Analytische Chemie
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Paper des Monats
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Anomalous surface composition in thin films of a poly(vinyl methyl ether) / polystyrene blend
(2017)
Highly surface-sensitive X-ray photoelectron spectroscopy at HE-SGM beamline revealed in the outermost region (< 2nm) of thin films (15 -65 nm) of PVME/PS blends a relative high amount of PS, whereas in slightly deeper regions PVME was enriched. Such enrichment of PVME in the whole near-surface region was proposed in former investigations based on conventional XPS studies.
Synchrotron X-ray refraction radiography (SXRR) is proven to identify different kinds of defects in Ti-Al6-V4 samples produces by selective laser melting. Namely, these defect types are empty pores and unprocessed powder, which are characteristic to the regions above and below the optimal laser energy density, respectively. Furthermore, SXRR detects small defects below the spatial resolution.
Material studies of inks
(2017)
The course presents panorama of historic writing inks, their use the methods of their identification. First, we discuss the possible types of the inks and show how one can determine these types using very simple instrumentation.
The change of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age constitutes the second half of the course.
The degradation of the chemotherapy drug 5-fluorouracil by a non-pristine metal surfaces is studied.Using density functional theory, X-ray photoelectron spectroscopy and X-ray absorption spectroscopy we show that the drug is entirely degraded by medical-grade silver surfaces, already at body temperature,and that all of the fluorine has left the molecule, presumably as HF. Remarkably, this degradation is even more severe than that reported previously for 5-fluorouracil on a pristine monocrystalline silver surface(in which case 80% of the drug reacted at body temperature) [1]. We conclude that the observed reaction is due to a reaction pathway, driven by H to F attraction between molecules on the surface, which results in the direct formation of HF; a pathway which is favoured when competing pathways involving reactive Ag surface sites are made unavailable by environmental contamination. Our measurements indicate that realistically cleaned, non-pristine silver alloys, which are typically used in medical applications, can result in severe degradation of 5-fluorouracil, with the release of HF – a finding which may have important implications for the handling of chemotherapy drugs.
Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis.
We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions.
The presentation deals with the progess, the use of beads brings with it when developing and using immunoanalytical methods. While with conventional assays (e.g. ELISA) fill/empty/wash steps have to be performed within the same microplate well, antibodies on beads bring the possibility of incubating the sample with the capture antibodies in one compartment and then transport it, e.g. in microfluidic channels, to the site of detection. Especially magnetic nanoparticles, that can be captured and released easily, have a wide field of application.
Laser thermography has its roots in the late-1960s when Kubiak first used a focused light source to raster-scan a specimen containing surface breaking cracks and employed an infrared detector to monitor the blocking effect of the cracks on the heat flow. Nowadays, this technique has evolved into the flying-spot laser thermography. In the mid-1970s, when Rosencwaig and Gersho worked out the theory for the photoacoustic effect, they laid the foundation for the development of the photothermal testing methodology. The decisive difference to the flying-spot technique is that in the photothermal methodology, a high-frequency modulated laser beam is used, which explicitly uses the concept of the thermal wave.
Starting in the 1980s, infrared cameras came into play and enabled full-field thermal imaging, but this time, slow thermal light sources were used. Today, flash lamps (pulsed planar heating) and halogen lamps (modulated planar heating) have been established as the standard light sources for the specific regimes of pulsed and lock-in thermography.
Only recently, the availability of novel technologies – fast and high-resolution infrared cameras, innovative brilliant laser sources and high-performance data acquisition and processing technology – has enabled a paradigm shift from the separated photothermal and thermographic methodologies to a versatile tool for NDE that combines both approaches. In addition, the heating can also be spatially structured using laser arrays. This new degree of freedom allows the development of completely new thermography NDE methods.
In the talk, we present current activities with kilowatt-class high-power laser sources for advanced flying-spot, pulsed, lock-in and laser-projected thermography.
Naturwissenschaftliche Verfahren sind zunehmend von Bedeutung bei der Untersuchung von Kunst- und Kulturgut und der Entwicklung von Konservierungskonzepten. Neben bildgebenden Verfahren sind materialanalytische Methoden von großer Wichtigkeit. Mobilen, zerstörungsfreien Verfahren ist grundsätzlich den Vorzug zu geben. Es ist jedoch zu konstatieren, dass Probenentnahmen unumgänglich sind, wenn spezielle Fragen an die Materialanalyse gestellt werden.
The modeling of waveguides by means of the Scaled Boundary Finite Element Method (SBFEM) has recently been addressed and is considered an effective procedure for the simulation of ultrasonic guided waves in plates and uniform structures, as well as their interaction with defects. This work presents the extension of the known applications like uniform concrete foundation cylinders to structures with more complex shapes and defects. The main focus is the required modeling of 3-D structures in SBFEM to solve these efficiently. Furthermore the coupling of different models is discussed. This involves models like a mainly uniform foundation cylinder with varying material behavior or geometry in certain areas which has to be modeled in 3-D SBFEM. With the presentation of numerical examples the accuracy and performance of the modeling is discussed and the advantages in improving numerical stability are shown.
This work addresses the computation of stiffness matrices for general prismatic structures with an arbitrary cross section. The presented approach is based on the scaled boundary finite element method (SBFEM), a semi-analytical method, which can be used to model structures by only discretizing the boundary of a domain. For prismatic structures, the process is further simplified, as only the cross section of the structure has to be discretized. Thus, a particular semi-analytical finite element is constructed for bounded and unbounded domains. The proposed approach leads to a frequency-dependent stiffness matrix. This stiffness matrix can easily be coupled to other prismatic SBFEM domains or general SBFEM domains. Necessary modifications to include forces along the scaling direction, such as body loads, are addressed. The results of the proposed approach are compared to those of traditional FEM models obtained using commercially available software.