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Planar and three-dimensional (3D) interdigitated electrodes (IDE) with electrode digits separated by an insulating barrier of different heights were electrochemically characterized and compared in terms of their sensing properties. Due to the impact of the surface resistance, both types of IDE structures display a non-linear behavior in low-ionic strength solutions. The experimental data were fitted to an electrical equivalent circuit and interpreted taking into account the surface-charge-governed properties. The effect of a charged polyelectrolyte layer electrostatically assembled onto the sensor surface on the surface resistance in solutions with different KCl concentration is studied. In case of the same electrode footprint, 3D-IDEs show a larger cell constant and a higher sensitivity to molecular adsorption than that of planar IDEs. The obtained results demonstrate the potential of 3D-IDEs as a new transducer structure for a direct label-free sensing of charged molecules.
It is well known that biochemical and biotechnological processes are strongly dependent and affected by a variety of physico-chemical parameters such as pH value, temperature, pressure and electrolyte conductivity. Therefore, these quantities have to be monitored or controlled in order to guarantee a stable process operation, optimization and high yield. In this work, a sensor chip for the multiparameter detection of three physico-chemical parameters such as electrolyte conductivity, pH and temperature is realized using barium strontium titanate (BST) as multipurpose material. The chip integrates a capacitively coupled four-electrode electrolyte-conductivity sensor, a capacitive field-effect pH sensor and a thin-film Pt-temperature sensor. Due to the multifunctional properties of BST, it is utilized as final outermost coating layer of the processed sensor chip and serves as passivation and protection layer as well as pH-sensitive transducer material at the same time. The results of testing of the individual sensors of the developed multiparameter sensor chip are presented. In addition, a quasi-simultaneous multiparameter characterization of the sensor chip in buffer solutions with different pH value and electrolyte conductivity is performed. To study the sensor behavior and the suitability of BST as multifunctional material under harsh environmental conditions, the sensor chip was exemplarily tested in a biogas digestate.
In this work, the catalyst manganese(IV) oxide (MnO2), of calorimetric gas sensors (to monitor the sterilization agent vaporized hydrogen peroxide) has been investigated in more detail. Chemical analyses by means of X-ray-induced photoelectron spectroscopy have been performed to unravel the surface chemistry prior and after exposure to hydrogen peroxide vapor at elevated temperature, as applied in the sterilization processes of beverage cartons. The surface characterization reveals a change in oxidation states of the metal oxide catalyst after exposure to hydrogen peroxide. Additionally, a cleaning effect of the catalyst, which itself is attached to the sensor surface by means of a polymer interlayer, could be observed.
It is well known that the degradation environment can strongly influence the biodegradability and kinetics of biodegradation processes of polymers. Therefore, besides the monitoring of the degradation process, it is also necessary to control the medium in which the degradation takes place. In this work, a micromachined multi-parameter sensor chip for the control of the polymer-degradation medium has been developed. The chip combines a capacitive field-effect pH sensor, a four-electrode electrolyte-conductivity sensor and a thin-film Pt-temperature sensor. The results of characterization of individual sensors are presented. In addition, the multi-parameter sensor chip together with an impedimetric polymer-degradation sensor was simultaneously characterized in degradation solutions with different pH and electrolyte conductivity. The obtained results demonstrate the feasibility of the multi-parameter sensor chip for the control of the polymer-degradation medium.
Die tert.-Butyloxycarbonyl-Gruppe (Boc) läßt sich mittels reiner Trifluoressigsäure nicht selektiv neben dem Benzyloxycarbonyl-Rest (Z) abspalten. Das gelingt auch nicht mit Lösungen von Trifluoressigsäure bzw. Chlorwasserstoff in organischen Lösungsmitteln. Kern-substituierte Z-Gruppen wie Z(pCl), Z(mCl) oder Z(pNO₂) sind zwar stabiler, werden aber von den obengenannten Reagenzien ebenfalls angegriffen bzw. sind nicht mehr acidolytisch abspaltbar. – Mit 70proz. wäßriger Trifluoressigsäure gelingt die Abspaltung von Boc neben Z dagegen fast selektiv; dabei werden aber Benzylester, besonders Glutaminsäure-γ-benzylester, teilweise hydrolysiert, während Methyl- sowie Äthylester nahezu beständig sind. Die Brauchbarkeit des Abspaltungsverfahrens wird anhand der schrittweise durchgeführten Synthese zweier Heptapeptid-Derivate gezeigt. – Ähnlich spezifisch gelingt die Abspaltung von Boc mit Bortrifluorid-ätherat in Eisessig; Benzylester sind gegenüber diesem Reagenz stabiler als gegen wäßrige Trifluoressigsäure. Das Bortrifluorid-Verfahren eignet sich besonders für die Abspaltung von Boc-Gruppen neben säurelabilen Thiol-Schutzgruppen (Tetrahydropyranyl- bzw. Trityl-Rest) sowie neben dem Cyclocystinyl-Rest. Die Leistungsfähigkeit der Methode wird durch die Synthese zweier Peptid-Derivate mit S-Trityl-Schutzgruppen belegt. Als Nebenreaktion ist die Acetylierung von aliphatischen Hydroxylgruppen möglich. Sie läßt sich vermeiden, wenn man die Spaltung in anderen Lösungsmitteln durchführt. Die als Modellverbindungen für Stabilitätsuntersuchungen verwendeten Nε-acylierten Lysin-Derivate werden mit dem Aminosäureanalysator quantitativ neben Lysin bestimmt.
Es wird die Synthese der Sequenz A 6–9 des Schafinsulins in der geschützten Form Boc-Cys-Cys-Ala-Gly-OBuᵗ (5) sowie das Verhalten dieses monomeren cyclischen Cystinpeptidderivates gegenüber den in der Peptidchemie gebräuchlichen Reagenzien Bortrifluorid/Eisessig, Triäthylamin und Hydrazinhydrat beschrieben.
Die Darstellung der N-[2-(p-Biphenylyl)isopropyloxycarbonyl]-Derivate (Bpoc-Derivate) des Cysteins unter Verwendung der Thiolschutzgruppen Tetrahydropyranyl (Thp) für 1, Diphenylmethyl (Dpm) für 2, Trityl (Trt) für 3 und S-tert.-Butyl (SBut) für 4 sowie die Synthese von aktivierten Estern der Bpoc-Derivate des Glycins (5), Isoleucins (6) und Prolins (7) werden beschrieben. An einem Beispiel wird die Möglichkeit aufgezeigt, die Bpoc-Gruppe über das Bpoc-Azid nachträglich in den Peptidverband einzuführen.
Die Synthese der Sequenzen A2—21 (13) und A1—21 (15) der Schafinsulin-A-Kette als monomere cyclische Dicystinpeptidderivate wird beschrieben. Die intrachenaren Cystinbrücken A6—7 und A 11 —20 vermitteln die Löslichkeit dieser Derivate in Dimethylformamid und ermöglichen erstmalig die Reindarstellung vollgeschützter Insulin-A-Kettenderivate. Die während der Synthese eingesetzten Schutzgruppen lassen sich mittels Trifluoressigsäure und 2-Mercaptoäthanol quantitativ entfernen.
The objectives of the present work are to characterize the Gas Metal Arc Welding process of DP 600 sheet steel and to summarize the modelling techniques. The time-temperature evolution during the welding cycle was measured experimentally and modelled with the softwaretool SimWeld. To model the phase transformations during the welding cycle dilatometer tests were done to quantify the parameters for phase field modelling by MICRESS®. The important input parameters are interface mobility, nucleation density, etc. A contribution was made to include austenite to bainite transformation in MICRESS®. This is useful to predict the microstructure in the fast cooling segments. The phase transformation model is capable to predict the microstructure along the heating and cooling cycles of welding. Tensile tests have shown the evidence of failure at the heat affected zone, which has the ferrite-tempered martensite microstructure.
In den letzten Jahrzehnten hat das Elektronenstrahlschweißen, das bereits im größeren Maßstab verwendet wird, seine Fähigkeit als qualitatives Werkzeug für die Verbindung verschiedener Materialen nachgewiesen. Das Non Vacuum Electron Beam Welding (NV-EBW) hat zahlreiche Vorteile im Vergleich zum Elektronenstrahlschweißen im Vakuum, da man unter normalem Atmosphärendruck arbeiten kann. Im Hinblick auf die reproduzierbare Qualität, insbesondere im Bereich der Massen-Fertigung, ist die Kontrolle der Strahlparameter sowie deren Einfluss auf das Schweißergebnis von großer Bedeutung. Durch eine genaue Kenntnis der Strahlkenngrößen wie des Strahldurchmessers und der Leistungsdichteverteilung kann eine Aussage über die sich ausbildende Schweißnaht sowie die Schweißbaddynamik getroffen werden. Messungen der Strahlkenngrößen im Prozess erlauben insbesondere die Untersuchung von Humping-Effekten. In diesem Beitrag wird der Prozess der Elektronenstrahlvermessung unter atmosphärischen Bedingungen beschrieben. Es wird zudem die Abhängigkeit der Elektronenstrahlcharakteristika von den verschiedenen Prozessparametern dargestellt.
Living cells are complex biological systems transforming metabolites taken up from the surrounding medium. Monitoring the responses of such cells to certain substrate concentrations is a challenging task and offers possibilities to gain insight into the vitality of a community influenced by the growth environment. Cell-based sensors represent a promising platform for monitoring the metabolic activity and thus, the “welfare” of relevant organisms. In the present study, metabolic responses of the model bacterium Escherichia coli in suspension, layered onto a capacitive field-effect structure, were examined to pulses of glucose in the concentration range between 0.05 and 2 mM. It was found that acidification of the surrounding medium takes place immediately after glucose addition and follows Michaelis–Menten kinetic behavior as a function of the glucose concentration. In future, the presented setup can, therefore, be used to study substrate specificities on the enzymatic level and may as well be used to perform investigations of more complex metabolic responses. Conclusions and perspectives highlighting this system are discussed.
Light-addressable potentiometric sensors (LAPS) are semiconductor-based potentiometric sensors, with the advantage to detect the concentration of a chemical species in a liquid solution above the sensor surface in a spatially resolved manner. The addressing is achieved by a modulated and focused light source illuminating the semiconductor and generating a concentration-depending photocurrent. This work introduces a LAPS set-up that is able to monitor the electrical impedance in addition to the photocurrent. The impedance spectra of a LAPS structure, with and without illumination, as well as the frequency behaviour of the LAPS measurement are investigated. The measurements are supported by electrical equivalent circuits to explain the impedance and the LAPS-frequency behaviour. The work investigates the influence of different parameters on the frequency behaviour of the LAPS. Furthermore, the phase shift of the photocurrent, the influence of the surface potential as well as the changes of the sensor impedance will be discussed.
Fledermäuse orientieren sich extrem schnell auch in absoluter Dunkelheit. Sie verwenden dazu eine Art Ultraschall Radar, um die Umgebung räumlich wahrzunehmen. Der Photo-Misch-Detektor (engl. Photonic Mixer Device, PMD) verwendet dieses Prinzip der Fledermäuse im optischen Bereich — dreidimensionale Szenen werden ohne Rechenaufwand kostengünstig, effizient und mit hoher Geschwindigkeit erfasst.
Deoxyribonucleic acid (DNA) and protein recognition are now standard tools in biology. In addition, the special optical properties of microsphere resonators expressed by the high quality factor (Q-factor) of whispering gallery modes (WGMs) or morphology dependent resonances (MDRs) have attracted the attention of the biophotonic community. Microsphere-based biosensors are considered as powerful candidates to achieve label-free recognition of single molecules due to the high sensitivity of their WGMs. When the microsphere surface is modified with biomolecules, the effective refractive index and the effective size of the microsphere change resulting in a resonant wavelength shift. The transverse electric (TE) and the transverse magnetic (TM) elastic light scattering intensity of electromagnetic waves at 600 and 1400 nm are numerically calculated for DNA and unspecific binding of proteins to the microsphere surface. The effect of changing the optical properties was studied for diamond (refractive index 2.34), glass (refractive index 1.50), and sapphire (refractive index 1.75) microspheres with a 50 µm radius. The mode spacing, the linewidth of WGMs, and the shift of resonant wavelength due to the change in radius and refractive index, were analyzed by numerical simulations. Preliminary results of unspecific binding of biomolecules are presented. The calculated shift in WGMs can be used for biomolecules detection.
Die Detektion von Schadstoffen repräsentiert in der Umweltanalytik eine wichtige Aufgabenstellung. Gerade die Abwasser- bzw. Brauchwasseranalytik sowie die Prozesskontrolle haben einen hohen Stellenwert. Siliziumbasierte Dünnschichtsensoren bieten eine kostengünstige Möglichkeit, „online“-Messungen bzw. Vor-Ort-Messungen zeitnah durchzuführen. In dieser Arbeit wird ein potentiometrisches Sensorarray auf der Basis von Chalkogenidgläsern zur Detektion von Schwermetallen in wässrigen Medien vorgestellt.
In industrial processes there is a variety of heavy metals (e.g., copper, zinc, cadmium, and lead) in use for wires, coatings, paints, alloys, batteries, etc. Since the application of these transition metals for industry is inevitable, it is a vital task to develop proper analytical techniques for their monitoring at low activity levels, especially because most of these elements are acutely toxic for biological organisms. The determination of ions in solution by means of a simple and inexpensive sensor array is, therefore, a promising task. In this work, a sensor array with heavy metal-sensitive chalcogenide glass membranes for the simultaneous detection of the four ions Ag⁺, Cu2⁺, Cd2⁺, and Pb2⁺ in solution is realized. The results of the physical characterization by means of microscopy, profilometry, Rutherford backscattering spectroscopy (RBS), and scanning electron microscopy (SEM) as well as the electrochemical characterization by means of potentiometric measurements are presented. Additionally, the possibility to expand the sensor array by polymeric sensor membranes is discussed.
Characterisation of polymeric materials as passivation layer for calorimetric H2O2 gas sensors
(2012)
Calorimetric gas sensors for monitoring the H₂O₂ concentration at elevated temperatures in industrial sterilisation processes have been presented in previous works. These sensors are built up in form of a differential set-up of a catalytically active and passive temperature-sensitive structure. Although, various types of catalytically active dispersions have been studied, the passivation layer has to be established and therefore, chemically as well as physically characterised. In the present work, fluorinated ethylene propylene (FEP), perfluoralkoxy (PFA) and epoxy-based SU-8 photoresist as temperature-stable polymeric materials have been investigated for sensor passivation in terms of their chemical inertness against H₂O₂, their hygroscopic properties as well as their morphology. The polymeric materials were deposited via spin-coating on the temperature-sensitive structure, wherein spin-coated FEP and PFA show slight agglomerates. However, they possess a low absorption of humidity due to their hydrophobic surface, whereas the SU-8 layer has a closed surface but shows a slightly higher absorption of water. All of them were inert against gaseous H₂O₂ during the characterisation in H₂O₂ atmosphere that demonstrates their suitability as passivation layer for calorimetric H₂O₂ gas sensors.
Two types of microvalves based on temperature-responsive poly(N-isopropylacrylamide) (PNIPAAm) and pH-responsive poly(sodium acrylate) (PSA) hydrogel films have been developed and tested. The PNIPAAm and PSA hydrogel films were prepared by means of in situ photopolymerization directly inside the fluidic channel of a microfluidic chip fabricated by combining Si and SU-8 technologies. The swelling/shrinking properties and height changes of the PNIPAAm and PSA films inside the fluidic channel were studied at temperatures of deionized water from 14 to 36 °C and different pH values (pH 3–12) of Titrisol buffer, respectively. Additionally, in separate experiments, the lower critical solution temperature (LCST) of the PNIPAAm hydrogel was investigated by means of a differential scanning calorimetry (DSC) and a surface plasmon resonance (SPR) method. Mass-flow measurements have shown the feasibility of the prepared hydrogel films to work as an on-chip integrated temperature- or pH-responsive microvalve capable to switch the flow channel on/off.
Label-free electrical detection of consecutive deoxyribonucleic acid (DNA) hybridization/denaturation by means of an array of individually addressable field-effect-based nanoplate silicon-on-insulator (SOI) capacitors modified with gold nanoparticles (Au-NP) is investigated. The proposed device detects charge changes on Au-NP/DNA hybrids induced by the hybridization or denaturation event. DNA hybridization was performed in a high ionic-strength solution to provide a high hybridization efficiency. On the other hand, to reduce the screening of the DNA charge by counter ions and to achieve a high sensitivity, the sensor signal induced by the hybridization and denaturation events was measured in a low ionic-strength solution. High sensor signals of about 120, 90, and 80 mV were registered after the DNA hybridization, denaturation, and re-hybridization events, respectively. Fluorescence microscopy has been applied as reference method to verify the DNA immobilization, hybridization, and denaturation processes. An electrostatic charge-plane model for potential changes at the gate surface of a nanoplate field-effect sensor induced by the DNA hybridization has been developed taking into account both the Debye length and the distance of the DNA charge from the gate surface.
Magnetotomography and Electric Currents in a Fuel Cell / Lustfeld, H. ; Reißel, M. ; Steffen, B.
(2009)
The absorption coefficient of VAI3, FeAI, NiAI, NiAl2, CuAI2, PrAl2, and of disordered V–AI (16 at% AI, 28%, 41%) and Fe–AI (11%) alloys has been measured in the region of the M₂,₃ absorption of the transition metals and the Labsorption of AI. The strong changes of the AI spectrum in the region of the 100 eV maximum upon alloying are explained as another evidence of the EXAFS (extended X-ray absorption fine structure) nature of these structures. The broad, prominent absorption peaks from the 3p excitations in V and Fe and from the 4d excitations in Pr are influenced only little on allyoing and thus appear to be of atomic origin. The fine structure at the onset of the Pr 4d transitions is identical in the metal and the alloy but differs from that of Pr oxide. The only M₂,₃ edge which is detectably shifted is that of Ni (up to 2.1 eV), whereas the onset of the AI L₂,₃ edge is shifted in all the alloys (up to 1.1 eV). The shifts are interpreted in accordance with X-ray fluorescence and nuclear resonance measurements as changes of the density of states in the valence band of the alloys.