Standard Test Method for Sulfur in Ash from Coal and Coke

SCOPE
1.1 This test method pertains to the determination of sulfate sulfur in coal or coke ash.  
1.2 The values stated in SI units (Practice E380) shall be regarded as the standard.  
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.

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Status
Historical
Publication Date
09-Apr-1996
Current Stage
Ref Project

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ASTM D1757-96 - Standard Test Method for Sulfur in Ash from Coal and Coke
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Designation: D 1757 – 96
Standard Test Method for
1
Sulfur in Ash from Coal and Coke
This standard is issued under the fixed designation D 1757; 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 3.2 Test Method B—Eschka Mixture—A specified quantity
of ash and Eschka mixture are ignited together in air. The
1.1 This test method pertains to the determination of sulfate
sulfates are dissolved in hot water and separated from undis-
sulfur in coal or coke ash.
solved ash residue and magnesium oxide by filtration. Sulfate
1.2 The values stated in SI units (Practice E 380) shall be
in the filtrate is determined gravimetrically as barium sulfate
regarded as the standard.
(BaSO ).
4
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 Laboratory furnace temperature and furnace ventilation
priate safety and health practices and determine the applica-
have an influence on SO retention in laboratory ash. Conse-
3
bility of regulatory limitations prior to use.
quently, sulfur in ash as determined in the laboratory cannot be
2. Referenced Documents assumed to be equivalent to sulfur present in the mineral matter
in coal or to the retention of sulfur in ash produced under the
2.1 ASTM Standards:
2
conditions of commercial utilization.
D 1193 Specification for Reagent Water
3 4.2 The sulfate sulfur determined by these test methods can
D 2795 Test Methods for Analysis of Coal and Coke Ash
be used to calculate the sulfur trioxide portion of ash so that the
D 3174 Test Method for Ash in the Analysis Sample of Coal
3 ash content or ash composition can be reported on a sulfur
and Coke from Coal
trioxide free basis.
D 3177 Test Methods for Total Sulfur in the Analysis
3
Sample of Coal and Coke
5. Interferences
D 3682 Test Method for Major and Minor Elements in Coal
3
5.1 Barium in coal ashes can result in incomplete recovery
and Coke Ash by Atomic Absorption
of sulfate sulfur.
D 4326 Test Method for Major and Minor Elements in Coal
3
5.2 High iron content can be encountered in coal and coke
and Coke Ash by X-Ray Fluorescence
ash and can introduce error if, during the sulfate precipitation,
E 380 Practice for Use of the International System of Units
4
the iron is either partially adsorbed by the BaSO precipitate or
4
(SI) (the Modernized Metric System)
coprecipitated as iron sulfate.
2.2 British Standard:
5
BS 1016, Part 14 Analysis of Coal Ash and Coke Ash
6. Apparatus
6.1 Muffle Furnace, electric, capable of maintaining a tem-
3. Summary of Test Methods
perature of 800 6 25°C for igniting barium sulfate.
3.1 Test Method A—Modified British Method—A specified
6.2 Crucibles or Capsules, porcelain, platinum, alundum, or
quantity of ash is digested in boiling dilute hydrochloric acid
silica of 10 to 15-mL capacity, for igniting BaSO .
4
solution to which bromine water is added to convert sulfite that
may be present to the sulfate form. After neutralization and
7. Purity of Reagents
precipitation of iron with ammonium hydroxide, the mixture is
7.1 Purity of Reagents—Reagent grade chemicals shall be
filtered and sulfate in the filtrate is determined gravimetrically
used in all tests. Unless otherwise indicated, it is intended that
as barium sulfate (BaSO ).
4
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
6
1
where such specifications are available.
This test method is under the jurisdiction of ASTM Committee D-5 on Coal and
Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
Ash and Trace Elements of Coal.
Current edition approved April 10, 1996. Published June 1996. Originally
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published as D 1757 – 60 T. Last previous edition D 1757 – 95. Reagent Chemicals, American Chemical Society Specifications, American
2
Annual Book of ASTM Standards, Vol 11.01. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
Annual Book of ASTM Standards, Vol 05.05. listed by the American Chemical Society, see Analar Standards for Laboratory
4
Annual Book of ASTM Standards, Vol 14.02. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5
Available from American National Standards Institute, 11 W. 42nd St., 13th and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Floor, New York, NY 10036. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 1757
NOTE 1—The excess of strong ammonium hydroxide minimizes the
7.2 Purity of Water—Unless otherwise indicated, references
possi
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