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 (30oC, 50oC, 70oC) 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.