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General Chapters: <191> IDENTIFICATION TESTS-GENERAL

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191

IDENTIFICATIONTESTSGENERAL

UnderthisheadingareplacedteststhatarefrequentlyreferredtointhePharmacopeiafortheidentificationofofficial articles.[NOTEThetestsarenotintendedtobeapplicabletomixturesofsubstancesunlesssospecified.] AcetateWhenaceticacidoranacetateiswarmedwithsulfuricacidandalcohol,ethylacetate,recognizablebyits characteristicodor,isevolved.Withneutralsolutionsofacetates,ferricchlorideTSproducesadeepredcolorthatis destroyedbytheadditionofmineralacids. AluminumWith6Nammoniumhydroxide,solutionsofaluminumsaltsyieldagelatinous,whiteprecipitatethatis insolubleinanexcessof6Nammoniumhydroxide.1NsodiumhydroxideorsodiumsulfideTSproducesthesame precipitate,whichdissolvesinanexcessofeitherofthesereagents. AmmoniumAmmoniumsaltsaredecomposedbytheadditionofanexcessof1Nsodiumhydroxide,withtheevolution ofammonia,recognizablebyitsodorandbyitsalkalineeffectuponmoistenedredlitmuspaperexposedtothevapor. Warmingthesolutionacceleratesthedecomposition. AntimonyWithhydrogensulfide,solutionsofantimony(III)compounds,stronglyacidifiedwithhydrochloricacid,yieldan orangeprecipitateofantimonysulfidethatisinsolublein6Nammoniumhydroxide,butissolubleinammoniumsulfideTS. BariumSolutionsofbariumsaltsyieldawhiteprecipitatewith2Nsulfuricacid.Thisprecipitateisinsolublein hydrochloricacidandinnitricacid.Bariumsaltsimpartayellowishgreencolortoanonluminousflamethatappearsblue whenviewedthroughgreenglass. BenzoateInneutralsolutions,benzoatesyieldasalmoncoloredprecipitatewithferricchlorideTS.Inmoderately concentratedsolutions,benzoatesyieldaprecipitateofbenzoicaciduponacidificationwith2Nsulfuricacid.This precipitateisreadilysolubleinethylether. BicarbonateSeeCarbonate. BismuthWhendissolvedinaslightexcessofnitricacidorhydrochloricacid,bismuthsaltsyieldawhiteprecipitateupon dilutionwithwater.Thisprecipitateiscoloredbrownbyhydrogensulfide,andtheresultingcompounddissolvesinawarm mixtureofequalpartsofnitricacidandwater. BisulfiteSeeSulfite. BorateTo1mLofaboratesolution,acidifiedwithhydrochloricacidtolitmus,add3or4dropsofiodineTSand3or4 dropsofpolyvinylalcoholsolution(1in50):anintensebluecolorisproduced.Whenaborateistreatedwithsulfuricacid,
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General Chapters: <191> IDENTIFICATION TESTS-GENERAL

methanolisadded,andthemixtureisignited,itburnswithagreenborderedflame. BromideSolutionsofbromides,upontheadditionofchlorineTS,dropwise,liberatebromine,whichisdissolvedby shakingwithchloroform,coloringthechloroformredtoreddishbrown.SilvernitrateTSproducesinsolutionsofbromidesa yellowishwhiteprecipitatethatisinsolubleinnitricacidandisslightlysolublein6Nammoniumhydroxide. CalciumSolutionsofcalciumsaltsforminsolubleoxalateswhentreatedasfollows.Toasolutionofthecalciumsalt(1in 20)add2dropsofmethylredTS,andneutralizewith6Nammoniumhydroxide.Add3Nhydrochloricacid,dropwise,until thesolutionisacidtotheindicator.UpontheadditionofammoniumoxalateTS,awhiteprecipitateisformed.This precipitateisinsolublein6Naceticacidbutdissolvesinhydrochloricacid.Calciumsaltsmoistenedwithhydrochloricacid impartatransientyellowishredcolortoanonluminousflame. CarbonateCarbonatesandbicarbonateseffervescewithacids,evolvingacolorlessgasthat,whenpassedintocalcium hydroxideTS,producesawhiteprecipitateimmediately.Acoldsolution(1in20)ofasolublecarbonateiscoloredredby phenolphthaleinTS,whileasimilarsolutionofabicarbonateremainsunchangedorisonlyslightlycolored. ChlorateSolutionsofchloratesyieldnoprecipitatewithsilvernitrateTS.Theadditionofsulfurousacidtothismixture producesawhiteprecipitatethatisinsolubleinnitricacid,butissolublein6Nammoniumhydroxide.Uponignition, chloratesyieldchlorides,recognizablebyappropriatetests.Whensulfuricacidisaddedtoadrychlorate,decrepitation occurs,andagreenishyellowgasisevolved.[CautionUseonlyasmallamountofchlorateforthistest,andexercise extremecautioninperformingit.] ChlorideWithsilvernitrateTS,solutionsofchloridesyieldawhite,curdyprecipitatethatisinsolubleinnitricacidbutis solubleinaslightexcessof6Nammoniumhydroxide.Whentestingamine(includingalkaloidal)hydrochloridesthatdonot respondtotheabovetest,addonedropofdilutednitricacidand0.5mLofsilvernitrateTStoasolutionofthesubstance beingexaminedcontaining,unlessotherwisedirectedinthemonograph,about2mgofchlorideionin2mL:awhite,curdy precipitateisformed.Centrifugethemixturewithoutdelay,anddecantthesupernatantlayer.Washtheprecipitatewith three1mLportionsofnitricacidsolution(1in100),anddiscardthewashings.AddammoniaTSdropwisetothis precipitate.Itdissolvesreadily.Whenamonographspecifiesthatanarticlerespondstothetestfordrychlorides,mixthe solidtobetestedwithanequalweightofmanganesedioxide,moistenwithsulfuricacid,andgentlyheatthemixture: chlorine,whichisrecognizablebytheproductionofabluecolorwithmoistenedstarchiodidepaper,isevolved. CitrateTo15mLofpyridineaddafewmgofacitratesalt,dissolvedorsuspendedin1mLofwater,andshake.Tothis mixtureadd5mLofaceticanhydride,andshake:alightredcolorisproduced. CobaltSolutionsofcobaltsalts(1in20)in3Nhydrochloricacidyieldaredprecipitatewhenheatedonasteambathwith anequalvolumeofahot,freshlypreparedsolutionof1nitroso2naphthol(1in10)in9Naceticacid.Solutionsofcobalt salts,whensaturatedwithpotassiumchlorideandtreatedwithpotassiumnitriteandaceticacid,yieldayellowprecipitate. CopperSolutionsofcupriccompounds,acidifiedwithhydrochloricacid,depositaredfilmofmetalliccopperupona bright,untarnishedsurfaceofmetalliciron.Anexcessof6Nammoniumhydroxide,addedtoasolutionofacupricsalt, producesfirstabluishprecipitateandthenadeepbluecoloredsolution.WithpotassiumferrocyanideTS,solutionsof cupricsaltsyieldareddishbrownprecipitate,insolubleindilutedacids. HypophosphiteWhenstronglyheated,hypophosphitesevolvespontaneouslyflammablephosphine.Hypophosphitesin solutionyieldawhiteprecipitatewithmercuricchlorideTS.Thisprecipitatebecomesgraywhenanexcessof hypophosphiteispresent.Solutionsofhypophosphites,acidifiedwithsulfuricacid,andwarmedwithcupricsulfateTSyield aredprecipitate. IodideSolutionsofiodides,upontheadditionofchlorineTS,dropwise,liberateiodine,whichcolorsthesolutionyellowto red.Whenthesolutionisshakenwithchloroform,thelatteriscoloredviolet.Theiodinethusliberatedgivesabluecolor withstarchTS.SilvernitrateTSproduces,insolutionsofiodides,ayellow,curdyprecipitatethatisinsolubleinnitricacid andin6Nammoniumhydroxide. IronFerrousandferriccompoundsinsolutionyieldablackprecipitatewithammoniumsulfideTS.Thisprecipitateis dissolvedbycold3Nhydrochloricacidwiththeevolutionofhydrogensulfide.
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General Chapters: <191> IDENTIFICATION TESTS-GENERAL

FerricSaltsAcidsolutionsofferricsaltsyieldadarkblueprecipitatewithpotassiumferrocyanideTS.Withanexcessof 1Nsodiumhydroxide,areddishbrownprecipitateisformed.WithammoniumthiocyanateTS,solutionsofferricsalts produceadeepredcolorthatisnotdestroyedbydilutemineralacids. FerrousSaltsSolutionsofferroussaltsyieldadarkblueprecipitatewithpotassiumferricyanideTS.Thisprecipitateis insolublein3Nhydrochloricacidbutisdecomposedby1Nsodiumhydroxide.With1Nsodiumhydroxide,solutionsof ferroussaltsyieldagreenishwhiteprecipitate,thecolorrapidlychangingtogreenandthentobrownwhenshaken. LactateWhensolutionsoflactatesareacidifiedwithsulfuricacid,potassiumpermanganateTSisadded,andthemixture isheated,acetaldehydeisevolved.Thiscanbedetectedbyallowingthevaportocomeintocontactwithafilterpaperthat hasbeenmoistenedwithafreshlypreparedmixtureofequalvolumesof20%aqueousmorpholineandsodium nitroferricyanideTS:abluecolorisproduced. LeadWith2Nsulfuricacid,solutionsofleadsaltsyieldawhiteprecipitatethatisinsolublein3Nhydrochloricor2N nitricacid,butissolubleinwarm1NsodiumhydroxideandinammoniumacetateTS.WithpotassiumchromateTS, solutionsofleadsalts,freeornearlyfreefrommineralacids,yieldayellowprecipitatethatisinsolublein6Naceticacid butissolublein1Nsodiumhydroxide. LithiumWithsodiumcarbonateTS,moderatelyconcentratedsolutionsoflithiumsalts,madealkalinewithsodium hydroxide,yieldawhiteprecipitateonboiling.TheprecipitateissolubleinammoniumchlorideTS.Lithiumsaltsmoistened withhydrochloricacidimpartanintensecrimsoncolortoanonluminousflame.Solutionsoflithiumsaltsarenotprecipitated by2Nsulfuricacidorsolublesulfates(distinctionfromstrontium). MagnesiumSolutionsofmagnesiumsaltsinthepresenceofammoniumchlorideyieldnomorethanaslightlyhazy precipitatewhenneutralizedwithammoniumcarbonateTS,butonthesubsequentadditionofdibasicsodiumphosphate TS,awhite,crystallineprecipitate,whichisinsolublein6Nammoniumhydroxide,isformed. ManganeseWithammoniumsulfideTS,solutionsofmanganoussaltsyieldasalmoncoloredprecipitatethatdissolvesin aceticacid. MercuryWhenappliedtobrightcopperfoil,solutionsofmercurysalts,freefromanexcessofnitricacid,yieldadeposit thatuponrubbing,becomesbrightandsilveryinappearance.Withhydrogensulfide,solutionsofmercurycompoundsyield ablackprecipitatethatisinsolubleinammoniumsulfideTSandinboiling2Nnitricacid. MercuricSaltsSolutionsofmercuricsaltsyieldayellowprecipitatewith1Nsodiumhydroxide.Theyyieldalso,inneutral solutionswithpotassiumiodideTS,ascarletprecipitatethatisverysolubleinanexcessofthereagent. MercurousSaltsMercurouscompoundsaredecomposedby1Nsodiumhydroxide,producingablackcolor.With hydrochloricacid,solutionsofmercuroussaltsyieldawhiteprecipitatethatisblackenedby6Nammoniumhydroxide.With potassiumiodideTS,ayellowprecipitate,thatmaybecomegreenuponstanding,isformed. NitrateWhenasolutionofanitrateismixedwithanequalvolumeofsulfuricacid,themixtureiscooled,andasolutionof ferroussulfateissuperimposed,abrowncolorisproducedatthejunctionofthetwoliquids.Whenanitrateisheatedwith sulfuricacidandmetalliccopper,brownishredfumesareevolved.Nitratesdonotdecolorizeacidifiedpotassium permanganateTS(distinctionfromnitrites ). NitriteWhentreatedwithdilutemineralacidsorwith6Naceticacid,nitritesevolvebrownishredfumes.Thesolution colorsstarchiodidepaperblue. OxalateNeutralandalkalinesolutionsofoxalatesyieldawhiteprecipitatewithcalciumchlorideTS.Thisprecipitateis insolublein6Naceticacidbutisdissolvedbyhydrochloricacid.Hotacidifiedsolutionsofoxalatesdecolorizepotassium permanganateTS. PermanganateSolutionsofpermanganatesacidifiedwithsulfuricacidaredecolorizedbyhydrogenperoxideTSandby sodiumbisulfiteTS,inthecold,andbyoxalicacidTS,inhotsolution. PeroxideSolutionsofperoxidesslightlyacidifiedwithsulfuricacidyieldadeepbluecolorupontheadditionofpotassium dichromateTS.Onshakingthemixturewithanequalvolumeofethyletherandallowingtheliquidstoseparate,theblue
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General Chapters: <191> IDENTIFICATION TESTS-GENERAL

colorisfoundintheethyletherlayer. Phosphate[NOTEWherethemonographspecifiestheidentificationtestforPhosphate,usethetestsfor orthophosphates,unlesstheinstructionsspecifytheuseofthepyrophosphatetestsorindicatethattheproductistobe ignitedbeforeperformingthetest.]WithsilvernitrateTS,neutralsolutionsoforthophosphatesyieldayellowprecipitatethat issolublein2Nnitricacidandin6Nammoniumhydroxide.WithammoniummolybdateTS,acidifiedsolutionsof orthophosphatesyieldayellowprecipitatethatissolublein6Nammoniumhydroxide.Thisprecipitatemaybeslowtoform. WithsilvernitrateTS,pyrophosphatesobtainedbyignitionyieldawhiteprecipitatethatissolublein2Nnitricacidandin6 Nammoniumhydroxide.WithammoniummolybdateTS,ayellowprecipitatethatissolublein6Nammoniumhydroxideis formed. PotassiumPotassiumcompoundsimpartavioletcolortoanonluminousflame,butthepresenceofsmallquantitiesof sodiummasksthecolorunlesstheyellowcolorproducedbysodiumisscreenedoutbyviewingthroughabluefilterthat blocksemissionat589nm(sodium)butistransparenttoemissionat404nm(potassium).Traditionally,cobaltglasshas beenused,butothersuitablefiltersarecommerciallyavailable.Inneutral,concentratedormoderatelyconcentrated solutionsofpotassiumsalts(dependinguponthesolubilityandthepotassiumcontent),sodiumbitartrateTSproducesa whitecrystallineprecipitatethatissolublein6Nammoniumhydroxideandinsolutionsofalkalihydroxidesandcarbonates. Theformationoftheprecipitate,whichisusuallyslow,isacceleratedbystirringorrubbingtheinsideofthetesttubewitha glassrod.Theadditionofasmallamountofglacialaceticacidoralcoholalsopromotestheprecipitation. SalicylateInmoderatelydilutesolutionsofsalicylates,ferricchlorideTSproducesavioletcolor.Theadditionofacidsto moderatelyconcentratedsolutionsofsalicylatesproducesawhite,crystallineprecipitateofsalicylicacidthatmelts between158 and161 . SilverWithhydrochloricacid,solutionsofsilversaltsyieldawhite,curdyprecipitatethatisinsolubleinnitricacid,butis readilysolublein6Nammoniumhydroxide.Asolutionofasilversalttowhich6Nammoniumhydroxideandasmall quantityofformaldehydeTSareaddeddeposits,uponwarming,amirrorofmetallicsilveruponthesidesofthecontainer. SodiumUnlessotherwisespecifiedinanindividualmonograph,prepareasolutiontocontain0.1gofthesodium compoundin2mLofwater.Add2mLof15%potassiumcarbonate,andheattoboiling.Noprecipitateisformed.Add4mL ofpotassiumpyroantimonateTS,andheattoboiling.Allowtocoolinicewaterand,ifnecessary,rubtheinsideofthetest tubewithaglassrod.Adenseprecipitateisformed.Sodiumcompoundsimpartanintenseyellowcolortoanonluminous flame. SulfateWithbariumchlorideTS,solutionsofsulfatesyieldawhiteprecipitatethatisinsolubleinhydrochloricacidandin nitricacid.WithleadacetateTS,neutralsolutionsofsulfatesyieldawhiteprecipitatethatissolubleinammoniumacetate TS.Hydrochloricacidproducesnoprecipitatewhenaddedtosolutionsofsulfates(distinctionfromthiosulfates ). SulfiteWhentreatedwith3Nhydrochloricacid,sulfitesandbisulfitesyieldsulfurdioxide,whichblackensfilterpaper moistenedwithmercurousnitrateTS. TartrateDissolveafewmgofatartratesaltin2dropsofsodiummetaperiodatesolution(1in20).Addadropof1N sulfuricacid,andafter5minutesaddafewdropsofsulfurousacidfollowedbyafewdropsoffuchsinsulfurousacidTS:a reddishpinkcolorisproducedwithin15minutes. ThiocyanateWithferricchlorideTS,solutionsofthiocyanatesyieldaredcolorthatisnotdestroyedbymoderately concentratedmineralacids. ThiosulfateWithhydrochloricacid,solutionsofthiosulfatesyieldawhiteprecipitatethatsoonturnsyellow,andsulfur dioxide,whichblackensfilterpapermoistenedwithmercurousnitrateTS.TheadditionofferricchlorideTStosolutionsof thiosulfatesproducesadarkvioletcolorthatquicklydisappears. ZincInthepresenceofsodiumacetate,solutionsofzincsaltsyieldawhiteprecipitatewithhydrogensulfide.This precipitateisinsolubleinaceticacid,butisdissolvedby3Nhydrochloricacid.AmmoniumsulfideTSproducesasimilar precipitateinneutralandinalkalinesolutions.WithpotassiumferrocyanideTS,zincsaltsinsolutionyieldawhite precipitatethatisinsolublein3Nhydrochloricacid.
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General Chapters: <191> IDENTIFICATION TESTS-GENERAL

AuxiliaryInformationStaffLiaison:AntonioHernandezCardoso,B.S.,Scientist,LatinAmericanSpecialist ExpertCommittee:(GC05)GeneralChapters05 USP29NF24Page2550 PharmacopeialForum:VolumeNo.27(6)Page3349 PhoneNumber:13018168308

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