A rapid and highly sensitive adsorptive stripping voltammetry method for the measurement of traces of nickel(u) in flowing systems is described. The method involves a mass-transport controlled preconcentration step, during which the Niu-dimethylglyoxime complex is adsorbed onto an in situ plated mercury film wall-jet electrode, followed by a reductive square wave stripping scan. The optimization of the experimental conditions and square wave parameters was carried out in order to achieve high sensitivity, reproducibility and fast response. The detection limit, restricted by the amount of nickel in the blank solution, was found to be 1.3 x lo-'' M, with a relative standard deviation of 2 12.2 % (n = 15), for a 1-min accumulation time. Linear calibration plots were obtained up to 8 x lo-'' M. This method can be applied to continuous on-line monitoring of trace levels of nickel in flowing systems, enabling easy automation.