ASTM D4326-11
(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
SIGNIFICANCE AND USE
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.
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.
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 standard. No other units of measurement are included in this 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: D4326 − 11
StandardTest 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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers the analysis of the commonly 3.1 Definitions—Definitions applicable to this test method
determinedmajorandminorelementsinashfromcoalorcoke are listed in D121, Terminology of Coal and Coke.
using X-ray fluorescence (XRF) techniques.
4. Summary of Test Method
NOTE 1—Test Method D1757 is used for determination of sulfur.
4.1 The coal or coke to be analyzed is ashed under standard
NOTE 2—Although not included in the present method, the determina-
tion of barium, strontium, and manganese may be required to yield
conditions and ignited to constant weight. Previously ashed
adequate totals.
materials are ignited to constant weight under standard condi-
1.2 The values stated in SI units are to be regarded as tions. The ash is fused with lithium tetraborate (Li B O)or
2 4 7
standard. No other units of measurement are included in this other suitable flux and either ground and pressed into a pellet
standard. or cast into a glass disk.The pellet or disk is then irradiated by
an X-ray beam of short wavelength (high energy). The char-
1.3 This standard does not purport to address all of the
acteristic X-rays of the atom that are emitted or fluoresced
safety concerns, if any, associated with its use. It is the
uponabsorptionoftheprimaryorincidentX-raysaredispersed
responsibility of the user of this standard to establish appro-
and intensities at selected wavelengths are measured by sensi-
priate safety and health practices and determine the applica-
tive detectors. Detector output is related to concentration by
bility of regulatory limitations prior to use.
calibration curves or by computerized data-handling equip-
ment.
2. Referenced Documents
2
4.2 The K spectral lines are used for all of the elements
2.1 ASTM Standards:
determined by this procedure.
D121Terminology of Coal and Coke
D1757Test Method for Sulfate Sulfur inAsh from Coal and
4.3 Allelementsaredeterminedastheelementandreported
3
Coke (Withdrawn 2009)
as the oxide and include Si,Al, Fe, Ca, Mg, Na, K, P, Ti, Mn,
D3174Test Method forAsh in theAnalysis Sample of Coal
Sr, and Ba.
and Coke from Coal
5. Significance and Use
E2Methods of Preparation of Micrographs of Metals and
Alloys (Including Recommended Practice for Photogra-
5.1 Acompositionalanalysisofashisusedindescribingthe
phy As Applied to Metallography); Replaced by E883
quality of coal for its complete characterization. Ash compo-
3
(Withdrawn 1983)
sition is useful in predicting slagging and fouling characteris-
E11Specification forWovenWireTest Sieve Cloth andTest
tics of combusted materials as well as the potential utilization
Sieves
of ash by-products.
5.2 The chemical composition of laboratory prepared coal
or coke ash is rarely, if ever, representative of the composition
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
ofthemineralmatterinthecoalbecausetheashingprocesscan
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
alter some minerals. However, it can approximate the compo-
Elements in Ash and Trace Elements of Coal.
Current edition approved April 1, 2011. Published April 2011. Originally
sition of the fly ash and slag resulting from commercial
approved in 1984. Last previous edition approved 2004 as D4326–04. DOI:
combustion of coal or coke.
10.1520/D4326-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6. Apparatus
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
6.1 Ashing Furnace, with air circulation as specified inTest
the ASTM website.
3
MethodD3174andcapableofhavingitstemperatureregulated
The last approved version of this historical standard is referenced on
www.astm.org. between 700 and 750°C.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
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D4326 − 11
6.2 Fusion Furnace or Fluxing Device, with an operating 8. Preparation of Coal Ash and Coke Ash
temperature of at least 1000°C.
8.1 Prepare the ash from a thoroughly mixed representative
6.3 Fusion Crucibles, either high-purity graphite (22 mm analysis sample of air-dried coal or coke that has been ground
to pass a 250-µm (No. 60) U.S.A standard sieve. Spread the
...
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:D4326–04 Designation:D4326–11
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
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.
1.2The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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: ASTM Standards:
D121 Terminology of Coal and Coke
D1757 Test Method for Sulfate Sulfur in Ash from Coal and Coke
D3174 Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
E2 MethodsofPreparationofMicrographsofMetalsandAlloys(IncludingRecommendedPracticeforPhotographyasApplied
3
to Metallography)
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions—Definitions applicable to this test method are listed in D121, Terminology of Coal and Coke.
4. Summary of Test Method
3.1The4.1 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.
3.2The K spectral lines are used for all of the elements determined by this procedure.
3.3All 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.
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 May 26, 2004. Published June 2004. Originally approved in 1984. Last previous edition approved 2003 as D4326–03. DOI: 10.1520/D4326-04.
Current edition approvedApril 1, 2011. PublishedApril 2011. Originally approved in 1984. Last previous edition approved 2004 as D4326 – 04. DOI: 10.1520/D4326-11.
2
Annual Book of ASTM Standards, Vol 05.05.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For
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.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4326–11
4.Significance and Use
4.1A 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.
4.2The chemical composition of laboratory prepared coal or coke ash is rarely, if ever, rep
...
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