A high performance novel extraction method for heavy metal ions from aqueous solutions is investigated using a microwave-assisted heating technique. The selected solid material is a functionalized nano magnetic iron oxide with 3-aminopropyltriethoxysilane [Nano-Fe3O4-SiO2-NH2] which is synthesized using a microwave-assisted procedure. The metal sorption properties of this magnetic nano-sorbent with four different divalent metal ions, viz. Pb(II), Cd(II) and Hg(II) were evaluated by heating the interacting metal ion solution in contact with the sorbent in a microwave oven for 5-30 s. Pb(II) was found the highest extracted metal ion and the capacity value was identified as 1250 mu mol g(-1) after heating for 5 s, while the equilibrium capacity value was obtained as 1300 mol g-1 at 15 s. The maximum capacity values of Cu(II), Cd(II) and Hg(II) were characterized as 1050, 350 and 350 after microwave heating for 25, 15 and 25 s, respectively. The collected data refer to an excellent and high performance solid phase extraction methodology of heavy metal ions from their matrices in few seconds based on using the microwave-enforced sorption technique. The functionalized Nano-Fe3O4-SiO2-NH2 sorbent was synthesized using the microwave-assisted preparation system and characterized by the FT-IR, SEM, HR-TEM, XRD-method and surface area determination. (C) 2016 Elsevier B.V. All rights reserved.