In the present study, Cd(II), Co(II), and Ni(II) ions were separated and preconcentrated via carrier element-free coprecipitation (CEFC) method by using an organic coprecipitating agent, 1,2-bis-(2-tosyl ethoxy) benzene (BTEB), prior to their flame atomic absorption spectrometric (FAAS) detections. The experimental conditions were optimized in terms of pH of the aqueous solution, BTEB amount, standing time, centrifugation rate and time, and sample volume. Under the optimum experimental conditions, the detection limits for Cd(II), Co(II), and Ni(II) ions were found to be 0.13, 0.67, and 0.46 mu g L-1, respectively, and the relative standard deviations for the analyte ions were found to be lower than 4.0%. The accuracy of the method was tested by analyzing certified reference material and spike tests. The method was applied to determine the levels of Cd(II), Co(II), and Ni(II) ions in sea and stream water, macaroni, red lentil, and cracked wheat samples.