Two new solid phase extraction methods have been developed for simultaneous separation and precon-centration of Cu(II) and Cd(II) in some food and environmental samples before their determination by flame atomic absorption spectrometry (FAAS). One of these methods is based on the absorption of the Cu(II) and Cd(II) complexes with [3-(cyanomethyl)-5-(4-methylphenyl)-4H-1,2,4-triazol-4-ylicarbamate (L1) and the other is based on the absorption of the Cu(II) and Cd(II) complexes with 4-(4-methylphenyl)-5-{[pyridine-4-yl-4H-1,2,4-triazole-3-yl)thio]methyl}-4H-1,2,4-triazole-3-thiol (L2) on Amberlite XAD-1180 resin. The metal complexes are retained on resin at pH 6.0 and eluted with 1.0 mol L-1 HCl in acetone in both methods. After the optimum conditions were determined, the methods were applied to seawater, stream water, rice, lentil, tea, tobacco, bulgur, chickpea, wheat, red pepper, black pepper, peppermint, and dried eggplant samples in order to determine the levels of copper and cadmium.