Coupled UV–Vis/FT–NIR Spectroscopy for Kinetic Analysis of Multiple Reaction Steps in Polymerizations

We couple UV–vis and FT–NIR spectroscopy for the real-time monitoring of polymerization reactions, allowing the simultaneous tracking of the rates of light absorption and initiator/monomer consumption, from which dynamic and previously difficult-to-measure parameters are calculated: quantum yields of initiator consumption, initiation and polymerization, photosensitivity, and residual content of leachable chromophore. Estimating these parameters from one set of experiments is not possible with any other probing technique. We demonstrate the potential of this technique using the free radical initiating system including camphorquinone as photoreducible chromophore and amines as reductants for the visible-light-triggered bulk polymerization of methacrylate monomers, important for dental and biomaterials. Photoinitiation by camphorquinone/amine pairs in two dimethacrylates serves to show the importance of obtaining quantum yields in the polymerizing medium instead of using inert solvents. Additionally, the oft...