ASTM_D_5987_-_96_2015.pdf

Designation:D598796(Reapproved 2015)Standard Test Method forTotal Fluorine in Coal and Coke by PyrohydrolyticExtraction and Ion Selective Electrode or IonChromatograph Methods1This standard is issued under the fixed designation D5987;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 total fluorine incoal and coke.1.2 This analysis was successfully tested on coals contain-ing 37%ash or less(see AS 1038.10.4 and Conrad2).1.3 The values stated in SI units shall be regarded asstandard.The values given in parentheses are for informationonly.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 and health practices and determine the applica-bility of regulatory limitations prior to use.For specific hazardstatements see Note 4.1.5 All accountability and quality control aspects of GuideD4621 apply to this test method.2.Referenced Documents2.1 ASTM Standards:3D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampleof CoalD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD4621 Guide for Quality Management in an OrganizationThat Samples or Tests Coal and Coke(Withdrawn 2010)4D5142 Test Methods for Proximate Analysis of the AnalysisSample of Coal and Coke by Instrumental Procedures(Withdrawn 2010)42.2 Australian Standard:5AS 1038.10.4 Determination of Trace ElementsCoal,Coke and Fly-Ash-Determination of Fluorine ContentPyrohydrolysis Method3.Summary of Test Method3.1 Total fluorine is determined in this test method by firstsubjecting the weighed test portion to pyrohydrolytic condi-tions which separate fluorine from the coal/coke matrix.Thepyrohydrolysate is then gravimetrically processed and finaldeterminations are made by either ion-selective electrode orion chromatographic techniques.4.Significance and Use4.1 This test method permits measurement of the fluorinecontent of coal and coke for the evaluation of potential fluorineemission from coal combustion or conversion processes.Whencoal samples are combusted in accordance with this testmethod,the fluorine is quantitatively released from the coaland retained in the pyrohydrolysate so that it is representativeof the total fluorine concentration in coal.5.Apparatus5.1 Laboratory WareExcept as noted,all laboratory ware,for example,volumetric flasks,beakers,bottles,etc.,used forsolutionscontainingfluorideionsmustbemadeofpolyethylene,polystyrene,or a heat-resistant polymer such aspolypropylene.5.2 VialsGlass or polystyrene,10 to 30-mL capacity withtightly fitting snap-on plastic lids.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 Nov.1,2015.Published December 2015.Originallypublished approved in 1996.Last previous edition approved in 2007 asD598796(2007).DOI:10.1520/D5987-96R15.2Conrad,V.B.,and Brownlee,W.D.,“HydropyrolyticIon ChromatographicDetermination of Fluoride in Coal and Geological Materials,”Analytical Chemistry,Vol 60,No.4,1988,pp.365369.3For 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.4The last approved version of this historical standard is referenced onwww.astm.org.5Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.3 BottlesPolypropylene,125-mL capacity,wide-mouth,with liner-less leakproof polyethylene screw cap,for tube-furnace pyrohydrolysate processing.5.4 VialsPolystyrene,70-mL capacity,with liner-lessleakproof polyethylene screw cap.5.5 Dispensing BottlesPolyethylene,250-mL capacity,forthe standard fluorine solution(6.3.1)and of 600-mL capacityfor the absorption solution(6.3.3)and buffer(6.3.5).5.6 MicropipettesPolypropyleneorothersuitablepolymer,variable volumes ranging from 0.1 mL to at least 2.0mL.This is a satisfactory alternative to the 250-mL dispensingbottle(5.5),for the delivery of small volumes of the standardfluorine solution.5.7 Glass Dropper Bottle30-mL capacity for dispensingglacial acetic acid.5.8 BalanceAnalytical,with a sensitivity o