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1、MethodIb(ResidualTitration)方法Ib(残留滴定)Principle—SeetheinformationgiveninthesectionPrincipleunderMethodIa.Intheresidualtitration,excessReagentisaddedtothetestspecimen,sufficienttimeisallowedforthereactiontoreachcompletion,andtheunconsumedReagentistitratedwithastandardsolutionofwat
2、erinasolventsuchasmethanol.Theresidualtitrationprocedureisapplicablegenerallyandavoidsthedifficultiesthatmaybeencounteredinthedirecttitrationofsubstancesfromwhichtheboundwaterisreleasedslowly.原理:见方法Ia项下原理部分给出的信息。在残留滴定中,额外的试剂被加入到供试样品中,为反应的完成留下了充分的时间,并且将未消耗掉的试剂与水和某种溶剂(例如,甲醇)的标准溶液一
3、起滴定。残留滴定程序通常是可行的,并避免了可能在直接滴定该物质过程中遇到的困难,这些物质中被束缚水分释放得很缓慢。Apparatus,Reagent,andTestPreparation—UseMethodIa.仪器、试剂、供试配制液:同方法Ia。StandardizationofWaterSolutionforResidualTitration—PrepareaWaterSolutionbydiluting2mLofwaterwithmethanolorothersuitablesolventto1000mL.Standardizethissolut
4、ionbytitrating25.0mLwiththeReagent,previouslystandardizedasdirectedunderStandardizationoftheReagent.Calculatethewatercontent,inmgpermL,oftheWaterSolutiontakenbytheformula:用于残留滴定的水溶液的标准化:以甲醇或其他适当溶剂将2mL水稀释至1000mL,以配制水溶液。使用此前已经按照试剂的标准化项下规定进行过标准化的试剂,对25mL此溶液进行滴定,从而对其进行标准化。按照下面的公式,计算
5、此水溶液中的水分含量(单位mg/mL):V¢F/25,inwhichV¢isthevolumeoftheReagentconsumed,andFisthewaterequivalencefactoroftheReagent.DeterminethewatercontentoftheWaterSolutionweekly,andstandardizetheReagentagainstitperiodicallyasneeded.其中,V¢是消耗掉的试剂,F是试剂的水平衡因子。每周测定水溶液的水分含量,并据此根据需要定期对试剂进行标准化。Procedure
6、—WheretheindividualmonographspecifiesthatthewatercontentistobedeterminedbyMethodIb,transfer35to40mLofmethanolorothersuitablesolventtothetitrationvessel,andtitratewiththeReagenttotheelectrometricorvisualendpoint.QuicklyaddtheTestPreparation,mix,andaddanaccuratelymeasuredexcessoft
7、heReagent.Allowsufficienttimeforthereactiontoreachcompletion,andtitratetheunconsumedReagentwithstandardizedWaterSolutiontotheelectrometricorvisualendpoint.Calculatethewatercontentofthespecimen,inmg,takenbytheformula:步骤:当具体各论中规定用方法Ib测定水分含量时,将35至40mL甲醇或其他适当溶剂转移至该滴定容器,并用试剂滴定至测电法或视觉
8、观察的终点。快速加入供试配制品,混匀,并加入精确称量的额外试剂。留下充分的时间以使该反应完成,