ASTM D3684-01(2006)
(Test Method)Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method (Withdrawn 2014)
Standard Test Method for Total Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method (Withdrawn 2014)
SIGNIFICANCE AND USE
The possible emission of mercury that may be found in coal from coal combustion is an environmental concern.
When test portions are burned according to this procedure, the total mercury is quantitatively retained and is representative of concentrations in the whole coal.
SCOPE
1.1 This test method describes a procedure for the analysis of total mercury in coal.
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.
1.2 The values stated in SI units (IEEE/ASTM SI 10) shall be regarded as the standard.
WITHDRAWN RATIONALE
This test method describes a procedure for the analysis of total mercury in coal.
Formerly under the jurisdiction of Committee D05 on Coal and Coke, this test method was withdrawn in September 2014. This standard is being withdrawn without replacement due to its limited use by industry.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 01(Reapproved 2006)
Standard Test Method for
Total Mercury in Coal by the Oxygen Bomb
Combustion/Atomic Absorption Method
This standard is issued under the fixed designation D3684; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This test method describes a procedure for the analysis 3.1 Total mercury is determined in this test method by
of total mercury in coal. combusting a weighed sample in an oxygen bomb with dilute
nitric acid absorbing the mercury vapors. The bomb is rinsed
1.2 This standard does not purport to address all of the
into a reduction vessel with dilute nitric acid, and the mercury
safety concerns, if any, associated with its use. It is the
is determined by the flameless cold vapor atomic absorption
responsibility of the user of this standard to establish appro-
technique.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
NOTE 1—Mercury and mercury salts can be volatilized at low tempera-
tionary statements are given in 8.3.1. tures. Precautions against inadvertent mercury loss should be taken when
using this method.
1.3 The values stated in SI units (IEEE/ASTM SI 10) shall
be regarded as the standard.
4. Significance and Use
4.1 The possible emission of mercury that may be found in
2. Referenced Documents
coal from coal combustion is an environmental concern.
2.1 ASTM Standards:
4.2 When test portions are burned according to this
D1193 Specification for Reagent Water
procedure, the total mercury is quantitatively retained and is
D2013 Practice for Preparing Coal Samples for Analysis
representative of concentrations in the whole coal.
D3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke
5. Apparatus
D3180 Practice for Calculating Coal and Coke Analyses
5.1 Combustion Bomb—The combustion bomb shall be
from As-Determined to Different Bases
constructedofmaterialsthatarenotaffectedbythecombustion
D5142 Test Methods for ProximateAnalysis of theAnalysis
process or products. The bomb must be designed so that all
Sample of Coal and Coke by Instrumental Procedures
liquid combustion products can be completely recovered by
(Withdrawn 2010)
washing the inner surfaces. There must be no gas leakage
E144 Practice for Safe Use of Oxygen Combustion Bombs
during the test. The bomb must be capable of withstanding a
IEEE/ASTM SI 10 Standard for Use of International System
hydrostatic pressure test to gage pressure of 20 MPa (approxi-
of Units (SI): The Modern Metric System
mately3000psig)atroomtemperaturewithoutstressinganyof
2.2 ISO Standards
the parts beyond the elastic limit.
ISO 5725-6:1994 Accuracy of measurement methods and
results-Part 6 5.2 Water Bath—A container shall be large enough to hold
the combustion bomb, and enough cooling water shall be used
to dissipate the heat generated during the combustion process.
This test method is under the jurisdiction of ASTM Committee D05 on Coal
The container should be designed to allow a constant flow of
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
water around the combustion bomb.
Elements in Ash and Trace Elements of Coal.
Current edition approved April 1, 2006. Published April 2006. Originally
5.3 Combustion Crucibles—Samples shall be burned in an
approved in 1978. Last previous edition approved in 2001 as D3684 – 01. DOI:
open crucible of platinum, quartz, or acceptable base-metal
10.1520/D3684-01R06.
2 alloy.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.4 Firing Wire, 100 mm of either No. 34 B&S (0.160-mm)
Standards volume information, refer to the standard’s Document Summary page on
nickel-chromium alloy, No. 34 B&S iron, or No. 38 B&S
the ASTM website.
The last approved version of this historical standard is referenced on (0.101-mm) gage platinum wire.
www.astm.org.
5.5 Firing Circuit—A 6- to 16-V alternating or direct
Available from International Organization for Standardization (ISO), 1 rue de
Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland. current is required for ignition purposes with an ammeter or
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3684 − 01 (2006)
pilot light in the circuit to indicate when current is flowing. A 7. Sample
stepdown transformer connected to an alternating current
7.1 Prepare the analysis sample in accordance with Method
lighting circuit or batteries may be used. The ignition circuit
D2013 by pulverizing the material to pass a 250-µm (No. 60)
switch shall be of the momentary double-contact type, nor-
sieve.
mally open, except when held closed by the operator. The
switchshouldbedepressedonlylongenoughtofirethecharge. 7.2 Analyze separate test portions for moisture content in
accordance with Test Methods D3173 or D5142 so that
5.6 Analytical Balance, with a sensitivity of 0.1 mg.
calculation to other bases can be made.
5.7 Atomic Absorption Spectrophotometer, with a flameless
cold-vapor mercury analysis system comprised of either a
8. Procedure for Bomb Combustion
closed recirculating system or an open one-pass system.
8.1 Thoroughly mix the analysis sample of coal in the
5.8 Reduction Vessels, biochemical oxygen demand (BOD)
sample bottle. Weigh a test portion of about 1 g, to the nearest
bottles, 300-mL capacity.
0.0001 g, into a preignited crucible.
6. Reagents
8.2 Transfer10mLofHNO (1+9)tothecombustionbomb,
attach the fuse wire to the bomb electrodes, place the crucible
6.1 Purity of Reagents—Reagent grade chemicals shall be
with sample into the electrode support of the bomb, and adjust
used in all tests. Unless otherwise indicated, it is intended that
the fuse wire to contact only the test portion.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
8.3 Assemble the bomb in conformance with the manufac-
where such specifications are available. Other grades may be
turer’s directions and charge it with oxygen to a pressure
used, provided it is first ascertained that the reagent is of
between 2 to 3 MPa (20 and 30 atm). If the oxygen should
sufficiently high purity to permit its use without lessening the
exceed the specified pressure, stop, detach the filling
accuracy of the determination.
connection, exhaust the bomb in the usual manner, and discard
6.2 Reagent Water—Reagent water, conforming to Type II the test portion.
of Specification D1193, shall be used for preparation of
8.3.1 Warning—The following precautions are recom-
reagents and washings of the bomb interior.
mended for safe oxygen bomb operation. Additional precau-
tions are given in Practice E144.
6.3 Hydroxylamine Hydrochloride Solution (1.5 g/100
8.3.1.1 Theweightofthetestportionandthepressureofthe
mL)—Dissolve 1.5 g of hydroxylamine hydrochloride
oxygen admitted to the bomb must not exceed the bomb
(NH OH·HCl) in water and dilute to 100 mL.
manufacturer’s recommendations.
6.4 Mercury Standard Stock Solution [1000 ppm (1000
8.3.1.2 Inspect the bomb parts carefully after each use.
µg/mL)]—Dissolve 1.080 g of mercury (II) oxide (HgO) in a
Check the bomb for thread wear on any closures; if an
minimum volume of HCl (1+1). Dilute to 1 L with water.
inspection reveals any wear, replace the worn parts or return
6.5 Mercury Standard Solution [0.1 ppm (µg/mL)]—Dilute
the bomb to the factory for testing or replacement of the
0.10 mL of mercury standard stock solution to 1 L with water.
defective parts. It is a good practice to replace the O-rings and
If micropipets are not available, this standard may be prepared
seals, inspect screw cap threads, and hydrostatically test the
by serial dilution of the mercury standard stock solution.
bomb as per the manufacturer’s recommendations.
Prepare the mercury standard solution daily.
8.3.1.3 Equip the oxygen supply cylinder with an approved
6.6 Nitric Acid(1+9)—Dilute100mLofconcentratednitric
type of safety device, such as a reducing valve, in addition to
acid (HNO , sp gr 1.42) to 1 L with water.
3 the needle valve and pressure gage used in regulating the
oxygenfeedtothebomb.Valves,gages,andgasketsmustmeet
6.7 Oxygen—Oxygen shall be free of combustible matter.
industry safety code. Suitable reducing valves and adaptors for
Only oxygen manufactured from liquid air, guaranteed to be
2.0- to 3.4-MPa (300- to 500-psi) discharge pressures are
greater than 99.5 % pure, will meet this requirement.
obtainable from commercial sources of compressed gas equip-
6.8 Potassium Permanganate Solution (5 g/100 mL)—
ment. Check the pressure gage periodically for accuracy.
Dissolve 5 g of potassium permanganate (KMnO ) in water
8.3.1.4 During ignition of a test portion, the operator must
and dilute to 100 mL.
not permit any portion of his body to extend over the oxygen
6.9 Stannous Chloride Solution (10 g/100 mL)—Dissolve
bomb.
10 g of stannous chloride dihydrate (SnCl ·2H O) in 45 mLof
2 2
8.3.1.5 Exercise extreme caution when combustion aids are
concentrated hydrochloric acid (HCl, sp gr 1.19) and cau-
used so as not to exceed the bomb manufacturer’s recommen-
tiously dilute to 100 mL with water.
dations and to avoid damage to the bomb. Do not fire loose
fluffy material such as unpelleted benzoic acid, unless thor-
oug
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