HE POSSIBILITY to reduce the levels of heavy metals from ……aqueous waste solutions by using polyacrylamide ferric antimonate ion-exchangers has been investigated in this study. These composite ion exchangers have high chemical stability and high loading capacity. The materials were characterized using X-ray diffraction analysis, infrared spectroscopy and thermogravemetric and differential thermal analysis. The distribution coefficients and separation factors of prepared materials were calculated for Fe (III), Pb (II), Cd (II), Cu (II), and Zn (II) ions. The samples prepared show high chemical stability in water, nitric and hydrochloric acids, as well as in potassium and sodium hydroxides. All these results support the suitability of the prepared material for removals of heavy metals from aqueous waste solutions.Keywords: Characterization,Organic-inorganic hybrid and Distribution studies.Composites ion exchangers consist of one or more ion exchangers combined with another materials, which can be inorganic or organic and it may be an ion exchanger. Thus, organic-inorganic hybrid materials are expected to provide many possibilities as new composite materials. The hybrid materials usually show intermediate properties between those of plastics and glasses (ceramics). Accordingly, hybridization can be used to modify organic polymer materials or to modify inorganic materials. In addition of these characteristics, the hybrid materials can be considered as new composite materials that exhibit very different properties from their original components (organic polymer and inorganic materials) (1)(2)(3)(4)(5)(6) . Attempts are focused in this study to prepare composite ion exchangers for treatment of aqueous waste solutions. Heavy metals are nondegradable in the environment and can be harmful to a variety of living species. For this reason, the removal of these metals from aqueous waste solutions is important in terms of protection of public health and environment. The heavy metals levels in aqueous waste solutions, drinking water, and water used for agriculture should be reduced to the maximum permissible concentration (7) . Ion exchange method is one of the important procedures for removal of the heavy metals from aqueous waste solutions.