Simultaneous determination of antimony and bismuth was performed from 0.5 M HCl solution that contained 0.1 M hydrazine, using the hanging mercury electrode by differential pulse anodic stripping voltammetry with very slow potential scan rate and small pulse amplitude. The influence of HCl and chloride concentrations on the peak shape of Bi and Sb and the influence of other ions and organic substances were investigated. For the determination of antimony and bismuth in water and snow samples, the UV irradiation and the reduction of Sb(V) to Sb(III) by hydrazine in boiling solution were applied. The detection limit for Bi and Sb is 20 ng L-1.