ASTM D4326-04
(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 D 1757 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.
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Designation:D4326–04
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 D4326; 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.
Note—Section 13 Precision and Bias, was corrected and the year date was changed on May 26, 2004.
1. Scope 3. Summary of Test Method
1.1 This test method covers the analysis of the commonly 3.1 The coal or coke to be analyzed is ashed under standard
determined major and minor elements in ash from coal or coke conditions and ignited to constant weight. Previously ashed
using X-ray fluorescence (XRF) techniques. materials are ignited to constant weight under standard condi-
tions. The ash is fused with lithium tetraborate (Li B O)or
2 4 7
NOTE 1—Test Method D1757 is used for determination of sulfur.
other suitable flux and either ground and pressed into a pellet
NOTE 2—Although not included in the present method, the determina-
or cast into a glass disk. The pellet or disk is then irradiated by
tion of barium, strontium, and manganese may be required to yield
an X-ray beam of short wavelength (high energy). The char-
adequate totals.
acteristic X-rays of the atom that are emitted or fluoresced
1.2 The values stated in SI units are to be regarded as the
uponabsorptionoftheprimaryorincidentX-raysaredispersed
standard. The values given in parentheses are for information
and intensities at selected wavelengths are measured by sensi-
only.
tive detectors. Detector output is related to concentration by
1.3 This standard does not purport to address all of the
calibration curves or by computerized data-handling equip-
safety concerns, if any, associated with its use. It is the
ment.
responsibility of the user of this standard to establish appro-
3.2 The K spectral lines are used for all of the elements
priate safety and health practices and determine the applica-
determined by this procedure.
bility of regulatory limitations prior to use.
3.3 All elements are determined as the element and reported
2. Referenced Documents as the oxide and include Si, Al, Fe, Ca, Mg, Na, K, P, Ti, Mn,
2 Sr, and Ba.
2.1 ASTM Standards:
D1757 TestMethodforSulfateSulfurinAshfromCoaland
4. Significance and Use
3
Coke
4.1 Acompositionalanalysisofashisusedindescribingthe
D3174 Test Method forAsh in theAnalysis Sample of Coal
quality of coal for its complete characterization. Ash compo-
and Coke from Coal
sition is useful in predicting slagging and fouling characteris-
E2 Methods of Preparation of Micrographs of Metals and
tics of combusted materials as well as the potential utilization
Alloys (Including Recommended Practice for Photography
3 of ash by-products.
as Applied to Metallography)
4.2 The chemical composition of laboratory prepared coal
E11 SpecificationforWovenWireTestSieveClothandTest
or coke ash is rarely, if ever, representative of the composition
Sieves
ofthemineralmatterinthecoalbecausetheashingprocesscan
alter some minerals. However, it can approximate the compo-
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
sition of the fly ash and slag resulting from commercial
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
combustion of coal or coke.
Elements in Ash and Trace Elements of Coal.
Current edition approved May 26, 2004. Published June 2004. Originally
5. Apparatus
approved in 1984. Last previous edition approved 2003 as D4326 – 03. DOI:
10.1520/D4326-04.
5.1 Ashing Furnace, with air circulation as specified in Test
2
Annual Book of ASTM Standards, Vol 05.05.
MethodD3174andcapableofhavingitstemperatureregulated
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
between 700 and 750°C.
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 5.2 Fusion Furnace or Fluxing Device, with an operating
the ASTM website.
temperature of at least 1000°C.
3
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
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D4326–04
1
5.3 Fusion Crucibles, either high-purity graphite (22 mm coal or coke in a layer not over 6 mm ( ⁄4 in.) in depth in a
high and 19 mm wide, inside diameter) or platinum-gold alloy fireclay, porcelain, or platinum roasting dish. Place the ash in a
of a similar or larger capacity. cold muffle furnace and heat gradually so
...
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:D4326–01 Designation:D4326–04
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 (´) indicates an editorial change since the last revision or reapproval.
Note—Section 13 Precision and Bias, was corrected and the year date was changed on May 26, 2004.
1. 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 D 1757 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1757 Test Methods for Sulfur in Ash from Coal and Coke
D 3174 Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
E2 Methods of Preparation of Micrographs of Metals and Alloys (Including Recommended Practice for Photography as
3
Applied to Metallography)
E11 Specification for Wire-Cloth Sieves for Testing Purposes
3. Summary of Test Method
3.1 The coal or coke to be analyzed is ashed under standard conditions and ignited to constant weight. Previously ashed
materials are ignited to constant weight under standard conditions. The ash is fused with lithium tetraborate (Li B O ) or other
2 4 7
suitable flux and either ground and pressed into a pellet or cast into a glass disk. The pellet or disk is then irradiated by an X-ray
beam of short wavelength (high energy). The characteristic X-rays of the atom that are emitted or fluoresced upon absorption of
the primary or incident X-rays are dispersed and intensities at selected wavelengths are measured by sensitive detectors. Detector
output is related to concentration by calibration curves or by computerized data-handling equipment.
3.2 The K spectral lines are used for all of the elements determined by this procedure.
3.3 All elements are determined as the element and reported as the oxide and include Si,Al, Fe, Ca, Mg, Na, K, P, Ti, Mn, Sr,
and Ba.
4. Significance and Use
4.1 Acompositional 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.
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 Oct. 10, 2001. Published October 2001. Originally published as D4326–84. Last previous edition D4326–97.
Current edition approved May 26, 2004. Published June 2004. Originally approved in 1984. Last previous edition approved 2003 as D 4326 – 03.
2
Annual Book of ASTM Standards, Vol 05.05.
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
Discontinued, see 1982 Annual Book of ASTM Standards, Part 11.
3
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4326–04
4.2 The chemical composition of laboratory prepared coal or coke 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 or coke.
5. Apparatus
5.1 Ashing Furnace, with air circulation as specified in Test Method D 3174 and capable of having its temperature regulated
between 700 and 750°C.
...
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