Coupling of a high throughput microelectrochemical cell with online multielemental trace analysis by ICP-MS

In this work, the successful coupling of a specially designed microelectrochemical cell and direct online multi-elemental trace analysis by ICP-MS is presented. The feasibility of this method is demonstrated by the example of copper dissolution in HCl (1 and 10 mM), showing very high sensitivity and an excellent congruency between electrochemical experiments and copper concentrations detected downstream. The complementary data allows for a precise determination of the valence of Cu ions released during anodic dissolution, which undergoes changes depending on the electrolyte and the applied current density. Moreover it provides a means of quantification of processes without net external currents that are not readily accessible by plain electrochemical techniques, in particular the exchange current densities at the open circuit potential, i.e. corrosion rate, and the dissolution of native oxides. The system presented combines full spectrum electrochemical capabilities, convection control, and highly sensitive electrolyte analysis in an integrated, miniaturized arrangement under full computer control and automation. (C) 2011 Elsevier B.V. All rights reserved.