The determination method of Ru, Rh and Pd in 30%TRPO-kerosene ICP-AES was studied by using aqueous calibration reference solution and choosing ethanol as diluent. The effects of the contents of 30%TRPO-kerosene and aqueous solution and the concentration of HNO3 in 30%TRPO-kerosene on the intensities of Ru, Rh and Pd were described. The optimized condition for preparing samples and calibration solutions was chosen as follows: The contents of 30%TRPO-kerosene and aqueous phase were 10%(Ｖ/Ｖ) and 5% (Ｖ/Ｖ) respectively and the concentration of HNO3 30%TRPO-kerosene was 0.20 mol·L-1. The determination method of Au, Ru and Pd was set up according to the above condition. The detection limit, precision and recovery ratio of Ru, Rh and Pd are well. The method is not only used in determination of Au, Ru and Pd in 30%TRPO-kerosene, but also used in other organic phases.