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The application of three analytical techniques, x-ray near grazing diffraction, infrared transmission and reflectance spectroscopy, and UV-visible-near-infrared reflectance spectroscopy, to the characterization of cobalt cobaltite, Co304, and of nickel cobaltite, NiCozO4 films, is reported. Thin films of CosO4 and NiCo204, in a 10-1000 nm thickness range were prepared by two methods: spraying and sputtering. Characteristic spectra and thickness limits are discussed based on theoretical considerations. Corresponding cyclic voltammograms are presented and discussed. Among the four methods of investigation of the cationic composition of the films, cyclic voltammetry appears to be the least sensitive.