ASTM D4326-01

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Designation: D 4326 – 01
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 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-
1.1 This test method covers the analysis of the commonly
acteristic X-rays of the atom that are emitted or fluoresced
determined major and minor elements in ash from coal or coke
upon absorption of the primary or incident X-rays are dispersed
using X-ray fluorescence (XRF) techniques.
and intensities at selected wavelengths are measured by sensi-
NOTE 1—Test Method D 1757 is used for determination of sulfur.
tive detectors. Detector output is related to concentration by
NOTE 2—Although not included in the present method, the determina-
calibration curves or by computerized data-handling equip-
tion of barium, strontium, and manganese may be required to yield
ment.
adequate totals.
3.2 The K spectral lines are used for all of the elements
1.2 The values stated in SI units are to be regarded as the
determined by this procedure.
standard. The values given in parentheses are for information
3.3 All elements are determined as the element and reported
only.
as the oxide and include Si, Al, Fe, Ca, Mg, Na, K, P, Ti, Mn,
1.3 This standard does not purport to address all of the
Sr, and Ba.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 A compositional analysis of ash is used in describing the
bility of regulatory limitations prior to use.
quality of coal for its complete characterization. Ash compo-
sition is useful in predicting slagging and fouling characteris-
2. Referenced Documents
tics of combusted materials as well as the potential utilization
2.1 ASTM Standards:
of ash by-products.
D 1757 Test Methods for Sulfur in Ash from Coal and
4.2 The chemical composition of laboratory prepared coal
2
Coke
or coke ash is rarely, if ever, representative of the composition
D 3174 Test Method for Ash in the Analysis Sample of Coal
of the mineral matter in the coal because the ashing process can
2
and Coke from Coal
alter some minerals. However, it can approximate the compo-
E 2 Methods of Preparation of Micrographs of Metals and
sition of the fly ash and slag resulting from commercial
Alloys (Including Recommended Practice for Photography
combustion of coal or coke.
3
as Applied to Metallography)
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
5. Apparatus
4
poses
5.1 Ashing Furnace, with air circulation as specified in Test
Method D 3174 and capable of having its temperature regu-
3. Summary of Test Method
lated between 700 and 750°C.
3.1 The coal or coke to be analyzed is ashed under standard
5.2 Fusion Furnace or Fluxing Device, with an operating
conditions and ignited to constant weight. Previously ashed
temperature of at least 1000°C.
materials are ignited to constant weight under standard condi-
5.3 Fusion Crucibles, either high-purity graphite (22 mm
tions. The ash is fused with lithium tetraborate (Li B O )or
2 4 7
high and 19 mm wide, inside diameter) or platinum-gold alloy
other suitable flux and either ground and pressed into a pellet
of a similar or larger capacity.
5.4 Pulverizers, including agate, mullite or tungsten carbide
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
mortar, and pestle, minimum capacity 25 mL.
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
5.5 Sieves, 250-μm (No. 60) and 75-μm (No. 200) U.S.A
Elements in Ash and Trace Elements of Coal.
standard sieve as specified in Specification E 11.
Current edition approved Oct. 10, 2001. Published October 2001. Originally
5.6 Compactor—A press equipped with a gage enabling
published as D 4326 – 84. Last previous edition D 4326 – 97.
2 8
Annual Book of ASTM Standards, Vol 05.05.
reproducible pressures (exceeding 1.72 3 10 Pa (25 000 psi))
3
Discontinued, see 1982 Annual Book of ASTM Standards, Part 11.
if pressed pellets are utilized.
4
Annual Book of ASTM Standards, Vol 14.02.
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