ASTM D6357-11
(Test Method)Test Methods for Determination of Trace Elements in Coal, Coke, & Combustion Residues from Coal Utilization Processes by Inductively Coupled Plasma Atomic Emission, Inductively Coupled Plasma Mass, & Graphite Furnace Atomic Absorption Spectrometry
Test Methods for Determination of Trace Elements in Coal, Coke, & Combustion Residues from Coal Utilization Processes by Inductively Coupled Plasma Atomic Emission, Inductively Coupled Plasma Mass, & Graphite Furnace Atomic Absorption Spectrometry
SIGNIFICANCE AND USE
Coal contains several elements whose individual concentrations are generally less than 0.01 %. These elements are commonly and collectively referred to as trace elements. These elements primarily occur as part of the mineral matter in coal. The potential release of certain trace elements from coal combustion sources has become an environmental concern.
The ash prepared in accordance with these provisional test methods quantitatively retains the elements listed in 1.1 and is representative of their concentrations in the coal or coke.
SCOPE
1.1 These test methods pertain to the determination of antimony, arsenic, beryllium, cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, vanadium, and zinc in coal and coke. These test methods can also be used for the analysis of residues from coal combustion processes.
Note 1—These test methods may be applicable to the determination of other trace elements.
1.2 The values stated in SI units shall be 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: D6357 − 11
Standard Test Methods for
Determination of Trace Elements in Coal, Coke, and
Combustion Residues from Coal Utilization Processes by
Inductively Coupled Plasma Atomic Emission Spectrometry,
Inductively Coupled Plasma Mass Spectrometry, and
1
Graphite Furnace Atomic Absorption Spectrometry
This standard is issued under the fixed designation D6357; 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 D7448 Practice for Establishing the Competence of Labora-
tories Using ASTM Procedures in the Sampling and
1.1 These test methods pertain to the determination of
Analysis of Coal and Coke
antimony, arsenic, beryllium, cadmium, chromium, cobalt,
D7582 Test Methods for Proximate Analysis of Coal and
copper, lead, manganese, molybdenum, nickel, vanadium, and
Coke by Macro Thermogravimetric Analysis
zinc in coal and coke. These test methods can also be used for
E691 Practice for Conducting an Interlaboratory Study to
the analysis of residues from coal combustion processes.
Determine the Precision of a Test Method
NOTE 1—These test methods may be applicable to the determination of
2.2 Other Documents:
other trace elements.
EPA/600/4-91/010 MethodsfortheDeterminationofMetals
3
1.2 The values stated in SI units shall be regarded as the
in Environmental Samples
standard.
3. Terminology
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1 Definitions—Definitions applicable to these test meth-
responsibility of the user of this standard to establish appro-
ods are listed in Terminology D121.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
4.1 The coal or coke to be analyzed is ashed under con-
2. Referenced Documents
trolled conditions, digested by a mixture of aqua-regia and
2
2.1 ASTM Standards:
hydrofluoric acid, and finally dissolved in 1 % nitric acid.
D121 Terminology of Coal and Coke
Combustion residues are digested on an as-received basis. The
D346 Practice for Collection and Preparation of Coke
concentration of individual trace elements is determined by
Samples for Laboratory Analysis
either inductively coupled atomic emission spectrometry (IC-
D1193 Specification for Reagent Water
PAES) or inductively coupled plasma mass spectrometry
D2013 Practice for Preparing Coal Samples for Analysis
(ICPMS).Selectedelementsthatoccuratconcentrationsbelow
D3173 Test Method for Moisture in the Analysis Sample of
the detection limits of ICPAES can be quantitatively analyzed
Coal and Coke
by graphite furnace atomic absorption spectrometry (GFAA).
D3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases
5. Significance and Use
5.1 Coal contains several elements whose individual con-
centrations are generally less than 0.01 %. These elements are
1
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
commonly and collectively referred to as trace elements.These
and Coke and are the direct responsibility of Subcommittee D05.29 on Major
elements primarily occur as part of the mineral matter in coal.
Elements in Ash and Trace Elements of Coal.
The potential release of certain trace elements from coal
Current edition approved April 1, 2011. Published April 2011. Originally
published in 1996. Last previous edition approved in 2004 as D6357 - 04. DOI:
combustion sources has become an environmental concern.
10.1520/D6357-11.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from Superintendent of Documents, U.S. Printing Office,
the ASTM website. Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6357 − 11
5.2 The ash prepared in accordance with these provisional 7.5 ICP Calibration Standards—Aqueous multielement so-
test methods quantitatively retains the elements listed in 1.1 lutions made up in 1 % HNO are used for calibration of
3
andisrepresentativeoftheirconcentrationsinthecoalorcoke. ICPAES and ICPMS systems.The standards may be purchased
or prepared from high-purity grade chemicals or metals.
7.5.1 GFAA Stock Standard Solution (1000 ppm)—Single-
6. Apparatus
element standards either purchased or prepared from high-
6.1 InductivelyCoupledPlasmaAtomicEmissionSpectrom-
purity
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6357–04 Designation: D6357 – 11
Standard Test Methods for
Determination of Trace Elements in Coal, Coke, and
Combustion Residues from Coal Utilization Processes by
Inductively Coupled Plasma Atomic Emission Spectrometry,
Inductively Coupled Plasma Mass Spectrometry, and
1
Graphite Furnace Atomic Absorption Spectrometry
This standard is issued under the fixed designation D6357; 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 pertain to the determination of antimony, arsenic, beryllium, cadmium, chromium, cobalt, copper, lead,
manganese, molybdenum, nickel, vanadium, and zinc in coal and coke. These test methods can also be used for the analysis of
residues from coal combustion processes.
NOTE 1—These test methods may be applicable to the determination of other trace elements.
1.2 The values stated in SI units shall be 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D121 Terminology of Coal and Coke
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
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
D4621Guide for Quality Management in an Organization That Samples or Tests Coal and Coke 7448 Practice for Establishing
the Competence of Laboratories Using ASTM Procedures in the Sampling and Analysis of Coal and Coke
D5142Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Procedures 7582 Test
Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Documents:
3
EPA/600/4-91/010 Methods for the Determination of Metals in Environmental Samples
3. Terminology
3.1 Definitions—Definitions applicable to these test methods are listed in Terminology D121.
4. Summary of Test Method
4.1 The coal or coke to be analyzed is ashed under controlled conditions, digested by a mixture of aqua-regia and hydrofluoric
acid, and finally dissolved in 1 % nitric acid. Combustion residues are digested on an as-received basis. The concentration of
individual trace elements is determined by either inductively coupled atomic emission spectrometry (ICPAES) or inductively
1
These test methods are under the jurisdiction ofASTM 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 Oct.April 1, 2004.2011. Published November 2004.April 2011. Originally published in 1996. Last previous edition approved in 20002004 as
D6357-00a.D6357 - 04. DOI: 10.1520/D6357-04.10.1520/D6357-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from Superintendent of Documents, U.S. Printing Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D6357 – 11
coupled plasma mass spectrometry (ICPMS). Selected elements that occur at concentrations below the detection limits of ICPAES
can be quantitatively analyzed by graphite furnace atomic absorption spectrometry (GFAA).
5. Significance and Use
5.1 Coal contains several elements whose individual concentrations are generally less than 0.01 %. These elements are
commonly and collectively referred to as trace elements. These elements primarily occur as part of the mineral matter in coal. The
potential release of certain trace elements from coal combustion sources has become an environmental concern.
5.2 The ash prepared in accorda
...
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