ASTM_D_8247_-_19.pdf

Designation:D824719Standard Test Method forDetermination of Total Fluorine and Total Chlorine in Coalby Oxidative Pyrohydrolytic Combustion Followed by IonChromatography Detection1This standard is issued under the fixed designation D8247;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 determination of totalfluorine and total chlorine in coal.Samples containing200 mg kg to 4000 mg kg of chlorine and 20 mg kg to100 mgkg of fluorine can be analyzed directly.1.1.1 It is possible for this method to be used for thedetermination of total bromine in coal.No precision and biasstatement will be given for the determination of total bromine.1.2 The values stated in SI units are to be regarded asstandard.The values given in parentheses after SI units areprovided for information only and are not considered standard.1.3 In determining the conformation of the test results usingthis method to applicable specifications,results shall berounded off in accordance with the rounding-off method fromPractice E29.1.4 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:3ISO 5725-6:1994 Accuracy(Trueness and Precision)ofMeasurement Methods and Results Part 6:Use inPractice of Accuracy Values3.Terminology3.1 DefinitionsDefinitions applicable to this test methodare listed in Terminology D121.3.2 Abbreviations:3.2.1 ICion chromatograph3.2.2 CICcombustion ion chromatography4.Summary of Test Method4.1 A 50 mg to 100 mg sample is weighed into a sampleboat and is introduced at a controlled rate into a hightemperature combustion tube where the sample is combusted ina humidified oxygen pyrohydrolytic environment.The gaseousby-products of the combusted sample are trapped in anabsorption solution where the hydrogen halides(HX)formedduring combustion disassociate into their respective ions(X-).An aliquot of known volume of the absorbing solution is theninjected into an ion chromatograph(IC).The halide anions areseparated by the anion separation column of the IC.Theconductivity of the eluent is reduced with an anion suppressiondevice prior to detection of the chloride and fluoride ions with1This 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 Feb.1,2019.Published April 2019.DOI:10.1520/D8247-19.2For 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.3Available from International Organization for Standardization(ISO),ISOCentral Secretariat,BIBC II,Chemin de Blandonnet 8,CP 401,1214 Vernier,Geneva,Switzerland,http:/www.iso.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 a conductivity detector.Quantification of the fluoride andchloride is achieved by first calibrating the ion chromatographwith a series of aqueous standards containing known amountsof fluoride and chloride.5.Significance and Use5.1 This test method covers the measurement of the chlorineand fluorine contents in coal.These halides can con