ASTM D6414-14

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
5.1 The emission of mercury during coal combustion can be an environmental concern.  
5.2 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 to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Warning:   Mercury has been designated by many regulatory agencies as a hazardous material that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Safety Data Sheet (SDS) for additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.  
1.4 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: 28-Feb-2014
• ICS: 73.040 - Coals
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 14
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.
1. Scope from As-Determined to Different Bases
D7582 Test Methods for Proximate Analysis of Coal and
1.1 These test methods cover procedures to determine the
Coke by Macro Thermogravimetric Analysis
total mercury content in a sample of coal or coal combustion
E691 Practice for Conducting an Interlaboratory Study to
residue.
Determine the Precision of a Test Method
1.2 The values stated in SI units are to be regarded as
IEEE/ASTM SI 10 Standard for Use of the International
standard. No other units of measurement are included in this
System of Units (SI): The Modern Metric System
standard. 3
2.2 ISO Standard
1.3 Warning: Mercury has been designated by many regu-
ISO 5725-6:1994 Accuracy of measurement methods and
latory agencies as a hazardous material that can cause serious results-Part 6
medical issues. Mercury, or its vapor, has been demonstrated to
3. Terminology
be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury contain-
3.1 For definitions of terms used in this standard, refer to
ing products. See the applicable product Safety Data Sheet
Terminology D121.
(SDS) for additional information. Users should be aware that
4. Summary of Test Method
selling mercury and/or mercury containing products into your
state or country may be prohibited by law.
4.1 Test Method A—Mercury in the analysis sample is
1.4 This standard does not purport to address all of the solubilized by heating the test sample at a specified tempera-
safety concerns, if any, associated with its use. It is the
ture in a mixture of nitric and hydrochloric acids. The acid
responsibility of the user of this standard to establish appro-
solutions produced are transferred into a vessel in which the
priate safety and health practices and determine the applica-
mercuryisreducedtoelementalmercury.Themercuryvaporis
bility of regulatory limitations prior to use.
determined by flameless cold-vapor atomic absorption spec-
troscopy.
2. Referenced Documents
4.2 Test Method B—Mercury in the analysis sample is
2
2.1 ASTM Standards:
solubilized by heating the test sample in a mixture of nitric and
4
D121 Terminology of Coal and Coke
sulfuric acids with vanadium pentoxide. The acid solutions
D1193 Specification for Reagent Water
produced are transferred into a vessel in which the mercury is
D2013 Practice for Preparing Coal Samples for Analysis
reduced to elemental mercury. The mercury vapor is deter-
D3173 Test Method for Moisture in the Analysis Sample of
mined by flameless cold-vapor atomic absorption spectros-
Coal and Coke
copy.
D3180 Practice for Calculating Coal and Coke Analyses
NOTE 1—Mercury and mercury salts can be volatilized at low tempera-
tures. Precautions against inadvertent mercury loss should be taken when
using this method.
1
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
5. Significance and Use
and Coke and are the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
5.1 The emission of mercury during coal combustion can be
Current edition approved March 1, 2014. Published March 2014. Originally
an environmental concern.
approved in 1999. Last previous edition approved in 2006 as D6414 - 01(2006).
DOI: 10.1520/D6414-14.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from International Organization for Standardization (ISO), 1 rue de
Standards volume information, refer to the standard’s Document Summary page on Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland.
4
the ASTM website. 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
1

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D6414 − 14
5.2 When representative test portions are analyzed accord- 8.2 Purity of Acids—Use trace metal purity grade acids or
ing to one of these procedures, the total mercury is represen- equivalent. Redistilled acids are acceptable.
tative of concentrations in the sample.
8.3 Purity of Water—UsewaterequivalenttoASTMTypeII
reagent water of Specification D1193.
6. Apparatus
8.4 Mercury Standard Stock Solution [100
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6414 − 01 (Reapproved 2006) D6414 − 14
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.
1. 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 to be regarded as standard. No other units of measurement are included
in this standard.
1.3 Warning: Mercury has been designated by many regulatory agencies as a hazardous material that can cause serious
medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Caution should
be taken when handling mercury and mercury containing products. See the applicable product Safety Data Sheet (SDS) for
additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country
may be prohibited by law.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D121 Terminology of Coal and Coke
D1193 Specification for Reagent Water
D2013 Practice for Preparing Coal Samples for Analysis
D3173 Test Method for Moisture in the Analysis Sample of Coal and Coke
D3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases
D5142D7582 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental ProceduresMacro
Thermogravimetric Analysis (Withdrawn 2010)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
IEEE/ASTM SI 10 Standard for Use of the International System of Units (SI): The Modern Metric System
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 ISO Standard
ISO 5725-6:1994 Accuracy of measurement methods and results-Part 6
3. Terminology
3.1 For definitions of terms used in this standard, refer to Terminology D121.
4. Summary of Test Method
4.1 Test Method A—Mercury in the analysis sample is solubilized by heating the test sample at a specified temperature in a
mixture of nitric and hydrochloric acids. The acid solutions produced are transferred into a vessel in which the mercury is reduced
to elemental mercury. The mercury vapor is determined by flameless cold-vapor atomic absorption spectroscopy.
1
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 Elements
in Ash and Trace Elements of Coal.
Current edition approved April 1, 2006March 1, 2014. Published April 2006March 2014. Originally approved in 1999. Last previous edition approved in 20012006 as
D6414 - 01.01(2006). DOI: 10.1520/D6414-01R06.10.1520/D6414-14.
2
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 the ASTM website.
3
Available from International Organization for Standardization (ISO), 1 rue de Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6414 − 14
4.2 Test Method B—Mercury in the analysis sample is solubilized by heating the test sample in a mixture of nitric and sulfuric
4
acids with vanadium pentoxide. The acid solutions produced are transferred into a vessel in which the mercury is reduced to
elemental mercury. The mercury vapor is determined by flameless cold-vapor atomic absorption spectroscopy.
NOTE 1—Mercury and mercury salts can be volatilized at low temperatures. Precautions against inadvertent mercury loss should be taken when using
this method.
5. Significance and Use
5.1 The emission of
...