An adsorptive differential pulse stripping method for the simultaneous determination of lead and tin is proposed. The procedure involves an adsorptive accumulation of lead and tin on a hanging mercury drop electrode (HMDE), followed by oxidation of adsorbed lead and tin by voltammetric scan using differential pulse modulation. The optimum experimental conditions are: 0.2 mol L−1 HNO3, accumulation potential of −900 mV versus Ag/AgCl, accumulation time of 200 s, scan rate of 20 mV s−1 and pulse height of 80 mV. Lead and tin peak currents were observed in the same potential region at about −400 mV. The simultaneous determination of lead and tin by using voltammetry is a difficult problem in analytical chemistry, due to voltammogram interferences. The resolution of a mixture of lead and tin by the application of orthogonal signal correction‐partial least squares (OSC‐PLS) was performed. The linear dynamic ranges were 0.003‐0.35 and 0.008‐0.50 μg mL−1 and detection limits were land 3 ng mL−1 for lead and tin, respectively. The RMSEP for lead and tin with OSC and without OSC were 2.8737, 6.0557 and 8.0941, 9.5151, respectively. The capability of the method for the analysis of real samples was evaluated by the determination of lead and tin in water samples with satisfactory results.
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