Nano structured zirconium phosphates (ZPs) of different sizes were synthesized using Tritron X-100 (polyethylene glycol-p-isooctylphenyl ether) surfactant. The materials were characterized by FTIR and Powdered X-ray diffraction (XRD). The structural and morphological details of the material were established by scanning  electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM study was followed by energy dispersive spectroscopic analysis (EDS) for elemental analysis of the sample. The particle sizes were determined by dynamic light scattering (DLS) method. Ion exchange capacity of these nano materials towards different metal ions was measured and size-dependention exchange property of the materials was investigated thoroughly. The nano material of the smallest size (ca. 21.04nm) was employed to separate carrier-free ^137mBa from ¹³⁷Cs in column chromatographic Technique using1.0MHNO3 as eluting agent at pH=5.