ASTM D6349-08
(Test Method)Standard Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of Coal and Coke by Inductively Coupled Plasma-Atomic Emission Spectrometry
Standard Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of Coal and Coke by Inductively Coupled Plasma-Atomic Emission Spectrometry
SIGNIFICANCE AND USE
A compositional analysis of coal and coke and their associated combustion residues are often useful in assessing their quality. Knowledge of the elemental composition of the associated residues is also useful in predicting the elemental enrichment/depletion compositional behavior of ashes and slags in comparison to the concentration levels in the parent coal. Utilization of the ash by-products and hazardous potential may also depend on the chemical composition and leachability of the inorganic constituents of the coal ash.
The chemical composition of laboratory-prepared ash may not exactly represent the composition of mineral matter in coal or the composition of fly ash and slag resulting from commerical-scale burning of the coal.
SCOPE
1.1 This test method covers a procedure for the analysis of the commonly determined major and minor elements in coal, coke, and solid residues from combustion of coal and coke. These residues may be laboratory ash, bottom ash, fly ash, flue gas desulfurization sludge, and other combustion process residues.
1.2 The values stated in SI units are to 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: D 6349 – 08
Standard Test Method for
Determination of Major and Minor Elements in Coal, Coke,
and Solid Residues from Combustion of Coal and Coke by
Inductively Coupled Plasma—Atomic Emission
1
Spectrometry
This standard is issued under the fixed designation D 6349; 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.
3
1. Scope 2.2 ISO Standard:
ISO/IECGuide99:2007 Internationalvocabularyofmetrol-
1.1 This test method covers a procedure for the analysis of
ogy -- Basic and general concepts and associated terms
the commonly determined major and minor elements in coal,
(VIM)
coke, and solid residues from combustion of coal and coke.
These residues may be laboratory ash, bottom ash, fly ash, flue
3. Summary of Test Method
gas desulfurization sludge, and other combustion process
3.1 The sample to be analyzed is ashed under standard
residues.
conditionsandignitedtoconstantweight.Theashisfusedwith
1.2 The values stated in SI units are to be regarded as the
a fluxing agent followed by dissolution of the melt in dilute
standard.
acid solution.Alternatively, the ash is digested in a mixture of
1.3 This standard does not purport to address all of the
hydrofluoric, nitric, and hydrochloric acids. The solution is
safety concerns, if any, associated with its use. It is the
analyzedbyinductivelycoupledplasma-atomicemissionspec-
responsibility of the user of this standard to establish appro-
trometry (ICP) for the elements. The basis of the method is the
priate safety and health practices and determine the applica-
measurement of atomic emissions. Aqueous solutions of the
bility of regulatory limitations prior to use.
samples are nebulized, and a portion of the aerosol that is
2. Referenced Documents produced is transported to the plasma torch where excitation
2
and emission occurs. Characteristic line emission spectra are
2.1 ASTM Standards:
produced by a radio-frequency inductively coupled plasma. A
D 346 Practice for Collection and Preparation of Coke
gratingmonochromatorsystemisusedtoseparatetheemission
Samples for Laboratory Analysis
lines, and the intensities of the lines are monitored by photo-
D 1193 Specification for Reagent Water
mutilplier tube or photodiode array detection. The photocur-
D 2013 Practice for Preparing Coal Samples for Analysis
rents from the detector are processed and controlled by a
D 3173 TestMethodforMoistureintheAnalysisSampleof
computer system. A background correction technique is re-
Coal and Coke
quired to compensate for variable background contribution to
D 3180 Practice for Calculating Coal and Coke Analyses
the determination of elements. Background must be measured
from As-Determined to Different Bases
adjacent to analyte lines of samples during analysis. The
D 5142 Test Methods for Proximate Analysis of the Analy-
positionselectedforthebackgroundintensitymeasurement,on
sis Sample of Coal and Coke by Instrumental Procedures
eitherorbothsidesoftheanalyticalline,willbedeterminedby
E 691 Practice for Conducting an Interlaboratory Study to
thecomplexityofthespectrumadjacenttotheanalyteline.The
Determine the Precision of a Test Method
position used must be free of spectral interference and reflect
the same change in background intensity as occurs at the
1
analyte wavelength measured.
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
4. Significance and Use
Current edition approved Feb. 1, 2008. Published February 2008. Originally
4.1 A compositional analysis of coal and coke and their
approved in 1998. Last previous edition approved in 2007 as D 6349 - 07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
associated combustion residues are often useful in assessing
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Available from International Organization for Standardization (ISO), 1 rue de
Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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D6349–08
TABLE 1 Recommended Wavelengths for Elements Determined
of potential spectral interferences. For this purpose, linear
by ICP
relations between concentration and intensity for the analytes
Element Wavelengths, nm
and the interferents can be assumed.Th
...
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:D6349–07 Designation: D 6349 – 08
Standard Test Method for
Determination of Major and Minor Elements in Coal, Coke,
and Solid Residues from Combustion of Coal and Coke by
Inductively Coupled Plasma—Atomic Emission
1
Spectrometry
This standard is issued under the fixed designation D 6349; 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
1.1 This test method covers a procedure for the analysis of the commonly determined major and minor elements in coal, coke,
and solid residues from combustion of coal and coke. These residues may be laboratory ash, bottom ash, fly ash, flue gas
desulfurization sludge, and other combustion process residues.
1.2 The values stated in SI units are to 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:
D 346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D 1193 Specification for Reagent Water
D 2013 Practice for Preparing Coal Samples for Analysis
D 3173 Test Method for Moisture in the Analysis Sample of Coal and Coke
D 3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases
D 5142 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Procedures
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 ISO Standard:
ISO/IEC Guide 99:2007 International vocabulary of metrology -- Basic and general concepts and associated terms (VIM)
3. Summary of Test Method
3.1 Thesampletobeanalyzedisashedunderstandardconditionsandignitedtoconstantweight.Theashisfusedwithafluxing
agent followed by dissolution of the melt in dilute acid solution. Alternatively, the ash is digested in a mixture of hydrofluoric,
nitric, and hydrochloric acids.The solution is analyzed by inductively coupled plasma-atomic emission spectrometry (ICP) for the
elements. The basis of the method is the measurement of atomic emissions. Aqueous solutions of the samples are nebulized, and
a portion of the aerosol that is produced is transported to the plasma torch where excitation and emission occurs. Characteristic
line emission spectra are produced by a radio-frequency inductively coupled plasma.Agrating monochromator system is used to
separate the emission lines, and the intensities of the lines are monitored by photomutilplier tube or photodiode array detection.
The photocurrents from the detector are processed and controlled by a computer system. A background correction technique is
required to compensate for variable background contribution to the determination of elements. Background must be measured
adjacent to analyte lines of samples during analysis. The position selected for the background intensity measurement, on either or
both sides of the analytical line, will be determined by the complexity of the spectrum adjacent to the analyte line. The position
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
Ash and Trace Elements of Coal.
Current edition approved JuneFeb. 1, 2007.2008. Published July 2007.February 2008. Originally approved in 1998. Last previous edition approved in 20012007 as
D 6349 - 017.
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
Methods for Chemical Analysis of Water and Wastes , (EPA-600/4-79-020), Metals-4, Method 200.7 CLP-M.
3
Available from International Organization for Standardization (ISO), 1 rue de Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D6349–08
used must be free of spectral interference and reflect the same change in backgrou
...
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