Copper (II) and lead (II) ions are complexed with 1-nitroso-2-naphthol and preconcentrated on the magnetic activated carbon cloth prior to its flame atomic absorption spectrometric detection. Analytical parameters such as model solution pH, adsorbent amount, eluent type and volume, ligand amount, sample volume and matrix effect were determined. As a result of these studies, quantitative recovery of analyte ions was obtained at pH 4.0. Quantitative recovery was observed with 2 mL 3 M HNO3 solution as eluent. The developed method has been applied to various water and food samples and the accuracy of the developed method has been confirmed by certified reference material analysis and addition recovery studies. The method has been applied to the separation and preconcentration of copper (II) and lead (II) ions in water and food samples.