ASTM D6414-99

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.

General Information

• Status: Historical
• Publication Date: 09-Oct-2001
• ICS: 73.040 - Coals
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaced By: ASTM D6414-01 - Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Acid Extraction or Wet Oxidation/Cold Vapor Atomic Absorption
• Effective Date: 10-Oct-2001

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D6414–99
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 (ε) 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
5
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
5. Significance and Use
2.1 ASTM Standards:
2
5.1 The emission of mercury during coal combustion can be
D 121 Terminology of Coal and Coke
3
an environmental concern.
D 1193 Specification for Reagent Water
2
5.2 When representative test portions are analyzed accord-
D 2013 Method of Preparing Coal Samples for Analyses
ing to one of these procedures, the total mercury is represen-
D 3173 Test Method for Moisture in theAnalysis Sample of
2
tative of concentrations in the sample.
Coal and Coke
D 5142 Test Methods for the Proximate Analysis of the
6. Apparatus
Analysis Sample of Coal and Coke by Instrumental
2 6.1 Apparatus for Test Method A:
Procedures
6.1.1 Analytical Balance, with a sensitivity of 0.1 mg.
D 3180 Practice for Calculating Coal and Coke Analyses
2 6.1.2 Atomic Absorption Spectrophotometer, with a flame-
from As-Determined to Different Bases
less cold-vapor mercury analysis system.
IEEE/ASTM SI 10 Standard for Use of the International
4 6.1.3 Digestion Vessels, 100- to 250-mL bottles with an
System of Units (SI): The Modern Metric System
O-ring seal and screw cap. Bottle must be compatible for use
3. Terminology with aqua regia. Polycarbonate and HDPE are acceptable.
Bottles and cap assemblies shall be washed in 1-to-1 HCl then
3.1 For definitions of terms used in this standard, refer to
dried before each use.
Terminology D 121.
NOTE 1—Other bottle and cap assemblies may be used provided they
4. Summary of Test Method
are compatible for use with aqua regia at a temperature of 80°C.
4.1 Test Method A—Mercury in the analysis sample is
6.1.4 Heat Source, a water bath capable of maintaining a
solubilized by heating the test sample at a specified tempera-
temperature of 80°C.
3
6.1.5 SyringeandFilter,a20-cm syringeanda1-µmPTFE
1
These Test Methods are under the jurisdiction of ASTM Committee D-5 on
filter to fit syringe.
Coal and Coke and are the direct responsibility of Subcommittee D05.29 on Major
6.2 Apparatus for Test Method B:
Elements in Ash and Trace Elements of Coal.
6.2.1 Analytical Balance, with a sensitivity of 0.1 mg.
Current edition approved April 10, 1999. Published May 1999.
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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D6414–99
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 tubes. 8.11 Certified Reference Material (CRM)—Use Certified
6.2.4 Heat Source, an aluminum block with 18-mm holes to
Reference Material (CRM) coals with dry-basis mercury val-
accommodate the disposable test tubes. The block shall be ues for which confidence limits are issued by a recognized
capable of slowly reaching and maintaining a final temperature
c
...