ASTM D1757-03

Standard Test Method for Sulfate Sulfur in Ash from Coal and Coke (Withdrawn 2009)

SIGNIFICANCE AND USE
Laboratory furnace temperature and furnace ventilation have an influence on SO3 retention in laboratory ash. Consequently, sulfur in ash as determined in the laboratory cannot be assumed to be equivalent to sulfur present in the mineral matter in coal or to the retention of sulfur in ash produced under the conditions of commercial utilization.
The sulfate sulfur determined by these test methods can be used to calculate the sulfur trioxide portion of ash so that the ash content or ash composition can be reported on a sulfur trioxide free basis.
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 E 380) 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.
WITHDRAWN RATIONALE
This test method pertains to the determination of sulfate sulfur in coal or coke ash.
Formerly under the jurisdiction of Committee D05 on Coal and Coke, this test method was withdrawn in October 2009.This standard is a classical gravimetric sulfate method that is sometimes improperly cited for use in contracts. In addition the Eschka's Mixture that is vital for the test method is no longer available commcercially.

General Information

• Status: Withdrawn
• Publication Date: 09-Apr-2003
• Withdrawal Date: 31-Aug-2009
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaces: ASTM D1757-96(2002) - Standard Test Method for Sulfur in Ash from Coal and Coke
• Effective Date: 10-Apr-2003
• Referred By: ASTM D3174-12(2018)e1 - Standard Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
• Effective Date: 10-Apr-2003

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 1757 – 03
Standard Test Method for
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Sulfate 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 solution to which bromine water is added to convert sulfite that
may be present to the sulfate form. After neutralization and
1.1 This test method pertains to the determination of sulfate
precipitation of iron with ammonium hydroxide, the mixture is
sulfur in coal or coke ash.
filtered and sulfate in the filtrate is determined gravimetrically
1.2 The values stated in SI units (Practice E 380) shall be
as barium sulfate (BaSO ).
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regarded as the standard.
3.2 Test Method B—Eschka Mixture—A specified quantity
1.3 This standard does not purport to address all of the
of ash and Eschka mixture are ignited together in air. The
safety concerns, if any, associated with its use. It is the
sulfates are dissolved in hot water and separated from undis-
responsibility of the user of this standard to establish appro-
solved ash residue and magnesium oxide by filtration. Sulfate
priate safety and health practices and determine the applica-
in the filtrate is determined gravimetrically as barium sulfate
bility of regulatory limitations prior to use.
(BaSO ).
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2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
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4.1 Laboratory furnace temperature and furnace ventilation
D 1193 Specification for Reagent Water
3
have an influence on SO retention in laboratory ash. Conse-
3
D 2795 Test Methods for Analysis of Coal and Coke Ash
quently, sulfur in ash as determined in the laboratory cannot be
D 3174 TestMethodforAshintheAnalysisSampleofCoal
3
assumedtobeequivalenttosulfurpresentinthemineralmatter
and Coke from Coal
in coal or to the retention of sulfur in ash produced under the
D 3177 Test Methods for Total Sulfur in the Analysis
3
conditions of commercial utilization.
Sample of Coal and Coke
4.2 The sulfate sulfur determined by these test methods can
D 3682 Test Method for Major and Minor Elements in
3
beusedtocalculatethesulfurtrioxideportionofashsothatthe
Combustion Residues from Coal Utilization Processes
ash content or ash composition can be reported on a sulfur
D 4326 Test Method for Major and Minor Elements in Coal
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trioxide free basis.
and Coke Ash by X-Ray Fluorescence
E 380 Practice for Use of the International System of Units
5. Interferences
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(SI) (the Modernized Metric System)
5.1 Barium in coal ashes can result in incomplete recovery
2.2 British Standard:
5 of sulfate sulfur.
BS 1016, Part 14 Analysis of Coal Ash and Coke Ash
5.2 High iron content can be encountered in coal and coke
3. Summary of Test Methods ash and can introduce error if, during the sulfate precipitation,
the iron is either partially adsorbed by the BaSO precipitate or
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3.1 Test Method A—Modified British Method—A specified
coprecipitated as iron sulfate.
quantity of ash is digested in boiling dilute hydrochloric acid
6. Apparatus
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This test method is under the jurisdiction of ASTM Committee D05 on Coal
6.1 Muffle Furnace, electric, capable of maintaining a tem-
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
perature of 800 6 25°C for igniting barium sulfate.
Elements in Ash and Trace Elements of Coal.
6.2 Crucibles or Capsules, porcelain, platinum, alundum, or
Current edition approved April 10, 2003. Published July 2003. Originally
approved in 1960. Last previous edition approved in 2000 as D 1757 – 96 (2000).
silica of 10 to 15-mL capacity, for igniting BaSO .
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2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 05.06.
4
Annual Book of ASTM Standards, Vol 14.04.
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Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D1757–03
7. Purity of Reagents 100 mL of dilute HCl and 5 mL of bromine water. Cover the
beaker, boil 15 min, and digest an additional 30 to 45 min at a
7.1 Purity of Reagents—Reagent grade chemicals shall be
temperature just below boiling.
used in all tests. Unless otherwise indicated, it is intended that
10.2 Precipitation of Iron—While the solution is hot, add a
all reagents shall conform to the specifications of the Commit-
few drops of methyl orange indicator. Precipitate iron by
tee onAnalytical Reagents of theAmerican Chemical Society,
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slowly adding concentrated NH OH (sp gr 0.90) until a slight
4
where such specifi
...