Electrochemical generation of the higher fullerene radicals C₇₆˙⁻, C₇₈˙⁻ and C₈₄˙⁻ under oxygen- and moisture-free conditions and their observation by EPR

Abstract

A low volume, three-compartment, three-electrode, oxygen- and moisture-free electrochemical cell which allows cyclic voltammetry and bulk electrolysis of minute quantities (<100 µg) of compounds is described. The electrolysed solution can be vacuum-line transferred to a suitable container for further spectroscopic characterization. The cell performances are exemplified by the reversibility study of the first reduction wave of C₆₀ and C₈₄ and the production of the higher fullerene radicals C₇₆˙⁻, C₇₈˙⁻ and C₈₄˙⁻ in benzonitrile and 1,1,2,2-tetrachloroethane (TCE), and their observation by electron paramagnetic resonance (EPR).