Three electrode materials (glassy carbon, gold, and platinum) were investigated for application in a non-aqueous single-metal redox flow battery based on vanadium (III) acetylacetonate, supported by tetraethylammonium tetrafluoroborate in acetonitrile. Redox couples associated with the one-electron disproportionation of V(acac)3 were observed in voltammetry for each metal tested. An elementary kinetic model was created and used to determine rates for oxidation or reduction of the vanadium complex. The oxidation rates for V(acac)3 were mass-transfer limited on all electrode materials, suggesting reversible kinetics. For the V(acac)3 reduction reaction, exchange-current densities of 1.3, 3.8, and 8.4 A m−2 were observed on glassy carbon, platinum, and gold electrodes, respectively.