Thin mercury film electrodes coated with poly(styrenesulfonate) (PSS-TMFE) were prepared by solvent evaporation of an aqueous solution of the polymer onto a glassy carbon electrode followed by electrolytic deposition of the mercury film through the polymer layer. The performance of these polymer modified mercury film electrodes is evaluated in a NaCl solution using lead(II) as a model heavy metal cation. This new methodology presents an improved sensitivity, mechanical stability, reproducibility, repeatibility and increased efficiency against surfactants when comparing to the conventional TMFE. Square-wave anodic stripping voltammetry at the ex situ mercury plated PSS-TMFE was successfully applied to the determination of total and labile amounts of lead and copper in estuarine water samples of variable and high salinity (23.5Ω ± 35.0Ω). Concentrations in the nanomolar region can be easily assessed using a 3 minutes accumulation time with low relative standard deviations (less than 3%).

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