Leaching yields from an activated aggregate, removal yields from leachate, and overall mass balance relevant to the chemical procedure were investigated on radionuclides of 59Fe, 60Co, and 152Eu to reduce volume of radioactive waste used in a nuclear reactor facility. The radioactive nuclides were leached with 7 M HNO3 from the aggregate, then the 7 M HNO3 solution was mixed with NaOH or NH3 water to remove the nuclides as a precipitate. 70–80% of 60Co and 60–70% of 152Eu were leached from an activated aggregate. 100% of 59Fe, more than 99% of 60Co, and 94–98 % of 152Eu were removed as a precipitate at pH higher than 4, 7, and 6, respectively. Removal rates became lower at pH lower than 4 for 59Fe, 7 for 60Co, and 6 for 152Eu. It is basically possible to separate 60Co and 152Eu from precipitate of Fe at pH ∼ 4. The further separation to reduce volume of waste is not practical, because 20% of 60Co and 152Eu contained in the precipitate. 93% of volume reduction was achieved with one-step separation.

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