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Autor

  • Guhl, Svetlana (2)
  • Kern, Simon (2)
  • Maiwald, Michael (2)
  • Meyer, Klas (2)
  • Paul, Andrea (2)
  • Engell, S. (1)
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  • Gottu Mukkula, A. R. (1)
  • Gräßer, Patrick (1)
  • Holtkamp, M. (1)
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  • 2019 (1)
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Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals (2019)
Kern, Simon ; Wander, Lukas ; Meyer, Klas ; Guhl, Svetlana ; Gottu Mukkula, A. R. ; Holtkamp, M. ; Salge, M. ; Fleischer, C. ; Weber, N. ; Engell, S. ; Paul, Andrea ; Pereira Remelhe, M. ; Maiwald, Michael
Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance.
Online low-field NMR spectroscopy for process control of an industrial lithiation reaction—automated data analysis (2018)
Kern, Simon ; Meyer, Klas ; Guhl, Svetlana ; Gräßer, Patrick ; Paul, Andrea ; King, R. ; Maiwald, Michael
Monitoring specific chemical properties is the key to chemical process control. Today, mainly optical online methods are applied, which require time- and cost-intensive calibration effort. NMR spectroscopy, with its advantage being a direct comparison method without need for calibration, has a high potential for closed-loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and rough environments for process monitoring and advanced process control strategies. We present a fully automated data analysis approach which is completely based on physically motivated spectral models as first principles information (Indirect Hard Modelling – IHM) and applied it to a given pharmaceutical lithiation reaction in the framework of the European Union’s Horizon 2020 project CONSENS. Online low-field NMR (LF NMR) data was analysed by IHM with low calibration effort, compared to a multivariate PLS-R (Partial Least Squares Regression) approach, and both validated using online high-field NMR (HF NMR) spectroscopy.
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