Analytische Chemie
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Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users.
The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively).
First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments.
Four materials were investigated in pH 13 solution for 14 days
- 3D-Printer-Polymer was completely resolved
- PVC has no noticeable decrease in weight
- (VitaPro) glass filter for the sensor protector, has weight loss 2.7 %
- The epoxy resin has increased by 1.8 % due to moisture expansion
Different concrete samples were prepared for the validation of the systems.
RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring.
Today, 40 % of the world’s population live in areas with a significant risk of dengue infection. Early and reliable diagnosis of dengue virus (DENV) is essential to provide the patients with the required medical care and prevent spreading of the disease. Conventional methods for DENV diagnosis like PCR and virus isolation can be used in laboratory settings, yet are difficult to implement in point-of-care diagnostics, requiring simple, selective, fast, and sensitive detection schemes. We present here a novel approach for the detection of DENV, via its RNA, with optical read-out that relies on RNA-catalyzed fluorophore transfer onto a semiconductor quantum dot (QD) and Förster resonance energy transfer (FRET).
For this RNA assay, peptide nucleic acid (PNA) oligomers were used as highly specific capture and reporter probes. PNA exhibits remarkable affinity towards RNA as well as extremely high chemical and enzymatic stability. The capture probe, which is immobilized on a QD acting as FRET donor, bears a nucleophile at the N-terminus and the reporter probe is modified with an organic dye acting as FRET acceptor. The presence of DENV genomic RNA in the sample triggers a transfer of the dye onto the QD, signaled by FRET between the QD and the dye. A unique advantage of this system is the ability of one RNA molecule to trigger multiple transfer reactions, thereby amplifying the fluorescence signal. This assay together with the exceptional brightness of QDs and outstanding hybridization properties of PNA allows for highly specific and sensitive detection of DENV RNA in the sub-nM range.
Several restoration projects of stained-glass windows have been performed in Poland since 2010.Chemical analysis of glass samples was performed with SEM/EDX on a FEI ESEM-XL 30, (EDX-EDAX) and with Micro-XRF (M4 Tornado, Bruker).The chemical composition of medieval glass samples and of glass samples of the 19th Century have been determined.
Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for energydispersive X-ray spectroscopy (EDX)?
Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmitted and Dark Field transmitted signals. By this method a pixel precise information of the particles surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined.
Basierend auf aktuellen Regelwerken (SEP1927 und ASTM E588) stehen Möglichkeiten zur nichtinvasiven Beurteilung des zu untersuchenden Werkstoffes, in verschiedenen Qualitätsstufen bis zu einer Vergleichsfehlergröße von bis zu 300 Mikrometer zur Verfügung. Allerdings ist der realistische Nachweis und die Beurteilung von künstlichen sowie von natürlichen Fehlern kleiner 500 Mikrometer nur unter optimalen Voraussetzungen (bspw. Wahl des Prüfkopfes, Geometrie des Prüfobjektes, orts- bzw. zeitliche Auflösung der Messdatenaufnahme) und unter Einsatz von geeigneten Signalverarbeitungsalgorithmen möglich. Im Rahmen von Ringversuchen wurden daher verschiedene Methoden zur Aufbereitung der zu erfassenden Messdaten entwickelt und an verschiedenen Bauteilgeometrieen und Werkstoffen getestet. Dabei stellten sich der spektrale Tiefenausgleich (SDAC) und die nichtlineare Bewertung einzelner Frequenzkomponenten des Nutzsignals als sehr vielversprechend heraus und die Nachweisbarkeit kleiner Fehler - im Bereich von 100 - 500 μm - konnte erfolgreich gesteigert werden.
Simple calibration concept of an online NMR module demonstrated in a modularised production plant
(2017)
Monitoring specific information (such as physico-chemical properties, chemical re-actions, etc.) is the key to chemical process control. Within the CONSENS Project, the challenge to adapt a commercially available benchtop NMR spectrometer to the full requirements of an automated chemical production environment was tack-led. The developed online NMR module was provided in an explosion proof housing and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit, a programmable logic controller for automated triggering, flow con-trol, as well as data communication.
First results of an aromatic coupling reaction in lab scale showed a general feasibil-ity according to the signal information in the acquired NMR spectra even though with a considerable overlap. Due to the comparatively low field strength of the NMR spectrometer multivariate methods had to be considered for the prediction of con-centration profiles based on spectral data. Typically, for industrial application of those methods, e.g. Partial Least Squares Regression (PLS-R) as well as Indirect Hard Modeling, large amount of calibration data is demanded, which must be ac-quired in time consuming lab-scale experiments and offline analytics. When it comes to changes in raw materials (e.g., varying functional groups, additional stabi-lizing agents) calibration experiments and data evaluation models are developed again. Here we present an approach of automated data analysis tools for low field NMR spectra with minimal calibration effort. The algorithms are based on Indirect Hard Modeling, whereby each component in each mixture spectra can be rep-resented by several flexible peak functions (pure component models). This means, that only pure component NMR spectra are needed to generate a first evaluation model. The flexibility of peak functions in the spectral model can be adjusted via constraints of peak parameters. The area of any pure component model can either be converted to concentrations based on a one-point calibration on raw material concentration or even neat solvent signals. In several cases it has been shown, the IHM works almost independently of the matrix of the real samples. Such a calibration can be repeated daily in the beginning of each process run with minimal time effort. Moreover, additional pure components can be added to the model or even substitut-ed while keeping the previously adjusted peak function constraints. The proposed method exhibited good agreement of resulting concentration data from low field NMR spectra, when compared to an online high field NMR spectrometer as refer-ence instrument.
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
Mycotoxins can be found worldwide in food and feed and cause a variety of mold-related health risks which makes it necessary to further examine their metabolic fate in human and other mammals. Beside standard in vitro assays with liver cell preparations an increasing interest in new simulation methods are playing a growing role. The online coupling of electrochemistry with mass spectrometry (EC/MS) is one of these novel techniques, successfully applied in pharmacological and drug research for several years now. The primary objective of this study was to investigate the capability of EC/MS to elucidate metabolic pathways of the mycotoxin citrinin as relevant food contaminant. For this purpose, a coulometric flow through cell equipped with a glassy carbon working electrode was used by applying a ramped potential between 0 and 2 V vs Pd/H2. The electrochemically generated oxidation products analyzed by EC/MS were compared to those obtained from in vitro assays. To receive a comprehensive assessment of EC/MS other non-microsomal oxidation techniques such as Fenton-like reaction and UV irradiation were applied. Several hydroxylated derivatives of citrinin were generated by EC/MS and Fenton-like reaction which are similar to microsomal biotransformation products. These data show that EC/MS is a versatile tool that can be easily applied in mycotoxin research to support metabolic investigations of known and unknown mycotoxins.
Die Methode der Spektral Induzierten Polarisation (SIP) wird eingesetzt, um hydraulische Parameter wie Porosität und Permeabilität von Gesteinen abzuleiten. Dabei wird ein Wechselstrom im Bereich von 1 mHz bis 45 kHz in das Gestein eingespeist und die Phasenverschiebung zwischen elektrischem Strom und Spannung gemessen, woraus die komplexe Leitfähigkeit berechnet wird.
In dieser Arbeit werden die komplexen Leitfähigkeiten von Fontainebleau Sandsteinen mittels einer am Leibnitz-Institut für Angewandte Geophysik (LIAG) hergestellten Messzelle und einer SIP Apparatur des Forschungszentrums Jülich (FZJ) gemessen. Die Fontainebleau Sandsteine stammen aus Frankreich, südlich von Paris und zeichnen sich durch eine nahezu homogene Zusammensetzung aus Quartz aus. Für die Messungen wurden vier Blöcke mit jeweils vier Proben ausgewählt, die in Porosität und Permeabilität variieren. Für die SIP-Messungen werden die Gesteinsproben mit Natriumchlorid Lösung unterschiedlicher Leitfähigkeiten gesättigt, um die Abhängigkeit der IP-Spektren von der Leitfähigkeit des Porenfluids zu untersuchen. Die Messungen werden mit anderen petrophysikalischen Untersuchungen ergänzt, wie z.B. der Bestimmung der Porenradienverteilung mittels Quecksilberporosimetrie und der spezifischen inneren Oberfläche mit Gassorption (BET). Mit dem Raster-Ektronen-Mikroskop werden hochauflösende Bilder der inneren Gesteinsstruktur erzeugt und ausgewertet.
Erste Ergebnisse der SIP-Messungen zeigen deutliche Phasenmaxima im niederfrequenten Bereich, die hinsichtlich ihrer Amplitude und Frequenzlage zwischen den Blöcken variieren.
Ziel der Arbeit ist eine systematische Untersuchung der Polarisationseigenschaften bezüglich der Variabilität von Porosität, Porenradienverteilung, spezifischen inneren Oberfläche und Fluidleitfähigkeit, um die Zusammenhänge qualitativ und quantitativ zu charakterisieren.