Integrated Microanalytical System Coupling Permeation Liquid Membrane and Voltammetry for Trace Metal Speciation. Technical Description and Optimization

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Abstract
A new minicell coupling the liquid‐liquid extraction technique called permeation liquid membrane (PLM) with an integrated Ir‐based Hg‐plated microelectrode array for voltammetric detection has been developed for the speciation of heavy metals in natural waters. Lead and cadmium have been used as model compounds. The PLM consists of a carrier (0.1 M 22DD+0.1 M lauric acid) dissolved in 1 : 1 mixture of toluene/phenylhexane held in the small pores (30 nm) of a hydrophobic polypropylene membrane (Celgard 2500). One side of this membrane is in contact with a flowing source solution, containing the metal ions of interest. An acceptor or strip solution (pyrophosphate) is placed on the other side of the PLM with the microelectrode array placed at 480 μm of the PLM. The analyte is transported by the carrier from the source solution to the strip solution. The originality of the new minicell is that accumulation in the strip solution is voltammetrically followed by the integrated microelectrode array in real time, and at low concentration level, using square‐wave anodic stripping voltammetry (SWASV). In order to protect the Hg microelectrodes from the adsorption of the hydrophobic carrier, the microelectrodes are embedded in a thin gel layer (280 μm) of 1.5% LGL agarose gel containing 10% of hydrophobic silica particles C18. The choice of optimum conditions is discussed in details in this article. Due to the very small effective strip volume of the new cell (less than 1 μL), high enrichment factor can be obtained (e.g., 330 for Pb) after 2 hours of accumulation. No deaeration of the solutions is required for SWASV measurements. Detection limits under these conditions are 2 pM and 75 pM for Pb and Cd, respectively, using a voltammetric deposition time of 5 min. In addition, no fouling effects were observed with natural water samples.