The hydrotalcite-like compound [Mg2Al(OH)(6)]NO3 center dot nH(2)O (shorted as MgAl-NO3) was intercalated with the chelating agent ethylenediaminetetraacetic acid (EDTA) and N,N'-1,2-ethanediylbis-1-aspartic acid (EDDS) by anion exchange to uptake heavy metal ions (Cu2+ , Pb2+) from aqueous solutions. These layered double hydroxides (LDHs) synthesized in this work were used to adsorb Cu2+ and Pb2+. The amount of Cu2+ or Pb2+ adsorbed at different pH, temperature, and the dosage of adsorbent was determined by atomic absorption spectrometry (AAS). The structure, the composition and the surface properties of precursor-LDHs and intercalated-LDHs (intercalated with the chelating agents) were characterized by chemical analysis, Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD) and a physical adsorption analyzer. Comparative experiments were carried out with commercially available LDH adsorbent (i.e., Kyowa DHT-4A). The adsorption behaviors of the MgAl-LDHs for Cu2+ and Pb2+ in aqueous were investigated by applying the adsorption results to the Freundlich isotherms model, and the data were well fitted by the model. The results suggested that MgAl-LDHs synthesized in this work could be suitable as sorbent materials for the adsorption and removal of heavy metal ions from aqueous solutions.