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Synthesis and purification of fullerenes

Posted on:1995-04-08Degree:Ph.DType:Thesis
University:University of South CarolinaCandidate:Scrivens, Walter AndrewFull Text:PDF
GTID:2461390014989018Subject:Chemistry
Abstract/Summary:
Chapter 1 describes the fabrication of a plasma discharge reactor constructed from a 1 L round-bottomed flask that allows for the preparation of gram-quantities of C{dollar}sb{lcub}60{rcub}{dollar} in an eight hour period. The modified reactor design (1) is inexpensive (2) requires almost no machining (3) has high thru-put (4) affords high yields of fullerenes (5) allows one to have near continuous feed of graphite rods and (6) permits control over four major reaction parameters important for the clean formation of fullerenes.; Chapter 2 describes potent solvents for fullerenes and their utility for the extraction and {dollar}sp{lcub}13{rcub}{dollar}C NMR analysis. The solubility of C{dollar}sb{lcub}60{rcub}{dollar} in a number of aromatic solvents is tabulated and details on the use of o-dichlorobenzene as an extraction and NMR solvent are given.; Chapter 3 describes the purification of gram quantities of C{dollar}sb{lcub}60{rcub}{dollar}and C{dollar}sb{lcub}70{rcub}{dollar} using activated charcoal flash chromatography columns. A detailed description on the packing and use of these columns as well as the analysis of the purified material is given.; Chapter 4 describes a method for the preparation of 0.3 {dollar}mu{dollar}m suspensions of C{dollar}sb{lcub}60{rcub}{dollar} in water and the synthesis of {dollar}sp{lcub}14{rcub}{dollar}C-labeled C{dollar}sb{lcub}60{rcub}{dollar} from Ba{dollar}sp{lcub}14{rcub}{dollar}CO{dollar}sb3{dollar}. Aqueous suspensions of the {dollar}sp{lcub}14{rcub}{dollar}C-labeled C{dollar}sb{lcub}60{rcub}{dollar} were then prepared to study the uptake of this material by human cells. The labeled C{dollar}sb{lcub}60{rcub}{dollar} becomes rapidly cell-associated and is retained by human keratinocytes in culture, with no significant loss of radioactivity over a period of 11 h.; Chapter 5 describes the synthesis of spiro-fused thiophene polymers.
Keywords/Search Tags:Describes, Synthesis, Chapter, Fullerenes
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