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Virginia Tech

Chromatography and purification of endohedral metallofullerenes

Abstract

dc:description.abstract

At 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).

Degree

thesis:*
Name thesis:degree_name
Ph. D.
Level thesis:degree_level
doctoral
Discipline thesis:degree_discipline
Chemistry
Department dc:contributor.department
Chemistry
Grantor dc:publisher
Virginia Tech
Year dc:date.issued
1995

Author and committee

dc:creator, dc:contributor.*
Author dc:creator
  • Stevenson, Steven A.
Chair dc:contributor.committeechair
  • Dorn, Harry C.
Committee members dc:contributor.committeemember
  • Anderson, Mark R.
  • Brewer, Karen J.
  • Taylor, Larry T.
  • Bell, Harold M.

Rights

dc:rights
Statement dc:rights
  • In Copyright
Language dc:language.iso
en

Identifiers

dc:identifier.*
Dc Identifier Other
etd-10032005-171425
OAI identifier oai:identifier
oai:vtechworks.lib.vt.edu:10919/29176

Chain of custody

source
Harvested from
Virginia Tech
Base URL
vtechworks.lib.vt.edu/oai/request
Last updated
2026-07-22
Source record
OAI-PMH GetRecord
related terms
citation

Stevenson, Steven A.. Chromatography and purification of endohedral metallofullerenes. doctoral thesis, Virginia Tech, 1995. http://hdl.handle.net/10919/29176