In this paper, the dependences of the semiconductors’ photoelectrochemical properties on the experimental conditions were studied for the solid solution of CdS and ZnS, graphitic carbon nitride, and the platinized carbon nitride. The cyclic voltammograms were obtained under different scan rates. The sample investigations were carried out by two ways, at the constant external voltage and varied amplitudes and at different external voltages and the fixed amplitude. The Mott – Schottky dependences were studied at different frequencies. The basic dependences of the changes in the photoelectrode target characteristics on the experimental condition were found. Some recommendations for the correct comparison of qualitative and quantitative photoelectrochemical data were formulated.