Online Measurement System in Reaction Monitoring for Determination of Structural and Elemental Composition Using Mass Spectrometry.

The monitoring of chemical reactions is an important task in chemical engineering, especially in quality control, pharmaceutical and biological processes, or industrial production. The development of new reactions such as catalyst-based procedures requires detailed knowledge about process steps and reaction kinetics. For qualitative and quantitative analysis of reactants and resulting products, proprietary online measurement systems are used, which were designed for special applications. A mobile online reaction monitoring system was developed for a flexible coupling to different mass selective measurement systems for structural (ESI-MS) and elemental (ICP-MS) analysis to determine chemical precursors, reaction products, and internal standard compounds and their elemental composition at any stage of the reaction. Chemical reactions take place in a tempered continuous-flow microreactor. The flow rate in the microreactor can be varied to adjust the residence times in the reactor. An online dilution module was integrated to adapt the concentration of the reaction solutions to the working range of the analyzers. The performance and limitations of the online reaction system were determined using standard solutions and a real chemical reaction. The control software with a graphical user interface enables the adjustment of reaction, sampling, and measurement parameters as well as the system and process control.