A continuous flow autoanalyzer for at-line monitoring of total grease and surfactant contents in alkaline degreasing baths is proposed. For this purpose, a simple, robust, automated configuration has been on-line coupled to an universal response detector, such as the evaporative light scattering one. The proposed autoanalyzer constitutes an advantageous alternative to manual procedures and achieves the determination of both indices in ca. 15 min. The parameters thus obtained can be used to evaluate the degree of exhaustion of the bath as therefore allows the timely decision-making about reusability, maintenance or renewal. The fractionation model has been validated using attenuated total reflection-Fourier transform-infrared (ATR-FT-IR) spectroscopy. The potential of the method was realized by applying it to the analysis of 15 real samples obtained from precleaning and cleaning alkaline baths from a production line of a metal industry.