A novel method is described for the determination of cobalt(II) by differential pulse voltammetry, based on accumulation of a cobalt complex, [CoSCNNO] + , on a hanging mercury drop electrode, followed by measurement of the catalytic current of the adsorbed complex. The effects of various experimental parameters on the catalytic current were investigated. The current was found to be linear for 0.3 nM to 100 nM Co, with a detection limit of 70 pM (4.1 ng 1 - 1 ) and a relative standard deviation of 1.6% for 50 nM Co (n = 25). The developed method showed considerable selectivity against nickel and zinc. A possible mechanism of the reduction process is proposed.