The steady-state fluorescence (SSF) technique was used to study the polymerization rate in free-radical crosslinking copolymerization (FCC) of methyl methacrylate (MMA) and ethylene glycol dimethacrylate (EGDM). Pyrene (Py) was used as a fluorescent probe for the in situ polymerization experiments. The increase in Py intensity was monitored during FCC. The Stern-Volmer kinetic was employed to determine the MMA consumption rate during gelation process for various EGDM contents and at different temperatures.