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New research applications involving the use of cellulosic material derived from maize stalk for on-site treatment of leachate were evaluated for specific removal of Cu(II) and Fe(III) from real, highly polluted tailing pond and mine wastewater samples. Two major issues generated by anthropic mining activities were also tackled: wastewater metal content decrease to improve water quality and subsequently metal specific recovery, increasing the economic efficiency of metal production by using a green technology for residual management. Rapid saturation of the maize stalk mass determined in batch studies and the mine pilot experiment led to diminished metal concentrations in the second pilot experiment, where Cu(II) and Pb(II) from synthetic solutions were monitored in order to test biomaterial performances. In addition, in the second pilot experiment, maize stalk removed Pb(II) in the first 36 h, below the determination limit of the analytical method. The biomaterial bed in the column was saturated after 252 h of inflow solution. FTIR-ATR, TG and SEM techniques probed the interaction between maize stalk polar groups C=O, –OH, C–O and tailing water metallic ions by large FTIR band displacements, intensity decrease and shape changes, modification of thermal stability and by changes in the appearance of adsorbent microstructure images owing mainly to ion exchange mechanism.