Heavy metal determination was carried out by applying the solid phase extraction (SPE) method in batch mode followed by atomic absorption spectroscopy (AAS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) from aqueous solutions using Ghezeljeh montmorillonite nanoclay as a new natural adsorbent. The Ghezeljeh clay is characterized by using Fourier Transform Infrared (FT-IR) Spectroscopy, Scanning Electron Microscopy-Energy Dispersive Spectrometry (SEM-EDS) and X-ray Diffractometry (XRD) and X-ray Fluorescence (XRF). The results of XRD and FT-IR of nanoclay confirm that montmorillonite is the dominant mineral phase. Based on SEM images of Ghezeljeh clay, it can be seen that the distance between the plates is Nano. The effects of varying parameters such as initial concentration of metal ions, pH and type of buffer solutions, amount of adsorbent, contact time, and temperature on the adsorption process were examined. The effect of various interfering ions was studied. The adsorption data correlated with Freundlich, Langmuir, Dubinin-Radushkevich (D-R), and Temkin isotherms. The Langmuir and Freundlich isotherms showed the best fit to the equilibrium data for Hg(II), but the equilibrium nature of Cu(II) adsorption has been described by the Langmuir isotherm. The kinetic data were described with pseudo-first-order, pseudo-second-order and double-exponential models. The adsorption process follows a pseudo-second-order reaction scheme. Calculation of Delta G(0),Delta H-0 and Delta S-0 showed that the nature of Hg(II) ion sorption onto the Ghezeljeh nanoclay was endothermic and was favored at higher temperature, and the nature of Cu(II) ion sorption was exothermic and was favored at lower temperature. (C) 2015 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.