A method based on 1H-NMR and 31P-NMR was established for the quantitative analysis of tris(3 sulfonatophenyl) phosphine sodium salt hydrate(TPPTS).Through one dimensional 1H-NMR,13C-NMR,31P-NMR and two-dimensional 1H-1H COSY,1H-13C HSQC, 1H-13C HMBC,the chemical shift of TPPTS including all the hydrogen atoms,carbon atoms and phosphorus atoms were assigned.Trioxane was selected as the internal standard compound while N,N-dimethylformamide-D7(DMF-D7) was used as solvent in the 1H-NMR test.Correspondingly,KH2PO4 and deuterium oxide(D2O-D2) were used in the 31P-NMR test.The pulse delay time(D1) of the mixing system was set reasonably based on results of the longitudinal relaxation time(T1) test.Quantitative analysis results of TPPTS by 1H-NMR and 31P-NMR were (58.72 ± 0.21)% and (58.51 ± 0.21)%,respectively,which are close and parallel.Meanwhile,there is no need for the standards of the samples to be detected in the process.Thus the rapid and effective determination of TPPTS in the mixing system could be realized.