A multiwalled carbon nanotube disk was used for the SPE of some toxic heavy metals from environmental samples. Metal ions were adsorbed on the disk as 8-hydroxquinoline complexes, then quantitatively desorbed from the disk by using 10 mL 2 M HNO(3). The effects of analytical parameters, including pH, sample volume, and flow rates, on the recoveries of Cd(II), Co(II), Ni(II), Pb(II), Fe(III), Cu(II), and Zn(II) were investigated. The influences of some 1A and 2A group elements and some other ions as concomitant ions on the recoveries of analyte ions were also examined. The LODs of the presented preconcentration-separation system for the analyte ions were found to be in the range of 1.0-5.2 mu g/L. In order to validate the procedure, SRM 1577B Bovine Liver, IAEA 336 Lichen, and HR-1 Humber river sediment certified reference materials were analyzed. The proposed method has been applied to the determination of understudy elements in some pharmaceutical samples and natural water samples from different sites in Turkey.