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- Automatic modal parameters identification (1)
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Organisationseinheit der BAM
The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale.
Microorganisms accumulate molar concentrations of compatible solutes like ectoine to prevent proteins from denaturation. Direct structural or spectroscopic information on the mechanism and about the hydration shell around ectoine are scarce. We combined surface plasmon resonance (SPR), confocal Raman spectroscopy, molecular dynamics simulations, and density functional theory (DFT) calculations to study the local hydration shell around ectoine and its influence on the binding of a gene-S-protein (G5P) to a single-stranded DNA (dT(25)). Due to the very high hygroscopicity of ectoine, it was possible to analyze the highly stable hydration shell by confocal Raman spectroscopy. Corresponding molecular dynamics simulation results revealed a significant change of the water dielectric constant in the presence of a high molar ectoine concentration as compared to pure water. The SPR data showed that the amount of protein bound to DNA decreases in the presence of ectoine, and hence, the protein-DNA dissociation constant increases in a concentration-dependent manner. Concomitantly, the Raman spectra in terms of the amide I region revealed large changes in the protein secondary structure. Our results indicate that ectoine strongly affects the molecular recognition between the protein and the oligonudeotide, which has important consequences for osmotic regulation mechanisms.
Nanotechnologien werden gegenwärtig als leistungsfähige Oberflächentechniken in erheblichem Umfange industriell genutzt. Dabei spielen dünne Schichten und deren Kenndaten eine wesentliche Rolle, z.B. als Röntgenspiegel oder optische und magnetooptische Datenträger. Die Schichtdicke zählt hierbei zu den technologisch wichtigen Parametern. Abgeleitet von Anwenderinteressen, werden für die Röntgenreflektometrie (XRR bzw. GIXR), Elektronenstrahl-Mikroanalyse (EPMA) und Röntgenfluoreszenzanalyse (XRF) einerseits und die Ellipsometrie andererseits zugeschnittene Schichtdickenmaßverkörperungen (SDM) entwickelt, gefertigt und untersucht. Das Ziel ist die Bereitstellung praxistauglicher, kalibrierter SDM, im weiteren Schichtdickennormale (SDN) genannt. SDN sind Maßverkörperungen, für die der Schichtdickenwert mit einer definierten Messunsicherheit bekannt und auf ein metrologisch anerkanntes Längennormal zurückgeführt ist. Berichtet wird über die Herstellung und messtechnische Charakterisierung der beiden spezifischen Varianten von Maßverkörperungen.
Three effects have been observed in wet-thermally grown structures under bombardement with energetic 15N ions: (1) Out-diffusion of H from the SiO2/Si system through the surface, (2) Accumulation of H at the SiO2/Si interface, (3) Changes in the optical fingerprint spectra of Ψ and Δ in dependence on λ (wavelength) obtained by ellipsometric measurements.
High-accuracy film thickness measurements in the range below 100 nm can be made by various complex methods like spectral ellipsometry (SE), scanning force microscopy (SFM), grazing incidence X-ray reflectometry (GIXR), or X-ray fluorescence analysis (XRF). The measurement results achieved with these methods are based on different interactions between the film and the probe. A key question in nanotechnology is how to achieve consistent results on a level of uncertainty below one nanometre with different techniques.
Two different types of thickness standards are realised. Metal film standards for X-ray techniques in the thickness range 10 to 50 nm are calibrated by GIXR with monochromatised synchrotron radiation of 8048 eV. The results obtained at four different facilities show excellent agreement. SiO2 on Si standards for SE and SFM in the thickness range 6 to 1000 nm are calibrated by GIXR with monochromatised synchrotron radiation of 1841 eV and with a metrological SFM. Consistent results within the combined uncertainties are obtained with the two methods. Surfaces and interfaces of both types of standards are additionally investigated by transmission electron microscopy (TEM).
Nach nationalen und internationalen Vorschriften müssen
Armaturen und Anlagenteile für hoch verdichteten Sauerstoff
ausbrennsicher sein. Diese Forderung kann technisch dadurch
erreicht werden, dass sicherheitstechnisch geeignete
nichtmetallische und metallische Werkstoffe verwendet werden.
Für die Auswahl geeigneter metallischer Werkstoffe sind
der Verwendungszweck der Armatur, die Betriebsbedingungen
sowie werkstoffspezifische Parameter zu berücksichtigen.
Einige metallische Werkstoffe besitzen gute Materialeigenschaften,
lassen sich leicht be- bzw. verarbeiten und
sind kostengünstig in der Beschaffung, dürfen aber aufgrund
ihres ungünstigen Abbrandverhaltens in Sauerstoff nicht eingesetzt
werden. Es besteht daher ein großes Interesse, den
sicherheitstechnischen Beschränkungen dieser Werkstoffe
durch geeignete Maßnahmen entgegenzuwirken. Eine mögliche
Lösung stellt die Beschichtung dieser Werkstoffe beispielsweise
mit Keramik dar, um den unmittelbaren Kontakt
mit dem Sauerstoff zu verhindern. Um den Einfluss dieser
Keramikschichten auf das Abbrandverhalten metallischer
Werkstoffe zu untersuchen, wird die im Standard ASTM G124
[1] beschriebene Apparatur und das in der einschlägigen
Literatur beschriebene Bewertungsverfahren verwendet. Die
Ergebnisse zeigen, dass für keramikbeschichtete metallische
Werkstoffe ein Abbrand erst bei höheren Sauerstoffdrücken
erfolgt.
Understanding the mechanism of interactions of nanomaterials at biointerfaces is a crucial issue to develop new antimicrobial vectors. In this work, a series of water-soluble fullerene-polyglycerol sulfates (FPS) with different fullerene/polymer weight ratios and varying numbers of polyglycerol sulfate branches are synthesized, characterized, and their interactions with two distinct surfaces displaying proteins involved in target cell recognition are investigated. The combination of polyanionic branches with a solvent exposed variable hydrophobic core in FPS proves to be superior to analogs possessing only one of these features in preventing interaction of vesicular Stomatitis virus coat glycoprotein (VSV-G) with baby hamster kidney cells serving as a model of host cell. Interference with L-selectin-ligand binding is dominated by the negative charge, which is studied by two assays: a competitive surface plasmon resonance (SPR)-based inhibition assay and the leukocyte cell (NALM-6) rolling on ligands under flow conditions. Due to possible intrinsic hydrophobic and electrostatic effects of synthesized compounds, pico- to nanomolar half maximal inhibitory concentrations (IC50) are achieved. With their highly antiviral and anti-inflammatory properties, together with good biocompatibility, FPS are promising candidates for the future development towards biomedical applications.
Today, short- and long-term structural health monitoring (SHM) of bridge infrastructures and their safe, reliable and cost-effective maintenance has received considerable attention. From a surveying or civil engineer’s point of view, vibration-based SHM can be conducted by inspecting the changes in the global dynamic behaviour of a structure, such as natural frequencies (i. e. eigenfrequencies), mode shapes (i. e. eigenforms) and modal damping, which are known as modal parameters. This research work aims to propose a robust and automatic vibration analysis procedure that is so-called robust time domain modal parameter identification (RT-MPI) technique. It is novel in the sense of automatic and reliable identification of initial eigenfrequencies even closely spaced ones as well as robustly and accurately estimating the modal parameters of a bridge structure using low numbers of cost-effective micro-electro-mechanical systems (MEMS) accelerometers. To estimate amplitude, frequency, phase shift and damping ratio coefficients, an observation model consisting of: (1) a damped harmonic oscillation model, (2) an autoregressive model of coloured measurement noise and (3) a stochastic model in the form of the heavy-tailed family of scaled t-distributions is employed and jointly adjusted by means of a generalised expectation maximisation algorithm. Multiple MEMS as part of a geo-sensor network were mounted at different positions of a bridge structure which is precalculated by means of a finite element model (FEM) analysis. At the end, the estimated eigenfrequencies and eigenforms are compared and validated by the estimated parameters obtained from acceleration measurements of high-end accelerometers of type PCB ICP quartz, velocity measurements from a geophone and the FEM analysis. Additionally, the estimated eigenfrequencies and modal damping are compared with a well-known covariance driven stochastic subspace identification approach, which reveals the superiority of our proposed approach. We performed an experiment in two case studies with simulated data and real applications of a footbridge structure and a synthetic bridge. The results show that MEMS accelerometers are suitable for detecting all occurring eigenfrequencies depending on a sampling frequency specified. Moreover, the vibration analysis procedure demonstrates that amplitudes can be estimated in submillimetre range accuracy, frequencies with an accuracy better than 0.1 Hz and damping ratio coefficients with an accuracy better than 0.1 and 0.2 % for modal and system damping, respectively.
Mit der Errichtung und der Inbetriebnahme des Windpark alpha ventus wurden umfangreiche Messungen an den Tragstrukturen und den Umgebungsparametern durchgeführt. Im Projekt Gigawind life wurde im TP1 ein Datenmanagementsystem zur kontinuierlichen und periodisch fortgeführten Datenauswertung für große Datenbestände (Big Data) entworfen und realisiert. Anhand von Performanceuntersuchungen konnte eine Verkürzung der Rechenzeit um den Faktor 10 in einem Rechencluster erreicht werden. Unter Anwendung einer Datenpipeline nach dem Publish/Subscribe Prinzip wird eine skalierbare Datenschnittstelle für Monitoringdaten vorgeschlagen.
The physical and chemical analysis of aerosols using reliable and physically traceable methods is important for the thorough investigation of airborne particles to support a better understanding of their origin as well as their health and climate impacts. Within the European Metrology Research AeroMet project,the aim of hysikalisch–Technische Bundesanstalt’s (PTB) X-ray spectrometry group is to develop and establish traceable and reliable X-ray methods to measure the elemental mass deposition per unit area, the elemental composition,and the chemical binding state of particulate matter supported by a flat substrate. This approach can substantially contribute to support quantitative analytical methods during on-site measurement campaigns where portable Instrumentation is employed by qualifying suitable calibration samples for commercial analytical X-ray instruments and by investigating samples collected during the field campaign.
At the Bundesanstalt für Materialforschung und -prüfung (BAM) full scale specimens for nuclear transport and storage containers (casks) are tested for their structural integrity in a series of drop tests on the Test Site Technical Safety in Horstwalde, 50 km south of Berlin. These drop tests cause a major stress not only on the casks, but also on the steel tower structure of the test facility, itself. The load pattern makes the structure very interesting for detailed investigation. The focus of the monitoring lies on the bolted joints of the flange connections that are a typical connection for cylindrical elements if welding is technical or economical unfavorable. The definition of the monitoring takes was done by investigating the existing documents and inspection results accompanied by building an initial digital representation of the structure, consisting of two finite element (FE) models and a geometrical 3D point cloud representation. As a first step the structures behavior during static and dynamic loading was analyzed using measurement data and an updated numerical FE Model. The idea behind is to use models for a digital planning and operation/evaluation of the structural health monitoring. A static FE simulation and a dynamic FE simulation are generated, to investigate how the structure behaves under the load conditions.