Analytische Chemie
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Das Ultraschall-Echo-Verfahren ist eine wichtige Methode der zerstörungsfreien Prüfung (ZfP). Prüfaufgaben im Bauwesen beinhalten unter anderem die korrekte Dickenbestimmung von Konstruktionen, sowie die Lokalisierung von Einbauteilen und Fehlstellen. Das Abbildungsverfahren RTM (Reverse Time Migration) liefert oft bessere Bilder als konventionelle Verfahren. Die Datenaufnahme am Betonprobekörper erfolgte mit einem Scannersystem der BAM, bei dem jeweils ein Ultraschall-Prüfkopf als Sender bzw. Empfänger diente. Es wurden senkrecht zur Profilrichtung horizontal polarisierte Scherwellen genutzt. Die RTM wurde mit dem Softwarepaket Madagascar gerechnet.
Die Ergebnis zeigt das Potential dieser Methode im Bezug auf komplexe Strukturen. Die lateralen Positionen der Risse im RTM-Bild sowie deren Höhe innerhalb des Probekörpers, entsprechen recht genau dem visuellen Befund.
Die Coda transmittierter Ultraschallsignale in Beton enthält Informationen zu Struktur und Zustand des Materials bzw. deren Änderung. Relevant sind u. a. Temperatur, Stress, Feuchtigkeit und verschiedene Schädigungsmechanismen. Die zahlreichen Einflussfaktoren sind nur schwer zu trennen und die Messeffekte oft zu Beginn sehr klein.Die CWI ermöglicht die Detektion kleinster Geschwindigkeitsveränderungen durch den Vergleich, der in kleinen Schritten gestauchten oder gestreckten Signalen mit eine Referenzmessung. Andere Indikatoren für Änderungen im Material sind:
• Kreuzkorrelation
• Laufzeit direkte Welle
• Energie/Amplitude
• Änderungen im Frequenzspektrum
Die beschriebene Technik wird von uns bisher primär in klein- und großskaligen Laborversuchen genutzt. Die Forschung konzentriert sich auf die Untersuchung und Trennung verschiedener Einflusseffekte. Aber auch erste reale Bauwerke wurden schon instrumentiert, z. B. Brücken und eine Tunneldecke.
Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture
(2017)
Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications.[1-2] Only a few thermoresponsive polymers have been reported that present an Upper Critical Solution Temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and “green” solvents such as water or ethanol.[3] Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing.
In this work, two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free-radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon are investigated using turbidimetry and temperature dependent dynamic light scattering.
Fluorescent nanoparticles that “light up”/”dim down” by applying external stimuli are of particular interest in the fields of sensing, diagnostics, photonics, protective coatings and microfluidics. The current challenge for these materials is to combine for instance fluorescence and its response to a stimulus such as temperature in a precise manner. Here we present such a system based on a core/shell/shell architecture consisting of a silica core with a fluorescent layer and a thermoresponsive shell.
The silica core nanoparticles were first coated with a fluorescent shell using surface initiated reversible addition-fragmentation chain transfer (RAFT) polymerization. The fluorescent nanoparticles were then completely engulfed by a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide). The fluorescence of the nanoparticles could be “switched on” at room temperature and “switched off” with increasing environmental temperature because of the presence of the thermoresponsive layer. Insights into this phenomenon will be given based on temperature dependent fluorescence measurements and dynamic light scattering.
Pollutants of low molecular weight, such as drug residues, are in the focus of water quality assessment: some of them, like carbamazepine are only partially degraded in wastewater treatment plants. Thus, these pollutants can serve as marker substances for elimination efficiencies. Monitoring water quality demands for selective, high-throughput and multi-target analytical methods. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the specific recognition by high affinity of target molecules to antibodies (Abs). Batch-wise processing in microtiter plates allows for the necessary high-throughput, however only a single analyte can be determined within one measurement.
To overcome these disadvantages, we developed a four-plex microbead-based flow cytometric assay, which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core/silica-shell particles. While, the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica shell creates a solid support for the immunoassay: The target analytes, three drugs, carbamazepine, diclofenac and caffeine and the fecal marker isolithocholic acid are coupled covalently to the surface via NHS chemistry to amino groups on the surface.
For determination of the pollutants, a mixture of specific Abs is incubated with the samples, to bind competitively on the “anchor” molecules on the surface of the beads or the analyte in solution. Bound antibodies are then visualized via fluorescent dye-labelled secondary Abs. Flow-cytometry allows for decoding of the beads and signal read-out, without washing the system. In order to decrease non-specific binding, we investigated different types of surface modifications, finding, that a PEG-based surface is suitable to support our immunoassay format. For maximum sensitivity, a design-of-experiment approach was chosen for optimization of the assay parameters. The resulting immunoassay is appropriate to quantify the pollutants in the low μg/L-range.
Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture
(2017)
Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and green solvents such as water or ethanol have been reported. Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of smart materials for sensing.
In this work two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon will be given based on turbidimetry and temperature dependent dynamic light scattering
Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range have been reported so far.
Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied. We propose a model for the temperature-induced aggregation behaviour of UCST-type poly(AAm-co-AN) copolymer in aqueous solution on the basis of turbidity measurements, SLS, DLS, SANS and cryo-TEM.
Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis
Vor einer geplanten Weiter- oder Wiedernutzung von Bestandsfundamenten stellt sich die Frage nach deren Lage, Geometrie und Zustand im Untergrund. Hierfür gibt es verschiedene Prüfverfahren. Im Projekt REFUND (2014-2016) wurden unter Berücksichtigung der aktuellen Normen und des Standes der Technik Ablaufdiagramme für die Planung der Wiedernutzung und die Untersuchung des Bestandes entwickelt. Dies geschah getrennt für Einzel- und Streifenfundamente, Platten und Pfähle. An zwei Praxisbeispielen wurden die Abläufe getestet und optimiert. Die Ergebnisse wurden in einem Handbuch kompiliert, das bei der TU Darmstadt erscheint.
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-to-aliphatic conversions or isomerisation’s 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).