ASTM_D_3179_-_02.pdf

Designation:D 3179 02Standard Test Methods forNitrogen in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D 3179;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover the determination of totalnitrogen in samples of coal and coke.The analytical data fromthese test methods shall be reported as part of ultimate analysiswhere ultimate analysis is requested.If ultimate analysis is notrequested,the value shall be reported according to the request.Two methods are included as follows:SectionsTest Method AKjeldahl-Gunning Macro Analysis,with an alter-native technique included9 to 16Test Method BKjeldahl-Gunning Semi-Micro Determination17 to 231.2 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.1.3 The values stated in SI units are to be regarded as thestandard.2.Referenced Documents2.1 ASTM Standards:D 121 Terminology of Coal and Coke2D 346 Practice for Collection and Preparation of CokeSamples for Laboratory Analysis2D 1193 Specification for Reagent Water3D 2013 Practice for Preparing Coal Samples for Analysis2D 3173 Test Method for Moisture in theAnalysis Sample ofCoal and Coke2D 3176 Practice for Ultimate Analysis of Coal and Coke2D 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different Bases2IEEE/ASTM SI 10Standard for Use of the InternationalSystem of Units(SI):The Modern Metric System43.Terminology3.1 For definitions of terms used in these test methods,referto Definitions D 121.For an explanation of the metric systemincluding units,symbols,and conversion factors,see IEEE/ASTM SI 10.4.Summary of Test Methods4.1 In these procedures,nitrogen is converted into ammo-nium salts by destructive digestion of the sample with a hot,catalyzed mixture of concentrated sulfuric acid and potassiumsulfate.These salts are subsequently decomposed in a hotalkaline solution from which the ammonia is recovered bydistillation and finally determined by alkalimetric or acidimet-ric titration.5.Significance and Use5.1 Nitrogen results obtained by these test methods arerequired to fulfill the requirements of the ultimate analysis,Practice D 3176.Also,results obtained may be used to evaluatethe potential formation of nitrogen oxides as a source ofatmospheric pollution.5.2 Nitrogen data are used in comparing coals and inresearch.When the oxygen content of coal is estimated bydifference,it is necessary to make a nitrogen determination.6.Interferences6.1 No significant interferences have been determined usingthese procedures.However,strict adherence is necessary whenusing these nitrogen procedures to obtain good reproducibleresults.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,1These test methods are under the jurisdiction ofASTM Committee D05 on Coaland Coke and are the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Oct.10,2002.Published January 2003.Originallypublished as D 3179 73.Last previous edition D 3179 89(2002)e1.2Annual Book of ASTM Standards,Vol 05.06.3Annual Book of ASTM Standards,Vol 11.01.4Annual Book of ASTM Standards,Vol 14.02.Excerpts appear in the gray pagesof all the volumes.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.where such specifications are available.5Other grades may beused,provided it is first ascertained that the reagent is ofsufficient purity to meet its use without lessening the accuracyof the determination.7.2 WaterUnless otherwise indicated,references to watershall be understood to mean Type II reagent water,conformingto Specification D 1193.8.Sampling and Preparation8.1 The sample shall be the material pulverized to pass No.60(250-m)sieve and well mixed in accordance with MethodD 346 or Method D 2013.In the case of coke and anthracite,grinding the sample to pass a No.200(75-m)or finer sieve isrecommended.8.2 A separate portion of the analysis sample should beanalyzed for moisture content in accordance with Test MethodD 3173,in order to allow calculation of the as-analyzed data toother bases.TEST METHOD AMACRO-NITROGENDETERMINATION WITH ALTERNATIVE METHODINCLUDED9.Scope and Application9.1 This test method describes a macro procedure for thedetermination of nitrogen in both coal and coke,by twoalternative procedures.In both procedur