ASTM D3177-89(1997)

Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke

SCOPE
1.1 These test methods cover two alternative procedures for the determination of total sulfur in samples of coal and coke. Sulfur is included in the ultimate analysis of coal and coke.  
1.2 The procedures appear in the following order:  Sections Method A---Eschka Method 6 to 9 Method B---Bomb Washing Method 10 to 11
1.3 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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. Specific precautionary statements are given in Sections 11.1.1 to 11.1.1.7.
1.4 The values stated in SI units are to be regarded as the standard.

General Information

• Status: Historical
• Publication Date: 31-Dec-1988
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.21 - Methods of Analysis

Relations

• Replaced By: ASTM D3177-89(2002) - Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke
• Effective Date: 29-Sep-1989

Standards Content (Sample)

Designation: D 3177 – 89 (Reapproved 1997)
Standard Test Methods for
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Total Sulfur in the Analysis Sample of Coal and Coke
This standard is issued under the fixed designation D 3177; 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 dissolved in hot water and then precipitated from the resulting
solution as barium sulfate (BaSO ). The precipitate is filtered,
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1.1 These test methods cover two alternative procedures for
ashed, and weighed.
the determination of total sulfur in samples of coal and coke.
3.2 Bomb Washing Method—Sulfur is precipitated as
Sulfur is included in the ultimate analysis of coal and coke.
BaSO from oxygen-bomb calorimeter washings, and the
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1.2 The procedures appear in the following order:
precipitate is filtered, ashed, and weighed.
Sections
Method A—Eschka Method 6-9
4. Significance and Use
Method B—Bomb Washing Method 10 and 11
4.1 Determination of sulfur is, by definition, part of the
1.3 This standard does not purport to address all of the
ultimate analysis of coal.
safety concerns, if any, associated with its use. It is the
4.2 Sulfur analysis results obtained by these methods are
responsibility of the user of this standard to establish appro-
used to serve a number of interests: evaluation of coal
priate safety and health practices and determine the applica-
preparation, evaluation of potential sulfur emissions from coal
bility of regulatory limitations prior to use. Specific precau-
combustion or conversion processes, evaluation of the coal
tionary statements are given in Sections 11.1.1-11.1.1.7.
quality in relation to contract specification, and other purposes
1.4 The values stated in SI units are to be regarded as the
of commercial or scientific interest.
standard.
5. Sample
2. Referenced Documents
5.1 The sample shall be the material pulverized to pass No.
2.1 ASTM Standards:
60 (250-μm) sieve in accordance with Method D 2013 or
D 346 Practice for Collection and Preparation of Coke
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Method D 346.
Samples for Laboratory Analysis
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5.2 A separate portion of the analysis sample should be
D 1193 Specification for Reagent Water
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analyzed for moisture content in accordance with Test Method
D 2013 Method of Preparing Coal Samples for Analysis
D 3173, so that calculation to other than the as-determined
D 2015 Test Method for Gross Calorific Value of Coal and
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basis can be made.
Coke by the Adiabatic Bomb Calorimeter
5.3 Procedures for converting as-determined sulfur values
D 3173 Test Method for Moisture in the Analysis Sample of
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obtained from the analysis sample to other bases are described
Coal and Coke
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in Practice D 3176 and Method D 3180.
D 3176 Practice for Ultimate Analysis of Coal and Coke
5.4 Standard Reference Material (SRM), such as SRM Nos.
D 3180 Practice for Calculating Coal and Coke Analyses
5
2
2682 through 2685—Sulfur in Coal which consist of four
from As-Determined to Different Bases
different coals that have been individually crushed and ground
D 3286 Test Method for Gross Calorific Value of Coal and
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to pass a No. 60 (250-μm) sieve, and bottled in 50-g units, or
Coke by the Isoperibol Bomb Calorimeter
other commercially available reference material coals with a
E 144 Practice for Safe Use of Oxygen Combustion
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certified sulfur content of6 0.0xx precision can be used. Sulfur
Bombs
values obtained by analyzing these coals, using any of the
3. Summary of Test Methods
methods described in this test method, may be used for
checking the accuracy of analytical results.
3.1 Eschka Method—A weighed sample and Eschka mix-
ture are intimately mixed and ignited together. The sulfur is
ALTERNATIVE PROCEDURES
TEST METHOD A—ESCHKA METHOD
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These test methods are under the jurisdiction of ASTM Committee D-5 on Coal
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of
6. Apparatus
Analysis.
6.1 Gas (Note 1) or Electric Muffle Furnace, or Burners,
Current edition approved Sept. 29, 1989. Published February 1990. Originally
published as D 3177 – 73. Last previous edition D 3177 – 84.
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Annual Book of ASTM Standards, Vol 05.05.
3 5
Annual Book of ASTM Standards, Vol 11.01. Available from National Institute of Standards and Technology, Gaithersburg,
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Annual Book of ASTM Standards, Vol 14.02. MD 20899.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 3177
for igniting the sample with the Eschka mixture and for solution required in accordance with 8.3. Transfer to a porce-
igniting the barium sulfate (BaSO ). lain capsule, or porcelain crucible, or a platinum crucible and
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cover with about1gof Eschka mixture.
NOTE 1—Gas can contain sulfur compounds.
8.2 Ignition—Heat the crucible over an alcohol, g
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