Table Of Content

DSEISCMIAUGTLNHTAOANNDNADEENOGDOULESSVOAMEMWULPLDOLTIPESIMSCEEHOLNAFETRMSGOEOEFNLTUEAMTAIMINSIOASCNLIRYROOSNECISASSIVYDOISUFTTEYESDMIHSOFCOLRRLETOEW CHERYLMORGAN OAFTDIHSESOUEFNRITTVAHTEEIROSRNIEDTQPOYURCIOETRFSOEEFRMNLETOONEFRTDISPDTHAFOIOILTRNOHSTPEOHAPGREHRTDYIAEADGLURFAEUTELEFOSIFCLHLOMOENLT UNIVERSITYOFFLORIDA 1993 UNIVERSITYOFFLORIDALIBRARIES ToWill,DaleandBarney-thanksforkeepingmyspiritsup ACKNOWLEDGMENTS studiesItatisthweitUhniavegrresaittyseonfseFloofriadca.comApligsrhamdeuantteadnedgrpereideinthcahtemIifsitnriyshsucepntmeyd almostanimpossibledream5or6yearsago.Butwithagreatdealof encouragementfrommyundergraduatechemistryprofessors.Dr.DavidBurgess andDr.WilliamTotherow,Itooktheplungeandenteredgraduateschoolinthe Gfaallgnoofn,19h89o.wcIotuhladsInhoatvaelgwiavyesnbuepe?neMaysyffaomrilmyehabsutshwiotwhnfmrieenadsgrleiaktedReaaclheolf support.Myparents,EllieandBingLonnroth,helpedmegetofftoagoodstart inFlorida.MychildrenLaurieandBrianhavestayedbymysideandhavegiven methreebeautifulgrandchildren-Alexis.AndrewandJamie.Mywonderful grandmother,EvelynLeard,hasbeenasaint(Iloveyou!).Myhusband.Will Morgan,hasbeenananchorforme.Hisundyingloveandsupportarewithme daily.Mybrother.DaleLonnroth,hasbeenmynumberonecheerleader.His faithinmethroughouttheyearshassustainedmyspiritandfocusedmyenergies. Mythankstoagreatfriend. Inadditiontomyfamilyandfriends,Igratefullyacknowledgethesupport andencouragementfrommyadvisorsandcoworkers.Mysincerethanksgotomy researchadvisor.Dr.JimWinefordner.forhisguidanceandsupportofmy research.IwouldalsoliketothankBenSmith.Hisexperimentalexpertisewas invaluable.CherylDaviswasagreathelpandsupportwiththisproject.Bill Spencergraciouslyallowedmetosharethephotodiodearraysystemwithhim. ItwasapleasuretoworkalongsideMikeWcnsinginCLB207.Finally,thanks gotoBenWomackwhotookmeunderhiswingwhenIfirstjoinedthegroup. Ithasbeenagreatresearchgrouptoworkwith. TABLEOFCONTENTS ACKNOWLEDGMENTS ABSTRACT CHAPTERS 1INTRODUCTION 1 4OHRSiecvIscoenteprsonetrvtiriocueDafmwleeDnvoiDtesfealstvIoeiehrpoeltmnaoeGtpnilmtooenswnitDniHsoclhlarogweCathodeGlowDischarge 4g1I1 2LOWPRESSUREDISCHARGES 13 CCDaaittshhcohodadirecgeGSepFouemtateteutrrrieynsgandCharacteristics 331153 3MDDIIESCSCRIHOGANCRAAGVNEIDTEYMPIAHSROSALIMLOENOTWSRYICSCATTEEHVMAOLDUEAGTLIOONWOFA 45 CEPaxhGrpalaemomrbeiwtemreDrinicatsnacEdlhvaaSCrleagutteauhtpSoiydosnetoDefemsaiMgincrocavityHollowCathode 455570 GARSELNISNODIGWDLLUEEDEAIESDSLBCEIYHNMAMENRINAGCTNERODOSECATAMEVRPIMLTIEYNSHAOOTLILUOLTNOIWOOFNCCAOTPHPOEDRE 108 5SDSCIOEAMLTTUUELHTRTOIMADOINENNEAGORTLUEISSOOIWNMDUUDOELIFSTSIDCBIEHYSLACMERRIMGECEETRNEEOTMCMIAISVCSIRITOOYNSAHMOPLLLEOW 138 111113354499500 6SUMMARY,CONCLUSIONSANDFUTUREWORK...159 BIOGRAPHICALSKETCH AobfRstetrqhauecitrUneoimfveeDnritsssistefyrotroatftihFoelnoDPreirgderaseeienntoePfdarDttoioacltthoFerulGofrfialdPluhmaietnletosSoocfphhtoyhoel DSEISCMIAUGTNLHTAOANNDNDAEENODGOUELSSVOAEMMWLUPODLLIPTESIMSCEEHOLNAFETRMSOGEOFENLTAEUMTAMIINISOASCNLIRYOROSNECISASSIVYDOISUTFTEYESDMIHSOFCLORLREOTEW By CherylMorgan August,1993 CMhaajiorrmaDnep:arPtrmoefn,t:JamCehsemDi.stWriynefordner Thehollowcathodeglowdischargeisarathermodestatomicemission source,but,nevertheless,hasmanydesirablecharacteristics.Thedischargeis easytoinitiateandmaintain,providingsharpatomiclineswithalowbackground continuum, Thelowpressureenvironmentvirtuallyeliminateschemical reactions,matrixeffectsandself-absorption.Thenontherinalsputtering atomizationprocessyieldsanatomcloudrepresentativeofthebulkmaterial. Althoughtheoreticallythehollowcathodeglowdischargeisnearlyanideal source,inrealityithassufferedfromweaksignaloutput.Ithasbeenshownthat cathodegeometryplaysanimportantroleintheatomicemissionsignalintensity. Thehollowcathodegeometryincreasestheemissionsensitivityovertheplanar cathode,butnotenoughtorivalotheratomicemissionsources.Thework presentedinthisdissertationfocusesontheuseofamicrocavityhollowcathode glowdischarge(MCHCGD)asamethodtoenhancesignaloutput. Althoughthereareseveraleffectivemultielementtechniquesinusetoday, theyallrequirelargesamplevolumes.Therearecircumstances,however,in whichonlyaverysmallsamplemaybeavailable(i.e.forensicsamplesand preciousbodilyfluids)butthedeterminationofmanyelementsonthetraceand uitratracelevelmayberequired.Thisprojectinvestigatestheapplicabilityof MCHCGDtothesimultaneousmultielementanalysisofdiscretenanosamplesof solutionresidues. Severalimportantdiagnosticparametersweredetermined,including pressure,voltage,current,sampledryingtime,slitwidthandchamberpurging. phaseeTvhaeluaetxepdertihmeeMntCaHlCinGveDsteimgaitsisoinonwsaysstpeemrfaosramesdourincetfwoorupihtarsaetsr.aceTanhaelysfiirss.t SingleelementanalysisofCuandPbwasperformedusingeachelement's dsetrmoonngsetsrtaetmeidsstihaotntlhiene.MCTHheCGliDmitsisoafndeetxeccetliloenn,t2sopugrcfeorfoCruuiatnrdat3ra6cefganfaolrysPibs,. ThesecondphaseevaluatedtheMCHCGDemissionsystemasamultielement source.SimultaneousdeterminationofPb,V,andCrwasachieved, demonstratingthattheMCHCGDisagoodmultielementsource. INCTHRAOPDTUECRTIION Theglowdischargeisarathermodestquasi-plasmawhichisgeneratedupon sparkbreakdownbetweentwoelectrodesimmersedinalowpressure,raregas environment.Itisaself-sustainingdischargeeasilymaintainableunderacertain setofconditions-pressuresrangingfroml-10Torr,appliedvoltagesrangingfrom 400-2000Vandcurrentsrangingfrom1-1000mA,dependingontheraregas- Inthislowpressureenvironment,theglowdischargeisvirtuallyfreefrom self-absorptionandself-reversal.1Ityieldsnarrowspectrallines2andprovidesan atomcloudrepresentativeofthebulkmaterialbeingsampled2withatomdensities rangingfrom109-1016cm'2.4 Thegroundstatefreeatompopulation,necessaryforatomicemission studies,isgeneratedbyanonthermal,nonselectivesputteringprocess.Because thesputteringprocessisnon-thermal.manyoftheinterferencesassociatedwith thermallyexcitedsources,suchasmatrixeffectsandsamplevaporization,arenot associatedwiththed.c.glowdischarge.Thesubsequentexcitationofthefree particlessputteredfromthesolidmatrixoccursasaresultoftheenergygenerated inanelectricfield.Consequently,theglowdischargefallsintothecategoryof electricdischarges.Thecategoriesofatomicemissionsourcesarepresentedin Table1-1. Table1-1.CategoriesofAtomicEmissionSources ThermalSources: HFilgahmeTsemperatureFurnaces ElectricDischargeSources: LowPressure GlGPHeoloiawlsnlsaDolriewsrCcCahEatlatherhocgodterdesoedeless AtmosphericPressure HighVoltagea.c.Arcs PlBRMaliFAPCCsIMocaalntmiwppardaDocaausnoismrcccmswioiitAacacittwtrhvviiracaHevveorsveeyngeDdseirsIsoncgdheuacnregdes

Design and development of a microcavity hollow cathode glow discharge emission system for simultaneous multielement analysis of discrete nanosamples of solution residues PDF

178 Pages·1993·1.4 MB·English

by Morgan, Cheryl

#americana #univ_florida_smathers #UFRDS

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