Abstract: Spectroelectrochemistry especially with in situ measurement in a cell provides a very useful mthodology for measuring the parameters of electrode process. In this paper, we report the determination of formal potentials, the number of electron transfer, the diffusion coefficient, the heterogeneous electron transfer rate constant and the transfer coefficient of some organic dyes (Methyelene blue, Neutral red, Indigo carmine) using spectroelectro chemical technique in situ.