納米氧化鋁材料在分離富集-原子吸收光譜法測(cè)定痕量貴金屬中的研究與應(yīng)用.pdf

1、湘潭大學(xué)碩士學(xué)位論文納米氧化鋁材料在分離富集原子吸收光譜法測(cè)定痕量貴金屬中的研究與應(yīng)用姓名：熊文明申請(qǐng)學(xué)位級(jí)別：碩士專業(yè)：分析化學(xué)指導(dǎo)教師：周方欽20060601AbstractInanalyticalsciencesseparationpreconcentrationisusuallyindispensabletoimprovethesensitivityivityoftheanalyticalmethod.Solidphaseext

2、raction(SPE)isasamplepreparationtechniquethatiginatedinthe1970sdevelopedfromthelateofthe1980shastheadvantageofhighpreconcentrationfactsimplicityofoperationlesspollutiontotheenvironmenteasyautomationcanbeappliedtothediffe

3、rentsamples.Nanometersizedmaterialasanovelfunctionmaterialwhichhascomeintothewldin1980shasmadeagreatprogressinrecentyears.Theregimeofnanoparticleisfrom1to100nmwhichfallsbetweentheclassicfieldsofchemistrysolidstatephysics

4、.Thesmallerthediametersarethemeatomsareontheirsurfacethebiggerthesurfaceareais.Thesurfaceatomsinnanometermaterialsareunsaturatedcanbindwithotheratoms.Alltheseacteristicsmakenanometermaterialsbeanidealsolidphaseadsptionma

5、terialsinmodernanalyticalchemistry.Theatomicadsptionspectrometry(AAS)whichhasthemeritsoflowcostdetectionlimitgoodprecisionaccuracywidelinearrangehasbeenwidelyappliedintraceanalysis.BycouplingSPEwithAAStheanalyticalperfma

6、nceoftheanalyticalmethodsuchassensitivitydetectionlimitantijammingcapabilitycouldbeefficientlyimproved.AtthesametimeitalsoextendstheapplicationfieldofSPE.InthisdissertationtheselfmadenanoaluminawasappliedinthefieldofSPEt

7、headsptionacteristicsmechanismofsomepreciouselementionsonnanoaluminamaterialwassystematicallystudiedwithFAAS.AnovelmethodwasdevelopedfdeterminationoftracepreciouselementswhichcombinedAASwithseparationpreconcentrationbyna

8、noaluminamaterialwithhighstabilityrelativehighivitylonglifepollutionfree.Themaincontentsweredescribedasfollows:1.ThesamplesofnanoaluminaofunifmparticaldiameterwerepreparedbyimprovedSolGelmethod.Thentheproductwastobedeter

9、minedbyIRTEM.Itwasfoundthattheproductisnanoalumina.Meoverthereislittleagglomerationtheparticlediameterisinthe20～80nmregionwithrectangulardistribution.Soitissuitablefsolidphaseadsbent.2.TheadsptionelutionbehavisofPdonnano

10、aluminaunderstationaryconditionwerestudiedindetail.FactsaffectingadsbingincludingpHvaluetemperatureadsbingtimeeluentscoexistingionswereexaminedtheoptimalexperimentalconditionswereestablished.BasedontheIRspetraofunadsbeda

11、dsbednanoaluminatheadsptionmechanismofPdonthenanoaluminawaspreliminaryprobed.AnewmethodfthedeterminationoftracePdinsyntheticwatersamplesbyAASafternanoaluminaseparationpreconcentrationwasproposed.Therecoveryrangedfrom95.0

12、%to97.6%.theresultsshowedthatthemethodissimplerapiditysensitivity.3.Usingamicrocolumnpackedwithimmobilizedpdimethylaminobenzalrhodanine(pDMABR)onnanoaluminaasadsbenttheretentionbehavisofAgonthemicrocolumnwerestudiedwithA

13、AS.TheconditionsfadsptionelutionofAgwereoptimized.Undertheoptimalconditionsthedetectionlimit（3σ）ofthemethodfAgwas1.7ngmLitsrelativestarddeviation(R.S.D.)was2.4%(n=12C=0.05gmL).Theproposedmethodwasappliedtothedeterminatio