Internal gelation process was employed for preparation of 0.3-1 mm sized microspheres of titania for their application in ion exchange columns. The- conventional internal gelation process was modified by adding surfactant and oil emulsion in the feed broth , which introduced large pores in the structure of the material. The effects of concentration of hydrochloric acid. titanium. surfactant and hexarncthylcretctraminc to titanium ratio in the feed broth and temperature of calcination on the surface characteristics of the final product were studied , The conditions of preparation were optimized to obtain physically stable porous microsphercs suitable for various applications, The resultant material was characterized by pore size distribution. Pore volume, thermogravimetry. X-ray diffract ion and SEM analyses . Ion exchange behaviour of the material was then studied by pH titration.