Styrene emulsion polymerization was performed in batch reactor using Raman spectroscopy for in situ monitoring of styrene conversion. The variation of the band of trigonal aromatic ring breathing at 1,000 cm−1 was analyzed in detail as a function of monomer conversion (wavenumber, integrated intensity, and half‐width at half‐maximum). The observed variation was described both qualitatively and quantitatively by a model assuming that the overall signal resulted from the addition of two close and distinct Gaussian signals, one originating from the monomer and the other one from the polymer repeat units. A reliable estimation of monomer conversion was obtained using the relative contributions of both components. The results were comparable to those obtained using the ratio of integrated intensities of the band at 1,000 cm−1 (overlapping signals of monomer and polymer) and the band at 1,631 cm−1 (signal specific to monomer). It was shown experimentally that information about monomer conversion could be obtained by applying linear model mixture to a single band of Raman spectrum, which provided an alternative method to the use of a ratio of integrated intensities.
Two complementary analytical techniques, Raman spectroscopy and drop tensiometry, were coupled in an original homemade experimental setup for in situ monitoring of radical polymerization in a single monomer droplet. Homopolymerizations of styrene and methyl methacrylate initiated by 2,2′‐azobisisobutyronitrile in a single droplet surrounded by an aqueous medium containing sodium dodecylsulfate were investigated. Monomer conversion (from Raman spectroscopy) and interfacial properties (interfacial tension and dilational moduli, from drop tensiometry) were simultaneously acquired in situ.
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