Herein, an efficient adsorbent based on intermetallics was developed for the adsorption of Pb(II) from aqueous solutions. Mesoporous FeSb 2 particles were synthesized via a costeffective co-precipitation method. The structural and morphological characterizations of FeSb 2 were evaluated using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Fourier transforms infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET), and zeta potential. The batch adsorption tests were performed as a function of initial Pb(II) concentration (5-70 mg L À 1 ), contact time (24 h), pH (2-9), FeSb 2 content (0.2-0.8 g L À 1 ), and recyclability (6 cycles), to evaluate the efficacy of FeSb 2 particles for Pb(II) removal. The adsorption behavior of FeSb 2 was found to match well with the pseudo-second-order kinetics and Freundlich isotherm model. The experimental maximum adsorption capacity (q m ) was achieved as 86.625 mg g À 1 for a Pb(II) concentration of 70 mg L À 1 . This value was found to be in good agreement with the value predicted by the Langmuir model, which was 88.26 mg g À 1 . Overall, this work documented the high potential of intermetallic FeSb 2 for the efficient removal of extremely dangerous Pb(II) ions and laid the foundation for other intermetallics in a new role of adsorbent for various wastewater treatments.