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              <p>Friedel's salt, a mineral anion exchanger belonging to the family of the layered double hydroxides (LDHs), was synthesized and used as a novel electrode modifier for the accumulation of iodide species and their subsequent voltammetric determination at carbon paste. Beside the preconcentration features of Friedel's salt towards iodide species, its presence at the electrode surface allowed to evidence the oxidation of molecular iodine into iodate (with transient IO−), contrary to most carbon‐based electrodes, as demonstrated by cyclic voltammetry. Preconcentration was achieved at open circuit and iodide was then detected by differential pulse voltammetry in unbuffered chloride medium. The sensing process was further improved by optimization of the carbon paste composition, the detection medium, and the accumulation time. The detection limit was 0.06 µM (3σ), with linear calibration ranges extending from 0.1 to 1 µM, 1 to 10 µM, and 10 to 50 µM, giving a dynamic range of over several orders of magnitude. The effect of anionic interferences was evaluated and the sensor was applied to iodide analysis in synthetic ground‐ and seawaters.</p>
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