ASTM D5987-96

Standard Test Method for Total Fluorine in Coal and Coke by Pyrohydrolytic Extraction and Ion Selective Electrode or Ion Chromatograph Methods

SCOPE
1.1 This test method covers the analysis of total fluorine in coal and coke.  
1.2 This analysis was successfully tested on coals containing 37% ash or less (see AS 1038.10.4 and Conrad).  
1.3 The values stated in SI units shall be regarded as standard. The values given in parentheses are for information only.  
1.4 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.  
1.5 All accountability and quality control aspects of Guide D 4621 apply to this test method.

General Information

• Status: Historical
• Publication Date: 09-Jul-1996
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaced By: ASTM D5987-96(2002) - Standard Test Method for Total Fluorine in Coal and Coke by Pyrohydrolytic Extraction and Ion Selective Electrode or Ion Chromatograph Methods
• Effective Date: 10-Jul-1996

Standards Content (Sample)

Designation: D 5987 – 96
Standard Test Method for
Total Fluorine in Coal and Coke by Pyrohydrolytic
Extraction and Ion Selective Electrode or Ion
1
Chromatograph Methods
This standard is issued under the fixed designation D 5987; 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.
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1. Scope 2.2 Australian Standard:
AS 1038.10.4 Determination of Trace Elements—Coal,
1.1 This test method covers the analysis of total fluorine in
Coke and Fly-Ash-Determination of Fluorine Content—
coal and coke.
Pyrohydrolysis Method
1.2 This analysis was successfully tested on coals contain-
2
ing 37 % ash or less (see AS 1038.10.4 and Conrad ).
3. Summary of Test Method
1.3 The values stated in SI units shall be regarded as
3.1 Total fluorine is determined in this test method by first
standard. The values given in parentheses are for information
subjecting the weighed test portion to pyrohydrolytic condi-
only.
tions which separate fluorine from the coal/coke matrix. The
1.4 This standard does not purport to address all of the
pyrohydrolysate is then gravimetrically processed and final
safety concerns, if any, associated with its use. It is the
determinations are made by either ion-selective electrode or
responsibility of the user of this standard to establish appro-
ion chromatographic techniques.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
4. Significance and Use
statements see Note 3 and Note 5.
4.1 This test method permits measurement of the fluorine
1.5 All accountability and quality control aspects of Guide
content of coal and coke for the evaluation of potential fluorine
D 4621 apply to this test method.
emission from coal combustion or conversion processes. When
coal samples are combusted in accordance with this test
2. Referenced Documents
method, the fluorine is quantitatively released from the coal
2.1 ASTM Standards:
and retained in the pyrohydrolysate so that it is representative
D 346 Practice for Collection and Preparation of Coke
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of the total fluorine concentration in coal.
Samples for Laboratory Analysis
4
D 1193 Specification for Reagent Water
5. Apparatus
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D 2013 Method for Preparing Coal Samples for Analysis
3 5.1 Laboratory Ware—Except as noted, all laboratory ware,
D 2234 Methods for Collection of a Gross Sample of Coal
for example, volumetric flasks, beakers, bottles, etc., used for
D 3173 Test Method for Moisture in the Analysis Sample of
3 solutions containing fluoride ions must be made of polyethyl-
Coal and Coke
ene, polystyrene, or a heat-resistant polymer such as polypro-
D 3180 Practice for Calculating Coal and Coke Analyses
pylene.
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from As-Determined to Different Bases
5.2 Vials—Glass or polystyrene, 10 to 30-mL capacity with
D 4621 Guide for Accountability and Quality Control in the
tightly fitting snap-on plastic lids.
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Coal Analysis Laboratory
5.3 Bottles—Polypropylene, 125-mL capacity, wide-mouth,
D 5142 Test Methods for the Proximate Analysis of the
with liner-less leakproof polyethylene screw cap, for tube-
Analysis Sample of Coal or Coke by Instrumental Proce-
3 furnace pyrohydrolysate processing.
dures
5.4 Vials—Polystyrene, 70-mL capacity, with liner-less
leakproof polyethylene screw cap.
5.5 Dispensing Bottles—Polyethylene, 250-mL capacity, for
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the standard fluorine solution (6.3.1) and of 600-mL capacity
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
for the absorption solution (6.3.3) and buffer (6.3.5).
Ash and Trace Elements of Coal.
5.6 Micropipettes—Polypropylene or other suitable poly-
Current edition approved July 10, 1996. Published September 1996.
2 mer, variable volumes ranging from 0.1 mL to at least 2.0 mL.
Conrad, V. B., and Brownlee, W. D., “Hydropyrolytic—Ion Chromatographic
Determination of Fluoride in Coal and Geological Materials,” Analytical Chemistry,
Vol 60, No. 4, 1988, pp. 365–369.
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Annual Book of ASTM Standards, Vol 05.05. Available from American National Standards Institute, 11 W. 42nd St., 13th
4
Annual Book of ASTM Standards, Vol 11.01. Floor, New York, NY 10036.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 5987
not have adequate thermal stress characteristics for operation with this test
This is a satisfactory alternative to the 250-mL dispensing
method.
bottle (5.5), for the delivery of small volumes of the standard
fluorine solution.
5.9.1.2 Silicone Stoppers—20 mm in diameter, positioned at
5.7 Glass Dropper Bottle—30-mL capacity for dispensing
inlet end and outlet, if applicable, of silica combustion tube
glacial
...