The concentration of As(total) in zinc plant electrolyte is determined by anodic stripping voltammetry (ASV) on a lateral gold electrode in HCl electrolyte. Due to the high excess of zinc in the sample the deposition potential has to be adapted. A second potential approx. 100 mV more negative than the arsenic signal has to be applied to selectively oxidize interfering antimony. For sample preparation the sample was passed through a cation exchange column to reduce the concentration of zinc in the measuring solution.