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ASTM D3684-94(2000)

(Test Method)

Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method

Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method

SCOPE
1.1 This test method describes a procedure for the analysis of total mercury 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. Specific precautionary statements are given in 8.3.1.
1.3 The values stated in SI units (IEEE/ASTM SI 10) shall be regarded as the standard.

General Information

Status
Historical
Publication Date
09-Oct-2001
ICS
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

Replaced By
ASTM D3684-01 - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method
Effective Date
10-Oct-2001

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ASTM D3684-94(2000) - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption MethodASTM D3684-94(2000) - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method
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ASTM D3684-94(2000) - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3684–94 (Reapproved 2000)
Standard Test Method for
Total Mercury in Coal by the Oxygen Bomb
1
Combustion/Atomic Absorption Method
This standard is issued under the fixed designation D 3684; 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 (ε) indicates an editorial change since the last revision or reapproval.
1. Scope into a reduction vessel with dilute nitric acid, and the mercury
is determined by the flameless cold vapor atomic absorption
1.1 This test method describes a procedure for the analysis
technique.
of total mercury in coal.
1.2 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 The possible emission of mercury that may be found in
responsibility of the user of this standard to establish appro-
coal from coal combustion is an environmental concern.
priate safety and health practices and determine the applica-
4.2 When test portions are burned according to this proce-
bility of regulatory limitations prior to use. Specific precau-
dure, the total mercury is quantitatively retained and is repre-
tionary statements are given in 8.3.1.
sentative of concentrations in the whole coal.
1.3 The values stated in SI units (IEEE/ASTM SI 10) shall
be regarded as the standard. 5. Apparatus
5.1 Combustion Bomb—The combustion bomb shall be
2. Referenced Documents
constructedofmaterialsthatarenotaffectedbythecombustion
2.1 ASTM Standards:
process or products. The bomb must be designed so that all
2
D 1193 Specification for Reagent Water
liquid combustion products can be completely recovered by
3
D 2013 Method of Preparing Coal Samples for Analysis
washing the inner surfaces. There must be no gas leakage
D 3173 Test Method for Moisture in theAnalysis Sample of
during the test. The bomb must be capable of withstanding a
3
Coal and Coke
hydrostatic pressure test to gage pressure of 20 MPa (approxi-
D 3180 Practice for Calculating Coal and Coke Analyses
mately3000psig)atroomtemperaturewithoutstressinganyof
3
from As-Determined to Different Bases
the parts beyond the elastic limit.
D 5142 Test Methods for the Proximate Analysis of the
5.2 Water Bath—A container shall be large enough to hold
Analysis Sample of Coal and Coke by Instrumental
the combustion bomb, and enough cooling water shall be used
3
Procedures
to dissipate the heat generated during the combustion process.
E 144 Practice for Safe Use of Oxygen Combustion
The container should be designed to allow a constant flow of
4
Bombs
water around the combustion bomb.
IEEE/ASTM SI 10 Standard for Use of International Sys-
5.3 Combustion Crucibles—Samples shall be burned in an
4
tem of Units (SI): The Modern Metric System
open crucible of platinum, quartz, or acceptable base-metal
3. Summary of Test Method alloy.
5.4 Firing Wire, 100 mm of either No. 34 B&S (0.160-mm)
3.1 Total mercury is determined in this test method by
nickel-chromium alloy, No. 34 B&S iron, or No. 38 B&S
combusting a weighed sample in an oxygen bomb with dilute
(0.101-mm) gage platinum wire.
nitric acid absorbing the mercury vapors. The bomb is rinsed
5.5 Firing Circuit—A 6- to 16-V alternating or direct
current is required for ignition purposes with an ammeter or
pilot light in the circuit to indicate when current is flowing. A
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
stepdown transformer connected to an alternating current
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
lighting circuit or batteries may be used. The ignition circuit
Elements in Ash and Trace Elements of Coal.
Current edition approved March 15, 1994. Published May 1994. Originally
switch shall be of the momentary double-contact type, nor-
published as D 3684 – 78. Last previous edition D 3684 – 78 (1988).
mally open, except when held closed by the operator. The
2
Annual Book of ASTM Standards, Vol 11.01.
3
switchshouldbedepressedonlylongenoughtofirethecharge.
Annual Book of ASTM Standards, Vol 05.06.
4
Annual Book of ASTM Standards, Vol 14.04. 5.6 Analytical Balance, with a sensitivity of 0.1 mg.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3684–94 (2000)
5.7 Atomic Absorption Spectrophotometer, with a flameless 8. Procedure for Bomb Combustion
cold-vapor mercury analysis system comprised of either a
8.1 Thoroughly mix the analysis sample of coal in the
closed recirculating system or an open one-pass system.
sample bottle. Weigh a test portion of about 1 g, to the nearest
5.8 Reduction Vessels, biochemical o
...

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4.1 Coke undergoes various degrees of degradation during removal from coke ovens, transportation, and its decent within a blast furnace to the combustion zone. These processes subject the coke to impact and abrasion. This test method is a relative measure of the resistance of coke to breakage when subjected to these degradation processes.
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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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1.3 While it is recognized that such a standard may be unwieldy for routine usage in commercial operations, it can provide a common base for agreement in cases of dispute or arbitration. The complete standard is referred to as the referee method. Embodied in the standard is the commercial method starting with the crushed and divided sample when the gross sample is not too wet to crush and divide. See Practice D2961/D2961M and Test Method D3173 for other moisture methods.  
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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.
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5.1 A compositional analysis of ash is used in describing the quality of coal for its complete characterization. Ash composition is useful in predicting slagging and fouling characteristics of combusted materials as well as the potential utilization of ash by-products.  
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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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1.1 This test method covers a procedure for the analysis of the commonly determined major and minor elements in coal, coke, and solid residues from combustion of coal and coke. These residues may be laboratory ash, bottom ash, fly ash, flue gas desulfurization sludge, and other combustion process residues.
Note 1: There are two interlaboratory studies associated with this test method. The first was conducted in 1997 ( RR:D05-1035)2 and the second was conducted in 2007 ( RR:D05-1032).3 Sulfur trioxide was only included in the 2007 study, and that study only included combustion residues derived from ash and no combustion residues derived from coke.  
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.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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