When working with an analytical method, one of the most important mome
nts is the setting up of the experimental conditions. Some techniques
of experimental design, together with some experimental matrices (Plac
kett-Burman, Fractional Factorial Design, Doehlert Design, 3/4 Designs
) are presented. They are illustrated by some drug studies, referring
to the optimization of their adsorptive stripping voltammetric determi
nation. It is shown how, starting with a relatively high number of fac
tors, a series of sequential experimental designs allows the required
information to be obtanined reducing the number of variables under stu
dy and/or their range at each step. In all cases examined, the final c
onditions give a much better result than would have been achieved with
a classical one-variable-at-a-time approach.