Polyvinyl alcohol solution in water-dimethyl sulphoxide will automatically change into gel. Auramine O as a fluorescence probe was added into the system. A self-catalytical curve

from which a gelation rate was taken out

of the gelation process was obtained by measuring fluorescence spectra of Auramine O. The effects of various component ratios in system on the gelation rate were examined. Kinetics of gelation was also studied by this method. It is found that the mole fraction of DMSO in the mixture solvent affected the rate of gelation. When the mole frac-tion of DMSO is 0.25

the rate of gelation reached the maximum. This phenomenon may be in-terpreted from the view of hydrogen bond formation. It is concluded that fluorescence probe method is efficient and easy for study of gelation process.