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- 1 Analytische Chemie; Referenzmaterialien (3)
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- 3.3 Sicherheit von Transportbehältern (3)
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- 9 Komponentensicherheit (2)
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- 1.2 Biophotonik (1)
Aim: To observe the variation in accumulation of Fusarium and Alternaria mycotoxins across a topographically heterogeneous field and tested biotic (fungal and bacterial abundance) and abiotic (microclimate) parameters as explanatory variables.
Methods and Results: We selected a wheat field characterized by a diversified topography, to be responsible for variations in productivity and in canopy-driven microclimate. Fusarium and Alternaria mycotoxins where quantified in wheat ears at three sampling dates between flowering and harvest at 40 points.
Tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), deoxynivalenol (DON), zearalenone (ZEN) and deoxynivalenol-3-Glucoside (DON.3G) were quantified. In canopy temperature, air and soil humidity were recorded for each point with data-loggers. Fusarium spp. as trichothecene producers, Alternaria spp. and fungal abundances were assessed using qPCR. Pseudomonas fluorescens bacteria were quantified with a culture based method. We only found DON, DON.3G, TeA and TEN to be ubiquitous across the whole field, while AME, AOH and ZEN were only occasionally detected. Fusarium was more abundant in spots with high soil humidity, while Alternaria in warmer and drier spots. Mycotoxins correlated differently to the observed explanatory variables: positive correlations between DON accumulation, tri 5 gene and Fusarium abundance were clearly detected.
The correlations among the others observed variables, such as microclimatic conditions, varied among the sampling dates. The results of statistical model identification do not exclude that species coexistence could influence mycotoxin production.
Conclusions: Fusarium and Alternaria mycotoxins accumulation varies heavily across the field and the sampling dates, providing the realism of landscapescale studies. Mycotoxin concentrations appear to be partially explained by biotic and abiotic variables.
Significance and Impact of the Study: We provide a useful experimental design and useful data for understanding the dynamics of mycotoxin biosynthesis in wheat.
While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture.
To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution.
However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample.
To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld.
Hydrogen in metals can cause a degradation of the mechanical properties with possible subsequent hydrogen assisted cracking (HAC). Though, the mechanism of HAC is not completely understood yet and thus suitable methods for in situ investigations to characterise the crack formation are needed. X-ray computed tomography (CT) is a well-known tool for analysing these properties. However, the effective resolution of the detector system limits the detection of small defects by CT. Analyser based imaging (ABI) takes advantage of x-ray refraction at interfaces between volumes of different density, i.e. of cracks, pores, inclusions, etc., within the sample to detect defects smaller than the resolution of the detector system. In this study, measurements on an aluminium alloy weld showed that ABI allows us to resolve the 3D structure of cracks undetected by absorption based CT. Prospective investigations will analyse HAC in steels.
3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT
(2016)
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
Aggregation-induced emission (AIE) has been meanwhile observed for many dye classes and particularly for fluorophores containing propeller-like groups. Herein, we report on the AIE characteristics of a series of four hydrophobic pyrrolidinylvinylquinoxaline (PVQ) derivatives with phenyl, pyrrolyl, indolyl, and methoxythienyl substituents used to systematically vary the torsion angle between this substituent at the quinoxaline C2 position and the planar PVQ moiety. These molecules, which are accessible via four- or five-component one-pot syntheses, were spectroscopically studied in organic solvents and solvent−water mixtures, as dye aggregates, solids, and entrapped in polystyrene particles (PSP). Steady-state and time-resolved fluorescence measurements revealed a strong fluorescence enhancement for all dyes in ethanol−water mixtures of high water content, accompanying the formation of dye aggregates with sizes of a few hundred nm, overcoming polarity and H-bonding-induced fluorescence quenching of the chargetransfer-type emission of these PVQ dyes. The size and shape of these dye aggregates and the size of the AIE effect are controlled by the water content and the substituent-dependent torsion angle that influences the nucleation process and the packing of the molecules during aggregation. Staining of 1 μm-sized carboxy-functionalized PSP with the PVQ dyes resulted also in a considerable increase in the fluorescence quantum yield and lifetime, reflecting the combined influence of the restricted molecular motion and the reduced polarity of the dye microenvironment.
Die Bestrebungen zur Verringerung der CO2-Emissionen erfordern hochbelastbare und effiziente Komponenten aus Stahl in der Anlagen-, Verfahrens- und Kraftwerkstechnik. Hierfür sind in zunehmendem Maße auf den Anwendungsfall und Stahlwerkstoff abgestimmte Verschleißschutzschich-ten und definierte, zerspante Oberflächen notwendig. Die hohen Härten dieser Schichten und der Einsatz konventioneller Co-basierter Verschleißwerkstoffe führen oftmals zu unwirtschaftlichen Bauteilen, gerade aufgrund hohen Werkzeugverschleißes bei der Zerspanung mit geometrisch bestimmter Schneide. Er-kenntnisse über den Einsatz Ni-basierter Verschleißwerkstoffe und die Optimierung der Zerspanbarkeit mittels Legierungsmodifikationen und moderner hybrider Fräsprozesse ohne Verschlechterung der Ver-schleißschutzeigenschaften sind deshalb für die Anwender und Verarbeiter zur wirtschaftlichen Fertigung hochbelasteter Stahlbauteile wesentlich. Der vorliegende Beitrag stellt die Untersuchungsmethodik eines aktuell laufenden Vorhabens der TU Clausthal und BAM, Berlin, vor. Fokus liegt hierbei auf den hochin-strumentierten Fräsexperimenten, die eine reproduzierbare Analyse und Korrelation zwischen den mik-rostrukturellen Eigenschaften der auftraggeschweißten Legierungen, dem Zerspanprozess und der Zer-spanbarkeit, insbesondere der resultierenden Oberflächenintegrität, ermöglichen sollen.
27Al nuclear magnetic resonance spectra of polycrystalline aluminium borate 9Al2O3 · 2B2O3 have been measured in double rotation at 11.7 and 7.0 T and high-speed magic-angle spinning at 7.0, 9.4, 11.7, 14.1 and 17.6 T. Spinning sidebands from the satellite transitions were observed at 7.0 and 14.1 T. Each of the four structural aluminium sites [Al(IV), Al(V)(1), Al(V)(2) and Al(VI)] are observed, characterised and assigned in the spectra. The obtained parameter set gives a fully consistent interpretation in agreement with the crystal structure of the compound.
This paper describes the analytical, numerical and experimental investigations on the phenomenon of
interactions between cask components and content of packages for the transport of radioactive material during drop
tests required according to the IAEA Regulations for the Safe Transport of Radioactive Material.
Radial and axial gaps between cask components and content are usually necessary for thermal reasons but larger
gaps can exist because of the geometrical dimensions of the specified content. Consequently interactions between
content and cask components (lid system, cask body, etc.) are possible and can not be excluded during drop tests.
Interactions in this context are relative movements between cask and content which are mainly due to elastic spring
effects after releasing the cask for the free drop. These relative movements can cause interior collisions between
content and cask during the main impact of the package onto the unyielding target.
Drop tests with various types of Type A and Type B packages fully instrumented with strain gauges and
accelerometers showed that these interactions respectively interior collisions can be considerable relating to high forces
acting on cask lids, lid bolts and the content. Of course the real quantitative consequences of the interactions depend
upon different conditions, among others the drop orientation, the design characteristics of the impact limiters, the
dimensions of the gaps, the material characteristics of the contents, etc. .
In order to investigate more precisely the phenomenon of interactions BAM carried out finite element
calculations for the named casks using the ABAQUS/ Standard and ABAQUS/ Explicit computer code comparing them
with results obtained from experiments. Additionally, tests with a simplified model instrumented with accelerometers
were carried out accompanied by finite element calculations and analytical calculations using MATHEMATICA.
The investigations on the mentioned phenomena of interaction show that they should be considered in approval design
tests and/ or calculations.
Long-term behaviour of geosynthetic drains - excavations on landfills after up to 12 years service
(2002)
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
Federal Institute for Materials Research and Testing (BAM) is the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste in Germany. In context with package design approval of the new German high level waste cask CASTOR® HAW28M, BAM performed several drop tests with a half scale model of the CASTOR® HAW/TB2. The cask is manufactured by Gesellschaft für Nuklear Service mbH and was tested under accident transport conditions on the 200 tons BAM drop test facility at the BAM Test Site Technical Safety. For this comprehensive test program, the test specimen CASTOR® HAW/TB2 was instrumented at 21 measurement planes with altogether 23 piezo resistive accelerometers, five temperature sensors and 131 triaxial strain gauges in the container interior and exterior respectively. The strains of four representative lid bolts were recorded by four uniaxial strain gauges per each bolt. Helium leakage rate measurements were performed before and after each test in the above noted testing sequence. The paper presents some experimental results of the half scale CASTOR® HAW/TB2 prototype (14 500 kg) and measurement data logging. It illustrates the extensive instrumentation and analyses that are used by BAM for evaluating the cask performance to the mechanical tests required by regulations. Although some of the quantitative deceleration, velocity and strain values cannot be shown because of confidentially issues, they are provided qualitatively to illustrate the types of measurements and methodologies used at BAM.
BAM (Federal Institute for Material Research and Testing) is the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste (HLW) in Germany. In context with package design approval of the new German HLW cask CASTOR HAW28M, BAM performed several drop tests with a half-scale model of the CASTOR HAW/TB2. The test model was manufactured by GNS (Gesellschaft fur Nuklear Service mbH) and tested under accident transport conditions on the 200 tons BAM drop test facility at the BAM Test Site Technical Safety. For this comprehensive test program the test specimen CASTOR HAW/TB2 was instrumented at 21 measurement planes with altogether 23 piezo-resistive accelerometers, five temperature sensors and 131 tri-axial strain gauges in the container interior and exterior, respectively. The strains of four representative lid bolts were recorded by four uniaxial strain gauges per each bolt. Helium leakage rate measurements were performed before and after each test in the above noted testing sequence. The paper presents some experimental results of the half-scale CASTOR HAW/TB2 prototype (14,500 kg) and measurement data logging.