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The polarography characteristic of uranyl ion in chromotropic acid solution was investigated systematically over the pH range 2.0 to 10.0 with ligand concentrations varying from 0.010 M to 0.200 M. At pH 5.5, the one‐electron reversible reduction waves were obtained. The temperature coefficient of the half‐wave potential was obtained to be −0.32 mV per degree and the mean value of id/h1/2 is 0.340 ± 0.003. The electrode reaction is UO2(HA)24− + c = UO2(HA)2− + HA3− Where pH 5.5, an irreversible and diffusion‐controlled wave was obtained. The diffusion coefficients and kinetic parameters of complex species were determined by deducing instantaneous equations.