A crystallization process has been under development for the recovery of U as uranyl nitrate hexahydrate (UNH) crystals. Two experiments, solubility of Cs
2Pu(NO
3)
6 and U crystallization, were performed to evaluate the influence of HNO
3 concentration in solution on the precipitation behavior of Cs
2Pu(NO
3)
6. The solubility of Cs
2Pu(NO
3)
6 in a uranyl nitrate solution has been found to decrease with increasing HNO
3 concentration in the solution. These experimental results imply that Cs
2Pu(NO
3)
6 is readily formed in high HNO
3 concentration solutions. Based on the solubility of Cs
2Pu(NO
3)
6 in uranyl nitrate solutions, U crystallization experiments were performed with a range of HNO
3 concentrations in the feed solution. At an HNO
3 concentration of 4.5 mol/dm
3 in the feed solution, the HNO
3 concentration of the mother liquor was 6.5 mol/dm
3. The decontamination factor (DF) of Cs for the UNH crystals was 8.61 after crystal washing. In this case, Cs
2Pu(NO
3)
6 precipitated upon cooling of the feed solution and was not separated from the UNH crystals after crystal washing. On the other hand, the DF of Cs was 174 after the UNH crystals were washed when the HNO
3 concentration in the feed solution was 3.2 mol/dm
3. With a lower HNO
3 concentration in the feed solution, nearly all Cs remained in the mother liquor during the U crystallization process. Therefore, to suppress Cs
2Pu(NO
3)
6 precipitation, a lower HNO
3 concentration must be maintained in the feed solution.
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