ASTM D4208-02e1

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Designation:D4208–02
Standard Test Method for
Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion
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Selective Electrode Method
This standard is issued under the fixed designation D4208; 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 (e) indicates an editorial change since the last revision or reapproval.
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e NOTE—Section 12.2 was editorially moved into footnote 8 in June 2004.
1. Scope useful in the evaluation of slagging problems, corrosion in
engineering processes, and in the total analysis of coal and
1.1 This test method covers the analysis of total chlorine in
coke. When coal samples are combusted in accordance with
coal.
this method, the chlorine is quantitatively retained and is
1.2 This standard does not purport to address all of the
representative of the total chlorine content of the whole coal.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Combustion Bomb, constructed of materials that are not
bility of regulatory limitations prior to use.
affected by the combustion process or products. The bomb
2. Referenced Documents must be designed so that all liquid combustion products can be
quantitatively recovered by washing the inner surfaces. There
2.1 ASTM Standards:
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must be no gas leakage during the test. The bomb must be
D1193 Specification for Reagent Water
capableofwithstandingahydrostatic-pressuretestto3000psig
D3173 TestMethodforMoistureintheAnalysisSampleof
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(approximately20MPa)atroomtemperaturewithoutstressing
Coal and Coke
any part beyond its elastic limit.
D3180 Practice for Calculating Coal and Coke Analysis
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5.2 Water Bath—A container large enough to hold the
from As-Determined to Different Bases
combustion bomb and enough cooling water to dissipate the
E 144 Practice for Safe Use of Oxygen Combustion
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heat generated during the combustion process. The container
Bombs
shall be designed to allow a constant flow of water around the
E691 Practice for Conducting an Interlaboratory Study to
5 combustion bomb.
Determine the Precision of a Test Method
5.3 Combustion Crucibles—Samples shall be burned in an
3. Summary of Test Method open crucible of platinum, quartz, or acceptable base-metal
alloy.
3.1 Total chlorine is determined in this method by combus-
5.4 Firing Wire, 100-mm, nickel-chromium alloy, No. 34B
ting a weighed sample in an oxygen bomb with dilute base
& S gage, or platinum, No. 34 or No. 38B & S gage.
adsorbingthechlorinevapors.Thebombisrinsedintoabeaker
5.5 Firing Circuit—A6to16-Valternatingordirectcurrent
with water and following the addition of an ionic strength
is required for ignition purposes with an ammeter or pilot light
adjuster, the chloride is determined by ion-selective electrode.
in the circuit to indicate when current is flowing.Astep-down
4. Significance and Use
transformer connected to an alternating-current lighting circuit
or batteries can be used. (Warning—The ignition circuit
4.1 The purpose of this test method is to measure the total
switch shall be of the momentary double-contact type, nor-
chlorine content of coal. The chlorine content of coals may be
mally open, except when held closed by the operator. The
switch should be depressed only long enough to fire the
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This test method is under the jurisdiction of ASTM Committee D05 on Coal
charge.)
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
5.6 Balance, analytical, with a sensitivity of 0.1 mg.
Analysis.
Current edition approved September 10, 2002. Published October 2002. Origi-
nally published as D4208–82. Last previous edition D4208–88 (2002).
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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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Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4208–02
5.7 Specific-Ion Meter—A pH meter with an expandable the bomb, and insert the fuse wire so that it just touches the
millivolt scale, specific-ion meter, sensitive to 0.1 mV, suitable surface of the sample.
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for method of standard addition determinations. 8.3 Assemble the bomb in the normal manner and charge it
5.8 Electrodes, chloride-sensing, with the appropriate withoxygentoapressurebetween20and30atm(2to3MPa).
reference-typeelectrodeasrecommendedbythemanufacturer. If the oxygen should exceed the specified pressure, do not
proceed with the combustion. In this case, detach the filling
6.
...