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A selective and sensitive method for simultaneous determination of lead and cadmium by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Pb (II) and Cd (II) ions with 2-mercaptobenzothiazole onto hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed species by differential pulse cathodic stripping voltammetry. Optimal conditions were obtained at pH 8.0, 2-mercaptobenzothiazole concentration of 1.0×10⁻⁴M, the accumulation potential of −0.4V (vs. Ag/AgCl), the accumulation time of 160s, and the scan rate of 100mV/s. Under optimised conditions, linear calibration curves were established for the concentration of Pb (II) and Cd (II) in the range of 0.5–70 and 0.2–30ng/ml, respectively, with detection limit of 0.017ng/ml for Pb (II) and 0.01ng/ml for Cd (II). The procedure was successfully applied …