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ASTM D4208-02

(Test Method)

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

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

SCOPE
1.1 This test method covers the analysis of total chlorine in coal.
1.2 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.

General Information

Status
Historical
Publication Date
09-Sep-2002
ICS
75.160.10 - Solid fuels
Technical Committee
D05 - Coal and Coke
Drafting Committee
D05.21 - Methods of Analysis
Current Stage
Ref Project

Relations

Replaced By
ASTM D4208-02e1 - Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
Effective Date
10-Sep-2002

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ASTM D4208-02 - Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode MethodASTM D4208-02 - Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
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ASTM D4208-02 - Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4208–02
Standard Test Method for
Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion
1
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 (ε) indicates an editorial change since the last revision or reapproval.
1. Scope engineering processes, and in the total analysis of coal and
coke. When coal samples are combusted in accordance with
1.1 This test method covers the analysis of total chlorine in
this method, the chlorine is quantitatively retained and is
coal.
representative of the total chlorine content of the whole coal.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Combustion Bomb, constructed of materials that are not
priate safety and health practices and determine the applica-
affected by the combustion process or products. The bomb
bility of regulatory limitations prior to use.
must be designed so that all liquid combustion products can be
2. Referenced Documents quantitatively recovered by washing the inner surfaces. There
must be no gas leakage during the test. The bomb must be
2.1 ASTM Standards:
2
capableofwithstandingahydrostatic-pressuretestto3000psig
D1193 Specification for Reagent Water
(approximately20MPa)atroomtemperaturewithoutstressing
D3173 TestMethodforMoistureintheAnalysisSampleof
3
any part beyond its elastic limit.
Coal and Coke
5.2 Water Bath—A container large enough to hold the
D3180 Practice for Calculating Coal and Coke Analysis
3
combustion bomb and enough cooling water to dissipate the
from As-Determined to Different Bases
heat generated during the combustion process. The container
E 144 Practice for Safe Use of Oxygen Combustion
4
shall be designed to allow a constant flow of water around the
Bombs
combustion bomb.
E691 Practice for Conducting an Interlaboratory Study to
5
5.3 Combustion Crucibles—Samples shall be burned in an
Determine the Precision of a Test Method
open crucible of platinum, quartz, or acceptable base-metal
3. Summary of Test Method
alloy.
3.1 Total chlorine is determined in this method by combus- 5.4 Firing Wire, 100-mm, nickel-chromium alloy, No. 34B
& S gage, or platinum, No. 34 or No. 38B & S gage.
ting a weighed sample in an oxygen bomb with dilute base
adsorbingthechlorinevapors.Thebombisrinsedintoabeaker 5.5 Firing Circuit—A6to16-Valternatingordirectcurrent
is required for ignition purposes with an ammeter or pilot light
with water and following the addition of an ionic strength
adjuster, the chloride is determined by ion-selective electrode. in the circuit to indicate when current is flowing.Astep-down
transformer connected to an alternating-current lighting circuit
4. Significance and Use
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
useful in the evaluation of slagging problems, corrosion in
switch should be depressed only long enough to fire the
charge.)
5.6 Balance, analytical, with a sensitivity of 0.1 mg.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
5.7 Specific-Ion Meter—A pH meter with an expandable
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
millivolt scale, specific-ion meter, sensitive to 0.1 mV, suitable
Current edition approved September 10, 2002. Published October 2002. Origi- 6
for method of standard addition determinations.
nally published as D4208–82. Last previous edition D4208–88 (2002).
2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 05.06.
4 6
Annual Book of ASTM Standards, Vol 14.04. Midgley, D., and Torrance, K., Potentiometric Water Analysis, John Wiley and
5
Annual Book of ASTM Standards, Vol 14.02. Sons, 1978.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4208–02
5.8 Electrodes, chloride-sensing, with the appropriate If the oxygen should exceed the specified pressure, do not
reference-typeelectrodeasrecommendedbythemanufacturer. proceed with the combustion. In this case, detach the filling
connection, exhaust the bomb in the usual manner, and discard
6. Reagents
the sample. (Warning—The following precautions are recom-
6.1 Purity of Reagents—Reagent grade chemicals shall
...

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This specification covers the classification of coals by rank, that is, according to their degree of metamorphism, or progressive alteration, in the natural series from lignite to anthracite. These coals are mainly composed of vitrinite. The classification shall be based on gradational properties that depend on the degree of metamorphism. The classification shall also be according to fixed carbon and gross calorific value calculated to the mineral-matter-free basis.
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Note 1: Coals rich in inertinite or liptinite (exinite), or both, cannot be properly classified because, in those macerals, the properties that determine rank (calorific value, volatile matter, and agglomerating character) differ greatly from those of vitrinite in the same coal. Often, such coals can be recognized by megascopic examination. In North America, these coals are mostly nonbanded varieties that contain only a small proportion of vitrain and consist mainly of attrital materials. The degree of metamorphism of nonbanded and other vitrinite-poor coals can be estimated by determining the classification properties of isolated or concentrated vitrinite fractions, or by determining the reflectance of the vitrinite (see Test Method D2798 and Appendix X1 of this classification). However, in the use of these vitrinite-poor coals, some properties normally associated with rank, such as rheology, combustibility, hardness, and grindability (as well as the rank determining properties) may differ substantially from those of vitrinite-rich coals of the same degree of metamorphism.  
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5.1 Reliable values of the plastic properties of coals are used to predict or explain the behavior of a coal or blends during carbonization or in other processes such as gasification, liquefaction, and combustion.
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Standard Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of Coal and Coke by Inductively Coupled Plasma—Atomic Emission Spectrometry

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5.1 A compositional analysis of coal and coke and their associated combustion residues are often useful in assessing their quality. Knowledge of the elemental composition of the associated residues is also useful in predicting the elemental enrichment/depletion compositional behavior of ashes and slags in comparison to the mass fraction in the parent coal. Utilization of the ash by-products and hazardous potential may also depend on the chemical composition and leachability of the inorganic constituents of the coal ash.  
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