ASTM D6414-01(2006)

Standard Test Methods for Total Mercury in Coal and Coal Combustion Residues by Acid Extraction or Wet Oxidation/Cold Vapor Atomic Absorption

SIGNIFICANCE AND USE
The emission of mercury during coal combustion can be an environmental concern.
When representative test portions are analyzed according to one of these procedures, the total mercury is representative of concentrations in the sample.
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.
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: 31-Mar-2006
• ICS: 73.040 - Coals
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaces: 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: 01-Apr-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 01(Reapproved 2006)
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 D6414; 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.
4
1. Scope 2.2 ISO Standard
ISO 5725-6:1994 Accuracy of measurement methods and
1.1 These test methods cover procedures to determine the
results-Part 6
total mercury content in a sample of coal or coal combustion
residue.
3. Terminology
1.2 The values stated in SI units are regarded as the
3.1 For definitions of terms used in this standard, refer to
standard.
Terminology D121.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 Test Method A—Mercury in the analysis sample is
priate safety and health practices and determine the applica-
solubilized by heating the test sample at a specified tempera-
bility of regulatory limitations prior to use.
ture in a mixture of nitric and hydrochloric acids. The acid
solutions produced are transferred into a vessel in which the
2. Referenced Documents mercuryisreducedtoelementalmercury.Themercuryvaporis
determined by flameless cold-vapor atomic absorption spec-
2
2.1 ASTM Standards:
troscopy.
D121 Terminology of Coal and Coke
4.2 Test Method B—Mercury in the analysis sample is
D1193 Specification for Reagent Water
D2013 Practice for Preparing Coal Samples for Analysis solubilized by heating the test sample in a mixture of nitric and
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sulfuric acids with vanadium pentoxide. The acid solutions
D3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke produced are transferred into a vessel in which the mercury is
reduced to elemental mercury. The mercury vapor is deter-
D3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases mined by flameless cold-vapor atomic absorption spectros-
copy.
D5142 Test Methods for ProximateAnalysis of theAnalysis
NOTE 1—Mercury and mercury salts can be volatilized at low tempera-
Sample of Coal and Coke by Instrumental Procedures
3
tures. Precautions against inadvertent mercury loss should be taken when
(Withdrawn 2010)
using this method.
IEEE/ASTM SI 10 Standard for Use of the International
System of Units (SI): The Modern Metric System
5. Significance and Use
E691 Practice for Conducting an Interlaboratory Study to
5.1 The emission of mercury during coal combustion can be
Determine the Precision of a Test Method
an environmental concern.
5.2 When representative test portions are analyzed accord-
ing to one of these procedures, the total mercury is represen-
1
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
tative of concentrations in the sample.
and Coke and are the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
6. Apparatus
Current edition approved April 1, 2006. Published April 2006. Originally
approved in 1999. Last previous edition approved in 2001 as D6414 - 01. DOI:
6.1 Apparatus for Test Method A:
10.1520/D6414-01R06.
2
6.1.1 Analytical Balance, with a sensitivity of 0.1 mg.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4
the ASTM website. Available from International Organization for Standardization (ISO), 1 rue de
3
The last approved version of this historical standard is referenced on Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland.
5
www.astm.org. 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 (2006)
6.1.2 Atomic Absorption Spectrophotometer, with a flame- Alternatively, use a commercially available stock solution
less cold-vapor mercury analysis system. specifically prepared for atomic absorption spectrometry.
6.1.3 Digestion Vessels, 100- to 250-mL bottles with an
8.5 Mercury Standard Solution (100 ng/mL)—Prepare the
O-ring seal and screw cap. Bottle must be compatible for use
mercury standard solution fresh daily. Dilute 5 mL of the
with aqua regia. Polycarbonate and HDPE are acceptable.
mercury standard stock solution to 500 mL with deionized
Bottles and cap assemblies shall be
...