External reflection FT-IR techniques allowed for in situ examination of interfacial electrochemical events occurring in a thin-layer spectroelectrochemical cell. The formation of an adsorbed hexacyanoferrate (HCF) species on a platinum electrode during potential cycling in the ferri-/ferrocyanide redox couple was investigated. At neutral pH with KCl as electrolyte, a hexacyanoferrate complex forms during potential cycling in the ferri-/ferrocyanide redox couple, but only if the potential limits are quite large. Characterization of the adsorbed complex indicates that it initially adsorbs as soluble Prussian Blue (KFe II [Fe III (CN) 6 ]) with no evidence of the presence of insoluble Prussian Blue [Fe 4 III (Fe 2 II (CN) 6 ]. This HCF complex can reversibly adsorb and grow on the electrode surface and desorb and decompose to reform solution-phase ferricyanide and ferrocyanide. Adsorption of the HCF complex decreases, but does not completely inhibit, electron transfer.
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Pharr et al. (1997) studied this question.
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