Abstract
The nature of the surface species produced in the first anodic peak at ca. +0.1 V/RHE in voltammetric sweeps of an iron electrode in alkaline sulphide solutions was studied using potential-modulated reflectance spectroscopy (PMRS). The observed PMRS signal was attributed to an electroreflectance effect, and the decrease in the signal with modulation frequency was interpreted as being due to the uncompensated ohmic resistance between the electrode and the tip of the Luggin capillary. A PMRS maximum at about 600 nm was attributed to an iron monosulphide, since the potential-modulated reflectance spectrum of the iron monosulphide pyrrhotite showed a maximum at 598 nm over a wide potential range. A PMRS maximum at 390–450 nm was attributed to FE(III) oxyhydroxides. It is concluded that both an iron monosulphide and an Fe(III) oxyhydroxide are formed in the first anodic peak of Fe in alkaline sulphide solution.
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