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The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/parameterization whenever our current automation landscape allows it. Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu).
Der Wandel von der aktuellen Automation zum smarten Sensor ist im vollen Gange. Automatisierungstechnik, sowie die Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Eine Topologie für smarte Sensoren, die das Zusammenwirken mit daten- und modellbasierten Steuerungen bis hin zur Softsensorik beschreibt gibt es bis heute jedoch noch nicht. Um zu einer störungsfreien Kommunikation aller Komponenten auf Basis eines einheitlichen Protokolls zu kommen sollte die Prozessindustrie die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen. Sie verwehrt stattdessen die Entwicklungen ihrer Zulieferer und wartet lieber ab. Der Beitrag greift die Anforderungen der Technologie-Roadmap „Prozess-Sensoren 4.0“ auf und zeigt Möglichkeiten zu ihrer Realisierung am Beispiel eines Online-NMR-Analysators, der im Rahmen eines EU-Projekts entwickelt wurde.
Modular plants using intensified continuous processes represent an appealing concept to produce pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes, and 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 includes a compact Nuclear Magnetic Resonance (NMR) spectrometer for online quality monitoring as well as a new model-based control approach. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including ro-bust evaluation of sensor data.
Here, we present alternatives for the quantitative determination of the analytes using modular, physically motivated models. These models can be adapted to new substances solely by the use of their corresponding pure component spectra, which can either be derived from experimental spectra as well as from quantum mechanical models or NMR predictors. Modular means that spec-tral models can simply be exchanged together with alternate reagents and products. Beyond that, we comprehensively calibrated an NIR spectrometer based on online NMR process data for the first time within an industrial plant. The integrated solution was developed for a metal organic reac-tion running on a commercial-scale modular pilot plant and it was tested under industrial conditions.
In case study one of the CONSENS project, two aromatic substances were coupled by a lithiation reaction, which is a prominent example in pharmaceutical industry. The two aromatic reactants (Aniline and o-FNB) were mixed with Lithium-base (LiHMDS) in a continuous modular plant to produce the desired product (Li-NDPA) and a salt (LiF). The salt precipitates which leads to the formation of particles. The feed streams were subject to variation to drive the plant to its optimum.
The uploaded data comprises the results from four days during continuous plant operation time. Each day is denoted from day 1-4 and represents the dates 2017-09-26, 2017-09-28, 2017-10-10, 2017-10-17.
In the following the contents of the files are explained.
Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual cam-paigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The re-sulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via compara-bly straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the ob-tained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s.
Currently, research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques.
Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16-inch polymer tubing working as a flow cell. Single scan 1H NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments.
Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods.
Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales ondemand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods.
Ugly Spectra and Lousy interfaces – Challenges for Compact NMR Spectroscopy in Process Control
(2016)
With the introduction of advanced process analytical technology, the closeness of key process variables to their limits can be directly controlled and the product can be classified or even released in real time.
Compact NMR instruments can make NMR spectroscopy accessible in industrial and harsh environments for process control.
Flexible, modulare Produktionsanlagen auf der Basis von verfahrenstechnischen Teilmodulen stellen einen vielversprechenden Ansatz für die kontinuierliche Produktion von Fein- und Spezialchemikalien dar. Der Schwerpunkt des Horizont-2020-Projekts der Europäischen Kommission CONSENS (Integrated Control and Sensing) liegt in der Implementierung von innovativen Sensorkonzepten zur Prozessüberwachung und -regelung innerhalb von containerbasierten modularen Produktionsan lagen. In diesem Artikel wird die Feldintegration eines Online-NMR-Sensors als smartes Modul für die Prozesskontrolle beschrieben. Dieses Modul basiert auf einem kommerziell erhältlichen Niederfeld-NMRSpektrometer, das zurzeit für die Anwendung im Laborbereich erhältlich ist. Für die Feldintegration wurde ein ATEX-zertifiziertes, explosionsgeschütztes Gehäuse entwickelt sowie Automationsschemen für den unbeaufsichtigten Betrieb und für die spektrale Datenauswertung erstellt. Nachdem die Machbarkeit und Leistungsfähigkeit des Sensorkonzeptes in Laborexperimente an einer aromatischen Substitutionsreaktion bereits erfolgreich demonstriert wurde, ist die Inbetriebnahme des NMR-Sensormoduls in
industrieller Umgebung für 2017 geplant.
Berichtet wird über die automatisierte und spektral-modellgestützte Datenauswertung quantitativer Online-NMR-Spektren von technischen Systemen, die einen grundlegenden Beitrag zum Thematik Smart Sensors im Sinne kalibrierarmer bzw. kalibrierfreier Verfahren liefern.
Die quantitative Online-NMR-Spektroskopie ist besonders reizvoll für diese Thematik: Sie kommt durch den direkten Nachweis der Kernspins ohne Kalibrierung aus und arbeitet auch in Konzentrationsrandbereichen äußerst linear. Als „absolute Vergleichsmethode“ (direkte Proportionalität der Signale zu den Stoffmengen innerhalb eines Spektrums) ist die NMR-Spektroskopie für die durchgeführten Grundlagenuntersuchungen im Zusammenhang mit spektralen Modellen prädestiniert.