Steady-state oxygen evolution measurements on a series of Ni.CoxO4 Teflon-bonded electrodes at 25~ 5N KOH showed that NiCo204 had the highest activity. Tafel plots on such electrodes are complicated by the formation of higher oxides, gas bubbles, and emptying of the electrocatalyst pores, and it is suggested that potentiostatic pulse techniques can give more reliable results, provided the electrodes are fully preanodized to form the higher metal oxide.* Electrochemical Society Student Member. ** Electrochemical Society Active Member.