0, reduction in an acid medium has been investigated on a transition metal macrocycle, CoNPc(l,2), impregnated on a carbon black support with a high dibutylphthalate adsorption value, using a rotating disk electrode and voltammetry techniques described previously, combined with X-ray photoelectron spectroscopy measurements. Optimal activity was found for a bilayer coverage (n = 2) at 17%-B% w/w loading. Heat treatment seems to be beneficial for n 6 3: it increases the overall number N of exchanged electrons and improves the electrode wetting. For the most active samples, mixed Co(II1/cdIIIl valencies were displayed.