ASTM D6414-01
(Test Method)Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Acid Extraction or Wet Oxidation/Cold Vapor Atomic Absorption
Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Acid Extraction or Wet Oxidation/Cold Vapor Atomic Absorption
SCOPE
1.1 These test methods cover procedures to determine the total mercury content in a sample of coal or coal combustion residue.
1.2 The values stated in SI units are regarded as the 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D 6414 – 01
Standard Test Methods for
Total Mercury in Coal and Coal Combustion Residues by
Acid Extraction or Wet Oxidation/Cold Vapor Atomic
1
Absorption
This standard is issued under the fixed designation D 6414; 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 ture in a mixture of nitric and hydrochloric acids. The acid
solutions produced are transferred into a vessel in which the
1.1 These test methods cover procedures to determine the
mercuryisreducedtoelementalmercury.Themercuryvaporis
total mercury content in a sample of coal or coal combustion
determined by flameless cold-vapor atomic absorption spec-
residue.
troscopy.
1.2 The values stated in SI units are regarded as the
4.2 Test Method B—Mercury in the analysis sample is
standard.
solubilized by heating the test sample in a mixture of nitric and
1.3 This standard does not purport to address all of the
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sulfuric acids with vanadium pentoxide. The acid solutions
safety concerns, if any, associated with its use. It is the
produced are transferred into a vessel in which the mercury is
responsibility of the user of this standard to establish appro-
reduced to elemental mercury. The mercury vapor is deter-
priate safety and health practices and determine the applica-
mined by flameless cold-vapor atomic absorption spectros-
bility of regulatory limitations prior to use.
copy.
2. Referenced Documents
NOTE 1—Mercury and mercury salts can be volatilized at low tempera-
2.1 ASTM Standards:
tures. Precautions against inadvertent mercury loss should be taken when
2
D 121 Terminology of Coal and Coke using this method.
3
D 1193 Specification for Reagent Water
2 5. Significance and Use
D 2013 Method of Preparing Coal Samples for Analyses
5.1 The emission of mercury during coal combustion can be
D 3173 Test Method for Moisture in theAnalysis Sample of
2
an environmental concern.
Coal and Coke
5.2 When representative test portions are analyzed accord-
D 3180 Practice for Calculating Coal and Coke Analyses
2
ing to one of these procedures, the total mercury is represen-
from As-Determined to Different Bases
tative of concentrations in the sample.
D 5142 Test Methods for the Proximate Analysis of the
Analysis Sample of Coal and Coke by Instrumental
6. Apparatus
2
Procedures
6.1 Apparatus for Test Method A:
IEEE/ASTM SI 10 Standard for Use of the International
4
6.1.1 Analytical Balance, with a sensitivity of 0.1 mg.
System of Units (SI): The Modern Metric System
6.1.2 Atomic Absorption Spectrophotometer, with a flame-
3. Terminology
less cold-vapor mercury analysis system.
6.1.3 Digestion Vessels, 100- to 250-mL bottles with an
3.1 For definitions of terms used in this standard, refer to
O-ring seal and screw cap. Bottle must be compatible for use
Terminology D 121.
with aqua regia. Polycarbonate and HDPE are acceptable.
4. Summary of Test Method
Bottles and cap assemblies shall be washed in 1-to-1 HCl then
dried before each use.
4.1 Test Method A—Mercury in the analysis sample is
solubilized by heating the test sample at a specified tempera-
NOTE 2—Other bottle and cap assemblies may be used provided they
are compatible for use with aqua regia at a temperature of 80°C.
1
6.1.4 Heat Source, a water bath capable of maintaining a
These Test Methods are under the jurisdiction of ASTM Committee D05 on
Coal and Coke and are the direct responsibility of Subcommittee D05.29 on Major
temperature of 80°C.
3
Elements in Ash and Trace Elements of Coal.
6.1.5 SyringeandFilter,a20-cm syringeanda1-µmPTFE
Current edition approved Oct. 10, 2001. Published December 2001. Originally
filter to fit syringe.
published as D6414-99. Last previous edition D 6414- 99.
2
Annual Book of ASTM Standards, Vol 05.05.
3
Annual Book of ASTM Standards, Vol 11.01.
4 5
Annual Book of ASTM Standards, Vol 14.04. Crock, J.G., Open-File Report, U.S. Geological Survey, 87–84, p.19.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D6414–01
6.2 Apparatus for Test Method B: 8.10 Stannous Chloride Solution (100 g/L)—Dissolve 100 g
6.2.1 Analytical Balance, with a sensitivity of 0.1 mg. of stannous chloride dihydrate (SnCl ·2 H O) in 300 mL of
2 2
6.2.2 Atomic Absorption Spectrophotometer, with a flame- concentrated hydrochloric acid (HCl, sp. gr. 1.19) and CAU-
less cold-vapor mercury analysis system. TIOUSLY dilute to 1 L with water. This solution is stable for
6.2.3 Digestion Vessels, 16- by 150-mm disposable glass approximately one week if refrigerated.
test
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