Abstract Synthesis of bismuth oxide synthesis through the precipitation method using H2C2O4 and Na2CO3 precipitating agents, identification of physicochemical properties and its photocatalysis activity for methyl orange degradation were conducted. The bismuth oxide synthesis was undertaken by dissolving Bi(NO3)3.5H2O in HNO3, then added precipitating agents to form precipitate. The results showed that bismuth oxide produced by H2C2O4 precipitating agent was a yellow powder containing a mixture of α-Bi2O3 (monoclinic) and β-Bi2O3 (tetragonal), porous with size of 28-85 μm. Meanwhile, the use of Na2CO3 as precipitating agent resulted in bismuth oxide consisting of α-Bi2O3 and β-Bi2O3 and Bi2O4, irregular shape without pore being 40-115 μm in size. Bismuth oxide synthesized with H2C2O4 precipitating agent showed higher photocatalytic activity compared to bismuth oxide synthesized using Na2CO3 on degrading methyl orange dye with degradation rate constants of 2.35x10-5 s-1 for H2C2O4 and 1.81x10-5 s-1 for Na2CO3.