AbstractThis work addresses the simultaneous determination of copper(II) and antimony(III) in real matrices by differential pulse (DPASV) and fundamental harmonic alternating current anodic stripping voltammetry (ACASV). The voltammetric measurements were carried out using as supporting electrolyte the same acidic mixture (nitric, hydrochloric and perchloric acids) used in the dissolution of the real matrices with proper dilution. The procedure of the sample preparation is thus reduced to one step hence avoiding errors from long and complex sample handlings prior to the instrumental measurement. The results were verified by the analysis of the standard reference materials NBS‐SRM 631 Spectrographic Zinc Spelter D‐2 and BCS 207/2 Gunmetal. The precision, expressed as relative standard deviation, and the accuracy, expressed as relative error, were, in all cases, less than 5; the detection limit, for each element and in the experimental conditions employed, was around 10−7M. The standard addition technique improved the resolution of the voltammetric method, even in the case of very high metal concentration r
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