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Mass Spectrometry of Metallofullerenes

Published online by Cambridge University Press:  25 February 2011

Mark M. Ross
Affiliation:
Chemistry Division, Naval Research Laboratory, Washington, D.C. 20375-5000.
H.H. Nelson
Affiliation:
Chemistry Division, Naval Research Laboratory, Washington, D.C. 20375-5000.
J.H. Callahan
Affiliation:
Chemistry Division, Naval Research Laboratory, Washington, D.C. 20375-5000.
S.W. Mcelvany
Affiliation:
Chemistry Division, Naval Research Laboratory, Washington, D.C. 20375-5000.
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Abstract

Fullerenes with a metal atom inside of the cage, metallofulierenes, were produced by either laser vaporization or a graphite arc and characterized using a variety of mass spectrometric methods. First, yttrium-fullerene adducts were formed by direct laser vaporization of samples consisting of graphite, yttrium oxide and fullerenes. Fragmentation and oxidation ion/molecule reactions showed that the laser-generated adducts are endohedral complexes (Yx@Cn), in contrast to externally-bound Y(Cn)+ species formed by gas-phase reactions. In addition, evidence was obtained for laserinduced bulk coalescence reactions yielding the metallofullerenes. Second, negative ion/desorption chemical ionization mass spectrometry was used to characterize metallofullerenes in arc-generated soot, pyridine extracts and the extract residue. The pyridine extracts of La2O3/graphite soot contain mostlyLa@C82 and La2@C80', in addition to (empty) fullerenes. However, the raw soot and the extract residue contain a broader range of metallofullerenes with relative abundances different than those observed from the extract (e.g. abundant La@C60', Lax@Cn') and La@C74). The thermal desorption behavior of the doped and undoped fullerenes indicate an interaction between the Cn and Lax@Cn species. Analysis of aqueous solutions of dried pyridine extracts of La2O3/graphite soot show Cn and Lax;@Cn' which is consistent with the possible presence ofmetallofullerene/ fullerene ionic complexes, (Lax@Cn)+C-n.

Type
Research Article
Copyright
Copyright © Materials Research Society 1992

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References

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