Abstract

Cumene hydroperoxide (CHP) is an important initiator in polymerization industry. The compound is potentially explosive, toxic, and mutagenic. Herein, an electrochemical sensor is developed for CHP detection. First, the mechanism of CHP electrode process was investigated by a combination of electrochemical methods and ex-situ characterization techniques (SEM, FTIR, LC-MS, 1H-NMR, and 13C-NMR). The electrochemically generated species became more easily reduced than CHP and deposited on the electrode surface, allowing the analyte to be detected at low overpotential in aqueous solutions (as opposed to organic solvents typically needed in organic peroxide detection). In addition to the newly developed method, the performance of the electrochemical sensor was further enhanced via the use of copper hexacyanoferrate (CuHCF), a Prussian blue analogue which showed strong electrocatalytic activity towards peroxide reduction. A number of different CuHCF samples were synthesized and tested. The crystalline nanostructured CuHCF with high surface area (31.92 m2 g−1) and large lattice parameter (10.1397(1) Å) yielded excellent analytical performance towards CHP detection. The optimized method showed high tolerance to interferences and was validated in tap water samples. The excellent reproducibility (%RSD = 1.81, n = 3), high sensitivity (44.03 μA cm−2 mM−1), and low detection limit (5.9 μM, 3S b/m) of the developed CHP sensor were demonstrated.

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