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The design of sample flow cells, commonly used in on-line analytics and especially for medium resolution NMR spectroscopy (MR-NMR) in low magnetic fields, was experimentally and theoretically investigated by 1H NMR and numerical simulations. The flow pattern was characterised to gain information about the residence time distribution and mixing effects. Both 1H NMR imaging and spectroscopy were used to determine the characteristics of flow cells and their significance for on-line measurements such as reaction monitoring or hyphenated separation spectroscopy. The volume flow rates investigated were in the range from 0.1 to 10 ml/min, typically applied in the above mentioned applications. The special characteristics of flow cells for MR-NMR were revealed by various NMR experiments and compared with CFD simulations and to flow cells commonly used in high-field NMR. The influence of the design of the inlet and outlet on the flow pattern was investigated as well as the effect of the length of the cell. For practical use, a numerical estimation of the inflow length was given. In addition, it was shown how experiments on the polarisation build-up revealed insight into the flow characteristics in MR-NMR.
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 Tutzing Symposium "100 % digital: survival strategies for the process industry" (see 4.1) in April 2018 was characterized by a great momentum which has been taken up and continued until today. The aim was to implement the ideas from the Tutzing Symposium in a coordinated and targeted manner. For this purpose, development needs as well as the numerous currently planned or already started research and development activities in the context of digitalisation were first compiled and analysed. This resulted in the current research landscape for digitalization in the process industry. It now enables to identify open topics and to translate them into research funding programs as well as to define new projects in the dialogue between users, suppliers and research, which are to be meaningfully interlinked and consolidated with existing projects.
Due to the strong interest in digitalisation, activities are constantly being added, so that this paper can only provide a snapshot of the situation in the period 2019-2020.
Immer im Bild mittels Prozess-Spektroskopie - Spektroskopische Methoden für die Prozessanalytik
(2012)
Zusammen mit der Genauigkeit von Messungen ist die ihnen zugeordnete Messunsicherheit Ausdruck und Maß von Vergleichbarkeit und Richtigkeit. Die Messunsicherheit spielt ebenso die Schlüsselrolle im Aufbau einer Rückführbarkeitskette, wie in diesem Beitrag beschrieben. Es ist der vierte und letzte Teil einer Artikelserie (siehe Infokasten), die Einblicke gibt in die Arbeit des DIN-Normenausschusses „Gasanalyse und Gasbeschaffenheit“ (DIN NA 062-05-73 AA) sowie der international tätigen Technical Committees 158 und 193 der ISO.
The application of compact NMR instruments to hot flowing samples or exothermically reacting mixtures is limited by the temperature sensitivity of permanent magnets. Typically, such temperature effects directly influence the achievable magnetic field homogeneity and hence measurement quality. The internal-temperature control loop of the magnet and instruments is not designed for such temperature compensation. Passive insulation is restricted by the small dimensions within the magnet borehole. Here, we present a design approach for active heat shielding with the aim of variable temperature control of NMR samples for benchtop NMR instruments using a compressed airstream which is variable in flow and temperature. Based on the system identification and surface temperature measurements through thermography, a model predictive control was set up to minimise any disturbance effect on the permanent magnet from the probe or sample temperature. This methodology will facilitate the application of variable-temperature shielding and, therefore, extend the application of compact NMR instruments to flowing sample temperatures that differ from the magnet temperature.
Calibration-Free Chemical Process and Quality Control Units as Enablers for Modular Production
(2021)
Modular chemical production is a tangible translation of the digital transformation of the process industry for specialty chemicals. In particular, it enables the speeding-up of process development and thus a quicker time to market by flexibly connecting and orchestrating standardised physical modules and bringing them to life (i.e., parameterising them) with digitally accumulated process knowledge.
We focus on the specific challenges of chemical process and quality control, which in its current form is not well suited for modular production and provide possible approaches and examples of the change towards direct analytical methods, analytical model transfer or machine-supported processes.