TY - CONF A1 - Wander, Lukas A1 - Paul, Andrea A1 - Rurack, Knut A1 - Biyikal, Mustafa A1 - Juritsch, Elevtheria A1 - Bernstein, Thomas A1 - Bartholmai, Matthias A1 - Noske, Reinhard T1 - Kompaktsensor zur Online-Überwachung von Nitroaromaten T2 - Tagungsband – 12. Kolloquium Prozessanalytik N2 - Nitroaromaten und insbesondere Trinitrotoluol (TNT) sind weit verbreitete Spreng- und Umweltschadstoffe. Die größte Herausforderung bei der Detektion von TNT in der Gasphase ist der geringe Dampfdruck. Derzeit werden vielerorts günstige, schnelle, handliche und einfach zu bedienende Alternativen zur klassischen TNT-Analytik entwickelt. Aktuell existieren keine einheitlichen Richtlinien für Sprengstoffsensoren. Hier wird die Entwicklung eines Messplatzes zur Validierung von Sprengstoffsensoren sowie die Erprobung eines kompakten Mustersensors vorgestellt. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Nitroaromaten KW - Fluoreszenzlöschung KW - Sensor PY - 2016 SP - P11, 61 EP - 62 AN - OPUS4-38402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koegler, M. A1 - Paul, Andrea A1 - Alborch, K. P. A1 - Birkholz, M. A1 - Junne, S. A1 - Neubauer, P. T1 - Raman on-line monitoring approach for bioprocess and bio-pharmaceutical manufacturing T2 - Tagungsband 12. Kolloquium Prozessanalytik N2 - There is a high demand of monitoring in the era of QbD in industrial scale require new approaches to gain data rapidly and of sufficient quality in real time. Raman spectroscopy technology has great potential but not yet shown it fully in process on-line monitoring due to limitations such as i) uncomplete separation between cells and growth media alone, ii) general weak Raman signals of analytes in complex solutions and iii) strong background signals such as the auto-fluorescence, cosmic rays and surrounding lights overlapping the weak Raman signals. Here we demonstrate a Proof-of-Concept on an the example lactic acid bacteria process using a Streptococcus thermophiles fermentation. Results from three different Raman approaches are presented: 1) Time-Gated Raman Spectroscopy (TG-Raman), 2) Surface Enhanced Raman Spectroscopy (SERS) and 3) Raman process spectroscopy with NIR excitation combined with multivariate data analysis (MVDA) using Principal Component Analysis (PCA) and Partial Least Squares Regression (PLSR). T2 - 12. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman KW - Chemometrics KW - SERS KW - TimeGate PY - 2016 SP - 91 EP - 93 CY - Berlin AN - OPUS4-38673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zientek, Nicolai A1 - Laurain, Clement A1 - Meyer, Klas A1 - Paul, Andrea A1 - Engel, D. A1 - Guthausen, G. A1 - Kraume, M. A1 - Maiwald, Michael T1 - Automated data evaluation and modeling of simultaneous 19F-1H medium resolution NMR spectra for online reaction monitoring T2 - Tagungsband - 10. Kolloquium Arbeitskreis Prozessanalytik N2 - Medium resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and process monitoring. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra were treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprised direct integration, automated line fitting, indirect hard modeling, and partial least squares regression. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Online NMR spectroscopy KW - Data evaluation KW - Reaction monitoring KW - Indirect hard modeling PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P04, 24 EP - 25 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Heilmann, M. T. A1 - Schmid, Thomas A1 - Maiwald, Michael T1 - Multivariate classification of Raman spectra from synthetic polymers – an approach for the improved detection of microplastics T2 - Tagungsband - 11. Kolloquium Arbeitskreis Prozessanalytik N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris, which leads to the accumulation of microscopic plastic particles of still unknown fate, is an upcoming problem of our time. In order to monitor the degree of contamination and to understand the underlying processes of degradation and internalization of plastic debris, analytical methods are urgently needed, which help to identify and quantify microplastics. Currently, expensive collected and purified materials enriched on filters are investigated by (micro) infrared spectroscopy (FTIR). Few studies using micro-Raman spectroscopy have been published as well. In contrast to FTIR, Raman spectroscopy can handle wet samples, but it suffers from interference of fluorescent materials. Both micro-FTIR- and micro-Raman, always include time consuming scanning and mapping procedures followed by the manual inspection and measurement of selected particles. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Prozessanalytik KW - Microplastics KW - Mikroplastik KW - Raman-Spektroskopie KW - Polymers KW - Multivariate classification PY - 2015 SP - 80 EP - 81 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krämer, D. A1 - Violet, N. A1 - Paul, Andrea A1 - Maiwald, Michael A1 - King, R. T1 - Robustification of partial least squares predictions based on near infrared spectroscopy trough nonlinear state estimation T2 - Tagungsband - 11. Kolloquium Arbeitskreis Prozessanalytik N2 - The Cultivation of “Saccharomyces cerevisiae” for enzyme production was monitored using Near-infrared spectroscopy. An inline NIR optrode was therefore immersed in a 15 L vessel. The calibration was done using a Partial Least Squares (PLS) model with reference measurements of glucose, ammonium, phosphate, ethanol, and optical density. A nonlinear biological process model based on an extended Kalman Filter (EKF) was used to describe the fermentation behavior. It was found that EKF corrects inaccurate PLS predictions. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - PLS-R KW - Near infrared spectroscopy KW - Prozess-Spektroskopie KW - Process analytical technology KW - Fermentation PY - 2015 SP - 77 EP - 77 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Wander, Lukas A1 - Paul, Andrea A1 - Bremser, Wolfram A1 - Maiwald, Michael T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes T2 - Advanced Mathematical and Computational Tools in Metrology and Testing XI N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which require excessive calibration effort. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environ¬ments for advanced process monitoring and control, as demonstrated within the European Union’s Horizon 2020 project CONSENS. We present a range of approaches for the automated spectra analysis moving from conventional multivariate statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants or derivatives and robust automation schemes. T2 - Advanced Mathematical and Computational Tools in Metrology and Testing conference CY - Glasgow, United Kingdom DA - 29.08.2017 KW - Online NMR Spectroscopy KW - Process Control KW - Partial Least Squares Regression KW - Indirect Hard Modelling KW - Quantum Mechanics KW - First Principles PY - 2018 SN - 978-9-813-27429-7 VL - 89 SP - 229 EP - 234 PB - World Scientific CY - New Jersey AN - OPUS4-51391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. A1 - Meyer, Klas A1 - Paul, Andrea A1 - Esche, E. A1 - Maiwald, Michael A1 - Repke, J.-U. T1 - Operation and Optimal Control of Multiphase Systems – Hydroformylation in Microemulsions on the Mini-plant Scale T2 - Processdings of 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) N2 - Hydroformylation of short-chained olefins has been established as a standard industrial process for the production of C2 to C6 aldehydes. Using aqueous solutions of transition metal complexes these processes are carried out homogeneously catalyzed. A biphasic approach allows for highly efficient catalyst recovery. Regarding renewable feedstocks, the hydroformylation of long-chained alkenes (> C10) in a biphasic system, using highly selective rhodium catalysts has yet not been shown. Therefore, the Collaborative Research Center SFB/TR 63 InPROMPT develops new process concepts, involving innovative tuneable solvent systems to enable rather difficult or so far nonviable synthesis paths. One possible concept is the hydroformylation of long-chained alkenes in microemulsions. For this, a modular mixer-settler concept was proposed, combining high reaction rates and efficient catalyst recycling via the application of technical grade surfactants. The feasibility of such a concept is evaluated in a fully automated, modular mini-plant system within which the characteristics of such a multiphase system pose several obstacles for the operation. Maintaining a stable phase separation for efficient product separation and catalyst recycling is complicated by small and highly dynamic operation windows as well as poor measurability of component concentrations in the liquid phases. In this contribution, a model-based strategy is presented to enable concentration tracking and phase state control within dynamic mini-plant experiments. Raman spectroscopy is used as an advanced process analytical tool, which allows for online in-situ tracking of concentrations. Combined with optical and conductivity analysis optimal plant trajectories can be calculated via the solution of dynamic optimization problem under uncertainty. Applying these, a stable reaction yield of 40 % was achieved, combined with an oil phase purity of 99,8 % (total amount of oily components in the oil phase) and catalyst leaching below 0.1 ppm. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Hydroformylation KW - Micoemulsion KW - Dispersion KW - Process Analytical Technology KW - Mini-plant KW - EuroPACT PY - 2017 SP - 92 EP - 92 CY - Frankfurt a. M. AN - OPUS4-40230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Spektroskopische Untersuchungen an Bioprozess- Simulationsproben T2 - Tagungsband - 10. Kolloquium Arbeitskreis Prozessanalytik N2 - Zur Onlineüberwachung von Fermentationsprozessen werden zunehmend schwingungsspektroskopische (Raman-, Mittel- und Nahinfrarotspektroskopie (NIRS) und UV-/VIS- Methoden(Absorptions- und Fluoreszenzspektroskopie) in Kombination mit multivariater Auswertung eingesetzt. Anliegen dieser Arbeit war es, zu testen, welche Verfahren für die spektroskopische On- und Offlineüberwachung des Fermentationsprozesses zur biotechnologischen Herstellung einer Malariavaccine grundlegend geeignet sind und welche Messbereiche und Genauigkeiten der Vorhersage im Idealfall bei der Abwesenheit von Hefezellen erzielt werden können. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Prozessanalytik KW - Prozess-Sensoren KW - Bioprozess KW - Prozess-Spektroskopie KW - Raman-Spektroskopie KW - Nahinfrarot-Spektroskopie KW - Fluoreszenz-Spektroskopie PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P13, 35 EP - 35 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38362 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Wander, Lukas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes T2 - Tagungsband 13. Dresdner Sensor-Symposium N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which require excessive calibration effort. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process Monitoring and control, as demonstrated within the European Union’s Horizon 2020 project CONSENS. We present a range of approaches for the automated spectra analysis moving from conventional multivariate statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants or derivatives and robust automation schemes. T2 - 13. Dresdner Sensor Symposium CY - Dresden, Germany DA - 04.12.2017 KW - Online NMR spectroscopy KW - Process control KW - Partial least squares regression KW - Indirect hard modeling KW - Quantum mechanics KW - First principles PY - 2017 UR - https://www.ama-science.org/proceedings/details/2748 SN - 978-3-9816876-5-1 DO - https://doi.org/10.5162/13dss2017/P2.07 SP - P2, 209 EP - 212 PB - AMA Service GmbH CY - Berlin AN - OPUS4-43254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Paul, Andrea A1 - Ruiken, J.-P. A1 - Westad, Frank A1 - Illner, M. A1 - Müller, D. A1 - Esche, E. A1 - Repke, J.-U. A1 - Maiwald, Michael T1 - Online Spectroscopy in Microemulsions – A Process Analytical Approach for a Hydroformylation Mini-plant T2 - Processdings of 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) 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 a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. 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 in the transfer lines. 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 high 1-dodecene content the formation of isomers as 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 both laboratory setup and mini-plant. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Microemulsions KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Online Raman Spectroscopy PY - 2017 SP - 64 EP - 64 CY - Frankfurt a. M. AN - OPUS4-40228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -