A simple, fast, and sensitive column solid phase extraction study has been proposed for flame atomic absorption spectrometric determination of lead, cadmium, chromium, nickel, copper, and manganese ions on XAD-4 as 1-(2-pyridylazo)2-naphthol (PAN) complexes. The analytes were sorbed as PAN complexes on Amberlite XAD-4 column at the pH range of 8.5-10, and then eluted with 1 M HNO3 in acetone. The effect of pH, reagent amount, sample volume, and matrix of the sample on the sorption of metal ions has also been investigated. The concentration of analytes after separation and preconcentration was in agreement with the added amount of ions. The present method was found to be applicable to the preconcentration of analyte ions in river water from Yesilirmak, lake water from Lake Van, bottled mineral waters, tap water, stream sediment, mushroom, tobacco, and black tea samples with good results (recoveries greater than 95%, relative standard deviations lower than 10%).