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Separation of trivalent minor actinides (MA(III): Am(III), Cm(III)) from fission products (FP) in high-level liquid waste (HLLW) is an important task in advanced nuclear-fuel reprocessing systems. For this purpose, an advanced aqueous partitioning process based on extraction chromatography method was studied. Because R-BTP extractants (R-BTP: 2,6-bis(5,6-dialkyl-1,2,4-triazin-3-yl)pyridine, R = alkyl group) exhibit high selectivity for MA(III) over trivalent rare-earth elements (RE(III)), a novel adsorbent isoHex-BTP/SiO2-P was prepared by impregnating isoHex-BTP extractant into the macroporous SiO2-P support with a mean diameter of 60 μm. The stability of isoHex-BTP/SiO2-P against nitric acid and γ-irradiation was investigated. It was found that isoHex-BTP/SiO2-P adsorbent shows good adsorption affinity to Dy(III). The hydrolytic and radiolytic stability of isoHex-BTP/SiO2-P adsorbent in 0.01 mol/L HNO3 was fairly promising. However, the adsorption amount Q of Dy(III) decreased dramatically in 3 mol/L HNO3 with the increase of the absorbed dose and became nearly zero at the absorbed dose over 46 kGy. These results suggest that with the synergetic effect of radiation and acidic hydrolysis, the adsorbent instantly loses its efficacy.