Abstract: Sampling, sample preparation and sample pretreatment method for electroplating sludge contained noble metals has been prepared, and related topics discussed. The direct determination of micro gold and palladium in the electroplating sludge using ICP-AES was studied. The result shows that under the optimal instrument parameters and working conditions, the detection limits of gold and palladium are 0.015～ 0.018 mg/L, respectively. The recovery rates are in the range of 94.0%～104.0%. The relative standard deviations (RSDs) are less than 3%. The method can be used to determine Au and Pd in electroplating sludge.