A novel thiosemicarbazide modified adsorbent (PAN(MW)-TSC) based on polyacrylonitrile fiber was successfully synthesized under microwave irradiation, which was applied for the uptake of Cd(II) and Pb(II) from aqueous solution subsequently. Microwave irradiation method is a new approach to achieve the modification and it turns out that just a 30 min process is enough for the anchoring of functional groups in the fiber matrix. The surface characterization was performed by fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) elemental analysis (EA) and thermogravimetric analysis (TGA), indicating that the modification was successfully accomplished. Batch adsorption experiments including equilibrium isotherms, kinetics and the effects of pH and temperature on the adsorption of Cd(II) and Pb(II) were systematically studied. Among three kinetic models, the pseudo-second-order kinetic model provides the best correlation for the process. The nonlinear resolution of the Langmuir isotherm equation has been found to show the closest fit to the equilibrium date. Thermodynamic parameters, involving Delta G, Delta H and Delta S were also calculated from graphical interpretation of the experimental data, which suggest that metal ions adsorption onto PAN(MW)-TSC fibers is spontaneous and exothermic. Regeneration of PAN(MW)-TSC fibers loaded with metal ions was efficiently done with 0.5 M HNO3, by which the investigated adsorbent could be used reproductively for five times with a small decrease in sorption capacity. The feasible preparation of PAN(MW)-TSC fibers with high adsorption capacities opens a new perspective in the potential application for wastewater treatment. (C) 2016 Published by Elsevier B.V.