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The modified sol-gel synthesis technique was used to created of nanostructured maghemite (γ-Fe2O3). It has been shown that the molar concentration of the original precursors during synthesis affects on the average particle sizes, specific surface area, pore size distributions, optical and conductivity properties. The XPS metod allowed to establish features of electronic structure of the synthesized materials. Optimal conditions for the synthesis of nanostructured maghemite with mesoporous structure were selected. The mechanism of electrical conductivity formation for synthesized mesoporous materials was established. The width of the band gap is determined and its dependence on the molar concentration of precursors is established. The positive correlation between the specific surface area of γ-Fe2O3 samples and photocatalytic activity was installed - the photocatalytic activity of synthesized γ-Fe2O3 increase with growth of specific surface area of γ-Fe2O3 samples.