In this book, lead adsorption efficiency of carboxylate-ferroxane nano structures from aqueous solutions have been studied. FTIR, SEM and DLS analysis characterized the synthesized samples. Performance evaluation of nano particles and nano composite in adsorption process was achieved using Taguchi and Box-Behnken experimental designs. Variables in adsorption process were initial pH, contact time, adsorbent dose and initial concentration of Pb(II) ions. Adsorption of lead was performed through two possible mechanisms; ion exchange and complex formation in case of both, the nano particles and the nano composite. Para amino benzoate-ferroxane nano particles performed the best among the other nano particles studied in lead adsorption. Also its corresponding nano composite with chitosan showed an improvement in Pb(II) uptake in comparison with the pure chitosan film.