We report the design of a thin-layer spectroelectrochemical cell that
has been optimized for obtaining spectral data under non-steady-state
electrochemical conditions. A variety of applications involving the si
multaneous use of cyclic voltammetry and W-visible spectroscopy is pos
sible. For example, scan rates as high as 25 mV/s have been used while
still maintaining peak separations of 165 mV or less for millimolar e
lectroactive species in acetonitrile. More importantly, under the same
conditions, the spectral and coulometric responses correlate temporal
ly. Because of flexibility in the design, the cell can be tailored for
specific solution applications. Its use can be further extended to el
ectropolymerization and the study of electroactive polymers.