ASTM_D_4326_-_13.pdf

Designation:D432613Standard Test Method forMajor and Minor Elements in Coal and Coke Ash By X-RayFluorescence1This standard is issued under the fixed designation D4326;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the analysis of the commonlydetermined major and minor elements in ash from coal or cokeusing X-ray fluorescence(XRF)techniques.NOTE1Test Method D5016 is used for determination of sulfur.NOTE2Although not included in the present method,the determina-tion of barium,strontium,and manganese may be required to yieldadequate totals.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD5016 Test Method for Total Sulfur in Coal and CokeCombustion Residues Using a High-Temperature TubeFurnace Combustion Method with Infrared AbsorptionD7348 Test Methods for Loss on Ignition(LOI)of SolidCombustion ResiduesD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE2 Methods of Preparation of Micrographs of Metals andAlloys(Including Recommended Practice for Photogra-phy As Applied to Metallography);Replaced by E 883(Withdrawn 1983)3E11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Terminology3.1 DefinitionsDefinitions applicable to this test methodare listed in D121,Terminology of Coal and Coke.4.Summary of Test Method4.1 The coal or coke to be analyzed is ashed under standardconditions and ignited to constant weight.Previously ashedmaterials are ignited to constant weight under standard condi-tions.The ash is fused with lithium tetraborate(Li2B4O7)orother suitable flux and either ground and pressed into a pelletor cast into a glass disk.The pellet or disk is then irradiated byan X-ray beam of short wavelength(high energy).The char-acteristic X-rays of the atom that are emitted or fluorescedupon absorption of the primary or incident X-rays are dispersedand intensities at selected wavelengths are measured by sensi-tive detectors.Detector output is related to concentration bycalibration curves or by computerized data-handling equip-ment.4.2 The K spectral lines are used for all of the elementsdetermined by this procedure.4.3 All elements are determined as the element and reportedas the oxide and include Si,Al,Fe,Ca,Mg,Na,K,P,Ti,Mn,Sr,and Ba.5.Significance and Use5.1 Acompositional analysis of ash is used in describing thequality of coal for its complete characterization.Ash compo-sition is useful in predicting slagging and fouling characteris-tics of combusted materials as well as the potential utilizationof ash by-products.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.29 on MajorElements in Ash and Trace Elements of Coal.Current edition approved Sept.1,2013.Published September 2013.Originallyapproved in 1984.Last previous edition approved 2011 as D4326 11.DOI:10.1520/D4326-13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 The chemical composition of laboratory prepared coalor coke ash is rarely,if ever,representative of the compositionof the mineral matter in the coal because the ashing process canalter some minerals.However,it can approximate the compo-sition of the fly ash and slag resulting from commercialcombustion of coal or coke.6.Apparatus6.1 Ashing Furnace,with an adequate air circulation andcapable of having its temperature regulated at 500C and750C.6.2 Fusion Furnace or Fluxing Device,with an operatingtemperature of at least 1000C.6.3 Fusion Crucibles,either high-purity graphite(22 mmhigh and 19 mm wide,inside diameter)or platinum-gold alloyof a similar or larger capacity.6.4 Pulverizers,including agate,mullite or