In homogeneous catalysis, the application of organic solvent nanofiltration (OSN) has become a well‐known alternative to common recycling methods. Even though some OSN membranes are commercially available, their classification and the scope of application have to be determined for the specific solvent mixture. The commercial membrane Evoniks DuraMem® 300 was tested in a mixture of ethanol, ethyl acetate, and cyclohexane with magnesium triflate as possible catalyst. The cross permeate fluxes were measured for two transmembrane pressures and the hydrodynamic radii of the components were determined. Some of the components in the ternary mixture are retained, which makes the membrane also suitable for fractioning thereof.

This work tries to close the gap between continuous synthesis, measurement, calibration, and analysis on R&D scale. By introducing new calibration methods, the full potential of inline ATR‐FTIR spectroscopy in continuous reactor setups is unraveled. A fast, fully automated calibration of the reaction mixtures is carried out at process conditions. The use of different compositions underlines the robustness of this calibration method, which was used for the determination of kinetic parameters. The conversion‐based calibration significantly increased the precision of the analysis. In difference, the new method only requires the preparation of two calibration mixtures. By that, this method can also be applied to large‐scale processes and allows the use of a single measurement setup from R&D to industrial scale.