A novel chemically modified electrode prepared by anodic electrodeposition of cobalt (III) film on the gold electrode substrate (Au-Co) was characterised by cyclic voltammetry and XPS techniques in both neutral and alkaline medium. Cobalt oxyhydroxide film was deposited by cycling the potential between 0.0 and 1.1 V versus SCE in 0.1 M sodium acetate solutions containing 10 mM CoCl2. The electrocatalytic properties of the Au-Co electrode were investigated in alkaline medium using glucose as a model compound. A comparative XPS study of bare gold, bare cobalt and Au-Co electrodes after electrochemical treatment in neutral and alkaline solutions has been carried out. A detailed XPS analysis of the Au4f(7.2), Co2p(3.2), O1s and C1s regions was performed to check the chemical composition of the Au-Co electrode upon electrochemical treatments. Film deposition is attributed to growth of conducting and compact CoOOH oxyhydroxide with significant insertion of carbonyl groups within the electrodeposited layer. The prolonged electrochemical treatment in alkaline medium produces a good stabilization of the Co-III oxyhydroxide film, with a dominant O1s feature at about 532.4 eV of BE corresponding to a non-stoichiometric surface oxygen. The absence of CoO species proves good conducting properties of the cobalt film and the absence of any passivation effects on the catalytic performance.