Due to the industrialization, especially in the developing countries, the emission of the heavy metals as lead, cadmium, chromium, nickel, arsenic, and mercury are highly concerned to public and aquatic health. Lead is released with the effluent from the paint, batteries, and automobiles manufacturing units. Lead is one of the toxic metals and largely affects the central, peripheral nervous system. In this study, a suitable and reliable method for the direct determination of Pb and Ni ions in environmental water is proposed. Pb and Ni ions were extracted and precocentrated with layered double hydroxides (LDHs) nano-particles. LDHs, relatively inexpensive and simply prepared material, was synthesized and used as a solid phase extraction (SPE) adsorbent to quantitatively determine the concentration of Pb and Ni ions in natural water samples. Several factors affecting the extraction efficiency, such as, eluent type, eluent volume, flow rate of sample, sample volume, and amount of adsorbent, were investigated and optimized in detail. Pb and Ni ions can be quantitatively retained by LDH nano-particles, then eluted completely by 1 mL of CO 3 2-(1.5 mol L-1) and1mL EtOH (65% v/v), respectively. The detection limit of this method for Pb and Ni ions was 17 ng mL−1with an enrichment factor of 100, and the relative standard deviation (RSD) was 1.4%.