Physical processes, online monitoring

As noted in the introduction, a major aim of the current research is the development of "black-box" automated reactors that can produce particles with desired physicochemical properties on demand and without any user intervention. In operation, an ideal reactor would behave in the manner of Figure 12. The user would first specify the required particle properties. The reactor would then evaluate multiple reaction conditions until it eventually identified an appropriate set of reaction conditions that yield particles with the specified properties, and it would then continue to produce particles with exactly these properties until instructed to stop. There are three essential parts to any automated system—(1) physical machinery to perform the process at hand, (2) online detectors for monitoring the output of the process, and (3) decision-making software that repeatedly updates the process parameters until a product with the desired properties is obtained. The effectiveness of the automation procedure is critically dependent on the performance of these three subsystems, each of which must satisfy a number of key criteria the machinery should provide precise reproducible control of the physical process and should carry out the individual process steps as rapidly as possible to enable fast screening the online detectors should provide real-time low-noise information about the end product and the decision-making software should search for the optimal conditions in a way that is both parsimonious in terms of experimental measurements (in order to ensure a fast time-to-solution) and tolerant of noise in the experimental system. 

Online Monitoring of Chemical Reactions (Poiymerization, Curing), Physical Processes (e.g., Aging), and Structure Formation... 

Spectroscopic techniques are powerful process analytical tools. They are unparalleled in terms of molecular specificity, minimal sample preparation that translates to speed, and are capable of inferring physical properties [63,67,68]. Mid-infrared Fourier transform spectroscopy (FTIR), near-IR (NIR), and Raman spectroscopic techniques are the workhorse tools commonly used to monitor online polymerization processes. 

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