Zitieren Sie bitte immer diesen URN: urn:nbn:de:kobv:b43-402822
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 online sensor dataMonitoring 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 Union’s 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.…
Autor*innen: | Simon KernORCiD |
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Weitere Person: | Svetlana Guhl, Klas MeyerORCiD, Andrea PaulORCiD, Lukas WanderORCiD, Patrick Gräßer, Michael MaiwaldORCiD |
Dokumenttyp: | Vortrag |
Veröffentlichungsform: | Präsentation |
Sprache: | Englisch |
Jahr der Erstveröffentlichung: | 2017 |
Veröffentlichende Institution: | Bundesanstalt für Materialforschung und -prüfung (BAM) |
DDC-Klassifikation: | Naturwissenschaften und Mathematik / Chemie / Analytische Chemie |
Freie Schlagwörter: | NMR spectroscopy; Online reaction monitoring |
Veranstaltung: | EuroPACT 2017 |
Veranstaltungsort: | Potsdam, Germany |
Beginndatum der Veranstaltung: | 10.05.2017 |
Enddatum der Veranstaltung: | 12.05.2017 |
URN: | urn:nbn:de:kobv:b43-402822 |
Verfügbarkeit des Dokuments: | Datei für die Öffentlichkeit verfügbar ("Open Access") |
Lizenz (Deutsch): | ![]() |
Datum der Freischaltung: | 18.05.2017 |
Referierte Publikation: | Nein |
Eingeladener Vortrag: | Nein |
Schriftenreihen ohne Nummerierung: | BAM Präsentationen |