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HPGe γ spectrometry sourceless efficiency calibration method is playing an important role in radioactive analysis,for its high accuracy and efficiency; it can be used without radioactive source,facilitated in situ measurement.By verification with the IAEA reference materials,we verified the reliability of γ spectrometry sourceless efficiency calibration method.And using this method,we analyzed the radioactive nuclides in rare earth residues of our province.The result shows that the radioactive equilibrium among the parents and the daughters in uranium (thorium) decay series of the rare earth residues has been destroyed and there are notable differences on radioactivity levels among them.Based on the results,this paper investigates and analyses the radioactive residues of rare earth smelting and separation plants in Jiangsu Province,and puts forward some suggestions on volume reduction.