The investigated nanometric magnetite powders were synthesized electrochemically, and examined by XRD and SEM techniques. Their reduction was conducted through the isothermal heating in hydrogen in the temperature range from 600 to 860 K. Kinetics of the hydrogen recovery process during oxidation of freshly formed Fe powders in a water vapor stream was also studied. It was assumed that the solid-gas reaction is diffusion controlled, and Jander’s model was applied to describe it. The experimental data suggest that the reoxidation process proceeds in two stages, at various activation energies. By changing the conditions of the electrochemical (EC) process we were able to produce the iron oxide powders with optimal particle size and activity, for pure hydrogen production through appropriate reduction/oxidation processes.