Nanocrystalline zirconia, a novel high capacity sorbent material was synthesized and tested for its utility in the preparation of 188 W/ 188 Re generators. The structural investigation of the material was carried out using X-ray diffraction, surface area determination, FTIR and TEM micrograph analysis. Various experimental parameters were optimized to separate 188 Re from 188 W. The capacity of the material was found to be ∼325mgW/g at the optimum pH. A chromatographic 188 W/ 188 Re generator was developed using this material from which >80% of 188 Re generated could be eluted with 0.9% saline solution, with high radionuclidic, radiochemical and chemical purity and appreciably high radioactive concentration suitable for radiopharmaceutical applications.