EPA METHOD 9000 Determination of Water in Waste Materials

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1、METHOD9000DETERMINATIONOFWATERINWASTEMATERIALSBYKARLFISCHERTITRATION1.0SCOPEANDAPPLICATION1.1TheKarlFischertitrationtechniqueiscapableofquantifyingthewatercontentofmaterialsfrom1ppmtonearly100%.Coulometrictitrationisusedfordirectanalysisofsampleswithwatercontentsbe

2、tween1ppmand5%,whilevolumetrictitrationismoresuitablefordirectanalysisofhigherlevels(100ppmto100%).Withpropersampledilution,therangeofthecoulometrictechniquecanalsobeextendedto100%water.Bothcoulometricandvolumetricproceduresarepresented.1.2Multiphasicsamplesshouldb

3、eseparatedintophysicalphases(liquid,solid,etc.)priortoanalysistoassurerepresentativealiquotsareanalyzed.1.3Establishingthewatercontentinasamplemaybeusefulforthereasonstofollow.1.3.1Itisusefulindeterminingthetotalcompositionofasample.Incombinationwithotheranalytical

4、results,themassbalanceofasamplecanbedetermined.1.3.2ItisusefulinidentifyingwhichsamplescanbeanalyzedbyInfraredSpectroscopyusingsodiumchloridecellsorwhichrequirezincselenidecells.1.3.3Itisusefulindeterminingtheamountofalcoholinanaqueoussolution.1.3.4Itisusefulwhendi

5、stinguishinganaqueousfromanonaqueoussolution.1.3.5Itisusefulwhensettingthepropermixtureoffeedmaterialsintheincinerationofwaste.2.0SUMMARYOFMETHOD2.1Inthevolumetricprocedure,thesampleoranextractofit,isaddedtoaKarlFischersolventconsistingofsulfurdioxideandanaminediss

6、olvedinanhydrousmethanol.Thissolutionistitratedwithananhydroussolventcontainingiodine.Theiodinetitrantisfirststandardizedbytitratingaknownamountofwater.2.2Inthecoulometricprocedure,thesampleoranextractofit,isinjectedintoanelectrolyticcellcontainingtheKarlFischersol

7、vent,wheretheiodinerequiredforreactionwithwaterisproducedbyanodicoxidationofiodide.Withthistechnique,nostandardizationofreagentsisrequired.2.3Inbothprocedures,theendpointisdeterminedamperometricallywithaplatinumelectrodethatsensesasharpchangeincellresistancewhenthe

8、iodinehasreactedwithallofthewaterinthesample.2.4Inthecoulometricprocedure,thecoulombsofelectricityrequiredtogeneratethenecessaryamountofiodineare