A preconcentration-separation procedure based on coprecipitation of palladium with thulium(III) hydroxide has been established prior to its flame atomic absorption spectrometric detection. The analytical parameters which are efficient on the quantitative recoveries of palladium were investigated. Palladium(II) ions was quantitatively recovered at pH 7.5 with 2.25 mg of thulium(III). The concomitant ions have not interference effect on the recoveries of palladium(II). The preconcentration factor was calculated as 150. The detection limit of the presented method was calculated as 1.5 mu g/L. The method was successfully applied to the determination of palladium contents of anodic slime and waste waters.