Abstract
We describe the use and characterization of a multilayer film, prepared via layer-by-layer deposition of cationic para-rosaniline acetate dye (i.e., PR) and the vanadium-containing Keggin-type polyoxometalate anion, [PMo11VO40]5− (i.e., PVMo11), on indium tin oxide (ITO) as an electrode for determination of chlorate. A linear cyclic voltammetry (CV) current response was observed for the 0μM≤[ClO3−]≤1000μM range with a detection limit of ∼220μM ClO3− (S/N>3) in a pH=2.5 solution of 100mM sodium acetate. Electrode response was insensitive to interference by oxygen and nitrogen-based explosives like TNT, a prerequisite for use in the field. A Taguchi L16 array was used to investigate the performance of the electrode as functions of number of PVMo11/PR bilayers (L; 3–6 bilayers), solution pH (H; pH ∼1.32–2.85), solution [ClO3−] (C; 250–1000μM), CV scan rate (S; 50–200mVs−1), and film age (A; 1–8 weeks). Maximum current response was obtained for a 1 week old 5 bilayer film immersed in a pH 2.85 0.10M NaCl (aq) solution containing 1000μM ClO3−. However, current response fell as films aged, requiring aging of films for approximately 8 weeks prior to use to obtain reproducible analyses. A two-level full factorial design using films aged 8 weeks identified the variables S, L, H, and C and variable interactions LS and HS as statistically significant contributors to the film current response and provided a model describing film performance.
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