Quality control and reaction monitoring are necessary to ensure the consistency of any kind of mixing or reaction process. In this context, a novel portable high-sensitivity sensor prototype based on the Raman effect is presented in this study. The elongated probe head is designed for (but not limited to) monitoring high temperature batch processes for quality assurance. Thanks to the highly sensitive special detectors, concentration differences of up to 50 mmol/L can currently be detected, which facilitates compliance with high product quality standards. In addition, seamless reaction tracking is possible. Small individual adjustments through simple, intuitive mechanical components provide a high degree of flexibility in reaction selection by the end user. Specially developed software automates the evaluation process and gives the user visual signals about the current status and progress of the batch as well as an emergency stop if temperature limits could damage individual components. By using all the individual components developed, the problem of the limited integration times of previous spectrometric measuring instruments could be reduced. The prototype was validated using concentration measurements of various substances that occur as standard in batch processes. In addition, this article provides an outlook on the fact that Raman measurements can also be carried out successfully and reliably in explosive environments in the future with the prototype presented.
To meet the demands of the chemical and pharmaceutical process industry for a combination of high measurement accuracy, product selectivity, and low cost of ownership, the existing measurement and evaluation methods have to be further developed. This paper demonstrates the attempt to combine future Raman photometers with promising evaluation methods. As part of the investigations presented here, a new and easy-to-use evaluation method based on a self-learning algorithm is presented. This method can be applied to various measurement methods and is carried out here using an example of a Raman spectrometer system and an alcohol-water mixture as demonstration fluid. The spectra’s chosen bands can be later transformed to low priced and even more robust Raman photometers. The evaluation method gives more precise results than the evaluation through classical methods like one primarily used in the software package Unscrambler. This technique increases the accuracy of detection and proves the concept of Raman process monitoring for determining concentrations. In the example of alcohol/water, the computation time is less, and it can be applied to continuous column monitoring.
With the goal to better process the monitoring of occurring fouling, a backscatter probe was developed to perform in-line measurements in a half-shell reactor during the reaction of N-vinylpyrrolidone (NVP) to polyvinylpyrrolidone (PVP). The measurement technique detects the changes of bands in the UV range, which allows a direct correlation with the concentration. Thus, the measured absorbance signal allows a conclusion on the accumulation of fouling in the reactor and on changes in the conversion at the measurement location.
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