Abstract
Ex situ and in situ mercury film formation was investigated in solutions containing NO3-, SCN-, Cl-, and ClO4-, and at glassy carbon macro- (3 mm) and micro- (10 μm) electrodes, a platinum macro- (1.6 mm) electrode, and a microfabricated Ir-ultramicroelectrode array (Ir-UMEA). The formation of mercury(I) chloride (calomel) during Hg deposition was investigated by varying the Cl- concentration. The performance of the Hg films was evaluated using Cd2+ and Pb2+ with square wave anodic stripping voltammetry. For ex situ Hg film formation on Ir and GC substrates, the highest efficiency was obtained when no Cl- or 1 M Cl- was present. The Pt surface was affected by the Cl- ions; thus for ex situ Hg film formation, the best results were obtained with no Cl- present. Calomel formation during in situ Hg deposition occurred for 0.001 > [Cl- ] < 0.5 M and was independent of the substrate. Calomel interference was identified by the presence of an anomalous cathodic peak between −0.6 and −0.3 V during the anodic scan....
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