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ASTM D4326-97

(Test Method)

Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence

Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence

SCOPE
1.1 This test method covers the analysis of the commonly determined major and minor elements in ash from coal or coke using X-ray fluorescence (XRF) techniques.  Note 1—Test Method D1757, 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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

Replaced By
ASTM D4326-01 - Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence
Effective Date
10-Oct-2001

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ASTM D4326-97 - Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray FluorescenceASTM D4326-97 - Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence
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ASTM D4326-97 - Standard Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4326–97
Standard Test Method for
Major and Minor Elements in Coal and Coke Ash By X-Ray
1
Fluorescence
This standard is issued under the fixed designation D 4326; 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 (ε) indicates an editorial change since the last revision or reapproval.
1. Scope tions. The ash is fused with lithium tetraborate (Li B O)or
2 4 7
other suitable flux and either ground and pressed into a pellet
1.1 This test method covers the analysis of the commonly
or cast into a glass disk. The pellet or disk is then irradiated by
determined major and minor elements in ash from coal or coke
an X-ray beam of short wavelength (high energy). The char-
using X-ray fluorescence (XRF) techniques.
acteristic X-rays of the atom that are emitted or fluoresced
NOTE 1—Test Method D 1757 is used for determination of sulfur.
uponabsorptionoftheprimaryorincidentX-raysaredispersed
NOTE 2—Although not included in the present method, the determina-
and intensities at selected wavelengths are measured by sensi-
tion of barium, strontium, and manganese may be required to yield
tive detectors. Detector output is related to concentration by
adequate totals.
calibration curves or by computerized data-handling equip-
1.2 The values stated in SI units are to be regarded as the
ment.
standard. The values given in parentheses are for information
3.2 The K spectral lines are used for all of the elements
only.
determined by this procedure.
1.3 This standard does not purport to address all of the
3.3 All elements are determined as the element and reported
safety concerns, if any, associated with its use. It is the
as the oxide and include Si, Al, Fe, Ca, Mg, Na, K, P, Ti, Mn,
responsibility of the user of this standard to establish appro-
Sr, and Ba.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Significance and Use
4.1 Acompositionalanalysisofashisusedindescribingthe
2. Referenced Documents
quality of coal for its complete characterization. Ash compo-
2.1 ASTM Standards:
sition is useful in predicting slagging and fouling characteris-
D 1757 Test Methods for Sulfur in Ash from Coal and
tics of combusted materials as well as the potential utilization
2
Coke
of ash by-products.
D 3174 TestMethodforAshintheAnalysisSampleofCoal
4.2 The chemical composition of laboratory prepared coal
2
and Coke from Coal
or coke ash is rarely, if ever, representative of the composition
E 2 Methods of Preparation of Micrographs of Metals and
ofthemineralmatterinthecoalbecausetheashingprocesscan
Alloys (Including Recommended Practice for Photography
alter some minerals. However, it can approximate the compo-
3
as Applied to Metallography)
sition of the fly ash and slag resulting from commercial
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
combustion of coal or coke.
4
poses
5. Apparatus
3. Summary of Test Method
5.1 Ashing Furnace, with air circulation as specified in Test
3.1 The coal or coke to be analyzed is ashed under standard
Method D 3174 and capable of having its temperature regu-
conditions and ignited to constant weight. Previously ashed
lated between 700 and 750°C.
materials are ignited to constant weight under standard condi-
5.2 Fusion Furnace or Fluxing Device, with an operating
temperature of at least 1000°C.
1
5.3 Fusion Crucibles, either high-purity graphite (22 mm
ThistestmethodisunderthejurisdictionofASTMCommitteeD-5onCoaland
Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
high and 19 mm wide, inside diameter) or platinum-gold alloy
Ash and Trace Elements of Coal.
of a similar or larger capacity.
Current edition approved Sept. 10, 1997. Published May 1998. Originally
5.4 Pulverizers, including agate, mullite or tungsten carbide
published as D 4326 – 84. Last previous edition D 4326 – 94.
2
Annual Book of ASTM Standards, Vol 05.05. mortar, and pestle, minimum capacity 25 mL.
3
Discontinued, see 1982 Annual Book of ASTM Standards, Part 11.
4
Annual Book of ASTM Standards, Vol 14.02.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4326–97
5.5 Sieves, 250-µm (No. 60) and 75-µm (No. 200) U.S.A standard sieve, and reignite at 750°C for 1 h. Immediately,
standard sieve as specified in Specification E 11. prepare the analysis sample or store the dry ash in a vacuum
5.6 Compactor—A press equipped with a gage enabling desiccator. If samples are stored under atmospheric conditions,
8
reproducible pressures (exceeding 1.723 10 Pa (25 000 psi)) they must be rehea
...

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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.  
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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.  
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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.
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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.  
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