Niobium and stibium in the diuranate were separated from uranium matrix by CL-TBP, and measured by ICP-AES. CL-TBP was filled into a chromatographic column with inner diameter of 8 mm by wet method, and the final height of the column was about 12 cm. The chromatographic column had been pre-balanced by 3 mol/L HNO3 before used. A certain amount of mixed solution of niobium and stibium was loaded onto the column; every 1 mL eluting solution was collected with the total of 15 mL. Niobium and stibium in the diuranate were separated from uranium matrix by CL-TBP, and measured by ICP-AES. CL-TBP was filled into a chromatographic column with inner diameter of 8 mm by wet method, and the final height of the column was about 12 cm. The chromatographic column had been pre-balanced by 3 mol / L HNO3 before used. A certain amount of mixed solution of niobium and stibium was loaded onto the column; every 1 mL eluting solution was collected with the total of 15 mL .