A new chelating resin, covalently linked 1,6-bis(2-carboxy aldehyde phenoxy)butane with the Amberlite XAD-16 was synthesized and used for preconcentration of Cu(II) and Cd(II) prior to their determination by flame atomic absorption spectrometry (FAAS). It was characterized by elemental analyses and Fourier Transform Infrared Spectroscopy (FT-IR). Cu(II) and Cd(II) ions were quantitatively preconcentrated on minicolumn loaded with synthesised resin at pH 4.00 and 6.00, respectively. They were eluated with 5mL of 0.5molL⁻¹ HCl. Recoveries of Cu(II) and Cd(II) were found to be 100±2.15, 100±1.40 (N=5), the limits of detection of Cu(II) and Cd(II) in the determination by FAAS (3s, N=20) were found to be 0.33 and 1.19μgL⁻¹, respectively. The effect of foreign ions on the recovery has been investigated. The proposed method has been applied for the determination of Cu(II) and Cd(II) ions to the real samples collected from Tigris river water in Diyarbakır and Elazığ cities in Turkey. Standard addition method and analysis of the certified reference material (NCS-DC 73350) was employed to check the accuracy of the method.