A separation-preconcentration procedure was developed for determination of trace amounts of palladium, rhodium and gold in dust and water samples by flame atomic absorption spectrometry after simultaneous coprecipitation by Mn(OH) 2 without chelating agent. The precipitate could be easily dissolved with concentrated nitric acid. The influence of the various analytical parameters such as pH, sample volume, centrifuge time, standing time, centrifugation rate and time, amounts of manganese and matrix effects were studied for the quantitative recoveries of the analyte ions. Under the optimized experimental conditions, the calibration curves for Pd(II), Rh ( , respectively. The proposed method has been applied for determination of trace amounts of palladium, rhodium and gold ions in the standard, road dust and water samples and satisfactory results were obtained.