A novel and simple magnetic solid phase extraction procedure for the separation-preconcentration of lead(II) and copper(II) at trace levels has been established by using Chromotrope FB impregnated magnetic multiwalled carbon nanotubes as a new adsorbent. The influences of critical analytical parameters like pH, flow rates, eluent, and sample volume were optimized. Matrix effects were also examined. Analyte elements were quantitatively recovered at pH 6.0. The limit of detection values were 11.7 mu g L-1 for lead and 3.7 mu g L-1 for copper. The (%) RSD values were generally found at < 7%. The validation was performed by the analysis of NCS-DC73349 Bush Branches and Leaves certified reference material. The method was applied to the FAAS determination of lead and copper concentrations in cigarette and hair samples.