RESUMO
The most important experimental parameters of the flow potentiometric stripping analysis (PSA) with oxygen as an oxidant were investigated and optimised. A simple, homemade flow system consisting of glassy carbon tubes, which served as a working and auxiliary electrode, was used. By applying a rest period before the stripping step (the flow stop mode) and by imposing a constant reductive current simultaneously with the interruption of potentiostatic control, significant increase of the flow PSA sensitivity was achieved. In the determination of cadmium and lead, quantitation limits of 0.11 and 0.82 µg/L were obtained. The precision of the method was evaluated in terms of repeatability and reproducibility, with values of relative standard deviation lower than 4.0% for cadmium and 4.2% for lead. This modified technique was applied for simultaneous determination of cadmium and lead in milk, after a simple pretreatment of the samples by dilution and acidification. The method accuracy was confirmed by analysing the certified reference material of skimmed milk powder (ERM-BD151).
RESUMO
Chronopotentiometric stripping analysis (CSA) was used for selective determination of As(III) and As(V) in different oilseeds. After the optimization of experimental parameters an appropriate procedure for sample pretreatment was developed. A detection limit of 2 microg/dm3 for As(III) was obtained with an electrolysis time of 600 s. This method was used for arsenic determination in sunflower, pumpkin, and flax seed, as well as for soy flakes and almond.