ASTM_D_2441_-_95.pdf

Designation:D 2441 95Standard Test Method forHydrolyzable Chlorine Compounds in Chlorinated AromaticHydrocarbons(Askarels)by Refluxing1This standard is issued under the fixed designation D 2441;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 covers the determination of hydrolyz-able chlorine compounds in chlorinated aromatic hydrocarbons(askarels).1.2 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.For a specifichazard statement,see Section 8.1.3 The values stated in SI units are to be regarded as thestandard.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2,3D 1820 Test Method for Hydrolyzable Chlorine Com-poundsinChlorinatedAromaticHydrocarbons(Askarels)43.Summary of Test Method3.1 This test method uses a quantitative potentiometrictitration using silver nitrate in an essentially nonaqueousmedium to determine chloride ions.These are obtained aftermethanolic sodium hydroxide hydrolysis of unstable chlorinecompounds in chlorinated aromatic hydrocarbons of theaskarel dielectric class.4.Significance and Use4.1 The measured chloride ion,reported as parts per millionin the askarel test specimen,is indicative of the relativestability of the askarel under prescribed conditions of test.4.2 Refluxing with methanolic sodium hydroxide offers thedetection of certain chlorine addition compounds that could bepresent as impurities and do not respond fully to hydrolysis atthe lower temperature used in Test Method D 1820.4.3 Many askarels contain polychlorinated biphenyls(PCBs).Manufacture and sale of PCBs has been prohibited byFederal regulation in the United States since 1978.Theconditions for continued use and the handling and disposal ofPCBs are also regulated.Users of this and other methods formeasuring the properties of askarels containing PCBs areresponsible for following applicable Federal,state,and localregulations.5.Interferences5.1 The presence of compounds containing hydrolyzablehalogen other than chlorine,that is,bromine and iodine,willgive positive results,as will also any other foreign substancecapable of forming an insoluble compound with silver nitrate.Such material would not normally be present in an askarel.5.2 The amount of chloride ions measured when the test isapplied to normally stable askarels is very small,ranging near1 ppm.Therefore,the test must be made in an area where theatmosphere is free of contaminating influences and it isessential to make a blank determination.The value obtained onthe blank will indicate the degree to which the test environ-ment,reagents,and glassware are satisfactory for this type oftesting.6.Apparatus6.1 Flask,borosilicate glass,500-mL,with 24/40 standard-taper joint.6.2 Reflux Condenser,with mated 24/40 standard-taperjoint.6.3 Combination Magnetic Stirrer5and Hot Plate.6.4 Magnetic Stirring Bar.66.5 Microburet,1.0-mL capacity,graduated in 0.01-mLdivisions.6.6 Electrodes,silver and glass.71This test method is under the jurisdiction of ASTM Committee D-27 onElectrical Insulating Liquids and Gasesand is the direct responsibility of Subcom-mittee D27.06on Chemical Test.Current edition approved June 15,1995.Published August 1995.Originallypublished as D 2441 65 T.Last previous edition D 2441 89.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 10.01.4Annual Book of ASTM Standards,Vol 10.03.5A Tempco,Aloe Scientific Co.,St.Louis 3,MO,Catalog No.V-75655 orequivalent is satisfactory.6A TFE-fluorocarbon-covered,1-in.long magnetic stirring bar from FisherScientific Co.,Catalog No.9-311-9 or equivalent is satisfactory.7Beckman Catalog No.39261 silver billet electrode and Catalog No.40498glass electrode have been found satisfactory for this purpose.Although the silverbillet-glass electrode system is preferred,a silver electrode with a mercurous sulfatereference electrode may be used.However,a silver-silver chloride electrode systemshould not be used.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMNOTICE:Thisstandardhaseitherbeensupersededandreplacedbyanewversionordiscontinued.ContactASTMInternational(www.astm.org)forthelatestinformation.6.7 Potentiometer,8suitable for use with the glass elec-trode.7.Reagents and Materials7.1 Purity of ReagentsUse reagent grade chemicals in alltests.Unless otherwise indicated,it is intended that all reagentsshall conform to the specifications of the Committee onAnalytical Reagents of the American