This research had two stages of development: during the first stage, the purpose of the research was to evaluate the adsorption properties of the natural polymer represented by shredded maize stalk (MS) and by Amberlite XAD7HP (XAD7HP) acrylic resin for removal of toxic diazo Acid Blue 113 (AB 113) dye from aqueous solutions. The AB 113 concentration was evaluated spectrometrically at 565 nm. In the second stage, the stability of MS loaded with AB 113 (MS-AB 113) and of XAD7HP loaded with AB 113 (XAD7HP-AB 113) in acidic medium suggests that impregnated materials can be used for selective removal of metal ions (Cr3+, Zn2+ and Mn2+). The metal ions using atomic absorption spectroscopy method (AAS) were determined. The use of MS-AB 113 ensures a high selectivity of divalent ions while the XAD7HP-AB 113 had excellent affinity for Cr3+ in the presence of Zn2+ and Mn2+. As a consequence, two advanced polymers, i.e., MS-AB 113 and XAD7HP-AB 113 that provide huge capacity for removal of Zn2+, Mn2+ and Cr3+ from acid polluted wastewater were obtained.