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ASTM D3761-96(2002)

(Test Method)

Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method

Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method

SIGNIFICANCE AND USE
This test method permits measurement of the fluorine content of coal for the evaluation of potential fluorine emission from coal combustion or conversion processes. When coal samples are combusted in accordance with this test method, the fluorine is quantitatively retained and is representative of the total fluorine concentration in whole coal.
SCOPE
1.1 This test method covers the analysis of total fluorine in coal.
1.2 This test method was successfully tested on coals containing 25 % ash or less.
1.3 The values stated in SI units are to be regarded as the 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. For specific hazard statements, see Section 7.
1.5 All accountability and quality control aspects of Guide D 4621 apply to this test method.

General Information

Status
Historical
Publication Date
09-Apr-1996
ICS
73.040 - Coals
75.160.10 - Solid fuels
Technical Committee
D05 - Coal and Coke
Drafting Committee
D05.29 - Major Elements in Ash and Trace Elements of Coal
Current Stage
Ref Project

Relations

Replaces
ASTM D3761-96 - Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
Effective Date
10-Apr-1996
Replaced By
ASTM D3761-10 - Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method (Withdrawn 2019)
Effective Date
01-Dec-2010
Referred By
ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
Effective Date
10-Apr-1996
Referred By
ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
Effective Date
10-Apr-1996

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ASTM D3761-96(2002) - Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode MethodASTM D3761-96(2002) - Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
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ASTM D3761-96(2002) - Standard Test Method for Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
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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:D3761–96 (Reapproved 2002)
Standard Test Method for
Total Fluorine in Coal by the Oxygen Bomb Combustion/Ion
1
Selective Electrode Method
This standard is issued under the fixed designation D3761; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope E144 Practice for Safe Use of Oxygen Combustion Bombs
1.1 This test method covers the analysis of total fluorine in
3. Summary of Test Method
coal.
3.1 Total fluorine is determined in this test method by
1.2 This test method was successfully tested on coals
2 combustingaweighedsampleinanoxygenbombwithadilute
containing 25% ash or less.
base absorbing the fluorine vapors. The bomb is rinsed into a
1.3 The values stated in SI units are to be regarded as the
beakerwithwaterandfollowingtheadditionofacitratebuffer,
standard. The values given in parentheses are for information
the fluorine is determined by ion-selective electrode.
only.
1.4 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 This test method permits measurement of the fluorine
responsibility of the user of this standard to establish appro-
contentofcoalfortheevaluationofpotentialfluorineemission
priate safety and health practices and determine the applica-
from coal combustion or conversion processes. When coal
bility of regulatory limitations prior to use. For specific hazard
samplesarecombustedinaccordancewiththistestmethod,the
statements, see Section 7.
fluorine is quantitatively retained and is representative of the
1.5 All accountability and quality control aspects of Guide
total fluorine concentration in whole coal.
D4621 apply to this test method.
5. Apparatus
2. Referenced Documents
3 5.1 Combustion Bomb, constructed of materials that are not
2.1 ASTM Standards:
affected by the combustion process or products. The bomb
4
D1193 Specification for Reagent Water
4 must be designed so that all liquid combustion products can be
D2013 Practice for Preparing Coal Samples for Analysis
quantitatively recovered by washing the inner surfaces. There
D3173 Test Method for Moisture in theAnalysis Sample of
4 must be no gas leakage during the test. The bomb must be
Coal and Coke
capable of withstanding a hydrostatic-pressure test to 20 MPa
D3180 Practice for Calculating Coal and Coke Analyses
4 (approximately 3000 psig) at room temperature without stress-
from As-Determined to Different Bases
ing any part beyond its elastic limit.
D4621 Guide for Quality Management in an Organization
4 5.2 Water Bath—A container large enough to hold the
That Samples or Tests Coal and Coke
combustion bomb and enough cooling water to dissipate the
D5142 TestMethodsforProximateAnalysisoftheAnalysis
5 heat generated during the combustion process. The container
Sample of Coal and Coke by Instrumental Procedures
shall be designed to allow a constant flow of water around the
combustion bomb.
5.3 Sample Holder—Samples shall be burned in an open
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
crucible of platinum, quartz, or acceptable base metal alloy.
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal. Base-metal alloy crucibles are acceptable if after a few
Current edition approved April 10, 2002. Published June 1996. Originally
preliminary firings the weight does not change significantly
published as D3761–79. Last previous edition D3761–96. DOI: 10.1520/D3761-
between tests.
96R02.
2
5.4 Ignition Wire, 100-mm, nickel-chromium alloy, No. 34
This standard is based on a published report by Thomas, J., Jr., and Gluskoter,
H.J.,“DeterminationofFluorideinCoalwiththeFluorideIon-SpecificElectrode,”
B & S gage, or platinum, No. 34 or No. 38B&S gage.
Analytical Chemistry, Vol 46, 1974, pp. 1321–23.
5.5 Ignition Circuit—A6 to 16-V alternating or direct cur-
3
Annual Book of ASTM Standards, Vol 11.01.
4
rent is required for ignition purposes with an ammeter or pilot
Annual Book of ASTM Standards, Vol 05.06.
5
Annual Book of ASTM Standards, Vol 14.04. light in the circuit to indicate when current is flowing. A
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3761–96 (2002)
step-down transformer connected to an alternating-current 7. Hazards
lighting circuit or batteries may be used.
7.1 Precautions—The following precautions are recom-
5.6 Balance, anal
...

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