美国药典USP32测试溶液配制.docx
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美国药典USP32测试溶液配制
TESTSOLUTIONS(TS)
Certainofthefollowingtestsolutionsareintendedforuseasacid-baseindicatorsinvolumetricanalyses.Suchsolutionsshouldbesoadjustedthatwhen0.15mLoftheindicatorsolutionisaddedto25mLofcarbondioxide-freewater,0.25mLof0.02Nacidoralkali,respectively,willproducethecharacteristiccolorchange.SimilarsolutionsareintendedforuseinpHmeasurement.Wherenospecialdirectionsfortheirpreparationaregiven,thesamesolutionissuitableforbothpurposes.
Whereitisdirectedthatavolumetricsolutionbeusedasthetestsolution,standardizationofthesolutionusedasTSisnotrequired.
Ingeneral,thedirectivetoprepareasolution“fresh”indicatesthatthesolutionisoflimitedstabilityandmustbepreparedonthedayofuse.
ForthepreparationofTestSolutions,usereagentsofthequalitydescribedunderReagents.
AcetaldehydeTS—Mix4mLofacetaldehyde,3mLofalcohol,and1mLofwater.Preparethissolutionfresh.
AcetateBufferTS—Dissolve320gofammoniumacetatein500mLofwater,add5mLofglacialaceticacid,dilutewithwaterto1000.0mL,andmix.ThissolutionhasapHbetween5.9and6.0.
AceticAcid,Glacial,TS—DeterminethewatercontentofaspecimenofglacialaceticacidbytheTitrimetricMethod(seeWaterDetermination921).Iftheacidcontainsmorethan0.05%ofwater,addafewmLofaceticanhydride,mix,allowtostandovernight,andagaindeterminethewatercontent.Iftheacidcontainslessthan0.02%ofwater,addsufficientwatertomakethefinalconcentrationbetween0.02%and0.05%,mix,allowtostandovernight,andagaindeterminethewatercontent.Repeattheadjustmentwithaceticanhydrideorwater,asnecessary,untiltheresultingsolutionshowsawatercontentbetween0.02%and0.05%.
AceticAcid,Strong,TS—Add300.0mLofglacialaceticacid,anddilutewithwaterto1000mL.Thissolutioncontainsabout30%(v/v)ofCH3COOHandhasaconcentrationofabout5N.
AceticAcid–AmmoniumAcetateBufferTS—Dissolve77.1gofammoniumacetateinwater,add57mLofglacialaceticacid,anddilutewithwaterto1000mL.
Acetone,Buffered,TS—Dissolve8.15gofsodiumacetateand42gofsodiumchlorideinabout100mLofwater,andadd68mLof0.1Nhydrochloricacidand150mLofacetone.Mix,anddilutewithwaterto500mL.
AcidFerricChlorideTS—Mix60mLofglacialaceticacidwith5mLofsulfuricacid,add1mLofferricchlorideTS,mix,andcool.
AcidFerrousSulfateTS—SeeFerrousSulfate,Acid,TS.
AcidStannousChlorideTS—SeeStannousChloride,Acid,TS.
AcidStannousChlorideTS,Stronger—SeeStannousChloride,Acid,TS.
AlbumenTS—Carefullyseparatethewhitefromtheyolkofastrictlyfreshhen'segg.Shakethewhitewith100mLofwateruntilmixedandallbutthechalazahasundergonesolution;thenfilter.Preparethesolutionfresh.
Alcohol–PhenolTS—Dissolve780mgofphenolinalcoholtomake100mL.
AlcoholicAmmoniaTS—SeeAmmoniaTS,Alcoholic.
AlcoholicMercuricBromideTS—SeeMercuricBromideTS,Alcoholic.
AlcoholicPotassiumHydroxideTS—SeePotassiumHydroxideTS,Alcoholic.
AlkalineCupricCitrateTS—SeeCupricCitrateTS,Alkaline.
AlkalineCupricCitrateTS2—SeeCupricCitrateTS2,Alkaline.
AlkalineCupricIodideTS—SeeCupricIodideTS,Alkaline.
AlkalineCupricTartrateTS(Fehling'sSolution)—SeeCupricTartrateTS,Alkaline.
AlkalineMercuric–PotassiumIodideTS—SeeMercuric–PotassiumIodideTS,Alkaline.
AlkalinePicrateTS—SeePicrateTS,Alkaline.
AlkalineSodiumHydrosulfiteTS—SeeSodiumHydrosulfiteTS,Alkaline.
AmaranthTS—Dissolve20mgofamaranthin10mLofwater.
AminonaphtholsulfonicAcidTS—Accuratelyweigh5gofsodiumsulfite,94.3gofsodiumbisulfite,and700mgof1,2,4-aminonaphtholsulfonicacid,andmix.PrepareaminonaphtholsulfonicacidTSfreshonthedayofusebydissolving1.5gofthedrymixturein10mLofwater.
Ammonia–AmmoniumChlorideBufferTS—Dissolve67.5gofammoniumchlorideinwater,add570mLofammoniumhydroxide,anddilutewithwaterto1000mL.
Ammonia–CyanideTS—Dissolve2gofpotassiumcyanidein15mLofammoniumhydroxide,anddilutewithwaterto100mL.
AmmoniaTS—Itcontainsbetween9.5%and10.5%ofNH3.Preparebydiluting350mLofAmmoniaWater,Stronger(seeinthesection,Reagents)withwatertomake1000mL.
AmmoniaTS,Alcoholic—Asolutionofammoniagasinalcohol.Clear,colorlessliquidhavingastrongodorofammonia.Specificgravity:
about0.80.Itcontainsbetween9%and11%ofNH3.Storeitinalkali-resistantcontainers,inacoldplace.
AmmoniaTS,Stronger—UseAmmoniaWater,Stronger(seeinthesectionReagents).
AmmoniacalPotassiumFerricyanideTS—Dissolve2gofpotassiumferricyanidein75mLofwater,add25mLofammoniumhydroxide,andmix.
AmmoniatedCupricOxideTS—SeeCupricOxide,Ammoniated,TS.
AmmoniumAcetateTS—Dissolve10gofammoniumacetateinwatertomake100mL.
AmmoniumCarbonateTS—Dissolve20gofammoniumcarbonateand20mLofammoniaTSinwatertomake100mL.
AmmoniumChlorideTS—Dissolve10.5gofammoniumchlorideinwatertomake100mL.
AmmoniumChloride–AmmoniumHydroxideTS—Mixequalvolumesofwaterandammoniumhydroxide,andsaturatewithammoniumchloride.
AmmoniumMolybdateTS—Dissolve6.5goffinelypowderedmolybdicacidinamixtureof14mLofwaterand14.5mLofammoniumhydroxide.Coolthesolution,andadditslowly,withstirring,toawell-cooledmixtureof32mLofnitricacidand40mLofwater.Allowtostandfor48hours,andfilterthroughafine-porosity,sintered-glasscrucible.Thissolutiondeterioratesuponstandingandisunsuitableforuseif,upontheadditionof2mLofdibasicsodiumphosphateTSto5mLofthesolution,anabundantyellowprecipitatedoesnotformatonceorafterslightwarming.Storeitinthedark.Ifaprecipitateformsduringstorage,useonlytheclearsupernatant.
AmmoniumOxalateTS—Dissolve3.5gofammoniumoxalateinwatertomake100mL.
AmmoniumPhosphate,Dibasic,TS(AmmoniumPhosphateTS)—Dissolve13gofdibasicammoniumphosphateinwatertomake100mL.
AmmoniumPolysulfideTS—Yellowliquid,madebysaturatingammoniumsulfideTSwithsulfur.
AmmoniumPyrrolidinedithiocarbamate,Saturated,TS—Addabout10gofammoniumpyrrolidinedithiocarbamatetoa1000-mLvolumetricflask,anddilutewithwatertovolume.
AmmoniumReineckateTS—Shakeabout500mgofammoniumreineckatewith20mLofwaterfrequentlyduring1hour,andfilter.Usewithin2days.
AmmoniumSulfideTS—SaturateammoniaTSwithhydrogensulfidebybubblinghydrogensulfidegasthroughthesolutionfor1minute.Thissolutionmustbefreshlyprepared.ThesolutionisnotrenderedturbideitherbymagnesiumsulfateTSorbycalciumchlorideTS(carbonate).Thissolutionisunstableforuseifanabundantprecipitateofsulfurispresent.
Residueonignition:
notmorethan0.05%.
AmmoniumThiocyanateTS—Dissolve8gofammoniumthiocyanateinwatertomake100mL.
AmmoniumVanadateTS—Dissolve2.5gofammoniumvanadatein500mLofboilingwater,cool,andadd20mLofnitricacid.Mix,cool,andaddwatertomake1L.Storeinpolyethylenecontainers.
AnthroneTS—Within12hoursofuse,rapidlydissolve35mgofanthroneinahotmixtureof35mLofwaterand65mLofsulfuricacid.Immediatelycoolinanicebathtoroomtemperature,andfilterthroughglasswool.Allowthesolutiontostandatroomtemperaturefor30minutesbeforeuse.
AntimonyTrichlorideTS—Dissolve20gofantimonytrichlorideinchloroformtomake100mL.Filterifnecessary.
BariumChlorideTS—Dissolve12gofbariumchlorideinwatertomake100mL.
BariumHydroxideTS—Asaturatedsolutionofbariumhydroxideinrecentlyboiledwater.Preparethesolutionfresh.
BariumNitrateTS—Dissolve6.5gofbariumnitrateinwatertomake100mL.
BetanaphtholTS—See2-NaphtholTS.
BiuretReagentTS—Dissolve1.5gofcupricsulfateand6.0gofpotassiumsodiumtartratein500mLofwaterina1000-mLvolumetricflask.Add300mLofcarbonate-freesodiumhydroxidesolution(1in10),dilutewithcarbonate-freesodiumhydroxidesolution(1in10)to1000mL,andmix.
BlueTetrazoliumTS—Dissolve500mgofbluetetrazoliuminalcoholtomake100mL.
BrilliantBlueGTS—Transfer25mgofbrilliantblueGtoa100-mLvolumetricflask,add12.5mLofalcoholand25mLofphosphoricacid,dilutewithwatertovolume,andmix.
BromineTS(BromineWater)—Asaturatedsolutionofbromine,preparedbyagitating2to3mLofbrominewith100mLofcoldwaterinaglass-stopperedbottle,thestopperofwhichshouldbelubricatedwithpetrolatum.Storeitinacoldplace,protectedfromlight.
Bromine–SodiumAcetateTS—Dissolve100gofsodiumacetatein1000mLofglacialaceticacid,add50mLofbromine,andmix.
p-BromoanilineTS—Add8gofp-bromoanilinetoamixtureof380mLofthiourea-saturatedglacialaceticacid,10mLofsodiumchloridesolution(1in5),5mLofoxalicacidsolution(1in20),and5mLofdibasicsodiumphosphatesolution(1in10)inalow-actinicglassbottle.Mix,andallowtostandovernightbeforeusing.Protectfromlight,andusewithin7days.
BromocresolBlueTS—UseBromocresolGreenTS.
BromocresolGreenTS—Dissolve50mgofbromocresolgreenin100mLofalcohol,andfilterifnecessary.
BromocresolGreen–MethylRedTS—Dissolve0.15gofbromocresolgreenand0.1gofmethylredin180mLofalcohol,anddilutewithwaterto200mL.
BromocresolPurpleTS—Dissolve250mgofbromocresolpurplein20mLof