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Principal components analysis (PCA), applied to differential-pulse anodic stripping voltammograms of a series of solutions containing various amounts of Pb²⁺ and Cd²⁺, revealed three principal components, accounted for by the presence of the two metal ions and of an appreciably curved baseline. The analysis of numerically simulated voltammograms showed that serious errors can arise from the use of incomplete target vectors unless a “tangent fit” procedure is used. By using so-modified voltammetric profiles of blank, lead and cadmium solutions as target vectors in the Procrustean analysis [target factor analysis (TFA)], it was possible to calculate accurately the concentrations of both metals in all solutions examined. Compared with the existing methods of evaluating voltammograms, the proposed PCA-TFA approach has the advantages of being global and, at the same time, simple (linear) and straightforward.