ABSTRACT. PVA/silica hybrid xerogels were synthesized by sonohydrolysis of a mixture of 2-way catalyzed TEOS and water solution of PVA. PVA was successfully removed from the xerogels through calcination and its removal was confirmed through TGA analysis of the calcined gel. Microstructure of the gels was studied through SEM, XRD and FTIR. Nitrogen sorption studies were conducted to find out surface area of different samples. It was found out that the samples having PVA removed through calcinations have higher surface area (411.64 m 2 /g) than the samples (353.544 m 2 /g) synthesized without any PVA. Adsorption properties of these xerogels synthesized by using different ratios of components were studied by taking Rhodamine G6 as a model adsorbate. The experiments were conducted at room temperature (25 o C). UV visible spectroscopy was used to measure the concentration of the dye before and after adsorption. The adsorption data of Rhodamine G6 on PVA modified silica is described by the Freundlich's adsorption model.