Substantial reductionIn analysis time has been achieved in anodic stripping analysis by eliminating the necessity lor oxygen removal. This was made possible by using square-wave voltammetry as a stripping technique in a low-pH electrolyte (0.1 M HCI04). Electroreduction of oxygen In acidic medium does not affect either the precision or the sensitivity of the method. Linear calibration plots were obtained for a model system at submicromolar concentration levels (0.1-1.3 µ Cd(II)) using short deposition times (5-240 s) at -0.7 V vs. SCE.

Normaland reverse-pulse voltammetry was used to investigate both the reduction and oxidation of SOCl2 at glassy carbon electrodes in jV,7V-dimethylformamide (DMF) with tetrabutylammonium hexafluorophosphate supporting electrolyte. NMR spectroscopy was used to probe for interactions between SOCl2 and DMF. NMR spectra and the quantitative treatment of normaland reverse-pulse voltammograms gave evidence for the displacement of Cl" in SOCl2 by DMF. The species SO2"1", solvated by DMF, and Cl" are responsible for the reduction and oxidation currents, respectively. The species S02+ is reduced via a two-electron process to "SO". Analyses of normal-pulse voltammograms for the S02+ reduction indicate that the rate-determining step is a one-electron transfer, and there is no evidence for an intermediate in the overall electroreduction.

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Results of further evaluation of the performance of the combination of square wave voltammetry and the COOL (Chernoff‐O'Dea‐Osteryoung‐Lane) algorithm are presented.