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ASTM D6349-01

(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

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.

General Information

Status
Historical
Publication Date
09-Oct-2001
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
Current Stage
Ref Project

Relations

Replaces
ASTM D6349-00 - 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
10-Oct-2001
Replaced By
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
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
10-Oct-2001
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
10-Oct-2001
Referred By
ASTM D8213-18 - Standard Test Method for Determination of Boron in Coal
Effective Date
10-Oct-2001
Referred By
ASTM D3174-12(2018)e1 - Standard Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
Effective Date
10-Oct-2001
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
10-Oct-2001
Referred By
ASTM D1857/D1857M-18 - Standard Test Method for Fusibility of Coal and Coke Ash
Effective Date
10-Oct-2001
Referred By
ASTM D7348-21 - Standard Test Methods for Loss on Ignition (LOI) of Solid Combustion Residues
Effective Date
10-Oct-2001

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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 SpectrometryASTM 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
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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
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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 – 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
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 3. Summary of Test Method
1.1 This test method covers a procedure for the analysis of 3.1 The sample to be analyzed is ashed under standard
the commonly determined major and minor elements in coal, conditionsandignitedtoconstantweight.Theashisfusedwith
coke, and solid residues from combustion of coal and coke. a fluxing agent followed by dissolution of the melt in dilute
These residues may be laboratory ash, bottom ash, fly ash, flue acid solution. Alternatively, the ash is digested in a mixture of
gas desulfurization sludge, and other combustion process hydrofluoric, nitric, and hydrochloric acids. The solution is
residues. analyzedbyinductivelycoupledplasma-atomicemissionspec-
1.2 The values stated in SI units are to be regarded as the trometry (ICP) for the elements. The basis of the method is the
standard. measurement of atomic emissions. Aqueous solutions of the
1.3 This standard does not purport to address all of the samples are nebulized, and a portion of the aerosol that is
safety concerns, if any, associated with its use. It is the produced is transported to the plasma torch where excitation
responsibility of the user of this standard to establish appro- and emission occurs. Characteristic line emission spectra are
priate safety and health practices and determine the applica- produced by a radio-frequency inductively coupled plasma. A
bility of regulatory limitations prior to use. gratingmonochromatorsystemisusedtoseparatetheemission
lines, and the intensities of the lines are monitored by photo-
2. Referenced Documents
mutilplier tube or photodiode array detection. The photocur-
2.1 ASTM Standards:
rents from the detector are processed and controlled by a
D 346 Practice for Collection and Preparation of Coke
computer system. A background correction technique is re-
2
Samples for Laboratory Analysis quired to compensate for variable background contribution to
3
D 1193 Specification for Reagent Water
the determination of elements. Background must be measured
2
D 2013 Method of Preparing Coal Samples for Analysis adjacent to analyte lines of samples during analysis. The
D 3173 Test Method for Moisture in theAnalysis Sample of
positionselectedforthebackgroundintensitymeasurement,on
2
Coal and Coke eitherorbothsidesoftheanalyticalline,willbedeterminedby
D 3180 Practice for Calculating Coal and Coke Analyses
thecomplexityofthespectrumadjacenttotheanalyteline.The
2
from As-Determined to Different Bases position used must be free of spectral interference and reflect
D 5142 Test Methods for Proximate Analysis of the Analy-
the same change in background intensity as occurs at the
2
sis Sample of Coal and Coke by Instrumental Procedures analyte wavelength measured.
E 691 Practice for Conducting an Interlaboratory Study to
4
4. Significance and Use
Determine the Precision of a Test Method
4.1 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
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
associated residues is also useful in predicting the elemental
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
enrichment/depletion compositional behavior of ashes and
Elements in Ash and Trace Elements of Coal.
Current edition approved Oct. 10, 2001. Published October 2001. Originally
slags in comparison to the concentration levels in the parent
published as D 6349 - 98. Last previous edition D 6349 - 00.
coal.Utilizationoftheashby-productsandhazardouspotential
2
Annual Book of ASTM Standards, Vol 05.06.
3
may also depend on the chemical composition and leachability
Annual Book of ASTM Standards, Vol 11.01.
4
Annual Book of ASTM Standards, Vol 14.02. of the inorganic constituents of the coal ash.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D6349–01
4.2 The chemical composition of laboratory-prepared ash intended for use only as a rudimentary guide for the indication
may not exactly represent the composition of mineral matter in of potential spectral interferences. For this purpose, linea
...

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4.1 Coke undergoes various degrees of degradation during removal from coke ovens, transportation, and its decent within a blast furnace to the combustion zone. These processes subject the coke to impact and abrasion. This test method is a relative measure of the resistance of coke to breakage when subjected to these degradation processes.
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This specification covers the classification of coals by rank, that is, according to their degree of metamorphism, or progressive alteration, in the natural series from lignite to anthracite. These coals are mainly composed of vitrinite. The classification shall be based on gradational properties that depend on the degree of metamorphism. The classification shall also be according to fixed carbon and gross calorific value calculated to the mineral-matter-free basis.
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Note 1: Coals rich in inertinite or liptinite (exinite), or both, cannot be properly classified because, in those macerals, the properties that determine rank (calorific value, volatile matter, and agglomerating character) differ greatly from those of vitrinite in the same coal. Often, such coals can be recognized by megascopic examination. In North America, these coals are mostly nonbanded varieties that contain only a small proportion of vitrain and consist mainly of attrital materials. The degree of metamorphism of nonbanded and other vitrinite-poor coals can be estimated by determining the classification properties of isolated or concentrated vitrinite fractions, or by determining the reflectance of the vitrinite (see Test Method D2798 and Appendix X1 of this classification). However, in the use of these vitrinite-poor coals, some properties normally associated with rank, such as rheology, combustibility, hardness, and grindability (as well as the rank determining properties) may differ substantially from those of vitrinite-rich coals of the same degree of metamorphism.  
1.3 The accuracy of the classification of impure coal may be impaired by the effect of large amounts of mineral matter on the determination of volatile matter and calorific value, and on their calculation to the mineral-matter-free basis.  
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5.1 Reliable values of the plastic properties of coals are used to predict or explain the behavior of a coal or blends during carbonization or in other processes such as gasification, liquefaction, and combustion.
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1.1 This test method covers a relative measure of the plastic behavior of coal when heated under prescribed conditions. This test method may be used to obtain semiquantitative values of the plastic properties of coals and blends used in carbonization and in other situations where determination of plastic behavior of coals is of practical importance.  
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1.3 While it is recognized that such a standard may be unwieldy for routine usage in commercial operations, it can provide a common base for agreement in cases of dispute or arbitration. The complete standard is referred to as the referee method. Embodied in the standard is the commercial method starting with the crushed and divided sample when the gross sample is not too wet to crush and divide. See Practice D2961/D2961M and Test Method D3173 for other moisture methods.  
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4.1 This test method permits measurement of the total mass fraction of arsenic and selenium in coal for the purpose of evaluating these elements where they can be of concern, for example, in coal combustion. When coal samples are prepared for analysis in accordance with this test method, the arsenic and selenium are quantitatively retained and are representative of the total mass fraction in the coal.
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1.2.1 All percentages are percent mass fractions unless otherwise noted.  
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ASTM D6349-21(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

SIGNIFICANCE AND USE
5.1 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 mass fraction 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.  
5.2 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.
Note 1: There are two interlaboratory studies associated with this test method. The first was conducted in 1997 ( RR:D05-1035)2 and the second was conducted in 2007 ( RR:D05-1032).3 Sulfur trioxide was only included in the 2007 study, and that study only included combustion residues derived from ash and no combustion residues derived from coke.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM D4326-21(Test Method)
Standard Test Method for Major and Minor Elements in Coal Ash By X-Ray Fluorescence

SIGNIFICANCE AND USE
5.1 A compositional analysis of ash is used in describing the quality of coal for its complete characterization. Ash composition is useful in predicting slagging and fouling characteristics of combusted materials as well as the potential utilization of ash by-products.  
5.2 The chemical composition of laboratory prepared coal ash is rarely, if ever, representative of the composition of the mineral matter in the coal because the ashing process can alter some minerals. However, it can approximate the composition of the fly ash and slag resulting from commercial combustion of coal.
SCOPE
1.1 This test method covers the analysis of the commonly determined major and minor elements in ash from coal using X-ray fluorescence (XRF) techniques.
Note 1: Test Method D5016 is used for determination of sulfur.
Note 2: Although not included in the present method, the determination of barium, strontium, and manganese may be required to yield adequate totals.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM D167/D167M-21a(Test Method)
Standard Test Method for Apparent and True Specific Gravity and Porosity of Lump Coke

SIGNIFICANCE AND USE
4.1 Apparent and true specific gravity, as determined by this test method, are influenced by the type of coals carbonized and the operating and preparational conditions of that carbonization, that is, charge bulk density, heating rate, and pulverization level. In turn, these properties directly influence the performance in processes using coke.
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1.1 This test method covers the determination of apparent specific gravity (Sections 5 to 9) and true specific gravity (Sections 10 to 14) of lump coke larger than 25 mm [1 in.] size and calculating porosity (Section 15) from the specific gravity data.  
1.2 Units—The values stated in either SI units or non-SI units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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