A Fe(OH)2 suspension was prepared by mixing iron sulfate and a weak alkali ammonia solution. Following this, iron oxides were synthesized by passing pure oxygen through the suspension (oxidation). The effects of different reaction temperatures (30˚C, 50˚C, 70˚C) and equivalent ratios (0.1~10.0) on the formation of iron oxides were investigated. An equilibrium phase diagram was established by quantitative phase analysis of the iron oxides using the Rietveld method. The equilibrium phase diagram showed a large difference from the equilibrium phase diagram of Kiyama when the equivalent ratio was above 1, and single Fe3O4 phase only formed above an equivalent ratio 2 at all reaction temperatures. Kiyama synthesized iron oxide using iron sulfate and a strong alkali NaOH solution.