Graphite oxide was synthesized and used as a solid-phase adsorbent for Cu(II) and Pb(II) in various samples. The characterization of the material was performed by X-ray diffraction, infrared spectroscopy, and Brunauer-Emmet-Teller measurements. The adsorption capacity of graphite oxide was 26.4 mg g(-1) for Cu(II) and 80.6 mg g(-1) for Pb(II). The detection limits of the method were 1.25 mu g L-1 for copper and 2.56 mu g L-1 for lead. Graphite oxide was used 150 times without any mass loss. A vortexing time of 30 s was sufficient for adsorption and elution contact times.