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Die Zusammensetzung der Malfarben Heinrich Campendonks in ihrer Kombination aus Farbpigmenten, Bindemitteln und Metallpulvern ist bislang nahezu unerforscht. Lediglich
für wenige Leinwandgemälde des Künstlers liegen publizierte Untersuchungen zu den Farbmitteln vor. Materialanalysen zu den Hinterglasarbeiten des Malers fehlten bisher. Im Rahmen eines Forschungs- und Restaurierungsprojektes im Zeitraum von 2014 bis 2016 wurden naturwissenschaftliche Untersuchungen an ausgewählten Hinterglasbildern durchgeführt, deren Ergebnisse in diesem Aufsatz vorgestellten werden. Die Untersuchungen erfolgten zunächst nicht-invasiv mit VIS-Spektroskopie, Röntgenfluoreszenzanalyse sowie Ramanspektroskopie, weiterhin mit Licht- und Fluoreszenzmikroskopie, Rasterelektronenmikroskopie mit energiedispersiver Röntgenmikroanalyse, Fourier-Transformations-Infrarotspektroskopie, Raman-Mikroskopie und Gas-Chromatografie/Massenspektrometrie.
Der Wandel von der aktuellen Automation zum smarten Sensor ist im vollen Gange. Automatisierungstechnik, sowie die Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Eine Topologie für smarte Sensoren, die das Zusammenwirken mit daten- und modellbasierten Steuerungen bis hin zur Softsensorik beschreibt gibt es bis heute jedoch noch nicht. Um zu einer störungsfreien Kommunikation aller Komponenten auf Basis eines einheitlichen Protokolls zu kommen sollte die Prozessindustrie die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen. Sie verwehrt stattdessen die Entwicklungen ihrer Zulieferer und wartet lieber ab. Der Beitrag greift die Anforderungen der Technologie-Roadmap „Prozess-Sensoren 4.0“ auf und zeigt Möglichkeiten zu ihrer Realisierung am Beispiel eines Online-NMR-Analysators, der im Rahmen eines EU-Projekts entwickelt wurde.
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. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/parameterization whenever our current automation landscape allows it. Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu).
A further improvement of the excellent properties of UHPC can be realized with thermal Treatment. Like for normal concrete, it accelerates the hardening and prevents shrinkage after the treatment. Additionally, an increase in strength can be achieved. Aim of this study was the optimisation of the thermal Treatment conditions of UHPC for very different Treatment methods; heat Treatment at 90 °C for unprotected and sealed samples, hot water bath at 90 °C and hydrothermal Treatment at 185 °C/1.1 MPa. The pre-storage time and the dwell time were systematically varied for each method to gain a higher strength. The compressive strength depends on the manner of Treatment at which higher water accessibility leads to higher strengths. The Phase composition changes considerably with different Treatment tempereatures. Finally, it can activate unhydrated binder components forming additional C-S-H, leading to higher strength.
Monitoring chemical reactions is the key to chemical process control. Today, mainly
optical online methods are applied. NMR spectroscopy has a high potential for direct
loop process control. Compact NMR instruments based on permanent magnets
are robust and relatively inexpensive analysers, which feature advantages like low
cost, low maintenance, ease of use, and cryogen-free operation. Instruments for
online NMR measurements equipped with a flow-through cell, possessing a good
signal-to-noise-ratio, sufficient robustness, and meeting the requirements for
integration into industrial plants (i.e., explosion safety and fully automated data
analysis) are currently not available off the rack.
Intensified continuous processes are in focus of current research. Flexible (modular)
chemical plants can produce different products using the same equipment with short
down-times between campaigns and quick introduction of new products to the
market. In continuous flow processes online sensor data and tight closed-loop control
of the product quality are mandatory. If these are not available, there is a huge risk of
producing large amounts of out-of-spec (OOS) products. This is addressed in the
European Unionʼs Research Project CONSENS (Integrated Control and Sensing)
by development and integration of smart sensor modules for process monitoring and
control within such modular plant setups.
The presented NMR module is provided in an explosion proof housing of 57 x 57 x
85 cm module size and involves a compact 43.5 MHz NMR spectrometer together
with an acquisition unit and a programmable logic controller for automated data
preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling
(IHM) was selected for data analysis of the low-field NMR spectra. A set-up for
monitoring continuous reactions in a thermostated 1/8” tubular reactor using
automated syringe pumps was used to validate the IHM models by using high-field
NMR spectroscopy as analytical reference method.
Process analytical techniques are extremely useful tools for chemical production and manufacture and are of particular interest to the pharmaceutical, food and (petro-) chemical industries.
Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack.
A major advantage of NMR spectroscopy is that the method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method which is independent of the matrix. This is an important prerequisite for robust data evaluation strategies within a control concept and reduces the need for extensive maintenance of the evaluation model over the time of operation. Additionally, NMR spectroscopy provides orthogonal, but complimentary physical information to conventional, e.g., optical spectroscopy. It increases the accessible information for technical processes, where aromatic-toaliphatic conversions or isomerizations occur and conventional methods fail due to only minor changes in functional groups.
As a technically relevant example, the catalytic hydrogenation of 2-butyne-1,4-diol and further pharmaceutical reactions were studied using an online NMR sensor based on a commercially available low-field NMR spectrometer within the framework of the EU project CONSENS (Integrated Control and Sensing).