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1、METHOD9077TESTMETHODSFORTOTALCHLORINEINNEWANDUSEDPETROLEUMPRODUCTS(FIELDTESTKITMETHODS)1.0SCOPEANDAPPLICATION1.1Themethodmaybeusedtodetermineifaneworusedpetroleumproductmeetsorexceedsrequirementsfortotalhalogenmeasuredaschloride.Ananalysisofthechlorinecontentofpetrol
2、eumproductsisoftenrequiredpriortotheiruseasafuel.Themethodisspecificallydesignedforusedoilspermittingonsitetestingatremotelocationsbynontechnicalpersonneltoavoidthedelaysforlaboratorytesting.1.2Inthesefieldtestmethods,theentireanalyticalsequence,includingsampling,sam
3、plepretreatment,chemicalreactions,extraction,andquantification,arecombinedinasinglekitusingpredispensedandencapsulatedreagents.Theoverallobjectiveistoprovideasimple,easytouseprocedure,permittingnontechnicalpersonneltoperformatestwithanalyticalaccuracyoutsideofalabora
4、toryenvironmentinunder10minutes.Oneofthekitsispresetat1,000µg/gtotalchlorinetomeetregulatoryrequirementsforusedoils.Theotherkitsprovidequantitativeresultsoverarangeof750to7,000µg/gand300to4,000µg/g.2.0SUMMARYOFMETHOD2.1Theoilsample(around0.4gbyvolume)isdispersedinaso
5、lventandreactedwithamixtureofmetallicsodiumcatalyzedwithnaphthaleneanddiglymeatambienttemperature.Thisprocessconvertsallorganichalogenstotheirrespectivesodiumhalides.Allhalidesinthetreatedmixture,includingthosepresentpriortothereaction,arethenextractedintoanaqueousbu
6、ffer,whichisthentitratedwithmercuricnitrateusingdiphenylcarbazoneastheindicator.Theendpointofthetitrationistheformationoftheblue-violetmercurydiphenylcarbazonecomplex.Bromideandiodidearetitratedandreportedaschloride.2.2Reagentquantitiesarepresetinthefixedendpointkit(
7、MethodA)sothatthecolorofthesolutionattheendofthetitrationindicateswhetherthesampleisabove1,000µg/gchlorine(yellow)orbelow1,000µg/gchlorine(blue).2.3Thefirstquantitativekit(MethodB)involvesareversetitrationofafixedvolumeofmercuricnitratewiththeextractedsamplesuchthatt
8、heendpointisdenotedbyachangefrombluetoyellowinthetitrationvesselovertherangeofthekit(750to7,000µg/g).Thefinalcalculationisbasedonth
