Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-36333 Zeitschriftenartikel Zientek, Nicolai; Meyer, Klas; Kern, Simon; Maiwald, Michael Quantitative online NMR spectroscopy in a nutshell Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced. Weinheim, Germany Wiley-VCH Verlag GmbH & Co. KGaA 2016 Chemie Ingenieur Technik 88 6 698 709 10.1002/cite.201500120 2016-06-02 OPUS4-37356 Zeitschriftenartikel Meyer, Klas; Kern, Simon; Zientek, Nicolai; Guthausen, G.; Maiwald, Michael Process control with compact NMR Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. To build an interdisciplinary bridge between "process control" and "compact NMR",we give a short overviewon current developments in the field of process Engineering such as modern process design, integrated processes, intensified processes along with requirements to process control, model based control, or soft sensing. Finally, robust field integration of NMR systems into processes environments, facing explosion protection or Integration into process control systems, are briefly discussed. Elsevier 2016 Trends in Analytical Chemistry 83 Part A / SI 39 52 urn:nbn:de:kobv:b43-373562 10.1016/j.trac.2016.03.016 https://creativecommons.org/licenses/by-nc-nd/4.0/deed.de 2016-09-15 OPUS4-44847 Zeitschriftenartikel Kern, Simon; Meyer, Klas; Guhl, Svetlana; Gräßer, Patrick; Paul, Andrea; King, R.; Maiwald, Michael Online low-field NMR spectroscopy for process control of an industrial lithiation reaction—automated data analysis 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. Berlin, Heidelberg Springer 2018 Analytical and Bioanalytical Chemistry 410 14 3349 3360 10.1007/s00216-018-1020-z 2018-05-07 OPUS4-43254 Beitrag zu einem Tagungsband Kern, Simon; Guhl, Svetlana; Meyer, Klas; Wander, Lukas; Paul, Andrea; Maiwald, Michael Mathematical and statistical tools for online NMR spectroscopy in chemical processes Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which require excessive calibration effort. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process Monitoring and control, as demonstrated within the European Union's Horizon 2020 project CONSENS. We present a range of approaches for the automated spectra analysis moving from conventional multivariate statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants or derivatives and robust automation schemes. Berlin AMA Service GmbH AMA Verband für Sensorik und Messtechnik e.V. 2017 Tagungsband 13. Dresdner Sensor-Symposium 978-3-9816876-5-1 13. Dresdner Sensor Symposium Dresden, Germany 04.12.2017 06.12.2017 P2, 209 212 10.5162/13dss2017/P2.07 2017-12-04 OPUS4-38364 Beitrag zu einem Tagungsband Guhl, Svetlana; Meyer, Klas; Kern, Simon; Gräßer, Patrick; Maiwald, Michael Maiwald, Michael Process monitoring of an intensified continuous production unit with compact NMR spectroscopy Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analyzers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are cur-rently not available off the rack. Recently, promising benchtop NMR instruments with acceptable performance came to market and process integrated sensors developed on basis of such laboratory instruments are on their way. 2016 Tagungsband – 12. Kolloquium Prozessanalytik 12. Kolloquium des Arbeitskreises Prozessanalytik Berlin, Germany 28.11.2016 30.11.2016 P17, 75 77 urn:nbn:de:kobv:b43-383646 http://creativecommons.org/licenses/by-nc-nd/3.0/de/deed.de 2016-11-21 OPUS4-39138 Posterpräsentation Guhl, Svetlana; Meyer, Klas; Kern, Simon Process monitoring of an intensified continuous production unit with compact NMR spectroscopy Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union's Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8" tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. 2017 Workshop for Process Industry - Tackling the Future of Plant Operation Frankfurt am Main, Germany 25.01.2017 25.01.2017 urn:nbn:de:kobv:b43-391386 http://creativecommons.org/licenses/by-nc-nd/3.0/de/deed.de 2017-02-10