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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).
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.
Monitoring specific chemical properties is the key to chemical process control. Today, mainly optical online methods are applied, which require time- and cost-intensive calibration effort. NMR spectroscopy, with its advantage being a direct comparison method without need for calibration, has a high potential for closed-loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and rough environments for process monitoring and advanced process control strategies.
We present a fully automated data analysis approach which is completely based on physically motivated spectral models as first principles information (Indirect Hard Modelling – IHM) and applied it to a given pharmaceutical lithiation reaction in the framework of the European Union’s Horizon 2020 project CONSENS. Online low-field NMR (LF NMR) data was analysed by IHM with low calibration effort, compared to a multivariate PLS-R (Partial Least Squares Regression) approach, and both validated using online high-field NMR (HF NMR) spectroscopy.
Atomically dispersed metal-nitrogen doped carbons (M-N-C) are
promising catalysts for the activation of small molecules such as O2
and CO2. These single atom catalysts (SAC) operate at the interface
between homogenous and heterogenous catalysts. Currently, many
examples of M-N-C are known with good oxygen reduction reaction
activity but lacking a controlled synthesis of the specific active sites of
the precatalyst. Recently, our group facilitated the synthesis of pure
pyrrolic M-N4 sites using Zn ions as imprinters.[1] These amorphous
materials obtained by active site imprinting method are characterized
at the BAMline (Bessy II) by X-ray absorption spectroscopy (XAS).
In-situ/operando measurements will be crucial in future work for a
better understanding of the dynamic changes of the active site.
Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectros-copy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical com-parison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory.
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.
Process monitoring of an intensified continuous production unit with compact NMR spectroscopy
(2016)
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 analyzers, 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 cur-rently not available off the rack. Recently, promising benchtop NMR instruments with acceptable performance came to market and process integrated sensors developed on basis of such laboratory instruments are on their way.
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).
This contribution presents the results of structural and compressive strength investigations on cured andhigh-temperature treated silica-based one-part geopolymer-zeolite composites. The specimens weresynthesized from two different silica sources, sodium aluminate and water. The phase content as well asthe compressive strength of the cured composites varied depending on the starting mix-design and thesilica feedstock. Besides geopolymeric gel, A-type zeolites and hydrosodalites were the major reactionproducts. One of the silica feedstocks yielded significantly higher compressive strength (19 MPa), whilethe other one appears to cause less variation in phase content. Strength testing indicated an improvementon heating up to
200–400 °C (28 MPa) followed by a moderate decrease up to 700 °C. Above 700 °C the sys-tems underwent new phase formation and shrinkage (volume decrease) deformations. After exposureat 1000 °C the different mixes consisted of a mix of several stuffed silica phases, almost pure hexago-nal nepheline or amorphous phase. Depending on the mix-design, the onset temperature of the hightemperature phase transformations varied.
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.
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.
Kontinuierliche Sensorbasierte Bauwerksmessungen leisten einen wichtigen Beitrag zur Sicherheit von Verkehrsbauwerken. Hierzu werden im Vorhaben AISTEC Referenzbauwerke und Referenzverfahren untersucht mit Schwerpunkt auf den Einfluss klimatischer Bedingungen. Der Vortrag stellt den aktuellen Projektstand des FB 7.2 vor.
Managing aging engineering structures requires damage identification, capacity reassessment, and prediction of remaining service life. Data from structural health monitoring (SHM) systems can be utilized to detect and characterize potential damage. However, environmental and operational variations impair the identification of damages from SHM data. Motivated by this, we introduce a Bayesian probabilistic framework for building models and identifying damage in monitored structures subject to environmental variability. The novelty of our work lies (a) in explicitly considering the effect of environmental influences and potential structural damages in the modeling to enable more accurate damage identification and (b) in proposing a methodological workflow for model‐based structural health monitoring that leverages model class selection for model building and damage identification. The framework is applied to a progressively damaged reinforced concrete beam subject to temperature variations in a climate chamber. Based on deflections and inclinations measured during diagnostic load tests of the undamaged structure, the most appropriate modeling approach for describing the temperature‐dependent behavior of the undamaged beam is identified. In the damaged state, damage is characterized based on the identified model parameters. The location and extent of the identified damage are consistent with the cracks observed in the laboratory. A numerical study with synthetic data is used to validate the parameter identification. The known true parameters lie within the 90% highest density intervals of the posterior distributions of the model parameters, suggesting that this approach is reliable for parameter identification. Our results indicate that the proposed framework can answer the question of damage identification under environmental variations. These findings show a way forward in integrating SHM data into the management of infrastructures.
Structural health monitoring (SHM) of civil structures often is limited due to changing environmental conditions, as those changes affect the structural dynamical properties in a similar way like damages can do. In this article, an approach for damage detection under changing temperatures is presentedand applied to a beam structure. The used stochastic subspace-based algorithm relies on a reference null space estimate, which is confronted to data from the testing state in a residual function. For damage detection the residual is evaluated by means of statistical hypothesis tests. Changes of the system due to temperature effects are handled with a model interpolation approach from linear parameter varying system theory. From vibration data measured in the undamaged state at some few reference temperatures, a model of the dynamic system valid for the current testing temperature is interpolated. The reference null space and the covariance matrix for the hypothesis test is computed from this interpolated model. This approach has been developed recently and was validated in an academic test case on simulations of a mass-spring-damper. In this paper, the approach is validated experimentally on a beam structure under varying temperature conditions in a climate chamber. Compared to other approaches, the interpolation approach leads to significantly less false positive alarms in the reference state when the structure is exposed to different temperatures, while faults can still be detected reliably.
The Bundesanstalt für Materialforschung und -prüfung (BAM) collaborates with TNO to develop a software framework for automated calibration of structural models based on monitoring data. The ultimate goal is to include such models in the asset management process of engineering structures. As a basis for developing the framework, a multi-span road bridge consisting of ten simply supported steel box girders was selected as a test case. Our group measured output-only vibration data from one box girder under ambient conditions. From the data, we determined eigenfrequencies and mode shapes. In parallel, we developed a preliminary structural model of the box girder for the purpose of predicting its modal properties. In this contribution, we provide an overview of the measurement campaign, the operational modal analysis, the structural modeling and qualitatively compare the identified with the predicted modes. As an outlook, we discuss the further steps in the calibration process and future applications of the calibrated model.
Inspection and maintenance contribute significantly to the lifetime cost of bridges. There is significant potential in using information obtained through structural health monitoring to update predictive models of the condition and performance of such structures, and thus ena-ble an improved decision-making regarding inspection and maintenance activities. Within the AISTEC project funded by the German Federal Ministry of Education and Research, we develop vibration-based structural health monitoring systems aimed at continuously provid-ing information on the structural condition of bridges. Environmental variations such as changing ambient temperatures can significantly influence the dynamic characteristics of bridges and thus mask the effect of structural changes and damages. It remains a challenge to account for such influences in structural health monitoring. To study the effect of ambient temperatures on the dynamic characteristics of beam structures, we monitor the vibration response of a reinforced concrete beam in the uncracked and cracked state at varying tem-peratures in a climate chamber. We postulate a set of competing parameterized probabilistic structural models, which explicitly account for the effect of varying ambient temperatures on the mechanical properties of the system. We then combine the information provided by the structural models with the information contained in the recorded vibration data to learn the parameters of the temperature-dependent structural models and infer the plausible state of the beam using Bayesian system identification and model class selection.
Brücken sind Teil der alternden Verkehrsinfrastruktur. Um die Nutzungsdauer zu verlängern und plötzliche Schäden zu detektieren kann Bauwerksmonitoring ("Structural Health Monitoring") eingesetzt werden. Der Einfluss von Umgebungsbedingungen, beispielsweise der Temperatur, auf das Bauwerksverhalten ist meist größer als der Einfluss von Schäden. Diese Einflüsse bestmöglich voneinander zu trennen und Veränderungen im Tragverhalten korrekt Schäden oder Umgebungsbedingungen zuzuordnen ist eine offene Forschungsfrage. Diese Arbeit zeigt eine mögliche Lösung, bei der gekoppelte Modelle von Umwelteinflüssen, Schäden und Tragverhalten des Bauwerks auf Grundlage von Monitoringdaten aktualisiert werden. Das Framework dazu wird vorgestellt und an einem Laborexperiment eines Stahlbetonbalkens in der Klimakammer angewandt. Die Ergebnisse bestätigen die Vorgehensweise. In nächsten Schritten müssen komplexere Tragwerke und die Sensitivität des Ansatzes untersucht werden.
Structural health monitoring (SHM) intends to improve the management of engineering structures. The number of successful SHM projects – especially SHM research projects – is ever growing, yielding added value and more scientific insight into the management of infrastructure asset. With the advent of the data age, the value of accessible data becomes increasingly evident. In SHM, many new data-centric methods are currently being developed at a high pace. A consequent application of research data management (RDM) concepts in SHM projects enables a systematic management of raw and processed data, and thus facilitates the development and application of artificial intelligence (AI) and machine learning (ML) methods to the SHM data. In this contribution, a case study based on an institutional RDM framework is presented. Data and metadata from monitoring the structural health of the Maintalbrücke Gemünden for a period of 16 months are managed with the RDM system BAM Data Store, which makes use of the openBIS data management software. An ML procedure is used to classify the data. Feature engineering, feature training and resulting data
are performed and modelled in the RDM system.
Die aktuelle Instandhaltungsstrategien von Ingenieurbauwerken arbeiten zustandsbasiert und stützen sich auf visuelle Inspektionen in kurzen, starren Intervallen. Beim Übergang zu Predicitive-Maintenance-Strategien können Sensordaten eigesetzt werden um Prognosemodelle der Bauwerke zu aktualisieren. Ein erster Schritt hierzu ist die sensorbasierte Systemidentifikation.
Changes in the measured response of structural systems can be an indication of structural damages. However, such changes can also be caused by the effect of varying environmental conditions. To detect, localize and quantify changes or damages in structural systems subject to varying environmental conditions, physics-based models of the structural systems have to be applied which explicitly account for the influence of ambient conditions on the structural behavior. Data obtained from the structural systems should be used to calibrate the models and update predictions. Bayesian system identification is an effective framework for this task. In this paper, we apply this framework to learn the parameters of two competing structural models of a reinforced concrete beam subject to varying temperatures based on static response data. The models describe the behavior of the beam in the uncracked and cracked condition. The data is collected in a series of load tests in a climate chamber. Bayesian model class selection is then applied to infer the most plausible condition of the beam conditional on the available data.