ASTM D4326-13

Standard Test Method for Major and Minor Elements in Coal and Coke 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 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 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 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.

General Information

• Status: Historical
• Publication Date: 31-Aug-2013
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4326 − 13
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D7582Test Methods for Proximate Analysis of Coal and
Coke by Macro Thermogravimetric Analysis
1.1 This test method covers the analysis of the commonly
E2Methods of Preparation of Micrographs of Metals and
determinedmajorandminorelementsinashfromcoalorcoke
Alloys (Including Recommended Practice for Photogra-
using X-ray fluorescence (XRF) techniques.
phy As Applied to Metallography); Replaced by E883
3
NOTE 1—Test Method D5016 is used for determination of sulfur.
(Withdrawn 1983)
NOTE 2—Although not included in the present method, the determina-
E11Specification forWovenWireTest Sieve Cloth andTest
tion of barium, strontium, and manganese may be required to yield
Sieves
adequate totals.
1.2 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions—Definitions applicable to this test method
standard.
are listed in D121, Terminology of Coal and Coke.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 The coal or coke to be analyzed is ashed under standard
priate safety and health practices and determine the applica-
conditions and ignited to constant weight. Previously ashed
bility of regulatory limitations prior to use.
materials are ignited to constant weight under standard condi-
tions. The ash is fused with lithium tetraborate (Li B O)or
2 4 7
2. Referenced Documents
other suitable flux and either ground and pressed into a pellet
2
2.1 ASTM Standards:
or cast into a glass disk.The pellet or disk is then irradiated by
D121Terminology of Coal and Coke
an X-ray beam of short wavelength (high energy). The char-
D346Practice for Collection and Preparation of Coke
acteristic X-rays of the atom that are emitted or fluoresced
Samples for Laboratory Analysis
uponabsorptionoftheprimaryorincidentX-raysaredispersed
D2013Practice for Preparing Coal Samples for Analysis
and intensities at selected wavelengths are measured by sensi-
D3173Test Method for Moisture in theAnalysis Sample of
tive detectors. Detector output is related to concentration by
Coal and Coke
calibration curves or by computerized data-handling equip-
D3174Test Method forAsh in theAnalysis Sample of Coal
ment.
and Coke from Coal
4.2 The K spectral lines are used for all of the elements
D5016Test Method for Total Sulfur in Coal and Coke
determined by this procedure.
Combustion Residues Using a High-Temperature Tube
4.3 Allelementsaredeterminedastheelementandreported
Furnace Combustion Method with Infrared Absorption
as the oxide and include Si,Al, Fe, Ca, Mg, Na, K, P, Ti, Mn,
D7348Test Methods for Loss on Ignition (LOI) of Solid
Sr, and Ba.
Combustion Residues
5. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal 5.1 Acompositionalanalysisofashisusedindescribingthe
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
quality of coal for its complete characterization. Ash compo-
Elements in Ash and Trace Elements of Coal.
sition is useful in predicting slagging and fouling characteris-
Current edition approved Sept. 1, 2013. Published September 2013. Originally
tics of combusted materials as well as the potential utilization
approved in 1984. Last previous edition approved 2011 as D4326–11. DOI:
10.1520/D4326-13.
of ash by-products.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4326 − 13
5.2 The chemical composition of laboratory prepared coal 7.3 Heavy Absorber—Where heavy absorbers, such as lan-
or coke ash is rarely, if ever, representative of the composition thanum oxide or barium oxide, are used they shall be a
ofthemineralmatterinthecoalbecausetheashingprocesscan minimum of 99.99% purity.
alter some minerals. However, it can approximate the compo-
7.4 Fluxes—
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 − 11 D4326 − 13
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.
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 D1757D5016 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D121 Terminology of Coal and Coke
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
D1757D3173 Test Method for Sulfate Sulfur in Ash from Moisture in the Analysis Sample of Coal and Coke (Withdrawn 2009)
D3174 Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
D5016 Test Method for Total Sulfur in Coal and Coke Combustion Residues Using a High-Temperature Tube Furnace
Combustion Method with Infrared Absorption
D7348 Test Methods for Loss on Ignition (LOI) of Solid Combustion Residues
D7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis
E2 Methods of Preparation of Micrographs of Metals and Alloys (Including Recommended Practice for Photography As Applied
3
to Metallography); Replaced by E 883 (Withdrawn 1983)
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
4.1 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.
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 April 1, 2011Sept. 1, 2013. Published April 2011 September 2013. Originally approved in 1984. Last previous edition approved 20042011 as
D4326 – 04.D4326 – 11. DOI: 10.1520/D4326-11.10.1520/D4326-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
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, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4326 − 13
4.2 The K spectral lines are used for all of the elements determined by this procedure.
4.3 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.
5. 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 materi
...