A versatile variable temperature thin layer reflectance spectroelectrochemical cell

Abstract

A specular reflectance cell for variable temperature thin layer spectroelectrochemistry in the infrared and UV–Vis regions was designed and tested. The cell was constructed to fit commercially available FTIRs or UV–Vis spectrophotometers. It requires only a small sample volume. It is simple, rugged, and suitable for use with either aqueous or non-aqueous solutions. The cell employs commercially available optical windows and gaskets. Temperature control was achieved with an external bath/circulator in the range from −55 to+80°C. The cell's performance was tested in cyclic voltammetry mode with K 4 Fe(CN) 6 and ferrocene. The variable temperature feature of the cell was used to observe for the first time the radical anion of the complex Fe(CO) 3 (η 4 -2,5-norbornadiene at −15°C.