In this study, rice husk and jatropha shell were employed as precursors for the production of activated carbon by thermal and chemical activation process using phosphoric acid (H3PO4). The thermally activated carbon derived rice husk (RH) and jatropha shell (JS) and phosphoric acid activated derived rice husk (RH-Ac) and jatropha shell (JS-Ac) were characterized using BET, XRD, FTIR, Raman spectroscopy, SEM and XPS analysis. It showed that the cavities developed on the surfaces of RH-Ac and JS-Ac were be more high than those RH and JS. The BET surface area of RH, JS, RH-Ac and JS-Ac were 694.3 m2/g, 723.1 m2/g, 1261.3 m2/g and 1327.7 m2/g, respectively. The XPS analysis revealed that RH and JS exhibited the relative lower contents of carbonyl and phenol carbon than RH-Ac and JC-Ac. The as-prepared RH-Ac and JC-Ac were employed for the adsorption of Cu2+ and Fe2+ due to it better physicochemical properties. The most important influencing factors the adsorption of these metal ions such as pH, contact time, initial concentration were systematically studied. Experimental results were well analyzed by Langmuir model with the maximum adsorption ability of Cu2+ (22.773 mg/g), Fe2+ (25.431 mg/g) onto RH-Ac and Cu2+ (32.458 mg/g) and Fe2+ (56.179 mg/g) onto JS-Ac, which showed to be high in comparison to the similar activated carbon available obtained by other researchers. The pseudo 2nd order model showed that adsorption kinetic of Fe2+ and Cu2+ ions onto the JS-AC and RH-Ac has domination towards chemisorption. Moreover, thermodynamic parameters suggested that RS-Ac and JS-Ac for Cu (II) and Fe (II) adsorption phenomenon was endothermic and spontaneous. The high availability, facile production along with high performance of RH-Ac and JS-Ac make it an economically adsorbent for Fe (II) and Cu (II) adsorption.