TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in microemulsions – Process analytical technology for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by data of offline GC analysis. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with a high content of 1-dodecene the formation of isomers based on a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in the laboratory setup, as well as in the field during the conducted mini-plant operation studies. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - Online-Raman-Spektroskopie KW - Mikroemulsionen PY - 2017 AN - OPUS4-39691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas A1 - Kern, Simon A1 - Zientek, Nicolai A1 - Guthausen, G. A1 - Maiwald, Michael T1 - Process control with compact NMR N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. To build an interdisciplinary bridge between “process control” and “compact NMR”,we give a short overviewon current developments in the field of process Engineering such as modern process design, integrated processes, intensified processes along with requirements to process control, model based control, or soft sensing. Finally, robust field integration of NMR systems into processes environments, facing explosion protection or Integration into process control systems, are briefly discussed. KW - Prozessanalytik KW - Quantitative NMR-Spektroskopie KW - Industrie 4.0 KW - Reaction monitoring KW - Process control KW - Online NMR spectroscopy KW - Compact NMR PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-373562 UR - http://www.sciencedirect.com/science/article/pii/S0165993616300073 DO - https://doi.org/10.1016/j.trac.2016.03.016 SN - 0165-9936 VL - 83 IS - Part A / SI SP - 39 EP - 52 PB - Elsevier AN - OPUS4-37356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Ruiken, J.-P. A1 - Illner, M. A1 - Paul, Andrea A1 - Müller, D. A1 - Esche, E. A1 - Repke, J.-U. A1 - Maiwald, Michael T1 - Prozessanalytik für die moderne Verfahrenstechnik – Online-NMR- und -Raman-Spektroskopie im mizellaren Stoffsystem N2 - Homogen katalysierte Reaktionen sind wichtige Werkzeuge der chemischen Industrie. Milde Reaktionsbedingungen und hohe Selektivitäten führen zu einer energie- und ressourcenschonenden Produktion. Ein bedeutender Prozessschritt ist die Hydroformylierung. Hier kommen Kobalt- und Rhodiumkomplexe mit mehrzähnigen Liganden zum Einsatz, die zumeist in wässriger Lösung vorliegen. Die Anwendbarkeit beschränkt sich demnach auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Hydroformylierung KW - Prozessanalytik KW - Prozess-Spektroskopie KW - NMR-Spektroskopie KW - Raman-Spektroskopie KW - Mizellen PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/cite.201650219/epdf DO - https://doi.org/10.1002/cite.201650219 SN - 1522-2640 VL - 88 SP - 1304 EP - 1317 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-37316 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Ugly Spectra and Lousy interfaces – Challenges for Compact NMR Spectroscopy in Process Control N2 - 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. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Online NMR Spectroscopy KW - Smart Sensors KW - Industrie 4.0 KW - Reaction Monitoring PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/cite.201650243/full DO - https://doi.org/10.1002/cite.201650243 SN - 1522-2640 VL - 88 SP - 1304 EP - 1317 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-37317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - High-pressure NMR spectroscopy in condensed- and gas- phase T2 - 8th Internatiomal Gas Analysis Symposium CY - Rotterdam, Netherlands DA - 2015-06-10 PY - 2015 AN - OPUS4-35056 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative online NMR spectroscopy for industrial reaction and process monitoring N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. Tis paves the way for industrial automation in real process environments. Automated data preparation and analysis are cornerstones for a breakthrough of NMR techniques for process control. Particularly, robust chemometrics as well as automated signal processing methods have to be (further) developed especially for NMR spectroscopy in process control. This becomes even more important for so called “smart sensors” providing the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. T2 - Syngenta Face to Face Meeting Process Analytical Technology CY - Münchwilen, Switzerland DA - 12.09.2017 KW - Process monitoring KW - Online NMR spectroscopy KW - Reaction monitoring KW - Hydroformylation KW - Gas analysis KW - CONSENS KW - Indirect hard modeling PY - 2017 AN - OPUS4-41946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR spectroscopy for gas analysis T2 - 7th International Gas Analysis Symposium CY - Rotterdam, Netherlands DA - 2013-06-05 PY - 2013 AN - OPUS4-29203 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative determination of methanol in FAME by Near-Infrared (NIRS) and qNMR spektroskopy T2 - 7th International Gas Analysis Symposium CY - Rotterdam, Netherlands DA - 2013-06-05 PY - 2013 AN - OPUS4-29205 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - NMR Spectroscopy of fluids and gases from moderate to high pressure T2 - 9. AK PAT CY - Ludwigshafen am Rhein, Germany DA - 2013-11-28 PY - 2013 AN - OPUS4-29613 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zientek, Nicolai A1 - Meyer, Klas A1 - Panne, Ulrich A1 - Kraume, M. A1 - Maiwald, Michael T1 - Untersuchung der Auflösungskinetik von pharmazeutischen Cokristallen mittels Onlilne-NMR-Spektroskopie N2 - Bei der Entwicklung pharmazeutischer Wirkstoffe werfen Substanzen mit einer geringen Löslichkeit, Auflösungsrate und damit einhergehend schlechten Bioverfügbarkeit immer größere Probleme auf. Diese Eigenschaften und nicht etwa toxikologische Eigenschaften oder schlechte Wirksamkeit sorgen dafür, dass es weniger als 1 % aller Wirkstoffe bis in die Markteinführung schaffen. Eine Reihe von Ansätzen zur Verbesserung der schlechten Wasserlöslichkeit konnten bereits etabliert werden. Hierunter zählen die gezielte Salzbildung bzw. Salzscreening, Solubilisierung mit Cosolventien oder die Nutzung von Polymeren als mögliche Transportwege. Eine weitere Möglichkeit bietet die Bildung verschiedener polymorpher Formen, sowohl der Einzelkomponente als auch von den verschiedenen Mehrkomponentenverbindungen. T2 - 7. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 24.02.2013 KW - Quantitative Online-NMR-Spektroskopie KW - Pharmazeutische Cokristalle PY - 2013 SN - 978-3-9815360-9-6 SP - 9 EP - 11 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) AN - OPUS4-28266 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -