A new method has been developed for the determination of gold based on separation and preconcentration with a microcolumn packed with nanometer TiO2 immobilized on silica gel (immobilized nanometer TiO2) prior to its determination by flame atomic absorption spectrometry. The optimum experimental parameters for preconcentration of gold, such as pH of the sample, sample flow rate and volume, eluent and interfering ions, have been investigated. Gold could be quantitatively retained by immobilized nanometer TiO2 in the pH range of 8-10, then eluted...