Analytische Chemie
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The Berlin Main Station was built between 2000 and 2006. At the occasion of the 10th anniversary after the Berlin Main Station was officially opened to train traffic, a view back on eight years of monitoring was given. For the period of the construction with different load cases, the monitoring system was required by the Railway Authorities (Eisenbahnbundesam, EBA) to survey differential vertical displacements between neighbouring supports of the glas roof and the partially prestressed middle bridges. 128 sensors were installed.The data was published in the Internet with access restricted to the BAM scientists and the owner of the station, the German Railways DB AG.
The paper addresses the “Conventional Single-Sample vs. Multiple-Sample Hardness Testing: Hardness Testing Machine vs. Centrifuge” and the follow points are discussed in more detail: Principle of the centrifuge test, components of the centrifuge test, indenter geometries, microscopic measurement of Brinell and Vickers indents, and hardness testing: conventional vs. centrifuge.
Active thermography has been developed into a well-established non-destructive testing method and is used to detect cracks, voids, or material properties. The spatial-temporal structure of the external heating: spatially: planar (e.g., halogen lamp) or local (e.g., focused laser), and temporally: pulsed (e.g., flash lamp) or periodical (e.g., halogen lamp), has led to different testing modalities, as for instance flash and lock-in thermography. In this work, we combine a high-power laser with a spatial light modulator (SLM) allowing us to merge all degrees of freedom into a spatially and temporally controlled heat source. This approach allows us to launch a set of individually controlled and fully coherent high-energy thermal waves into the sample volume. As one possible application, we demonstrate the interference of two phase shifted thermal wave patterns in order to detect the position and depth of hidden defects, which is still a challenging task in thermographic and photothermal techniques. The patterns are positioned with a certain distance and a phase shift of pi to each other, creating an amplitude depletion zone that is centered between them. Now, when a defect is brought into the depletion zone, the destructive interference is disturbed and the defect can be recognized. This approach means that we intentionally exploit the vertical and lateral propagation directions of the thermal waves. In a more general view, controlling simultaneously control of phase and amplitude of a set of thermal waves enables us to have a defined propagation of the thermal wave field within the sample, which means that thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable spatial resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mm-range for modulation frequencies below 10 Hz which is perfectly met by present SLM technology. Eventually, this offers the opportunity to transfer known technologies from wave shaping techniques to thermography methods and to exploit the possibilities of coherent thermal wave shaping.
In recent years, the optimization of the imaging stations at research reactors and especially the further development of the neutron detectors allowed the measurement of hydrogen distributions with increasing spatial and temporal resolution at lower detection limits at the same time. Hydrogen has compared to iron a high total neutron cross section, which allows with basic radiographic methods the visualization of hydrogen in two and three dimensions inside the microstructure of components. This enables the in situ measuring of hydrogen mass flows inside cm thick steel samples with a temporal resolution of 20 s as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples. For the first time, we detected directly gaseous hydrogen in the crack cavities and we could measure the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of damage mechanisms, e.g. of hydrogen embrittlement. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm, which is not accessible with common methods as e.g. thermal desorption spectroscopy.
In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography method in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching.
The paper addresses the ‘Determining the influence of preparation and measurement conditions on bonding strength using CAT-Technology’ and the follow points are discussed in more detail: Motivation, CAT – Technology, Influence of bonding area on bonding strength, Influence of storing & measurement temperatures and Influence of substrate thickness and coating support.
The comprehensive knowledge of material properties as engineered and the material behavior in use is of huge importance for the functionality and reliability of processes and products. Hence, the accurate determination of material properties is a prerequisite for the applicability of a given material. Nowadays, macroscopic product features are originated by material properties on the microscopic and nanoscopic scale. This is a general challenge for uncertainty budgets in measurement and testing based on a conformity assesment.
Testing labs accreditated according to DIN EN ISO/IEC 17025 have to meet these demands. This paper focuses on the measurement of physical quantities (measurand with value and unit) and on the testing of material properties (qualitative, semi-quantitative or quantitative characteristics) of solid state materials. For both measurement and testing, the expression of uncertainty according to GUM is essential. Regarding the object/sample one has to subdivide in surface and bulk features, from the measurement/testing point of view destructive vs. nondestructive procedures have to be distinguished. Moreover, direct mesurement/testing and model-based determination of quantities/properties of interest require different approaches regarding the expression of uncertainty. For surface quantities and properties as discussed here, further considerations have to be made with respect to localized (lateral extension, native or artificial) or stratified (homogeneity and isotropy) material features vs. mapping (integration area) and imaging (lateral resolution and field of analysis) specifications of the measurement/testing procedure.
The concept of uncertainty budgets and the expression of uncertainty is introduced and discussed in more detail for the nondestructive model-based determination of thickness by spectroscopic ellipsometry (SE), the destructive determination of adhesion by means of centrifugal adhesion testing (CAT). It is shown that the expression of uncertainty for these examples and real materials requires different approaches resulting in either quantitity values with unit or qualitative/quantititative attributes with calculated/estimated uncertainties in agreement with GUM.
Economic industrial spray drying of ceramic slurries aims for as high as possible solids content. Investigated slurries of up to 80 wt% solids content were analyzed regarding stability while staying processable for granule production via spray drying.
Preliminary stability examinations were carried out on the one hand via zeta potential measurements and on the other hand by optical centrifuge analysis for determination of suitable additive type, quantity and composition while even allowing the detection of potential side effects. The processability of the slurry for spraying has primarily been quantified by viscosity measurements.
Early spray dried granules turned out to have internal voids and/or hard shells leading to defective sinter bodies and low density. Focusing on the root of these voids, the “hollow hard granules”, a controlled destabilization and flocculation was initiated by weakening electrostatic repulsion and approaching the isoelectric point. Destabilization, quantifiable by optical centrifugation, leaded to a change in speed of clarification as well as packing density, influencing movement speed of the phase boundary and the final height of the sediment, respectively. For sufficient destabilization, the solids content needed to be reduced in order to keep the viscosity suitable for the following spray drying procedure.
The versatile controlled destabilization of the ceramic slurry finally leaded to a significantly reduced fraction of hollow granules featuring a sinter body of higher density with smaller pores and a narrower pore size distribution, additionally this destabilization approach has shown to be transferrable with excellent results to zirconia and even ZTA (zirconia toughened alumina) composite materials.
Durch das alkalische Porenwassermilieu ist Stahl im Beton vor Korrosion geschützt. Unter ungünstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deckschicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich korrosionsbedingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanierungsmaßnahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeldmessung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszustandes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz.
Reference-free XRF is a SI traceable technique for the
determination of the mass deposition (mass per unit area) of elements in films on the nano- and micro scale. The method is radiometrically calibrated instrumentation (PTB@BESSY II, Germany) and based on reliable knowledge of all relevant atomic fundamental, experimental and instrumental parameters. No calibration sample or reference materials are necessary. The approach had been validated in the CCQM-P140 pilot study and the K129 key comparison by determination of mole fractions in Cu(In,Ga)Se2 thin films.