Vitamin B3 (nicotinic acid, NA) is selected as an example of a promising environmental eco-friendly metal sequestering reagent to functionalize the surface of nanoalumina-loaded sodium dodecyl sulfate (nano-Al 2 O 3 -SDS) sorbent. This reaction is accomplished via microwave-assisted heating using a solvent-free approach for the formation of a novel nano-Al 2 O 3 -SDS-NA sorbent. The functionalized nanomaterials are characterized by Fouriertransform infrared spectroscopy, thermogravimetric analysis, and scanning electron microscopy. A comparative study is performed to explore and evaluate the sorption behaviors of nano-Al 2 O 3 , nano-Al 2 O 3 -SDS, and nano-Al 2 O 3 -SDS-NA sorbents for removal of Cu(II), Zn(II), and Pb(II) from aqueous solutions by the batch adsorption technique. The desired selectivity characteristics in the evaluated nanosorbents are confirmed from the determined maximum metal sorption capacity values of Cu(ΙΙ), Zn(II), and Pb(II) as 5700, 900, and 700 mmol g À1 by nano-Al 2 O 3 -SDS-NA sorbent, respectively, using a 5 mg dosage. The optimum contact pH, time, initial metal ion concentration and competing species are also investigated. The Langmuir, Brunauer-Emmet-Teller and Dubinin-Radushkevich adsorption isotherm models are applied to evaluate the interaction processes of Cu(II), Zn(II), and Pb(II) by nano-Al 2 O 3 , nano-Al 2 O 3 -SDS, and nano-Al 2 O 3 -SDS-NA sorbents. The potential applications of these nanosorbents for adsorptive removal of metal cations from real samples are successfully optimized via a micro-column technique.