TY - CONF A1 - Kern, Simon A1 - Maiwald, Michael T1 - Low field NMR spectroscopy for process control - robust automated data preparation and analysis as prerequisites T1 - Niederfeld NMR-Spektroskopie für die Prozesskontrolle – Robuste und automatisierte Datenvorbehandlung und Datenanalyse als Grundvoraussetzungen N2 - 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. T2 - Seminar des Institut für Mathematik, Universität Rostock CY - Rostock, Germany DA - 12.07.2017 KW - Prozessanalytik KW - Prozess-Sensoren 4.0 KW - Online NMR Spektroskopie KW - Indirect Hard Modeling PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-409694 AN - OPUS4-40969 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Wander, Lukas A1 - Guhl, Svetlana A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Process monitoring of intensified continuous production units with compact NMR spectroscopy N2 - 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 (www.consens-spire.eu) 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. T2 - Seminar, Institute of Technical Biocatalysis, Hamburg University of Technology CY - Hamburg, Germany DA - 13.01.2017 KW - Process monitoring KW - Online NMR spectroscopy KW - Indirect hard modeling KW - Process control KW - Process analytical technology KW - CONSENS PY - 2017 AN - OPUS4-43551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Wander, Lukas A1 - Guhl, Svetlana A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Online low-field NMR spectroscopy in modular plants for chemical production N2 - Die Online-Reaktionsverfolgung ist der Schlüssel zur chemischen Prozesskontrolle. Heute werden in diesem Bereich hauptsächlich Methoden der optischen Spektroskopie eingesetzt. Durch aktuelle Entwicklungen im Bereich kompakter Niederfeld-NMR-Spektrometer auf Basis von Permanentmagnetsystemen ist erstmals auch die Integration unmittelbar in einer industriellen Produktionsumgebung möglich. Diese Geräte sind robuste und relativ preiswerte Analysatoren, welche die Vorteile eines wartungsfreundlichen Betriebs ohne Notwendigkeit von kryogenen Flüssigkeiten, sowie eine einfache Handhabung vereinen. Aktuell auf dem Markt verfügbare Geräte sind jedoch ausschließlich auf den Einsatz im Laborbetrieb ausgerichtet. Für die Kopplung als Online-Methode im Prozesseinsatz ist die Entwicklung geeigneter Durchflusszellen notwendig. Diese ermöglichen idealerweise ein gutes Signal-Rausch-Verhältnis, eine ausreichende Robustheit und müssen die Anforderungen an die Integration in industrielle Anlagen erfüllen (z.B. Explosionsschutz, Temperierung). Intensivierte kontinuierliche Prozesse stehen im Fokus der aktuellen Forschung. Im Vergleich zu etablierten Batch-Verfahren besteht in modularen chemischen Anlagen die Möglichkeit durch kurze Umrüstzeiten zwischen Kampagnen effektiv auf die Marktentwicklung zu reagieren. Bei kontinuierlicher Prozessführung sind Online-Sensoren und eine zuverlässige und schnelle Regelung der Produktqualität essentiell. Andernfalls besteht ein großes Risiko, große Mengen nicht-spezifikationskonformer Produkte zu erhalten. Dies wird im Rahmen des Forschungsprojekts CONSENS (Integrated Control and Sensing) der Europäischen Union durch die Entwicklung und Integration intelligenter Sensormodule zur Prozessüberwachung und -steuerung in modularen Anlagenkonzepten thematisiert. Das vorgestellte NMR-Analysatormodul mit der Baugröße von 57 x 57 x 85 cm basiert auf einem kompakten 43,5-MHz-NMR-Spektrometer. Dieses ist zusammen mit einem Akquisitionsrechner und einer programmierbaren Steuerung für die automatisierte Daten-aufbereitung (Phasing, Baseline-Korrektur) und Auswertung in ein explosionsgeschütztes Gehäuse integriert. Für die automatisierte Datenanalyse kommt die Methode des Indirect Hard Modelings (IHM) zum Einsatz. Die entwickelten IHM-Modelle werden mittels Online-Hochfeld-NMR-Spektroskopie als Referenzverfahren in einem Versuchsaufbau zur Überwachung kontinuierlicher Reaktionen auf Basis eines mit Spritzenpumpen betriebenen 1/8" Rohrreaktors validiert. N2 - 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 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 [3]) 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. T2 - Praktische Probleme der Kernresonanzspektroskopie CY - Erlangen, Germany DA - 16.01.2017 KW - Online NMR spectroscopy KW - Automated data evaluation KW - NMR sensor KW - Process control PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-389819 AN - OPUS4-38981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gräßer, Patrick A1 - Wander, Lukas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Low field NMR spectroscopy for sustainable and flexible production of high quality chemical products N2 - The main development goal of process industries is to advance the continuous production of high-value products that meet high quality demands in flexible intensified continuous plants by introducing novel online sensing equipment and closed-loop control (CONSENS – integrated control and sensing- is funded from the European Union’s Horizon 2020 research and innovation programme). Therefore, we present the field integration of a benchtop NMR instrument into a modular production environment, focussing on suitable equipment for operation in hazardous areas with risk of explosive atmospheres. We investigated a pharmaceutical reaction step in order to describe challenges for the experimental design, the evaluation of complex NMR spectra and demonstrate automated data analysis tools. T2 - 5th Panic - Practical Applications of NMR in Industry Conferece CY - Hilton Head Island, SC 29928, USA DA - 20.02.2017 KW - Online NMR spectroscopy KW - Automated data evaluation KW - Process control PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-392333 AN - OPUS4-39233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Paul, Andrea A1 - Wander, Lukas A1 - Gräßer, Patrick A1 - Maiwald, Michael T1 - Design and validation of a compact NMR analyser N2 - 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 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. T2 - EuroPACT 2017 CY - Potsdam, Germany DA - 10.05.2017 KW - Online reaction monitoring KW - NMR spectroscopy PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-402822 AN - OPUS4-40282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Maiwald, Michael T1 - Automated data preparation and spectral modeling N2 - For reaction monitoring and process control using NMR instruments, in particular, after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. Conventionally, sensors have to be calibrated in a first step to find a response curve between the sensor signal and physical or chemical properties of the sample. In a second step, a model of the response between these parameters (e.g., concentrations) and the targeted quality specifications is needed. Thanks to the direct proportionality of the molar concentrations and the NMR signal, it could directly be used in the near future to relate the process target quality specification to sensor data – also in combination with multiple other sensor or process information. T2 - qNMR Summit 2017 CY - Berlin, Germany DA - 16.03.2017 KW - Quantitative NMR spectroscopy KW - Automated data evaluation PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-393998 AN - OPUS4-39399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -