ASTM D4239-04a

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.

General Information

• Status: Historical
• Publication Date: 30-Jun-2004
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.21 - Methods of Analysis

Relations

• Replaces: ASTM D4239-04 - Standard Test Methods for Sulfur in the Analysis Sample of Coal and Coke Using High Temperature Tube Furnace Combustion Methods
• Effective Date: 01-Jul-2004
• Replaced By: ASTM D4239-05 - Standard Test Methods for Sulfur in the Analysis Sample of Coal and Coke Using High Temperature Tube Furnace Combustion Methods
• Effective Date: 01-Oct-2005
• Referred By: ASTM D2799-23 - Standard Test Method for Microscopical Determination of the Maceral Composition of Coal
• Effective Date: 01-Jul-2004
• Referred By: ASTM D1412/D1412M-20 - Standard Test Method for Equilibrium Moisture of Coal at 96 to 97 Percent Relative Humidity and 30 °C
• Effective Date: 01-Jul-2004
• Referred By: ASTM D3176-15 - Standard Practice for Ultimate Analysis of Coal and Coke
• Effective Date: 01-Jul-2004
• Referred By: ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
• Effective Date: 01-Jul-2004
• Referred By: ASTM D6700-19 - Standard Guide for Use of Scrap Tires as Tire-Derived Fuel
• Effective Date: 01-Jul-2004
• Referred By: ASTM D5865/D5865M-19 - Standard Test Method for Gross Calorific Value of Coal and Coke
• Effective Date: 01-Jul-2004
• Referred By: ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
• Effective Date: 01-Jul-2004
• Referred By: ASTM D388-23 - Standard Classification of Coals by Rank
• Effective Date: 01-Jul-2004
• Referred By: ASTM D8214-18 - Standard Test Method for Forms of Sulfur in Coal by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 01-Jul-2004
• Referred By: ASTM D7448-16 - Standard Practice for Establishing the Competence of Laboratories Using ASTM Procedures in the Sampling and Analysis of Coal and Coke
• Effective Date: 01-Jul-2004

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D4239–04a
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 2361 Test Method for Chlorine in Coal
D 3173 Test Method for Moisture in theAnalysis Sample of
1.1 These test methods cover two alternative procedures
Coal and Coke
using high-temperature tube furnace combustion methods for
D 3176 Practice for Ultimate Analysis of Coal and Coke
the rapid determination of sulfur in samples of coal and coke.
D 3180 Practice for Calculating Coal and Coke Analyses
1.2 These test methods appear in the following order:
from As-Determined to Different Bases
Sections
D 4208 Test Method for Total Chlorine in Coal by the
Method A—High-Temperature Combustion
Oxygen Bomb Combustion/Ion Selective Electrode
Method withAcid Base Titration Detec-
Method
tion Procedures 6-9
D 4621 Guide for Quality Management in an Organization
Method B—High-Temperature Combustion
Method with InfraredAbsorption Detec-
that Samples or Tests Coal and Coke
tion Procedures 10–12
D 5142 Test Methods for the Proximate Analysis of the
NOTE 1—High Temperature Combustion Method with Iodimetric De-
Analysis Sample of Coal and Coke by Instrumental
tectionprocedures,formallyMethodBinthe2000versionofthisstandard
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 7.8 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
of each acid present have been determined, the percentage of
2.1 ASTM Standards:
sulfur contained in the coal may be calculated.
D 346 Practice for Collection and Preparation of Coke
3.1.1 This method is written to include commercially avail-
Samples for Laboratory Analysis
able sulfur analyzers that must be calibrated with appropriate
D 1193 Specification for Reagent Water
certified reference materials to establish recovery factors or a
2
D 2013 Method of Preparing Coal Samples for Analysis
calibration curve based on the range of sulfur in the coal or
coke samples being analyzed.
1
NOTE 2—ElementsordinarilypresentincoaldonotinterfereinMethod
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 A (3.1), with the exception of chlorine; results must be corrected for
Analysis.
chlorine content of the samples (9.1).
Current edition approved July 1, 2004. Published July 2004. Originally approved
3.2 Method B—High-Temperature Combustion Method with
in 1983. Last previous as D 4239 – 83. Last previous edition approved in 2004 as
D 4239 – 04. Infrared Absorption Detection Procedures—The sample is
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
burned in a tube furnace at a minimum operating temperature
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
of1350°Cinastreamofoxygentooxidizethesulfur.Moisture
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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