A simple, rapid and inexpensive method for separation and preconcentration of some traces of hazardous elements is presented prior to their flame atomic absorption spectrometric determinations. At pH 6.5; cadmium(II), cobalt(II) and lead(II) were separated simultaneously with 1,2-bis((1H-benzo[d]imidazol-2-yl)methoxy)benzene (BBIMB) as a new complexing agent and floated after adding sodium dodecyl sulfate (SDS) as a foaming reagent. The floated layer was then eluted by concentrated nitric acid in methanol and introduced to the flame atomic absorption spectrometer (FAAS). The effects of pH, concentration of BBIMB, type and amount of surfactant as the floating agent, type and amount of eluting agent and influence of foreign ions on the recoveries of the analyte ions were investigated. Also, by using a non-linear curve fitting method the formation constants of Cd(II), Co(II) and Pb(II) complexes were obtained 1.02 × 10 6 , 1.17 × 10 6 and 1.46 × 10 6 , respectively. The detection limits of Cd(II), Co(II) and Pb(II) ions were 1.2, 0.7 and 0.5 mg/L, respectively. The enrichment factors were 45.0, 42.0 and 39.0 for Cd(II), Co(II) and Pb(II) ions, respectively. The proposed procedure was then successfully applied for determination of those heavy metals in colored human hair and dryer agents of paint samples.