Abstract: A method used for the determination of Na, K, Ca, Sc, Cr, Fe, Co, Ni, Zn, As, Se, Rb, Mo, Ag, Cd, In, Sn, Sb, Ba, Cs, Ir, Au, Th and rare earth elements in biological materials is described. The freeze-dried samples are irradiated in the core channel of a heavy water reactor with a flux of about 5 ×1013n/cm2s for 40 h.The radiochemical group separation is carried out after 3 days' cooling. The procedure is as follows: After dissolution with HNO3 and H2O2, the irradiated samples are passedthrough three columns——the HAP, the anion resin and the cation resin successively. Byusing different eluting solution, the interested elements are divided into six groups. About 25 trace elements can be rapidly determined with Ge (Li) semi-conductor detector.For examining the accuracy of this method, standard reference materials rice (NBS-SRM-1568) and bovine liver (NBS-SRM-1577) are analysed. Our results are quite consistent with NBS's value.Some samples of normal human whole blood are analysed and the results reported.The chemical yield of 24 elements are given.