In this study, activated bentonite was used for the separation and preconcentration of cobalt, copper and manganese prior to their determination by flame atomic absorption spectrometry (FAAS). The bentonite used in this study was obtained from west part of Turkey, Enez, Edirne. Optimum conditions for the separation and preconcentration of analyte elements were investigated. Bentonite was further purified by treating the material with 4.0 mol L-1 hydrochloric acid for the removal of contaminants before use. Both batch and column methods were used for the separation of the above metals. In the batch method, the effects of pH and shaking time on retention and elution were investigated. The elements were quantitatively retained by the collector at pH 4 and again quantitatively eluted with of 0.1 mol L-1 EDTA for Cc and Mri and 2.0 mol L-1 HCl for Cu and Mn.