Zirconium phosphate, HZr 2 (PO 4 ) 3 (HZP), was synthesized in inner pores of highly porous silica beads, and the ion exchange properties of HZPloaded silica beads (HZP-SiO 2 ) thus obtained were examined. The ion exchange properties of HZP-SiO 2 were basically equivalent to those of HZP in the form of powders. Chromatographic lithium isotope separation was attempted using HZP-SiO 2 as column packing material. The heavier isotope was effectively accumulated in the frontal part of the lithium chromatogram. However, the tailing phenomenon was observed at the rear boundary of the chromatogram, and no effective accumulation of the isotope separation effect was observed in the tail.