulfur in samples of coal and coke.
2
that Samples or Tests Coal and Coke
1.2 These test methods appear in the following order:
D 5142 Test Methods for the Proximate Analysis of the
Sections
Analysis Sample of Coal and Coke by Instrumental
2
Method A—High-Temperature Combustion Method with Acid
Procedures
Base Titration Detection Procedures 6-9
Method B—High-Temperature Combustion Method with Iodi-
3. Summary of Test Methods
metric Titration Detection Procedures 10-13
Method C—High-Temperature Combustion Method with Infra-
3.1 Method A—High-Temperature Combustion Method with
red Absorption Detection Procedures 14-16
Acid-Base Titration Detection Procedures—A weighed sample
1.2.1 When automated equipment is used to perform any of
is burned in a tube furnace at a minimum operating temperature
the three methods of this test method, the procedures can be of 1350°C in a stream of oxygen. During combustion, all sulfur
classified as instrumental methods. There are several manufac-
contained in the sample is oxidized to gaseous oxides of sulfur
turers that offer to the coal industry equipment with instrumen- (sulfur dioxide, SO , and sulfur trioxide, SO ) and the chlorine
2 3
tal analysis capabilities for the determination of the sulfur
in the sample is released as Cl . These products are then
2
content of coal and coke samples. absorbed into a solution of hydrogen peroxide (H O ) where
2 2
1.3 This standard does not purport to address all of the
they dissolve forming dilute solutions of sulfuric (H SO ) and
2 4
safety concerns, if any, associated with its use. It is the hydrochloric (HCl) acids. The quantities of both acids pro-
responsibility of the user of this standard to establish appro-
duced are directly dependent upon the amounts of sulfur and
priate safety and health practices and determine the applica- chlorine present in the original coal sample. Once the amounts
bility of regulatory limitations prior to use. See 7.8 and 15.2.
of each acid present have been determined, the percentage of
sulfur contained in the coal may be calculated.
2. Referenced Documents
3.1.1 This method is written to include commercially avail-
2.1 ASTM Standards:
able sulfur analyzers that must be calibrated with appropriate
D 346 Practice for Collection and Preparation of Coke certified reference materials to establish recovery factors or a
2
Samples for Laboratory Analysis
calibration curve based on the range of sulfur in the coal or
3
D 1193 Specification for Reagent Water
coke samples being analyzed.
2
D 2013 Method of Preparing Coal Samples for Analysis
NOTE 1—Elements ordinarily present in coal do not interfere in Method
2
D 2361 Test Method for Chlorine in Coal
A (3.1), with the exception of chlorine; results must be corrected for
D 3173 Test Method for Moisture in the Analysis Sample of
chlorine content of the samples (9.1).
2
Coal and Coke
3.2 Method B—High-Temperature Combustion Method with
2
D 3176 Practice for Ultimate Analysis of Coal and Coke
Iodimetric Detection Procedures—A weighed sample is
D 3180 Practice for Calculating Coal and Coke Analyses
burned in a tube furnace at a minimum operating temperature
2
from As-Determined to Different Bases
of 1350°C in a stream of oxygen to ensure the oxidation of
sulfur. The combustion products are absorbed in an aqueous
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
solution that contains iodine. When sulfur dioxide is scrubbed
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
by the diluent, the trace iodine originally present in the solution
Analysis.
Current edition approved April 10, 2002. Published July 2002. Originally
is reduced to iodide, thus causing an increase in resistance. The
published as D 4239 – 83. Last previous edition D 4239 – 00.
detection system of the instrument consists of a polarized dual
2
Annual Book of ASTM Standards, Vol 05.06.
3 platinum electrode. Any change in resistance of the solution in
Annual Book of ASTM
...
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