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.…
Autor*innen: | Simon KernORCiD, Svetlana Guhl, Klas MeyerORCiD, Andrea PaulORCiD, Lukas WanderORCiD, Patrick Gräßer, Michael MaiwaldORCiD |
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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 |
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 |
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 |