<p>A radiochemical methodology was developed for the separation and purification of ⁶⁵Zn from irradiated Y₂O₃ targets used for ⁸⁹Sr production in the Fast Breeder Test Reactor. Y₂O₃ pellets containing 0.1&#xa0;wt.% ZnO as a sintering aid were irradiated for 30 d at a fast neutron flux of about10¹⁵ n cm⁻²&#xa0;s⁻¹ and subsequently processed under remote hot-cell conditions. Following dissolution of irradiated pellets in 9&#xa0;M HNO₃, ⁸⁹Sr was selectively separated using 4,4’(5’) di-tert-butylcyclohexano-18-crown-6. Distribution ratio studies using Dowex 50WX8 cation and Dowex 1X8 anion exchange resins demonstrated superior selectivity of the anion exchange system in mixed HCl–HNO₃ medium for ⁶⁵Zn separation over Y, Mn and Co. Under optimized 4.5&#xa0;M of [H⁺], obtained by mixing equal volumes of HNO₃ and HCl, Zn formed stable anionic chloro-complexes [ZnCl₄]⁻² and was selectively retained on the anion exchange resin, while ⁸⁸Y, ⁶⁰Co, ⁵⁸Co, and ⁵⁴Mn were effectively removed. Quantitative recovery of ⁶⁵Zn was achieved by water elution, followed by final purification using cation exchange chromatography to remove trace ⁸⁸Y contamination. The developed process yielded high-purity ⁶⁵Zn with nearly 100% recovery and without any detectable radionuclide impurities. The methodology eliminates complete nitrate-to-chloride conversion and minimizes bulk volume evaporation steps, thereby reducing operational complexity and improving suitability for remote hot-cell applications. Bulk-level demonstration confirmed the scalability and practical applicability of the process for routine radiochemical production and recovery of ⁶⁵Zn from secondary radioactive waste streams.</p>