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A method to facilitate the analysis of the complex formation by a polybasic acid has been applied to the study of uranyl citrate complexes. The amount of the uranyl ion in equilibrium with the complexing agent was determined by the cation-exchange method. In this experiment, the uranyl-ion concentration was kept within a 105–106 M range in order to eliminate polymeric species. By using a series of solutions prepared so as to keep [H3Cit−] nearly constant and to vary [H2Cit2−] and [HCit3−] in the 2.2–2.9 pH range, it has been found that three kinds of complexes, UO2H3Cit+, UO2H2Cit, and UO2HCit−, were present in the solution. Approximate values of their formation constants were obtained.