A simple and sensitive adsorptive stripping voltammetry method was developed for determination of Zn using N-nitrozo-N-phenylhydroxylamine (cupferron) as a selective complexing agent. This complex absorbed on the hanging mercury drop electrode and created a sensitive peak current. The peak current and concentration of zinc accorded with a linear relationship in the range of 0.85–320 ng mL1. The influence of pH and the nature of supporting electrolytes, concentration of ligand, preconcentration time and applied potential were investigated. The relative standard deviation at a concentration level of 50 ng mL1 was 1.8%. The method was applied to the determination of zinc in city, river and mineral water samples, with satisfactory results.