Abstract: Seven elements, i.e., Ca, Co, Cr, Cu, Mo, V and W, in P/M ferrous alloy were determined by ICP-AES with microwave assisted sample digestion. The sample was digested in a digestion vessel with 6 mL of mixed acid of H2SO4-H3PO4-H2O(1+2+7) and 3 mL of conc. HNO3 in a microwave digestor under the condition of 800 W and 0.6 MPa. Analytical spectral lines of 317.993 nm (for Ca), 228.616 nm (for Co), 205.552 nm (for Cr), 324.754 nm (for Cu), 204.598 nm (for Mo), 311.071 nm (for V) and 207.911 nm (for W) were chosen for the analysis. Matrix effect was compensated by the matching method in preparation of calibration curves. For verification of accuracy of the present method, a checking analytical program was carried out among 3 analytical laboratories on 3 samples by different analytical methods, the results obtained by the present method were found to be in consistency with the results given by the other laboratories.