Separation/preconcentration of copper and cadmium using TiO2 core-Au shell nanoparticles modified with 11-mercaptoundecanoic acid and their slurry analysis by flame atomic absorption spectrometry were described. For this purpose, at first, titanium dioxide nanoparticles were coated with gold shell by reducing the chloroauric acid with sodium borohydride and then modified with 11-mercaptoundecanoic acid. The characterization of modified nanoparticles was performed using ultra-violet spectroscopy and dynamic light scattering. Copper and cadmium were then collected on the prepared sorbent by batch method. The solid phase loaded with the analytes was separated by centrifugation and the supernatant was removed. Finally, the precipitate was slurried and directly aspirated into the flame for the determination of analytes. Thus, elution step and its all drawbacks were eliminated. The effects of pH, amount of sorbent, slurry volume, sample volume and diverse ions on the recovery were investigated. After optimization of experimental parameters, the analytes in different certified reference materials and spiked water samples were quantitatively recovered with 5% RSD. The analytes were enriched up to 20-fold. Limits of detection (N = 10, 3 sigma) for copper and cadmium were 0.28 and 0.15 ng mL(-1) respectively. (C) 2010 Elsevier B.V. All rights reserved.