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Corrosion resistant structural materials of both iron and nickel based alloys are used in the electric power industry for the construction of the coolant loops of both conventional and nuclear power generating stations. These materials, in the presence of high temperature (e.g. 287° C), high pH (e.g. 10.0 @ 20°C) water with dissolved hydrogen will oxidize and form corrosion films that are double metal oxides (or spinels) of the form AB 2 O 4. This work describes optical reflectivity techniques that have been developed to study the growth of these films in situ. The optical technique uses a dualbeam specular reflection spectrometer to measure the spectrum of reflected light in small angle (i.e. < 15°) scatter. The reflection spectra are then calibrated using a set of corrosion coupons with corrosion films that are well known. Results are compared with models based on multilayer reflection and Mie scattering from a particle size distribution. Surface roughness is found to be the dominant cause of reduced reflection as the films grow.