A sodium diuranate (SDU) process was studied to determine how completely it would recover uranium from a UF6 transport cylinder wash solution and convert it into pure uranyl peroxide solid for recycle into the nuclear fuel cycle and fuel fabrication. The initial process separated residual iron from the wash solution by precipitating it out as Fe(OH)(3), then precipitated the uranium from the solution as SDU. A carbonate extraction was used to strip the uranium from the SDU as a uranyl carbonate complex solution, and the uranium was separated from this carbonate complex solution as a UO4 center dot nH(2)O solid precipitate. Experimentation showed the process to be generally successful, but led to modifications and improvements to enhance the separation of uranium. The modified process did recover essentially all of the uranium from the wash solution and converted it into a very pure UO4 solid. The purity of the separated product was confirmed with mass spectrometry. An analogous potassium diuranate (KDU) process was also attempted to evaluate for any significant differences or advantages as compared to the SDU process. This process proved ineffective during the carbonate extraction phase and was abandoned.