ASTM_D_2361_-_02.pdf

Designation:D 2361 02Standard Test Method forChlorine in Coal1This standard is issued under the fixed designation D 2361;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 This test method pertains to the determination of totalchlorine content in a coal sample.1.2 The values stated in SI units are regarded as thestandard.The values shown in parentheses are for informationonly.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.For specific hazardstatements,see Note 2 and Section 8.2.Referenced Documents2.1 ASTM Standards:D 121 Terminology of Coal and Coke2D 1193 Specification for Reagent Water3D 2013 Test Method of Preparing Coal Samples for Analy-sis2D 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different Bases2E 144 Practice for Safe Use of Oxygen CombustionBombs4E 832 Specification for Laboratory Filter Paper43.Terminology3.1 For definitions of terms used in this test method,refer toTerminology D 121.4.Summary of Test Method4.1 The specimen is oxidized by combustion and the con-tained chlorine is absorbed in alkaline reagents using one of thefollowing two procedures:4.1.1 A weighed specimen is burned in a combustion bombcontaining oxygen under pressure and a small amount ofammonium carbonate solution.4.1.2 A weighed specimen is mixed with Eschka mixtureand heated at a specified temperature in an oxidizing atmo-sphere.4.2 The chlorides contained in the ammonium carbonatesolution noted in 4.1.1 or extracted from the incinerated Eschkamixture noted in 4.1.2 are determined by potentiometrictitration.5.Significance and Use5.1 The purpose of this test method is to measure the totalchlorine content of coal.The chlorine content of coals may beuseful in the evaluation of slagging problems,corrosion inengineering processes,and in the total analysis of coal andcoke.When coal specimens are combusted in accordance withthis test method,the chlorine is quantitatively retained and isrepresentative of the total chlorine content of the whole coal.6.Apparatus6.1 Balance,analytical,with a sensitivity of 0.1 mg.6.2 Apparatus for Bomb Combustion of the Specimen:6.2.1 Combustion Bomb,constructed of materials that arenot affected by the combustion process or products.The bombshall be designed so that all liquid combustion products can becompletely recovered by washing the inner surfaces.Thereshall be no gas leakage during a test.The bomb shall becapable of withstanding a hydrostatic pressure test of 20 MPa(300 psig)at room temperature without stressing any partbeyond its elastic limit.6.2.2 Combustion CrucibleAn open crucible of platinum,quartz,or acceptable base-metal alloy.Base-metal alloy cru-cibles are acceptable,if after a few preliminary firings,theweight does not change significantly between tests.NOTE1Stable crucible weight may be obtained by heat treatingbase-metal crucibles in a muffle furnace for 4 h at a temperature of 500C.6.2.3 Ignition Wire,nickel-chromium(Chromel C)alloy oriron,100 mm length,0.16-mm diameter(No.34 B&S gage).Platinum or palladium wire,0.10-mm diameter(No.38 B&Sgage),may be used.1This test method is under the jurisdiction of ASTM Committee D05 on CoalCoke and is the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Sept.10,2002.Published December 2002.Originallypublished as D 2361 65T.Last previous edition D 2361 95(Reapproved 2001).2Annual Book of ASTM Standards,Vol 05.05.3Annual Book of ASTM Standards,Vol 11.01.4Annual Book of ASTM Standards,Vol 14.02.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.6.2.4 Ignition Circuit,for ignition purposes,capable ofproviding 6 to 16-V ac or dc to the ignition wire.The ignitioncircuit shall be controlled with a momentary switch to avoidelectrical shock to the operator.An ammeter or pilot light isrequired in the circuit to indicate when current is flowing.Astep-down transformer,connected to an ac lighting circuit orbatteries,may be used.6.2.5 Water BathA container large enough to hold thecombustion bomb with enough cooling water to cover thebomb and dissipate the heat generated during the combustionprocess.The container shall be designed to allow a constantflow of water around the combustion bomb.6.3 Apparatus for Eschka Combustion of Specimen:6.3.1 Crucibles,porcelain,30-mL capacity,high or low-form,or platinum or silica crucibles of similar size,for ignitingthe specimen with the Eschka mixture.6.3.2 Muffle Furnace,electrically heated,capable of main-ta