The quantitatively detection of uranyl in30%TBP/kerosene in Purex process was studied.The baseline of the Raman spectra was corrected,and the Raman band of uranyl which is considered as symmetric stretching mode v_(U-O)~8(860 cm~(-1))and the band of the organic solvent located at 1 065 cm~(-1)were selected as quantitative peak and internal standard reference peak, The quantitatively detected of uranyl in 30% TBP / kerosene in Purex process was studied. The baseline of the Raman spectra was corrected, and the Raman band of uranyl which was considered as symmetric stretching mode v_ (UO) ~ 8 (860 cm ~ (- 1)) and the band of the organic solvent located at 1 065 cm -1 were selected as quantitative peak and internal standard reference peak,