The synthesis and characterization of ethylenediaminetetraacetic acid immobilized activated carbon cloth was performed in the present work. It was used for preconcentration-separation of lead(II), cobalt(II), and nickel(II) at trace levels as an adsorbent. Factors including pH, concentration and volume of eluent, sample and eluent flow rates, sample volume, and effect of coexisting ions on the solid phase extraction of analytes were examined. The preconcentration factor was 50. The detection limits for Pb(II), Co(II), and Ni(II) were 4.39, 0.99 and 0.91 mu g L-1, respectively. The adsorption capacity for Pb(II), Co(II), and Ni(II) ions was found as 11.0, 11.2, and 10.2 mg g(-1), respectively. The validation of the method was performed by the analysis of certified reference materials (SPS-WW2 wastewater and BCR-146R sewage sludge amended soil (industrial origin)). The method was successfully applied for the determination of lead, cobalt, and nickel in fertilizer and water samples from Kayseri, Turkey.