A liquid-liquid extractive preconcentration procedure for cobalt, nickel and manganese in human hair samples has been developed. Preconcentration preceded FAAS determination of these elements. These ions were extracted into toluene after chelation with 5,7-diiodo-8-hydroxyquinoline and stripped into 0.1 mol L^-1 EDTA solution. The method was optimised with respect to the pH, 5,7-diiodo-8-hydroxyquinoline concentration, the choice of the solvent and stripping agent, aqueous phase volume, and equilibrium time. The method was evaluated using the standard human hair reference material IAEA.086. The obtained results were in good agreement with the certified values. For the comparison purpose typical hair samples were analysed by the standard inductively coupled plasma atomic emission spectrometric method.