ASTM D4239-00

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:  Sections Method A---High Temperature Combustion Method with Acid Base Titration Detection Procedures 6 to 9 Method B---High Temperature Combustion Method with Iodimetric Titration Detection Procedures 10 to 13 Method C---High Temperature Combustion Method with In- frared Absorption Detection Procedures 14 to 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.

General Information

• Status: Historical
• Publication Date: 09-Apr-2000
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.21 - Methods of Analysis

Relations

• Replaced By: ASTM D4239-02 - Standard Test Methods for Sulfur in the Analysis Sample of Coal and Coke Using High Temperature Tube Furnace Combustion Methods
• Effective Date: 10-Apr-2002

Standards Content (Sample)

ASTM-D4239
ADOPTION NOTICE
ASTM-D4239, "SULFUR IN THE ANALYSIS SAMPLE OF COAL AND COKE USING
HIGH TEMPERATURE TUBE FURNACE COMBUSTION METHODS", was adopted on
03-OCT-94 for use by the Department of Defense (DoD). Proposed
changes by DoD activities must be submitted to the DoD Adopting
Activity: Commander, Naval Sea Systems Command, SEA 03R42, 2531
Jefferson Davis Highway, Arlington, VA 22242-5160. Copies of
this document may be purchased from the American Society for
Testing and Materials 100 Barr Harbor Drive West Conshohocken,
Pennsylvania, United States, 19428-2959. http://www.astm.org/____________________
Custodians: Adopting Activity:
Army - CR4 Navy - SH
Navy - SH
Air Force - 68
FSC 9110
Approved for public release; distribution
DISTRIBUTION STATEMENT A:
is unlimited.

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