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ASTM D2361-95(2001)

(Test Method)

Standard Test Method for Chlorine in Coal

Standard Test Method for Chlorine in Coal

SCOPE
1.1 This test method pertains to the determination of total chlorine content in a coal sample.
1.2 The values stated in SI units are regarded as the standard. The values shown in parentheses are for information only.
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.  For specific hazard statements, see Note 2 and Section 8.

General Information

Status
Historical
Publication Date
31-Dec-2000
ICS
75.160.10 - Solid fuels
Technical Committee
D05 - Coal and Coke
Drafting Committee
D05.21 - Methods of Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D2361-95 - Standard Test Method for Chlorine in Coal
Effective Date
01-Jan-2001
Replaced By
ASTM D2361-02 - Standard Test Method for Chlorine in Coal (Withdrawn 2008)
Effective Date
10-Sep-2002
Referred By
ASTM D6700-19 - Standard Guide for Use of Scrap Tires as Tire-Derived Fuel
Effective Date
01-Jan-2001

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ASTM D2361-95(2001) - Standard Test Method for Chlorine in Coal
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 2361 – 95 (Reapproved 2001)
Standard Test Method for
Chlorine in Coal
This standard is issued under the fixed designation D 2361; 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 4.2 The chlorides contained in the ammonium carbonate
solution noted in 4.1.1 or extracted from the incinerated Eschka
1.1 This test method pertains to the determination of total
mixture noted in 4.1.2 are determined by potentiometric
chlorine content in a coal sample.
titration.
1.2 The values stated in SI units are regarded as the
standard. The values shown in parentheses are for information
5. Significance and Use
only.
5.1 The purpose of this test method is to measure the total
1.3 This standard does not purport to address all of the
chlorine content of coal. The chlorine content of coals may be
safety concerns, if any, associated with its use. It is the
useful in the evaluation of slagging problems, corrosion in
responsibility of the user of this standard to establish appro-
engineering processes, and in the total analysis of coal and
priate safety and health practices and determine the applica-
coke. When coal specimens are combusted in accordance with
bility of regulatory limitations prior to use. For specific hazard
this test method, the chlorine is quantitatively retained and is
statements, see Note 2 and Section 8.
representative of the total chlorine content of the whole coal.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
2 6.1 Balance, analytical, with a sensitivity of 0.1 mg.
D 121 Terminology of Coal and Coke
3 6.2 Apparatus for Bomb Combustion of the Specimen:
D 1193 Specification for Reagent Water
6.2.1 Combustion Bomb, constructed of materials that are
D 2013 Test Method of Preparing Coal Samples for Analy-
2 not affected by the combustion process or products. The bomb
sis
shall be designed so that all liquid combustion products can be
E 144 Practice for Safe Use of Oxygen Combustion
4 completely recovered by washing the inner surfaces. There
Bombs
shall be no gas leakage during a test. The bomb shall be
E 832 Specification for Laboratory Filter Paper
capable of withstanding a hydrostatic pressure test of 20 MPa
3. Terminology (300 psig) at room temperature without stressing any part
beyond its elastic limit.
3.1 For definitions of terms used in this test method, refer to
6.2.2 Combustion Crucible—An open crucible of platinum,
Terminology D 121.
quartz, or acceptable base-metal alloy. Base-metal alloy cru-
4. Summary of Test Method
cibles are acceptable, if after a few preliminary firings, the
weight does not change significantly between tests.
4.1 The specimen is oxidized by combustion and the con-
tained chlorine is absorbed in alkaline reagents using one of the
NOTE 1—Stable crucible weight may be obtained by heat treating
following two procedures:
base-metal crucibles in a muffle furnace for4hata temperature of 500°C.
4.1.1 A weighed specimen is burned in a combustion bomb
6.2.3 Ignition Wire, nickel-chromium (Chromel C) alloy or
containing oxygen under pressure and a small amount of
iron, 100 mm length, 0.16-mm diameter (No. 34 B&S gage).
ammonium carbonate solution.
Platinum or palladium wire, 0.10-mm diameter (No. 38 B&S
4.1.2 A weighed specimen is mixed with Eschka mixture
gage), may be used.
and heated at a specified temperature in an oxidizing atmo-
6.2.4 Ignition Circuit, for ignition purposes, capable of
sphere.
providing 6 to 16-V ac or dc to the ignition wire. The ignition
circuit shall be controlled with a momentary switch to avoid
This test method is under the jurisdiction of ASTM Committee D05 on Coal
electrical shock to the operator. An ammeter or pilot light is
Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
required in the circuit to indicate when current is flowing. A
Analysis.
step-down transformer, connected to an ac lighting circuit or
Current edition approved Sept. 10, 1995. Published November 1995. Originally
batteries, may be used.
published as D 2361 – 65 T. Last previous edition D 2361 – 91.
Annual Book of ASTM Standards, Vol 05.05.
6.2.5 Water Bath—A container large enough to hold the
Annual Book of ASTM Standards, Vol 11.01.
combustion bomb with enough cooling water to cover the
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.
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 2361
bomb and dissipate the heat generated during the combustion 8.1.2 Inspect the bomb parts carefully after each use.
process. The container shall be designed to allow a constant Frequently check the threads on the main closure for wear.
flow of water around the combustion bomb. Replace the cracked or significantly worn parts. Return the
6.3 Apparatus for Eschka Combustion of Specimen: bomb to the manufacturer occasionally for inspection and
6.3.1 Crucibles, porcelain, 30-mL capacity, high or low- proof testing.
form, or platinum or silica crucibles of similar size, for igniting 8.1.3 The oxygen supply cylinder should be equipped with
the specimen with the Eschka mixture. an approved type of safety device, such as reducing valve, in
6.3.2 Muffle Furnace, electrically heated, capable of main- addition to the needle valve and pressure gage used in
taining a uniform hot zone at 675 6 25°C, and with good regulating the oxygen feed to the bomb. Valves, gages, and
circulation of air. gaskets shall meet industry safety code. Check the pressure
6.4 Apparatus for Potentiometric Titration: gage periodically for accuracy.
6.4.1 Potentiometric Titration Assembly, using silver and 8.1.4 During ignition of a specimen, the operator shall not
silver-silver chloride electrodes. permit any portion of his body to extend over the combustion
bomb or its container.
7. Reagents
8.1.5 Exercise extreme caution when combustion aids are
7.1 Purity of Reagents—Reagent grade chemicals conform- employed so as not to exceed the bomb manufacturer’s
ing to the specifications of the Committee on Analytical
recommendations and to avoid damage to the bomb.
Reagents of the American Chemical Society shall be used in all 8.1.6 Admit oxygen slowly into the bomb to avoid blowing
tests.
powdered material from the crucible.
7.2 Purity of Water—Unless otherwise indicated, references 8.1.7 Do not fire the bomb if it has been filled to greater than
to water shall be understood to mean reagent water conforming 3-MPa (30 atm) pressure with oxygen, if the bomb has been
to Type II of Specification D 1193. dropped or turned over after loading, or if there is evidence of
a gas leak when the bomb is submerged in the water bath.
NOTE 2—Warning: Some reagents used in this test method are hazard-
ous. Follow the precautions listed in the Material Safety Data Sheet of the
9. Sample
manufacturer for each reagent.
9.1 The sample shall be the material pulverized to pass a
7.3 Ammonium Carbonate Solution—Dissolve 10 g of am-
250-μm (No. 60) sieve in accordance with Method D 2013.
monium carbonate ((NH ) CO ·H O) in 100 mL of water. Use
4 2 3 2
only a freshly prepared solution.
10. Procedure
7.4 Eschka Mixture—Thoroughly mix two parts by weight
10.1 Procedure for Bomb Combustion Method:
of light calcined magnesium oxide (MgO) with one part of
10.1.1 Thoroughly mix the analysis sample of coal. Care-
anhy
...

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ABSTRACT
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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5.2 The ash prepared in accordance with these provisional test methods quantitatively retains the elements listed in 1.1 and is representative of their mass fractions in the coal or coke.
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1.1 These test methods pertain to the determination of antimony, arsenic, beryllium, cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, vanadium, and zinc in coal and coke. These test methods can also be used for the analysis of residues from coal combustion processes. Additionally, there are specific test methods outlined that pertain to the determination of rare earth elements in coal and coal combustion residues.
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1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.2.1 All percentages are percent mass fractions unless otherwise noted.  
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ASTM D4606-21(Test Method)
Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method

SIGNIFICANCE AND USE
4.1 This test method permits measurement of the total mass fraction of arsenic and selenium in coal for the purpose of evaluating these elements where they can be of concern, for example, in coal combustion. When coal samples are prepared for analysis in accordance with this test method, the arsenic and selenium are quantitatively retained and are representative of the total mass fraction in the coal.
SCOPE
1.1 This test method2 covers the determination of total arsenic in the range of 0.7 ug/g to 12 ug/g and selenium in the range of 0.6 ug/g to 5 ug/g in coal.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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