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In most chemical reactions, stable isotopes are fractionated in a mass-dependent manner, yielding correlated isotope ratios in elements with three or more stable isotopes. The proportionality between isotope ratios is set by the triple isotope fractionation exponent θ that can be determined precisely for, e.g., sulfur and oxygen by IRMS, but not for metal(loid) elements due to the lower precision of MC-ICP-MS analysis and smaller isotopic variations. Here, using Mg as a test case, we compute a complete metrologically robust uncertainty budget for apparent θ values and, with reference to this, present a new measurement Approach that reduces uncertainty on θ values by 30%. This approach, namely, direct educt-product bracketing (sample−sample bracketing), allows apparent θ values of metal(loid) isotopes to be determined precisely enough to distinguish slopes in three-isotope space. For the example of Mg, we assess appropriate quality Control standards for interference-to-signal ratios and Report apparent θ values of carbonate−seawater pairs. We determined apparent θ values for marine biogenic carbonates, where the foraminifera Globorotalia menardii yields 0.514 ± 0.005 (2 SD), the coral Porites, 0.515 ± 0.006 (2 SD), and two specimens of the giant clam Tridacna gigas, 0.508 ± 0.007 (2 SD) and 0.509 ± 0.006 (2 SD), documenting differences in the uptake pathway of Mg among marine calcifiers. The capability to measure apparent θ values more precisely adds a new dimension to metal(loid) δ values, with the potential to allow us to resolve different modes of fractionation in industrial and natural processes.
Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering as well as of acrylonitrile butadiene styrene (ABS) by Fused Layer Modelling, were characterised with active thermography directly after manufacturing and after artificial weathering. For this, two different excitation methods (flash and pulse heating) were used and compared, regarding their suitability for the detection of constructed and imprinted defects inside the test specimens. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier Transformation after TSR were applied. To further investigate the long-term stability of the additively manufactured test specimens towards environmental stress, like UV radiation, heat, humidity, water contact and frost with active thermography, an artificial weathering test over 2000 hours (~3 months) was applied to the specimens. The monitoring of the changes in the optical properties of the weathered plastics was supplemented by spectral reflectance and UV/VIS spectroscopy.
The authors describe and interpret curvature-related changes to the ellipsometric readout. As model system for a concave curvature, a set of three spherical microscopic indents in silicon (100) of different sizes was prepared by instrumented indentation testing using a spherical indenter. For reference, these samples were characterized by AFM to reveal the topography of each structure. The concavelike indents were analyzed by Mueller-Matrix imaging ellipsometry to extract lateral intensity images of 12 elements of the Mueller-Matrix. As a result of the detailed analysis of the image elements m22, m23, and m14, it was possible to correlate intensity changes and symmetry properties to depolarization and cross polarization induced by the edge threshold and the curved surface of the indent.
In this contribution, we present three models to capture singularities in combination with the Spectral Element Method. The first model, the continued-fraction-based Scaled Boundary Finite Element Method, the second model, a new approach based on enrichment with static modes, and the third model, which uses an hp-refinement near the singularity, are compared among each other and evaluated in terms of their respective efficiency and accuracy.
Elementanalytische Verfahren werden heute zu mehr eingesetzt als bloß zur Bestimmung von Metallgesamtgehalten in diversen Probenmatrizes. Sie stellen heute ein wichtiges Werkzeug zur Beantwortung lebenswissenschaftlicher Fragen aus Umwelt, Medizin und Biologie dar. In der vorliegenden Arbeit kommt die single-cell-ICP-Flugzeitmassenspektrometrie (single-cell-ICP-TOF-MS) zur Multielementanalytik in einzelnen Kieselalgen (Diatomeen) zum Einsatz und wird zukünftig ein wichtiges Werkzeug z.B. bei der Beantwortung
ökotoxikologischer Fragestellung sein.
Ceramics and their composites are in general brittle materials because they are predominantly made up of ionic and covalent bonds that avoid dislocation motion at room temperature. However, a remarkable ductile behavior has been observed on newly developed 11 mol.% ceria-stabilized zirconia (11Ce-TZP) composite containing fine alumina (8 vol.% Al2O3) and elongated strontium hexa-aluminate (8 vol.% SrAl12O19) grains. The as-synthesized composite also has shown full resistance to Low Temperature Degradation (LTD), relatively high strength and exceptionally high Weibull modulus, allowing its use in a broader range of biomedical applications. In this study, to deepen the understanding of plastic deformation in Ce-TZP based composites that could soon be used for manufacturing dental implants, different mechanical tests were applied on the material, followed by complete microstructural characterization. Distinct from pure Ce-TZP material or other zirconia-based ceramics developed in the past, the material here studied can be permanently strained without affecting the Young modulus, indicating that the ductile response of tested samples cannot be associated to damage occurrence. This ductility is related to the stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation, analogue to Transformation-Induced Plasticity (TRIP) steels, where retained austenite is transformed to martensite. The aim of this study is to corroborate if the observed plasticity can be associated exclusively to the zirconia t-m phase transformation, or also to microcraking induced by the transformation. The t-m transformed-zones produced after bending and biaxial tests were examined by X-ray refraction and SEM/TEM coupled with Raman. The results revealed that the observed elastic-plastic behavior occurs without extensive microcracking, confirming a purely elastic-plastic behavior driven by the phase transformation (absence of damage).
Bruchmechanische Untersuchungen werden zur Vorhersage der Lebensdauer und der Wartungszyklen benutzt. Dabei wird davon ausgegangen, dass auch Objekte ohne detektierte Anzeigen Materialfehler mit einer Reflektivität kleiner der Nachweisgrenze aufweisen können. Keine detektierte Anzeige bedeutet daher für Bauteilauslegung, dass sie eine konservative Annahme machen müssen: es wird angenommen, dass das Bauteil Materialfehler in Größe der Nachweisgrenze enthält. Dies macht die Nachweisgrenze zu dem die Lebensdauer limitierenden Faktor. Bei probabilistischen Methoden wird zusätzliches Wissen, wie Zuverlässigkeit und Fehlerauffindwahrscheinlichkeiten bei der zerstörungsfreien Prüfung mit in die Berechnung einbezogen, um zu konservative Annahmen zu vermeiden. Ziel ist es eine Model-Assisted-POD aufzubauen mit der die reale volumetrische Ultraschallprüfung großer Schmiedeteile nachgebildet werden kann. Die resultierende POD soll im Weiteren in bruchmechanischen Betrachtungen Verwendung finden. In vorangegangenen Arbeiten [Preißel2015] wurde dazu der Einfluss des Prüfrasters nach der DGZfP-Richtlinie US 07:2014 auf die Fehlerauffindwahrscheinlichkeit (parametrisch) simulativ betrachtet und die Simulationstechnik experimentell validiert. In diesem Paper werden die Ergebnisse von Preißel überprüft und um eine Prüfraster-Summen-POD, die das Szenario der realen Bauteilprüfung beschreibt, erweitert. Zudem wird eine experimentell validierte, simulative, nicht-parametrische POD für schrägliegende Defekte aufgebaut. Schließlich werden erste Untersuchungen zur Defektmorphologie vorgestellt. Diese Arbeit ist im Rahmen eines Studenten-Stipendiums der DGZfP entstanden.
Digital Volume Correlation (DVC) is a powerful set of techniques used to compute the local shifts of 3D images obtained, for instance, in tomographic experiments. It is utilized to analyze the geometric changes of the investigated object as well as to correct the corresponding image misalignments for further analysis. It can therefore be used to evaluate the local density changes of the same regions of the inspected specimens, which might be shifted between measurements. In recent years, various approaches and corresponding pieces of software were introduced. Accuracies for the computed shift vectors of up to about 1‰of a single voxel size have been reported. These results, however, were based either on synthetic datasets or on an unrealistic setup. In this work, we propose two simple methods to evaluate the accuracy of DVC-techniques using more realistic input data and apply them to several DVC programs. We test these methods on three materials (tuff, sandstone, and concrete) that show different contrast and structural features.
In this in vitro study, we got a first insight of a possible potential of Hypericin for the treatment of pediatric soft tissue sarcoma. By coupling with radioiodine, we developed a novel approach for a combined anti-tumor treatment. The in vitro experiments lay the foundation for further in vivo experiments, which are needed to study the effects of a sequential administration of 131I-HYP and HYP.