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ASTM D3684-01

(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

Replaces
ASTM D3684-94(2000) - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method
Effective Date
10-Oct-2001
Replaced By
ASTM D3684-01(2006) - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method (Withdrawn 2014)
Effective Date
01-Apr-2006
Referred By
ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
Effective Date
10-Oct-2001
Referred By
ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
Effective Date
10-Oct-2001

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ASTM D3684-01 - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption MethodASTM D3684-01 - Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method
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ASTM D3684-01 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 3684 – 01
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 (e) indicates an editorial change since the last revision or reapproval.
NOTE 1—Mercury and mercury salts can be volatilized at low tempera-
1. Scope
tures. Precautions against inadvertent mercury loss should be taken when
1.1 This test method describes a procedure for the analysis
using this method.
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
alloy.
3. Summary of Test Method
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
into a reduction vessel with dilute nitric acid, and the mercury
current is required for ignition purposes with an ammeter or
is determined by the flameless cold vapor atomic absorption
pilot light in the circuit to indicate when current is flowing. A
technique.
stepdown transformer connected to an alternating current
lighting circuit or batteries may be used. The ignition circuit
switch shall be of the momentary double-contact type, nor-
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
mally open, except when held closed by the operator. The
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
switchshouldbedepressedonlylongenoughtofirethecharge.
Current edition approved October 10, 2001. Published December 2001. Origi-
5.6 Analytical Balance, with a sensitivity of 0.1 mg.
nally published as D 3684 – 78. Last previous edition D 3684 – 94 (2000).
2
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3684–01
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 re
...

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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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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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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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