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SynthesisofPotassiumTrioxalatoferrate1242617~1242624Objective：1.Tolearnbasicoperationssuchassynthesis,characterizationandchemicalanalysisofcoordinationcompounds.

2.Todevelopanalyticalandproblemsolvingskillsthroughthepracticeofexperimentaldesign

3.TolearnthesynthesisofPotassiumTrioxalatoferrate(lll)PotassiumTrioxalatoferrate(III)Chemicalformula:2K3·[Fe(C2O4)3]·3H2OColor：brightgreenSolubility:Water(0℃4.7g/100g；100℃117.7g/100g)Ethanol(hard)Stability:110℃itloesitscrystalwater230℃itisdecomposedUsageAsachemicalphotometricagent,sinceitissensitivetolightanddecomposestoyellowcolorwhenexposedtolight:

2K3·[Fe(C2O4)3]·3H2O→3K2C2O4+2FeC2O4+2CO2↑+6H2OAsaneffectivecatalystforsomeorganicreactionsPRINCIPLESSTEP1：Combineammoniumferroussulfateandoxalateacid(NH4)2Fe(SO4)2·6H2O+H2C2O4→FeC2O4·2H2O↓+(NH4)2SO4+H2SO4+4H2OSTEP2:Withthepresenceofexcessamountofoxalateanions,oxidationofferrousoxalatebyhydrogenperoxideproducespotassiumtrioxalatoferrateandferrichydroxide:6FeC2O4·2H2O+3H2O2+6K2C2O4→2Fe(OH)3↓+2K3·[Fe(C2O4)3]+12H2OStep3:Fe(OH)3canbeconvertedtotrioxalatoferratecoordinationcompoundwithproperamountofoxalateacid2Fe(OH)3+3H2C2O4+3K2C2O4→2K3·[Fe(C2O4)3]·3H2OStep4:Theproductcrystallizesaftertheadditionofethanol.Theoverallchemicalequation:

2FeC2O4·2H2O+H202+3K2C2O4+H2C2O4===2K3[Fe(C2O4)3]·3H2OEquipment:Platformbalance，filterflask,thermostaticwaterbath,Buchnerfunnel,phtestpaper,alcoholburner

Chemicals:ammoniumferroussulfate,sulfuricacid(3mol/l),saturatedoxalicacid,saturatedpotassiumoxalate,6％hydrogenperoxide,95％ethanol,potassiumnitrate

solidProcedures:

2.5g(NH4)2Fe(SO4)2·6H20in50mlbeakerAdd3dropsof1mol/LH2SO4Add10mLH2OHeatDissolvecompletelyAdd12.5mlH2C2O4heatinaboilingwaterbathprecipitateAdd25mlH2ORemovethesolutionbytilt-pourprocessRepeat3timesFeC2O4·2H2O(yellowprecipitate)Add5mlsaturatedK2C2O4Heatinthewaterbathat40℃Add5ml6%H2O2,Stirkeeptemperatureat40℃

Fe(Ⅱ)isoxidizedtoFe(Ⅲ)Heatthesolutiontillitboils+4mlH2C2O4

keepboilingand

stirConcentratebysmallsoftfire20mlemeraldsolutioncoolingtoroomtemperature+10ml95％ethanolandalittleKNO3

solidStandingfor1~2hoursFiltratebysuctionWashtheprecipitatewithsomeethanolProductweighNotesWhendissolvingferrousammoniumsulfate,alittleamountofH2SO4shouldbeaddedtopreventtheFe(II)hydrolysisandoxidation.WhenFeC2O4·H20isformed,maintainingtheboilingforafewminutesisrequiredinfavorofcrystalgrainsgrowinguptomakeiteasiertofilter.Keepstirringand(6%)H202shouldbedroppedslowlyundertheconstanttemperatureof40℃.Ifthetemperatureistoolow,theoxidationrateofFe(II)istooslow;buttoohightemperaturecanleadtothedecompositionofH202toaffecttheresultsofFe(II)oxidation.The

timeforboilingtoremoveexcessH2O2shouldnotbetoolong,otherwisetheformedFe(OH)3

precipitation

particleswillbecomelarge,whichisbadforthecoordinationreaction.Duringthecoordinationprocess,H2C2O4shouldbeaddeddropwiseandthePHshouldbecontrolledat3~3.5.IfpHistoolow,thesidereactionswilloccur,sothattheproductsmayhaveyellowpowder

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