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Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). 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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme.
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.
Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations).
Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu).
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
Industry 4.0, IIoT, or Lab 4.0 will enable us to handle more complex processes in shorter time. Intensified production concepts require for adaptive analytical instruments and control technology to realize short set-up times, modular control strategies. They are based on a digitized Laboratory 4.0.
Der Vortrag stellt einige aktuelle Herausforderungen für die Prozessanalytik und mögliche Antworten vor.
Gepulste Raman-Spektrometer akkumulieren das Raman-Signal mit Hilfe schneller optischer Schalter im Picosekunden-Bereich, bevor langlebigere Fluoreszenzanregung entsteht. Damit lassen sich stark fluoreszierende Materialien untersuchen, die bislang nicht zugänglich sind. Eine weitere interessante Entwicklung ist etwa die Shifted excitation Raman difference spectroscopy (SERDS) die besonders für biologische Anwendungen interessant ist.
Flexible, modulare Produktionsanlagen stellen einen vielversprechenden Ansatz für die kontinuierliche Produktion von Fein- und Spezialchemikalien dar. In einem EU-Projekt wurde die Feldintegration eines Online-NMR-Sensormoduls als smartes Modul für die Prozesskontrolle vorangebracht. Dieses Modul basiert auf einem kommerziell erhältlichen Niederfeld-NMR-Spektrometer, welche 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 kalibrierfreie spektrale Datenauswertung erstellt.
Eine sehr gut anwendbare analytische Messtechnik zur Kontrolle der elementaren Zusammensetzung von verschiedensten Materialien ist die laserinduzierte Plasmaspektroskopie (LIPS, engl. LIBS - Laser-induced Breakdown Spectroscopy). Bei der LIBS wird ein kurz gepulster Laser auf eine Probe fokussiert, um ein Leuchtplasma zu erzeugen. Das dabei erzeugte Atomemissionsspektrum ermöglicht eine qualitative und quantitative Analyse der Zusammensetzung der Probe bezüglich praktisch aller Elemente des Periodensystems. In einem aktuellen Projekt wird diese Methode neben anderen zur Online-Analyse von Ackerböden für die ortsspezifischer Bewirtschaftung (Precision Agriculture) weiterentwickelt und bewertet.
Von der zunehmenden Digitalisierung sind alle Bereiche von Wirtschaft, Industrie und Gesellschaft betroffen. Die Digitalisierung führt zu einer verstärkten virtuellen Nutzung von Ressourcen und zu einer hochdynamischen Entwicklung der zugehörigen Forschungs- und Technologiefelder. Neue Technologien sind die Basis für die erfolgreiche Weiterentwicklung des Wirtschaftsstandortes Deutschland und für eine Wertschöpfung in globalen Märkten. Die nachhaltige Sicherheit neuer Technologien schafft das Vertrauen der Bürger in den Wandel und sichert unsere Zukunft.
Im Vortrag werden Anforderungen und Lösungsvorschläge für das Labor der Zukunft diskutiert. Industrie 4.0 bzw. das Labor 4.0 hilft uns, komplexere Prozesse schneller umzusetzen. Entwicklung von Anlagen und Prozessen beginnt im Labor 4.0. Dazu werden offene, nicht proprietäre Schnittstellen und Standards bei Laborgeräten und Feldgeräten dringend benötigt. Der Standard OPC-UA wird derzeit als gesetzt gesehen. Als nächstes ist die Festlegung der Semantik (Companion Specification) erfordert. Als Bitte an die Zulieferer und Geräterhersteller wird gerichtet, möglichst keine Alleingänge hinsichtlich Schnittstellen, Standards oder GUI zu unternehmen, sondern diese mit den Anwendern abzustimmen. Auf diese Weise ergibt sich das in Industrie 4.0 geforderte "durchgehende Engineering“.
Die Sicherung der Wettbewerbsfähigkeit des Standorts Deutschland/Europa ergibt sich dann gleich in doppelter Hinsicht: Sichere, verfügbare und effiziente Herstellung international wettbewerbsfähiger Produkte für die Anwender sowie weltweiter Export von Mess- und Regeltechnik für die Messtechnikbranche.
qNMR provides the most universally applicable form of direct concentration or purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties.
The workshop presents basic terms of statistics and uncertainty analysis, which are the basis for qNMR spectroscopy and data analysis such as, e.g., standard deviations, linear regression, significance tests, etc. and gives typical examples of applications in qNMR spectroscopy.
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control and gives also an overview on direct dissolution studies of API cocrystals.
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.
Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations).
Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu).
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control giving an overview from direct dissolution studies of API cocrystals to studies of emulsions for a hydroformylation.
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. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control giving also an overview on direct dissolution studies of API cocrystals.