A new method using multiwalled carbon nanotubes as an SPE adsorbent was developed for the sensitive determination of trace iron and lead prior to flame atomic absorption spectrometry analysis. Iron and lead as 2,9-dimethyl-4, 7-diphenyl-1, 10-phenanthroline chelates were adsorbed quantitatively on multiwalled carbon nanotubes at a pH of 6.0 and easily eluted with 10 mL 1 M HNO3. The influences of matrix ions were also examined. The LOD values for iron and lead were calculated as 1.3 and 2.9 mu g/L, respectively. Validation of the presented procedure was performed by the analysis of TMDA 54.4 fortified lake water and HR-1 Humber River sediment certified reference materials. The method was successfully applied to the determination of trace iron and lead in real environmental samples, and excellent results were achieved.