A new adsorbent for determination of Pb and Cu by flame atomic absorption spectrometry (FAAS) was synthesized and characterized with different techniques. The effect of various parameters such as the pH, the type and volume of eluent, amount of adsorbent, sample volume and interfering ions were optimized. Under the optimized conditions, a linear calibration graph was obtained for determination of Pb(II) and Cu(II). The linear ranges were found to be 15-500 µg L−1and 18-500 µg L−1 for lead and copper, respectively. The limit of detection and limit of quantification were 4.3 and 14.5 µg L−1for lead and 5.0 and 16.7 µg L−1for copper, respectively. The relative standard deviation for eight replicate determinations of 80 and 200 µg L−1of Pb(II) were 2.9 and 1.4% and for Cu(II) were 3.5 and 1.9%, respectively. Applicability of the method was evaluated by analyzing trace amounts of lead and copper in different water samples.