Abstract: The new separation and purification method for~(177)Lu~m is investigated: the solution of 30 mg natural Lu_2O_3 target irradiated with thermal neutron for 26 d and decayed for 11 months is passed through a NH~+_4 type cation exchange column,~(177)Lu~m and other radionuclides are separated with 0.12 mol/L α-hydroxyisobytyric acid eluent. The~(177)Lu~m is purified from the 0.12 mol/L α-hydroxyisobytyric acid by elution 0.1 mol/L HCl from a H~+ type cation exchange column. The labeling of EDTMP with~(177)Lu~m is obtained. The results show radioactivity of purified~(177)Lu~m is 18.17 MBq, special (activity) 0.624 MBq/mg Lu_2O_3, radioactive purity over 99%, the yield is 97%. The fast paper chromatography of~(177)Lu~m-EDTMP is established, the labeling efficiency of~(177)Lu~m-EDTMP is more than 97% with the optimized labeling condition: ρ(EDTMP)>0.15 mg/mL, ρ(Lu_2O_3)=0.047 mg/mL, pH=5～10, the room temperature, 5 min.~(177)Lu~m-EDTMP can be used in the further study of~(177)Lu~m-(EDTMP), which a potential therapeutic agent for bone metastases.