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Chromatography and purification of endohedral metallofullerenes

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dc.contributor.authorStevenson, Steven A.en
dc.contributor.committeechairDorn, Harry C.en
dc.contributor.committeememberAnderson, Mark R.en
dc.contributor.committeememberBrewer, Karen J.en
dc.contributor.committeememberTaylor, Larry T.en
dc.contributor.committeememberBell, Harold M.en
dc.contributor.departmentChemistryen
dc.date.accessioned2014-03-14T20:17:02Zen
dc.date.adate2005-10-03en
dc.date.available2014-03-14T20:17:02Zen
dc.date.issued1995en
dc.date.rdate2005-10-03en
dc.date.sdate2005-10-03en
dc.description.abstractAt the conception of this research, a separation methodology for obtaining purified mctallofullerene [A<sub>m</sub>@C<sub>2n</sub>, m = # of metal atoms, A, and C<sub>2n</sub> = # of carbons in the surrounding cage] samples was not yet developed. Isolation of these metal-encapsulated fullerenes was strongly desired for characterization of their physical and chemical properties. Predicted applications for these novel species include their use as possible superconductors, catalysts, and non-linear optical devices. However, initial purification efforts have been hindered by several difficulties. These factors include a low abundance (< 1%) in the raw extract, uncertain stability in aerobic environments, co-elution of A<sub>m</sub>@C<sub>2n</sub> with empty-cage fullerenes, and the need for selective chromatographic detection. In this research, these difficulties have been overcome with the development of a continuous-flow, on-line HPLC-EPR apparatus. Advantages include a selective, non-invasive detector with chromatographic separations being performed in a controlled anaerobic environment. This on-line approach permits the selective detection of only those metallofullerenes with an odd-number of encapsulated atoms. The ability to continually monitor separations of these paramagnetic species ultimately permits the optimization of chromatographic parameters. The methodology developed from this on-line HPLC-EPR approach has ultimately resulted in purified empty-cage (C₆₀, C₇₀...C₉₆) and metallofullerene samples (Sc₂@C₇₄, Sc₂@C₇₆, Sc₂@C₇₈, Sc₂@C₈₀, Sc₂@C₈₂, Sc₂@C₈₄ - two isomers, Sc₂@C₈₆, Sc₂@C₈₈, Sc₂@C₉₀, Sc₃@C₈₂, Sc₄@C₈₂, La₂@C₇₂, Er@C₈₂, Er₂@C₈₂ - two isomers, and Er₂@C₉₂).en
dc.description.degreePh. D.en
dc.format.extentxx, 171 leavesen
dc.format.mediumBTDen
dc.format.mimetypeapplication/pdfen
dc.identifier.otheretd-10032005-171425en
dc.identifier.sourceurlhttp://scholar.lib.vt.edu/theses/available/etd-10032005-171425/en
dc.identifier.urihttp://hdl.handle.net/10919/29176en
dc.language.isoenen
dc.publisherVirginia Techen
dc.relation.haspartLD5655.V856_1995.S748.pdfen
dc.relation.isformatofOCLC# 34648512en
dc.rightsIn Copyrighten
dc.rights.urihttp://rightsstatements.org/vocab/InC/1.0/en
dc.subject.lccLD5655.V856 1995.S748en
dc.titleChromatography and purification of endohedral metallofullerenesen
dc.typeDissertationen
dc.type.dcmitypeTexten
thesis.degree.disciplineChemistryen
thesis.degree.grantorVirginia Polytechnic Institute and State Universityen
thesis.degree.leveldoctoralen
thesis.degree.namePh. D.en

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