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- Process analytical technology (6)
- Prozessanalytik (6)
- Hydroformylation (5)
- Reaction monitoring (5)
- Online NMR Spectroscopy (4)
- Online NMR spectroscopy (4)
- Process Analytical Technology (4)
- Prozess-Spektroskopie (4)
- CONSENS (3)
- Chemometrics (3)
- Indirect hard modeling (3)
- Partial least squares regression (3)
- Raman spectroscopy (3)
- Raman-Spektroskopie (3)
- Reaction Monitoring (3)
- EuroPACT (2)
- Industrie 4.0 (2)
- Microemulsions (2)
- Mini-plant (2)
- PLS-R (2)
- Partial Least Squares Regression (2)
- Smart Sensors (2)
- 19F-NMR (1)
- 1H-NMR (1)
- Automation (1)
- Baustoffe (1)
- Benchtop NMR Spectroscopy (1)
- Bioprozess (1)
- Chemometrie (1)
- Continuous Manufacturing (1)
- Continuous processes (1)
- Data Fusion (1)
- Data evaluation (1)
- Data processing (1)
- Dispersion (1)
- Emulsions (1)
- Emuslions (1)
- Escherichia coli (1)
- Fermentation (1)
- First Principles (1)
- First principles (1)
- Fluorescence (1)
- Fluoreszenz-Spektroskopie (1)
- Hydroformylierung (1)
- IHM (1)
- Indirect Hard Modeling (1)
- Indirect Hard Modelling (1)
- Medium-resolution NMR (1)
- Metabolite quantification (1)
- Micoemulsion (1)
- Microemulsion (1)
- Microplastics (1)
- Mikroplastik (1)
- Mizellen (1)
- Multivariate Data Analysis (1)
- Multivariate classification (1)
- Multivariate data analysis (1)
- NIR (1)
- NIR Spectroscopy (1)
- NIR spectroscopy (1)
- NMR (1)
- NMR Spectroscopy (1)
- NMR-Spektroskopie (1)
- Nahinfrarot-Spektroskopie (1)
- Near Infrared Spectroscopy (1)
- Near infrared spectroscopy (1)
- Nuclear Magnetic Resonance (1)
- Online (1)
- Online NMR (1)
- Online NMR Spectrsocopy (1)
- Online Raman Spectroscopy (1)
- Online-spectroscopy (1)
- Pichia pastoris (1)
- Polymers (1)
- Process Control (1)
- Process control (1)
- Prozess-Sensoren (1)
- Quantitative NMR (1)
- Quantitative NMR spectroscopy (1)
- Quantum Mechanics (1)
- Quantum mechanics (1)
- Raman (1)
- Real-time process monitoring (1)
- Real-time quality control (1)
- Recycling (1)
- Surface-enhanced Raman spectroscopy (SERS) (1)
- Time-gated Raman (TG-Raman) (1)
- UV/VIS spectroscopy (1)
Organisationseinheit der BAM
Für die Rückführung von aus Rückbauprojekten anfallender künstlicher Mineralwolle in ihren Herstellungsprozess ist es notwendig, Stein- und Glaswolle zu unterscheiden und voneinander getrennt zu halten. Zu diesem Zweck wurde das Potential von NIR-Spektroskopie (NIRS) für einen werks- oder baustellenseitigen Einsatz getestet. NIRS wird aufgrund kurzer Messzeiten, minimaler Probenvorbereitung und hoher Robustheit der Spektrometer häufig in der Prozessanalytik eingesetzt. Untersucht wurden 70 verschiedene Mineralwollen, wobei sich der Probenumfang sowohl aus werksneuen Proben mit Herstellerangaben als auch unbekannten Proben ohne Spezifikation zusammensetzen, die auf verschiedenen Baustellen in den Jahren 2016–2017 entnommen oder von Deponien zur Verfügung gestellt worden waren. Als Referenzmethode wurde die Röntgenfluoreszenzanalyse verwendet, um den Mineralwolle-Typ über den Elementgehalt nach VDI 3492 zu identifizieren. Mit Hilfe eines multivariaten Datenanalyseverfahrens konnte schließlich eine Methode etabliert werden, die eine zuverlässige Identifikation von unbekannten Mineralwollen anhand deren NIR-Spektren als Stein- bzw. Glaswolle ermöglicht.
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.
Supernatants from a fermentation process of Pichia pastoris were investigated by Raman spectroscopy. Using partial least squares regression, the principal substrates glycerol and methanol could be predicted, however not the expressed protein. To gain further insight, a priori prepared calibration samples were studied by vibrational-, UV/Vis-, and fluorescence spectroscopy. For the quantification of glycerol and methanol, Raman spectroscopy was identified as the most sensitive technique, and superior to near-infrared spectroscopy, but not for protein contents below 1 g L–1. Both UV/Vis absorption and fluorescence spectroscopy are well suited for the quantification of protein, however, best results were obtained with UV/Vis absorption.
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.
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.
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.
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.
A major industrial reaction based on homogeneous catalysis is hydroformylation for the production of aldehydes from alkenes and syngas. Hydroformylation in microemulsions, which is currently under investigation at Technische Universität Berlin on a mini-plant scale, was identified as a cost efficient approach which also enhances product selectivity. Herein, we present the application of online Raman spectroscopy on the reaction of 1-dodecene to 1-tridecanal within a microemulsion. To achieve a good representation of the operation range in the mini-plant with regard to concentrations of the reactants a design of experiments was used. Based on initial Raman spectra partial least squares regression (PLSR) models were calibrated for the prediction of 1-dodecene and 1-tridecanal. Limits of predictions arise from nonlinear correlations between Raman intensity and mass fractions of compounds in the microemulsion system. Furthermore, the prediction power of PLSR models becomes limited due to unexpected by-product formation. Application of the lab-scale derived calibration spectra and PLSR models on online spectra from a mini-plant operation yielded promising estimations of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions suggesting Raman spectroscopy as a suitable technique for process analytics in microemulsions.
Reaction monitoring in disperse systems, such as emulsions, is of significant technical importance in various disciplines like biotechnological engineering, chemical industry, food science, and a growing number other technical fields. These systems pose several challenges when it comes to process analytics, such as heterogeneity of mixtures, changes in optical behavior, and low optical activity. Concerning this, online nuclear magnetic resonance (NMR) spectroscopy is a powerful technique for process monitoring in complex reaction mixtures due to its unique direct comparison abilities, while at the same time being non-invasive and independent of optical properties of the sample. In this study the applicability of online-spectroscopic methods on the homogeneously catalyzed hydroformylation system of 1-dodecene to tridecanal is investigated, which is operated in a mini-plant scale at Technische Universität Berlin. The design of a laboratory setup for process-like calibration experiments is presented, including a 500 MHz online NMR spectrometer, a benchtop NMR device with 43 MHz proton frequency as well as two Raman probes and a flow cell assembly for an ultraviolet and visible light (UV/VIS) spectrometer. Results of high-resolution online NMR spectroscopy are shown and technical as well as process-specific problems observed during the measurements are discussed.