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Design and Validation of a Compact NMR Analyser

  • 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 analysers, 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 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 onlineMonitoring 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 analysers, 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 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. If these are not available, there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Unionʼs Research Project CONSENS (Integrated Control and Sensing) 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 of 57 x 57 x 85 cm module size 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.zeige mehrzeige weniger

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  • EuroPACT_2017_Kern_et_al_72-73.pdf
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  • BoA_EuroPACT_2017_titel.pdf
    eng

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Metadaten
Autoren/innen:Simon KernORCiD, Svetlana Guhl, Klas MeyerORCiD, Andrea PaulORCiD, Lukas WanderORCiD, Patrick Gräßer, Michael MaiwaldORCiD
Dokumenttyp:Beitrag zu einem Tagungsband
Veröffentlichungsform:Graue Literatur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Processdings of 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017)
Jahr der Erstveröffentlichung:2017
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
Herausgeber (Institution):DECHEMA e. V., Frankfurt
Verlagsort:Frankfurt a. M.
Erste Seite:72
Letzte Seite:73
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Industrie 4.0; Prozessanalytik
EuroPACT; Online NMR Spectrsocopy; Process Analytical Technology; Reaction Monitoring
Themenfelder/Aktivitätsfelder der BAM:Analytical Sciences
Analytical Sciences / Sensorik
Veranstaltung:4th European Conference on Process Analytics and Control Technology (EuroPACT 2017)
Veranstaltungsort:Potsdam, Germany
Beginndatum der Veranstaltung:10.05.2017
Enddatum der Veranstaltung:12.05.2017
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:15.05.2017
Referierte Publikation:Nein