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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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
D 1193 Specification for Reagent Water
liquid combustion products can be completely recovered by
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
Coal and Coke
hydrostatic pressure test to gage pressure of 20 MPa (approxi-
D 3180 Practice for Calculating Coal and Coke Analyses
mately3000psig)atroomtemperaturewithoutstressinganyof
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
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
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
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
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
Annual Book of ASTM Standards, Vol 11.01.
switchshouldbedepressedonlylongenoughtofirethecharge.
Annual Book of ASTM Standards, Vol 05.06.
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.
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 oxygen demand (BOD)
0.0001 g, into a preignited crucible.
bottles, 300-mL capacity.
8.2 Transfer 10 mLof HNO (1+9) to the combustion bomb,
attach the fuse wire to the bomb electrodes, place the crucible
6. Reagents
with sample into the electrode support of the bomb, and adjust
the fuse wire to contact only the test portion.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 8.3 Assemble the bomb in conformance with the manufac-
all reagents shall conform to the specifications of the Commit-
turer’s directions and charge it with oxygen to a pressure
tee onAnalytical Reagents of theAmerican Chemical Society, between 2 to 3 MPa (20 and 30 atm). If the oxygen should
where such specifications are available. Other grades may be
exceed the specified pressure, stop, detach the filling connec-
used, provided it is first ascertained that the reagent is of
tion,exhaustthebombintheusualmanner,anddiscardthetest
sufficiently high purity to permit its use without lessening the
portion.
accuracy of the determination.
8.3.1 Warning—The following precautions are recom-
6.2 Reagent Water—Reagent water, conforming to Type II
mended for safe oxygen bomb operation. Additional precau-
of Specification D 1193, shall be used for preparation of tions are given in Practice E 144.
reagents and washings of the bomb interior.
8.3.1.1 Theweightofthetestportionandthepressureofthe
6.3 Hydroxylamine Hydrochloride Solution (1.5 g/100
oxygen admitted to the bomb must not exceed the bomb
mL)—Dissolve 1.5 g of hydroxylamine hydrochloride manufacturer’s recommendations.
(NH OH·HCl) in water and dilute to 100 mL.
2 8.3.1.2 Inspect the bomb parts carefully after each use.
6.4 Mercury Standard Stock Solution [1000 ppm (1000
Check the bomb for thread wear on any closures; if an
µg/mL)]—Dissolve 1.080 g of mercury (II) oxide (HgO) in a inspection reveals any wear, replace the worn parts or return
minimum volume of HCl (1+1). Dilute to 1 L with water.
the bomb to the factory for testing or replacement of the
defective parts. It is a good practice to replace the O-rings and
6.5 Mercury Standard Solution [0.1 ppm (µg/mL)]—Dilute
seals, inspect screw cap threads, and hydrostatically test the
0.10 mL of mercury standard stock solution to 1 L with water.
bomb as per the manufacturer’s recommendations.
If micropipets are not available, this standard may be prepared
by serial dilution of the mercury standard stock solution. 8.3.1.3 Equip the oxygen supply cylinder with an approved
Prepare the mercury standard solution daily. type of safety device, such as a reducing valve, in addition to
the needle valve and pressure gage used in regulating the
6.6 Nitric Acid (1+9)—Dilute 100 mL of concentrated
oxygenfeedtothebomb.Valves,gages,andgasketsmustmeet
nitric acid (HNO , sp gr 1.42) to 1 L with water.
industry safety code. Suitable reducing valves and adaptors for
6.7 Oxygen—Oxygen shall be free of combustible
...

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5.1 Coal contains several elements whose individual mass fractions are generally less than 0.01 %. These elements are commonly and collectively referred to as trace elements. These elements primarily occur as part of the mineral matter in coal. The potential release of certain trace elements from coal combustion sources has become an environmental concern.  
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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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Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method

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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.
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.  
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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