ASTM D6349-07

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

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.
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-May-2007
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaces: ASTM D6349-01 - 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
• Effective Date: 01-Jun-2007
• Replaced By: ASTM D6349-08 - 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 Spectrometry
• Effective Date: 01-Feb-2008
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Jun-2007
• Referred By: ASTM D8088-16(2022) - Standard Practice for Determination of the Six Major Rare Earth Elements in Fluid Catalytic Cracking Catalysts, Zeolites, Additives, and Related Materials by Inductively Coupled Plasma Optical Emission Spectroscopy
• Effective Date: 01-Jun-2007
• Referred By: ASTM D1857/D1857M-18 - Standard Test Method for Fusibility of Coal and Coke Ash
• Effective Date: 01-Jun-2007
• Referred By: ASTM D8213-18 - Standard Test Method for Determination of Boron in Coal
• Effective Date: 01-Jun-2007
• Referred By: ASTM D3174-12(2018)e1 - Standard Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
• Effective Date: 01-Jun-2007
• Referred By: ASTM D7348-21 - Standard Test Methods for Loss on Ignition (LOI) of Solid Combustion Residues
• Effective Date: 01-Jun-2007
• Referred By: ASTM D5016-16 - Standard Test Method for Total Sulfur in Coal and Coke Combustion Residues Using a High-Temperature Tube Furnace Combustion Method with Infrared Absorption
• Effective Date: 01-Jun-2007

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: D 6349 – 07
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 E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers a procedure for the analysis of
the commonly determined major and minor elements in coal,
3. Summary of Test Method
coke, and solid residues from combustion of coal and coke.
3.1 The sample to be analyzed is ashed under standard
These residues may be laboratory ash, bottom ash, fly ash, flue
conditionsandignitedtoconstantweight.Theashisfusedwith
gas desulfurization sludge, and other combustion process
a fluxing agent followed by dissolution of the melt in dilute
residues.
acid solution.Alternatively, the ash is digested in a mixture of
1.2 The values stated in SI units are to be regarded as the
hydrofluoric, nitric, and hydrochloric acids. The solution is
standard.
analyzedbyinductivelycoupledplasma-atomicemissionspec-
1.3 This standard does not purport to address all of the
trometry (ICP) for the elements. The basis of the method is the
safety concerns, if any, associated with its use. It is the
measurement of atomic emissions. Aqueous solutions of the
responsibility of the user of this standard to establish appro-
samples are nebulized, and a portion of the aerosol that is
priate safety and health practices and determine the applica-
produced is transported to the plasma torch where excitation
bility of regulatory limitations prior to use.
and emission occurs. Characteristic line emission spectra are
2. Referenced Documents produced by a radio-frequency inductively coupled plasma. A
2
gratingmonochromatorsystemisusedtoseparatetheemission
2.1 ASTM Standards:
lines, and the intensities of the lines are monitored by photo-
D 346 Practice for Collection and Preparation of Coke
mutilplier tube or photodiode array detection. The photocur-
Samples for Laboratory Analysis
rents from the detector are processed and controlled by a
D 1193 Specification for Reagent Water
computer system. A background correction technique is re-
D 2013 Practice for Preparing Coal Samples for Analysis
quired to compensate for variable background contribution to
D 3173 TestMethodforMoistureintheAnalysisSampleof
the determination of elements. Background must be measured
Coal and Coke
adjacent to analyte lines of samples during analysis. The
D 3180 Practice for Calculating Coal and Coke Analyses
positionselectedforthebackgroundintensitymeasurement,on
from As-Determined to Different Bases
eitherorbothsidesoftheanalyticalline,willbedeterminedby
D 5142 Test Methods for Proximate Analysis of the Analy-
thecomplexityofthespectrumadjacenttotheanalyteline.The
sis Sample of Coal and Coke by Instrumental Procedures
position used must be free of spectral interference and reflect
the same change in background intensity as occurs at the
analyte wavelength measured.
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
4. Significance and Use
Elements in Ash and Trace Elements of Coal.
4.1 A compositional analysis of coal and coke and their
CurrenteditionapprovedJune1,2007.PublishedJuly2007.Originallyapproved
in 1998. Last previous edition approved in 2001 as D 6349 - 01.
associated combustion residues are often useful in assessing
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
their quality. Knowledge of the elemental composition of the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
associated residues is also useful in predicting the elemental
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. enrichment/depletion compositional behavior of ashes and
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1

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D6349–07
TABLE 1 Recommended Wavelengths for Elements Determined
5.1.2 Table 1 lists the elements determined by this method
by ICP
and the recommended wavelengths using conventional nebu-
Element Wavelengths, nm
lization. Sulfur may only be determined if the sample is
dissolved by the mixed acid dissolution described in 10.3.2.
Aluminum 396.152, 256.80, 308.215, 309.271
3
Barium 45
...