Abstract: | The anionic dispersion block copolymerization of styrene and 1,3‐butadiene has proved a suitable technique to synthesize block copolymers of tailor‐made blocklength under technically relevant conditions. For this purpose, however, an efficient analytical on‐line technique is required to control the concentrations of individual reactants and product. The present communication shortly outlines the potential of non‐invasive light‐fiber Fourier‐transform Raman spectroscopy in combination with a self‐modeling curve‐resolution analysis to monitor the polymerization progress and to derive concentration profiles of the two monomers and polybutadiene without prior calibration of the investigated system. |