We present electrochemical studies of tetraalkylammonium (R4N+) reduction chemistry at Highly Orientated Pyrolytic Graphite (HOPG) and glassy carbon (GC) electrodes. We show that by electrochemically controlled intercalation and formation of a graphite intercalation complex (GIC) into layered HOPG, the irreversible reduction of the tetraalkylammonium cation can be prevented and subsequent de-intercalation of the GIC via the use of potentiostatic control is achievable. R4N+ cations with varying alkyl chain lengths (methyl, ethyl and butyl) have been shown to exhibit excellent charge recovery effects during charge/discharge studies. Finally the effects of electrode expansion on the degree of recovered charge have been investigated and the observed effects of R4N+ intercalation on the graphite cathode have been probed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). (C) 2014 The Authors. Published by Elsevier B.V.