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The polarography of uranyl ion in 2,3‐cresotic acid solution has been studied at 25°C under varying conditions of ligand concentration and pH. The ligands species were proved to be a 2,3‐cresotate anion. The half‐wave potential vs. pH value interpreted on the basis of pK value for the acid ionization, and resulted in agreement with the deduction. The mole ratio of metal to ligand was found to be 1:1 and 1:2 by conductometric titration. At pH < pK1, the complex species of UO2(H2A)2+ and UO2(HA)+ was identified. At pK1 < pH < pK2, the co‐existence of UO2(HA)+, UO2(OH)(HA)2− and UO2(A)22– was confirmed. At pH > pK2, the complex species of UO2(OH) (A)23– was formed.