The determination of cobalt and nickel in aqueous solutions by strippi
ng voltammetry after adsorptive preconcentration is an established pro
cedure. The method is highly sensitive, but there is some controversy
concerning the reasons for the excellent sensitivity. Using a variety
of voltammetric techniques, we have determined that the reduction of n
ickel dimethylglyoximate in an ammonia buffer is consistent with an ov
erall process involving 16 or possibly 18 electrons. This hypothesis i
s confirmed by independently measuring the total quantity of metal ads
orptively deposited on the mercury electrode and comparing the amount
with the quantity of electricity required for its reduction.