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Electrochemistry is a well established field in analytical chemistry. One property of great interest in electrochemistry is the apparent charge transfer diffusion coefficient of polymer thin films. Combining electrochemical techniques with spectroscopy, new insights can be gained on the characteristics of the polymer film. Cyclic voltammetry was used to prepare polymer films of tris(5-amino-1,10-phenanthroline)ruthenium(II) and iron(II) on Indium Tin Oxide (ITO) surfaces. When the film was electrochemically reduced, a visible color change was measured spectroscopically and related to the charge transfer rate. A correlation was studied between the spectrochemical, electrochemical and impedance measurements. While under diffusion controlled conditions, this correlation was used to find the apparent charge transfer diffusion coefficient. This coefficient is useful for applications in other research and provides a better understanding of polymer thin films.