A novel enrichment-separation procedure based on solid phase extraction of copper(II) and lead(II) at ultratrace levels on 1-nitroso-2-naphthol impregnated multiwalled carbon nanotubes (NNMWCNTs) has been established. The effective critical parameters like pH and eluent type etc. on the quantitative recoveries of the analyte elements were optimized. The matrix effects are also investigated. The procedure was validated by analysing water certified reference materials and addition-recovery tests. The relative standard deviation of the presented procedure was below 10%. The application of the presented solid phase extraction procedure was successfully performed for copper and lead determination in some food and water samples.