文獻(xiàn)-電化學(xué)氧化處理水體及廢水中有機(jī)污染物的sb摻雜鈦基sno2陽(yáng)極的制備條件的優(yōu)化_第1頁(yè)
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OPTIMIZATIONOFTI/SNO2SB2O5ANODEPREPARATIONFORELECTROCHEMICALOXIDATIONOFORGANICCONTAMINANTSINWATERANDWASTEWATERRICHARDJWATTS,MEGANSWYETH,DENNISDFINN,AMYLTEELRECEIVED17JANUARY2007/REVISED23JULY2007ACCEPTED26JULY2007PUBLISHEDONLINE23AUGUST2007SPRINGERSCIENCEBUSINESSMEDIABV2007ABSTRACTTHEPREPARATIONOFANTIMONYDOPEDTINOXIDEANODESONATITANIUMSUBSTRATETI/SNO2SB2O5ANODESBYDIPPINGINASOLUTIONOFTINCHLORIDEANDANTIMONYCHLORIDEANDANNEALINGATHIGHTEMPERATURESWASOPTIMIZEDFORTHEPOTENTIALAPPLICATIONSOFDRINKINGWATERDISINFECTION,WASTEWATEREFUENTDISINFECTION,ANDINDUSTRIALWASTESTREAMTREATMENTTHEEFFECTIVENESSOFTI/SNO2SB2O5ANODESPREPAREDUNDERDIFFERENTCONDITIONSWASEVALUATEDBYUSINGHEXANOLASAPROBEMOLECULETOMEASURETHEEXTENTOFOXIDATIVEREACTIONS,ANDANODEPERFORMANCEWASMONITOREDBYCYCLICVOLTAMMETRYALARGEFACTORIALMATRIXCONSISTINGOFTINCHLORIDECONCENTRATIONANTIMONYCHLORIDECONCENTRATIONANNEALINGTEMPERATUREWASRSTEVALUATED,ANDTHEOPTIMUMCONDITIONSWEREFOUNDTOBE20TINCHLORIDEAND1ANTIMONYCHLORIDEINTHEDIPSOLUTIONANDANANNEALINGTEMPERATUREOF500FURTHERINVESTIGATIONSHOWEDTHATTHERATEOFWITHDRAWALFROMTHEDIPSOLUTION,THENUMBEROFCOATINGSOFTHEDIPSOLUTION,ANDTHEADDITIONOFOXYGENDURINGANNEALINGDIDNOTSIGNICANTLYAFFECTANODEPERFORMANCEUNDEROPTIMUMPREPARATIONCONDITIONS,TI/SNO2SB2O5ANODESSHOWEDNOLOSSOFPERFORMANCEOVER1,280CYCLESOFCYCLICVOLTAMMETRY,SUGGESTINGTHATTHEIRPERFORMANCECANBESUSTAINEDOVERLONGPERIODSOFUSETHERESULTOFTHISRESEARCHISASIMPLEPREPARATIONMETHODFOREFFECTIVEANDLONGLIVEDTI/SNO2SB2O5ANODESTHISMETHODCOULDBEEASILYADOPTEDBYAUTILITYFORPILOTORFULLSCALEDISINFECTIONOFWATERANDWASTEWATERANDTHETREATMENTOFINDUSTRIALWASTESTREAMSKEYWORDSANODEPREPARATIONTINOXIDEANODESDRINKINGWATERDISINFECTIONELECTROCHEMICALDISINFECTIONINDUSTRIALWASTETREATMENTWASTEWATEREFUENTDISINFECTION1INTRODUCTIONNUMEROUSCHEMICALANDPHYSICALAGENTSHAVEBEENUSEDFORTHEDISINFECTIONOFDRINKINGWATERANDWASTEWATEREFUENTSHOWEVER,ALLOFTHEPROCESSESCURRENTLYINUSEHAVEDISADVANTAGESCHLORINEISTHEMOSTCOMMONLYUSEDDISINFECTANTBECAUSEOFITSLOWCOSTHOWEVER,ITISNOTEFFECTIVEAGAINSTGIARDAANDCRYPTOSPORIDIUM1FURTHERMORE,THEFORMATIONOFCHLORINATEDBYPRODUCTS2,3ANDTHEPOSSIBILITYOFTANKRUPTURESANDTHERELEASEOFTOXICGASTOTHEATMOSPHERE4CREATESIGNICANTSAFETYCONCERNSOZONEANDULTRAVIOLETUVLIGHTARESOMETIMESUSEDASALTERNATIVESTOCHLORINE,BUTTHESETECHNOLOGIESARELIMITEDBYHIGHOPERATIONANDMAINTENANCECOSTS5ASANALTERNATIVETOTHESETECHNOLOGIES,SEVERALELECTROCHEMICALSYSTEMSHAVERECENTLYBEENSTUDIEDFORWATERDISINFECTIONUSINGELECTRODESCOMPOSEDOFTITANIUM6,CARBONCLOTH7,8,GRAPHITE9,TITANIUMNITRIDE10,PLATINUM11,PLATINUMCOATEDWITHNIOBIUM12,TITANIUMCOATEDWITHRUTHENIUMOXIDERUO21316,ANDBORONDOPEDDIAMOND17,18HYDROXYLRADICALGENERATEDATTHEANODESURFACEISLIKELYTHEDISINFECTINGAGENTINTHESESYSTEMS12,19,20TITANIUMANODESCOATEDWITHANTIMONYDOPEDTINOXIDETI/SNO2SB2O5ALSOGENERATEHYDROXYLRADICAL21,22RECENTLY,LOGEETAL23INVESTIGATEDTHEEFCACYOFTI/SNO2SB2O5ANODESFORWASTEWATEREFUENTDISINFECTIONTHEYWEREABLETOACHIEVEMULTILOGDISINFECTIONOFCOLIFORMBACTERIA,ANDPROVIDEDANECONOMICANALYSISDEMONSTRATINGTHATFULLSCALEEFUENTDISINFECTIONWITHTI/SNO2SB2O5ANODESMAYBEMOREECONOMICALTHANUVDISINFECTIONTHEIRRESULTSSUGGESTTHATTI/SNO2SB2O5ANODESHAVEAHIGHDEGREEOFPOTENTIALFORTHEFULLSCALEDISINFECTIONOFWASTEWATEREFUENTSTHESEANODESHAVEALSOBEENUSEDTOTREATCODINWASTEWATER24ANDTOTREATLANDLLLEACHATERESULTINGINDECOLORIZATION,CODREMOVAL,ANDCOMPLETEELIMINATIONOFAMMONIA25FURTHERMORE,TINOXIDEANDANTIMONYDOPEDTINOXIDEANODESCANALSOOXIDIZEORGANICCOMPOUNDSSUCHASPHENOL2628PMETHOXYPHENOL29,PENTACHLOROPHENOL30,BISPHENOLA31,ANILINE32,ANDACETOMINOPHEN33THESERESULTSSUGGESTTHATTI/SNO2SB2O5ANODESCANDESTROYORGANICCONTAMINANTSINWATERSIMULTANEOUSLYWITHTHEINACTIVATIONOFPATHOGENSRESULTSTODATEOBTAINEDINBENCHSCALEINVESTIGATIONSSUGGESTTHATTI/SNO2SB2O5ANODESMAYPROVIDEANEFFECTIVEANDECONOMICALALTERNATIVETOOTHERTREATMENTSYSTEMSFORCONTAMINANTDESTRUCTIONANDWATERANDWASTEWATEREFUENTDISINFECTIONTHESEANODESAPPEARTOHAVETHEGREATESTPOTENTIALFORFULLSCALEAPPLICATIONINWATERTREATMENTANDWASTEWATEREFUENTSYSTEMSTHATUSESINGLECHAMBERSYSTEMS,SUCHASPLUGOWPFORCONTINUOUSLYSTIRREDTANKREACTORSANTIMONYDOPEDTINOXIDEANODESHAVEASIGNICANTADVANTAGEOVEROTHERELECTRODESYSTEMSFORSUCHSINGLECHAMBERAPPLICATIONSBECAUSEOFTHEMINIMALBACKREACTIONSTHATOCCURATTHECATHODE34HOWEVER,SCALEUPANDLONGTERMUSEOFTI/SNO2SB2O5ANODESYSTEMSREQUIRETHATTHEELECTRODESBEPREPAREDUSINGCONDITIONSTHATPROVIDETHEMOSTEFFECTIVEANDEFCIENTPERFORMANCEANTIMONYDOPEDTINOXIDEANODESHAVEPREVIOUSLYBEENPREPAREDONTITANIUMSUBSTRATESBYSPRAYPYROLYSIS35,SOLGELAPPLICATION36,CHEMICALVAPORDEPOSITION37,ANDMANUALAPPLICATIONOFTINANTIMONYSOLUTIONSUSINGAPAINTBRUSH38HOWEVER,LOGEETAL23REPORTEDTHATMECHANICALDIPCOATINGOFTITANIUMRODSINATINANTIMONYSOLUTIONWASASIMPLEANDCOSTEFFECTIVEPREPARATIONMETHODBECAUSETI/SNO2SB2O5ANODESARENOTCURRENTLYCOMMERCIALLYAVAILABLE,UTILITIESWOULDNEEDANEFFECTIVEMETHODTOPREPARETHEANODESFORPILOTORFULLSCALEUSETHEPURPOSEOFTHISRESEARCHWASTODETERMINETHEMOSTEFFECTIVECONDITIONSFORTHEPREPARATIONOFSUCHDIPCOATEDTI/SNO2SB2O5ANODESFORTHEELECTROCHEMICALDISINFECTIONOFDRINKINGWATERANDWASTEWATEREFUENTSANDTHETREATMENTOFINDUSTRIALWASTESTREAMS2EXPERIMENTAL21MATERIALSHEXANOL,CARBONTETRACHLORIDE,CHLOROFORM,HEXACHLOROETHANE,HEXANE,SODIUMBICARBONATE,SODIUMSULFATE,SODIUMPERCHLORATE,ISOPROPANOL,TINCHLORIDEPENTAHYDRATE,ANTIMONYCHLORIDE,ANDTINSULFATEWEREPURCHASEDFROMSIGMAALDRICHHYDROCHLORICACIDANDSULFURICACIDWEREOBTAINEDFROMJTBAKERTITANIUMRODS2MMDIAMETERWEREPURCHASEDFROMGOODFELLOWMETALS22DEVELOPMENTOFPREPARATIONMETHODSFORTI/SNO2SB2O5ANODESTHEINITIALCONDITIONSFORINVESTIGATINGTHEPREPARATIONOFTI/SNO2SB2O5ANODESWEREBASEDONTHEPROCEDURESOFLIPPANDPLETCHER38ANDLOGEETAL23TITANIUMRODSWEREPREPAREDBYBEADBLASTING,SONICATIONINISOPROPANOL,BOILINGIN115MHCL,RINSINGINDISTILLEDWATER,ANDAIRDRYINGLAYERSOFTINANTIMONYWERETHENAPPLIEDBYDIPPINGTHERODSINISOPROPANOLCONTAININGTINCHLORIDEANDANTIMONYCHLORIDE,DRYINGAT100FOR10MIN,ANDANNEALINGINAMUFEFURNACEFOR20MINBECAUSETI/SNO2SB2O5ANODESARENOTCOMMERCIALLYAVAILABLE,AMATRIXOFCONDITIONSWASEMPLOYEDTOEVALUATETHEMOSTEFFECTIVEPROCEDUREFORPREPARINGTHEANODESTHEVARIABLESINVESTIGATEDINCLUDEDTINCHLORIDECONCENTRATIONINTHEDIPPINGSOLUTION520MGL1,ANTIMONYCHLORIDECONCENTRATIONINTHEDIPPINGSOLUTION0110GL1,ANNEALINGTEMPERATURES400600,ANDOXYGENOWRATESDURINGANNEALING08LMIN1ANODESWEREDRIEDFOR20MINBETWEENEACHDIPAFTERTHEPREPARATIONOFAGROUPOFEIGHTANODESWASCOMPLETE,THEANODESWEREPLACEDINAHOLDERTTEDTOA200MLBATCHREACTORMATCHEDWITHSTAINLESSSTEELCATHODESTHEANODESANDCATHODESWERECONNECTEDTOATENMA724045ADCPOWERSOURCEWITHCONSTANTCURRENTOF200MATHECURRENTWASMONITORED,ANDCURRENTFALLINGBELOW200MASIGNIEDTHEENDOFTHEANODESERVICELIFEANODESERVICELIFETIMESARELISTEDINTABLE123REACTORSYSTEMSTWOREACTORSYSTEMSWEREUSEDTOINVESTIGATETHEOXIDATIONEFFECTIVENESSOFTI/SNO2SB2O5ANODESASINGLECHAMBERREACTORWASUSEDTOASSESSTHEEFFECTIVENESSOFTHEANODESUNDERTHEPRACTICALCONSTRAINTSOFATYPICALEFUENTDISINFECTIONSYSTEMEG,APFREACTORINWHICHBOTHTHEANODESANDTHECATHODESARECONGUREDINASINGLEREACTORINADDITION,ADUALCHAMBERREACTORWASUSEDFORCYCLICVOLTAMMETRYTHEDUALCHAMBERREACTORCONSISTEDOFTWO200MLBEAKERSJOINEDBYATTEDGLASSTUBETTOGETHERBYAJUNCTIONHOLDINGANORINGANDABRACKETTHATHELDTHEJUNCTIONINPLACEANAONMEMBRANEWASPLACEDINTHEJUNCTIONTOSEPARATEREACTIONSATTHEANODEANDCATHODETHEANODESANDCATHODESWERECONNECTEDTOACYCLICVOLTAMMETERALLREACTIONSWERECONDUCTEDINTRIPLICATE,ANDCONTROLSYSTEMSWEREEVALUATEDINTHESAMEREACTORSWITHOUTTHEAPPLICATIONOFCURRENT24EVALUATIONOFOXIDATIONBYTI/SNO2SB2O5ANODES1HEXANOLWASCHOSENFORITSHIGHREACTIVITYWITHOHANDOTHEROXIDANTSKOH60109M1S139,ANDITSLOWPOTENTIALFORREACTIVITYWITHREDUCTANTSKE180205501742060022ANTIMONYCHLORIDE20MASS/VOLUME550034555057560024105005510550961060082045082050011220550144206002425EFFECTOFNUMBEROFSNO2SB2O5LAYERSANTIMONYDOPEDTINOXIDEANODESWEREPREPAREDWITH8,16,AND24COATINGSOFTHEDIPPINGSOLUTIONUSINGTHEOPTIMUMTINCHLORIDECONCENTRATION,ANTIMONYCHLORIDECONCENTRATION,DRYINGTIME,ANDOXYGENOWRATEDURINGANNEALINGEACHOFTHESETSOFANODESWASTHENEVALUATEDFOREFFECTIVENESSBYMONITORINGHEXANOLOXIDATION26EFFECTOFDIPWITHDRAWALRATETHEEFFECTOFTHERATEATWHICHTHETITANIUMRODSWEREWITHDRAWNFROMTHETINCHLORIDEANTIMONYCHLORIDESOLUTIONWASINVESTIGATEDUSINGAPULLEYSYSTEMWITHAVARIABLESPEEDMOTORFIVEDIFFERENTRATESWEREUSED003,01,03,07,AND17CMS1THEPERFORMANCEOFTHEANODESWASEVALUATEDBYCYCLICVOLTAMMETRYANDTHEACTIVITYWASEVALUATEDBYMEASURINGTHEOXIDATIVELOSSOFHEXANOLINDUALCHAMBERREACTORS27ANODESERVICELIFEATI/SNO2SB2O5ANODEPREPAREDUSINGTHEOPTIMALCONDITIONSWASEVALUATEDBYCONTINUOUSCYCLICVOLTAMMETRYTHECYCLESWEREREPEATEDCONTINUOUSLYFOR1,280CYCLES28CYCLICVOLTAMMETRYANTIMONYDOPEDTINOXIDEANODESPREPAREDUNDERVARIOUSCONDITIONSWERECHARACTERIZEDBYCYCLICVOLTAMMETRYUSINGANEGTHEANODEBEINGEVALUATEDANDACALOMELREFERENCEELECTRODEWERESUSPENDEDINONECELL,ANDAPLATINUMWIRECATHODEWASSUSPENDEDINTHEOTHERCELLTHEELECTROLYTEINTHECELLSCONSISTEDOFANAQUEOUSSOLUTIONOF05MSODIUMSULFATEAND10MMPOTASSIUMFERRICYANIDEVOLTAMMAGRAMSWERECONDUCTEDATSCANRATESOF5,10,20,AND50MVS1,WITHTHEEXCEPTIONOFTHEREPEATEDVOLTAMMAGRAMSFORASSESSINGANODELONGEVITY,WHICHWERECONDUCTEDUSINGASCANRATEOF20MVS129STATISTICALANALYSISTHEMOSTCOMMONDATAOBTAINEDINTHISSTUDYFEATUREDCONCENTRATIONSOFACONSTITUENTASAFUNCTIONOFTIMEAFFECTEDBYAGIVENVARIABLEEG,THERATEOFOXIDATIONOFHEXANOLAFFECTEDBYDIFFERENTANODEPREPARATIONMETHODSTHESEDATAWEREANALYZEDUSINGCOMPLETELYRANDOMIZEDDESIGNANALYSISOFVARIANCEWITHONEWAYTREATMENTSTRUCTUREANDREPEATEDMEASURESUSINGA95CONDENCEINTERVAL3RESULTSANDDISCUSSION31OPTIMIZATIONOFTI/SNO2SB2O5ANODEPREPARATIONATHREELEVELFACTORIALDESIGNWASUSEDTODETERMINETHEOPTIMALCONDITIONSFORTI/SNO2SB2O5ANODEPREPARATIONTHEFACTORSEVALUATEDINCLUDEDTINCHLORIDECONCENTRATIONANTIMONYCHLORIDECONCENTRATIONANNEALINGTEMPERATURETHEMOSTEFFECTIVERESULTSFROMTHEOPTIMIZATIONARELISTEDINTABLE1ANODESERVICELIFETIMESVARIEDSIGNICANTLYBASEDONTHEPREPARATIONCONDITIONSFORALLDOSESOFTINCHLORIDEANDANTIMONYCHLORIDE,ANNEALINGTEMPERATURES500RESULTEDINSHORTSERVICELIVESFORTHEANODESIE,05HFURTHERMORE,ANNEALINGAT600ALSORESULTEDINSHORTSERVICELIFETIMESOF0124HDEPENDINGONTHETINCHLORIDEANDANTIMONYCHLORIDECONCENTRATIONSINTHEDIPPINGSOLUTION,500OR550WASTHEOPTIMUMANNEALINGTEMPERATURETHEMOSTEFFECTIVECONDITIONFORTI/SNO2SB2O5ANODEPREPARATIONWAS20TINCHLORIDE,1ANTIMONYCHLORIDE,ANDANANNEALINGTEMPERATUREOF500THISFORMULATIONISSLIGHTLYDIFFERENTFROMTHE2ANTIMONYCHLORIDEREPORTEDINAPREVIOUSSTUDY23THEOPTIMIZEDCONDITIONSPROVIDEDASERVICELIFETHATEXCEEDEDTHE180HOFTESTING32EFFECTOFOXYGENOWRATEDURINGANODEANNEALINGTHEEFFECTOFTHEOXYGENOWRATEONTHEOXIDATIONEFFECTIVENESSOFTHETI/SNO2SB2O5ANODES,USINGHEXANOLASAPROBEMOLECULEFOROXIDANTDETECTION,ISSHOWNINFIG1STATISTICALANALYSESCONRMEDTHATTHEOXIDANTGENERATIONRATESFOREACHOFTHETWOAIROWRATESUSEDINTHEANNEALINGPROCESSWERENOTSIGNICANTLYDIFFERENTTHESERESULTSINDICATETHATTHEREWASNOSIGNICANTDIFFERENCEINTHEEFFECTOFAIROWRATESONTI/SNO2SB2O5ANODEPERFORMANCE,ANDSUGGESTTHATTHEAMBIENTOXYGENCONCENTRATIONINTHEMUFEFURNACEIE,21ISSUFCIENTTOPROMOTETHEOXIDATIONOFTINIITOTINIVOXIDETHEREFORE,ASUPPLEMENTALOXYGENSUPPLYWOULDNOTBENEEDEDATADECENTRALIZEDLOCATION,SUCHASATAUTILITYPUBLICWATERFACILITY,TOPREPARETI/SNO2SB2O5ANODESWITHOPTIMALPERFORMANCECHARACTERISTICSFIG1RELATIVEOXIDANTACTIVITYOFTI/SNO2SB2O5ANODES,MEASUREDBYLOSSOFTHEOXIDANTPROBEHEXANOL,WITHANDWITHOUTOXYGENOWDURINGANNEALINGEXPERIMENTALCONDITIONSSINGLECHAMBERREACTORCONTAINING1MSODIUMSULFATEAND1MMHEXANOL,WITH200MAAPPLIEDCURRENTEFFECTOFNUMBEROFTINANTIMONYCOATINGSONANODEPERFORMANCETHEEFFECTOFTHENUMBEROFTINCHLORIDEANTIMONYCHLORIDECOATINGSONOXIDANTACTIVITYWASEVALUATEDUSINGANODESPREPAREDUNDERTHEOPTIMUMPREPARATIONCONDITIONSOF20TINCHLORIDE,1ANTIMONYCHLORIDE,ANDANANNEALINGTEMPERATUREOF500ANTIMONYDOPEDTINOXIDEANODESPREPAREDWITH8,16,AND24LAYERSOFTINCHLORIDEANTIMONYCHLORIDECOATINGSWEREEVALUATEDFOROXIDATIVEACTIVITYUSINGHEXANOLASTHEOXIDANTPROBETHEEFFECTOFTHENUMBEROFCOATINGSONOXIDANTGENERATIONISSHOWNINFIG2FIG2RELATIVEOXIDANTACTIVITYOFTI/SNO2SB2O5ANODES,MEASUREDBYLOSSOFTHEOXIDANTPROBEHEXANOL,FORANODESWITH8,16,AND24LAYERSOFTINOXIDECOATINGEXPERIMENTALCONDITIONSSINGLECHAMBERREACTORCONTAINING1MSODIUMSULFATEAND1MMHEXANOL,WITH200MAAPPLIEDCURRENTEXPERIMENTSORNOCURRENTCONTROLTHESEDATASUGGESTTHATTHENUMBEROFTINANTIMONYCOATINGSHADNOEFFECTONOXIDANTACTIVITYSTATISTICALANALYSISCONRMEDTHATTHEOXIDANTGENERATIONRATESFOREACHOFTHETHREENUMBERSOFCOATINGSWERENOTSIGNICANTLYDIFFERENTTHERESULTSSHOWNINFIG2WEREALSOCONRMEDBYEVALUATINGCYCLICVOLTAMMOGRAMSONTI/SNO2SB2O5ANODESPREPAREDWITHTHETHREEDIFFERENTLEVELSOFCOATINGSFIG3ACTHESETHREEESSENTIALLYIDENTICALVOLTAMMOGRAMSCONRMTHATTHEINCREASEDNUMBERSOFTINANTIMONYCOATINGSHADMINIMALEFFECTONTHECHARACTERISTICSOFTHETI/SNO2SB2O5ANODESFIG3CYCLICVOLTAMMOGRAMSFORTI/SNO2SB2O5ANODESWITHVARIABLENUMBERSOFCOATINGLAYERSA,8COATINGSB,16COATINGSC,24COATINGS34EFFECTOFDIPWITHDRAWALRATETHEEFFECTOFANODEWITHDRAWALRATEFROMTHETINANTIMONYDIPSOLUTIONWASEVALUATEDBYMEASURINGOXIDANTACTIVITYUSINGHEXANOLASANOXIDANTPROBEANDBYCOMPARINGCYCLICVOLTAMMOGRAMSTHEOXIDATIONOFHEXANOLINDUALCHAMBERREACTORSFORDIPWITHDRAWALRATESOF003,01,03,07,AND17CMS1ARESHOWNINFIG4AETHESEDATASUGGESTTHATDIPWITHDRAWALRATEHADNOEFFECTONTHEPOTENTIALOFTI/SNO2SB2O5ANODESTOGENERATEOXIDANTSSTATISTICALANALYSESCONRMEDTHATTHEOXIDANTGENERATIONRATESFOREACHOFTHEVEDIPWITHDRAWALRATESWERENOTSIGNICANTLYDIFFERENTTHEINUENCEOFDIPRATEWASALSOINVESTIGATEDUSINGCYCLICVOLTAMMETRYTHEVOLTAMMOGRAMSWEREESSENTIALLYIDENTICAL,WHICHINCONCERTWITHTHEDATAOFFIG4,INDICATESTHATDIPSOLUTIONWITHDRAWALRATEDIDNOTHAVEASIGNICANTINUENCEONANODECHARACTERISTICSANDTHERELATIVEDEGREEOFOXIDANTPRODUCTIONTHEINITIALHYPOTHESISRELATEDTOTHEINUENCEOFDIPWITHDRAWALRATEWASTHATASLOWERDIPRATEMIGHTPROVIDEMOREUNIFORMCOATINGOFTHEANODESHOWEVER,DIPWITHDRAWALRATEHADNOEFFECTONTI/SNO2SB2O5ANODEPERFORMANCE,WHICHWILLSIMPLIFYTHEIRPREPARATIONFIG4RELATIVEOXIDANTACTIVITYQUANTIEDBYLOSSOFHEXANOLINTHEANODECELLANDTHECATHODECELLFORTI/SNO2SB2O5ANODESWITHDRAWNFROMTHETINCHLORIDEANTIMONYCHLORIDEISOPROPANOLSOLUTIONATDIFFERENTRATESA,003CMS1B,01CMS1C,03CMS1D,07CMS1E,17CMS1EXPERIMENTALCONDITIONSDUALCHAMBERREACTORCONTAINING1MSODIUMSULFATEAND1MMHEXANOL,WITH200MAAPPLIEDCURRENT35ANODELONGEVITYVARYINGRESULTSHAVEBEENREPORTEDFORTHESERVICELIFEOFTI/SNO2SB2O5ANODESCORREALOZANOETAL41REPORTEDASERVICELIFEOFLESSTHAN12HFORTI/SNO2SB2O5ANODESATACURRENTDENSITY100MACM1WHENUSEDFORTHEELECTROLYSISOFAQUEOUSACIDICSOLUTIONSTHEDEACTIVATIONOFTHESEELECTRODESHASBEENPROPOSEDTOBEDUETOTHEFORMATIONOFANONCONDUCTIVETINHYDROXIDEINTHEOUTERLAYEROFTHEANODE42,43CHENETAL44REPORTEDTHATTI/SNO2SB2O5ANODESUNDERWENTSOMEIRREVERSIBLEDAMAGEWITHINSECONDS,ASMEASUREDBYABILITYTOTREATCHEMICALOXYGENDEMAND,ALTHOUGHTHEYWERESTILLABLETOTREATCODBY75INSUBSEQUENTUSAGEINCONTRAST,LIPPANDPLETCHER38FOUNDTHATTI/SNO2SB2O5ANODESSHOWEDNOCHANGEINFUNCTIONOVER48DAYS,ANDSCANNINGELECTRONMICROSCOPYSHOWEDNOCHANGEINTHESURFACEAPPEARANCEOFTHEANODESINADDITION,LOGEETAL23REPORTEDASERVICELIFETIMEOFGREATERTHAN30DAYSFORTI/SNO2SB2O5ANODESALONGSERVICELIFEOFTI/SNO2SB2O5ANODESISCRITICALFORTHESEELECTROCHEMICALSYSTEMSTOBECOSTEFFECTIVEANODESSTUDIEDFORTHEOPITMIZATIONMATRIXTABLE1WERETESTEDFORONLY180HTHEREFORE,ANANODEPREPAREDUSINGTHEOPTIMUMCONDITIONSWASEVALUATEDBYREPEATINGCYCLICVOLTAMMETRYTHROUGH1,280CYCLESTHEVOLTAMMOGRAMSWEREGRAPHEDSEQUENTIALLYON26SEPARATEGURES,ALLOFWHICHWERENEARLYIDENTICALTHERSTANDLAST50CYCLESARESHOWNINFIG5ABTHESERESULTSCONRMALONGSERVICELIFEFORTI/SNO2SB2O5ANODESPREPAREDUS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