The reduction of hexavalent to trivalent uranium by mercury cathode electrolysis in hydrochloric acid solution was investigated. The dependence of the reducton ratio on the different media, the acid and uranium concentrations, and on the time of electrolysis was determined. It was found that hexavalent uranium can be reduced quantitatively to trivalent state by mercury cathode electrolysis. The absorption spectra of U(III) and U(IV) in 1M and 9M hydrochloric acid solutions were examined. The molar extinction coefficient of U(III) at 521 nm was 16.7 m2·mol–1 within the HCl concentration range of 0.5–4.5M. U(IV) practically does not interfere in the photometric determination of U(III) at this wavelength. A good linear dependence of absorbance on the concentration of U(III) was found.