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- 6 Materialchemie (4)
- 6.1 Oberflächen- und Dünnschichtanalyse (4)
- 1 Analytische Chemie; Referenzmaterialien (3)
- 3 Gefahrgutumschließungen; Energiespeicher (3)
- 3.3 Sicherheit von Transportbehältern (3)
- 8 Zerstörungsfreie Prüfung (3)
- 1.7 Organische Spuren- und Lebensmittelanalytik (2)
- 9 Komponentensicherheit (2)
- 9.4 Integrität von Schweißverbindungen (2)
- 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.
Aktuell wird die Ultraschallechotechnik für Holzbauteile genutzt, indem aus der Abschattung eines ansonsten stabilen Rückwandechos auf Auffälligkeiten im Holzbauteil geschlossen wird. Dabei werden Transversalwellen (Mittenfrequenz 50 kHz) mit der Polarisationsrichtung in Faserrichtung (L) angewendet. In einem 2012 abgeschlossenen Forschungsvorhaben wurde nun die direkte Abbildung von Streuern durch anisotrope SAFT-Rekonstruktion entwickelt.
Dazu werden flächig aufgenommene Ultraschallmessdaten mit automatisiert scannenden Druck- und Scherwellenköpfen erzeugt und auf Basis anisotroper Geschwindigkeitsverteilungen rekonstruiert. Benutzt werden die auch häufig für Beton eingesetzten trocken ankoppelnden Punktkontakt-Prüfköpfe. Da damit auch intensive Wellen an der Oberfläche erzeugt werden, entstehen im Material zusätzliche Kopfwellen, die ebenfalls bei der Rekonstruktion berücksichtigt werden.
Da die Wellengeschwindigkeiten in Holz individuell stark schwanken, wird eine interaktive Auswertetechnik zur Ermittlung der Materialkonstanten benutzt. Für die Messungen werden Druckwellen sowie Scherwellen in zwei Polarisationsrichtungen verwendet. Die Messungen erfolgen sowohl mit automatischen Scannersystemen als
auch mit einem linearen Prüfkopf-Array (kommerziell erhältlicher multistatischer Messkopf). Gezeigt werden Ergebnisse an Bauteilen mit künstlichen und realen Fehlstellen. Das Forschungsprojekt wurde gefördert vom Bundesamt für Bau- und Raumordnung (BBR, Zukunft Bau).
For validation of structural integrity under normal and hypothetical accident conditions during transport and storage of dangerous goods the Federal Institute for Materials Research and Testing (BAM) focuses its safety related scientific research on advanced mechanical safety assessment methods including simulation of high rate impact of model components and structures.
An impact and crash test facility was recently developed for performing dynamic impact tests with component size specimen, or to crash specimens of impact limiter materials and structural components.
The paper presents experimental techniques of BAM drop test machine and options of several measurement methods and advancements in order to characterize typical shock-absorbing materials under impact loading conditions. Instrumented drop weight tests are performed to complete materials data base and energy absorption of shock-absorbing materials as well as to implement materials and structural parameters into FEA of reference structures.
Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration
(2011)
The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS.
Drop and fire testing of spent fuel and HLW transport casks at 'BAM test site technical safety'
(2011)
BAM, as a competent German government institute for the mechanical and thermal testing of radioactive material transport and storage containers, operates unique drop and fire test facilities for experimental investigations on the open air BAM Test Site Technical Safety. To be able to perform even drop tests with full scale spent fuel or HAW casks (i.e. the German CASTOR cask designs), BAM constructed in 2004 a large drop test facility capable to handle 200 ton test objects, and to drop them onto a steel plate covered unyielding target with a mass of nearly 2600 ton. Drop test campaigns of the 181 ton GNS CONSTOR V/TC, the 129 ton MHI MSF-69BG and a 1:2 scale model of the GNS CASTOR HAW28M (CASTOR HAW/TB2) have been performed since then. The experimental BAM drop testing activities can be supported also by drop testing of smaller packages (up to 2 ton) in an in-house test facility and by dynamic, guided impact testing of package components and material specimen inside a new drop test machine. In May 2008, a new modern fire test facility was put into operation. The facility provides two test stands fired with liquid propane. Testing in every case has to be completed by computational investigations, where BAM operates appropriate finite element modelling on appropriate computer codes, e.g. ABAQUS, LS-DYNA, ANSYS and other analytical tools.
Instrumented measurements on radioactive waste disposal containers during experimental drop testing
(2011)
In context with disposal container safety assessment of containers for radioactive waste the German Federal Institute for Materials Research and Testing (BAM) performed numerous drop tests in the last years. The tests were accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers. The instrumentation of a specimen is an important tool to evaluate its mechanical behavior during impact. Test results as deceleration-time and strain-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of calculations based on finite-element methods. Strain gauges are useful to determine the time dependent magnitude of any deformation and the associated stresses. Accelerometers are widely used for the measuring of motion i.e. speed or the displacement of the rigid cask body, vibration and shock events. In addition high-speed video technique can be used to visualize and analyze the kinematical impact scenario by motion analysis. The paper describes some selected aspects on instrumented measurements and motion analysis in context with low level radioactive waste (LLW) container drop testing
The paper presents technical details of the drop test performance as well as some experimental results of tests carried out with the Japanese 'Yoyushindo-disposal' waste container for intermediate depth disposal. The tests were accompanied by various metrology to collect data as basis for safety assessment.
Evaluating porosity in cordierite diesel particulate filter materials, part 1 X-ray refraction
(2013)
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, with porosity and solid matter being intermingled. Mechanical, thermal, and filtration properties can only be precisely estimated if the morphology of both solid matter and porosity can be quantitatively determined. Using x-ray absorption and refraction, we quantitatively evaluate porosity and pore orientation in cordierite diesel particulate filter ceramics. Porosity values turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data.
Because of its mobility and ability to investigate exposed surfaces, single-sided (SiS) nuclear magnetic resonance (NMR) technology enables new application fields in geosciences. To test and assess its corresponding potential, we compare longitudinal (T1) and transverse (T2) data measured by SiS NMR with those of conventional geoscientific laboratory NMR. We use reference sandstone samples covering a broad range of pore sizes. Our study demonstrates that the lower signal-to-noise ratio of SiS NMR data generally tends to slightly overestimated widths of relaxation time distributions and consequently pore size distributions. While SiS and conventional NMR produce very similar T1 relaxation data, unbiased SiS NMR results for T2 measurements can only be expected for fine material, i.e. clayey or silty sediments and soils with main relaxation times below 0.05s. This limit is given by the diffusion relaxation rate due to the gradient in the primary magnetic field associated with the SiS NMR. Above that limit, i.e. for coarse material, the relaxation data is strongly attenuated. If considering the diffusion relaxation time of 0.2 s in the numerical data inversion process, the information content >0.2s is blurred over a range larger than that of conventional NMR. However, our results show that principle range and magnitudes of the relaxation time distributions are reconstructed to some extent. Regarding these findings, SiS NMR can be helpful to solve geoscientific issues, e.g. to assess the hydro-mechanical properties of the walls of underground facilities or to provide local soil moisture data sets for calibrating indirect remote techniques on the regional scale. The greatest opportunity provided by the SiS NMR technology is the acquisition of profile relaxation data for rocks with significant bedding structures at the µm scale. With this unique feature, SiS NMR can support the understanding and modeling of hydraulic and diffusional anisotropy behavior of sedimentary rocks.
Barium silicate glass powders 4 h milled in CO2 and Ar and sintered in air are studied with microscopy, total carbon analysis, differential thermal Analysis (DTA), vacuum hot extraction mass spectroscopy (VHE-MS), Fourier-transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary-ion mass spectrometry (TOF-SIMS). Intensive foaming of powder compacts is evident, and VHE studies prove that foaming is predominantly caused by carbonaceous species for both milling gases. DTA Shows that the decomposition of BaCO3 particles mix-milled with glass powders occurs at similar temperatures as foaming of compacts. However, no carbonate at the glass surface could be detected by FTIR spectroscopy, XPS, and TOF-SIMS after heating to the temperature of sintering. Instead, CO2 molecules unable to rotate identified by FTIR spectroscopy after milling, probably trapped by mechanical dissolution into the glass bulk. Such a mechanism or microencapsulation in cracks and particle aggregates can explain the contribution of Ar to foaming after intense milling in Ar atmosphere. The amount of CO2 molecules and Ar, however, cannot fully explain the extent of foaming. Carbonates mechanically dissolved beneath the surface or encapsulated in cracks and micropores of particle aggregates are therefore probably the major foaming source.
Reliability analysis of the ultrasonic inspection system for the inspection of hollow railway axles
(2016)
Axles are safety critical train components that are subjected to significant cyclic loading during operation. If the crack is initiated in the axle, cyclic loading will lead to crack propagation. To maintain structural integrity, axles must be periodically inspected for fatigue cracks in the material. Deutsche Bahn uses mechanized ultrasonic inspection system to inspect hollow railway axles. The inspections are performed from the bore surface, using several conventional transducers with different incident angles, inspecting the axle along the entire length. As with the every safety critical system, the reliability of these inspections must be determined with regard to their flaw detection capabilities. Traditionally this is done according to the relevant standards for railway vehicles. To investigate the capability of the NDT system more thoroughly, we want to evaluate the capability of the inspection system to detect flaws by means of probability of detection (POD) curves. It will be shown that other parameters, beside the size of the crack, for example crack position in the axle, influence the detection of the crack. The influence of these parameters was evaluated using ultrasonic simulation. The evaluation served as an input for the manufacturing of the flaws in the real scale axle. Once these axles are inspected and the data evaluated, using data from both measurement and simulation, we will express the POD of the crack as function of influencing parameters using the multiparameter POD model.
Complementary to Part 1 of this work, the bi-continuous microstructure of porous synthetic cordierite ceramics for filtration applications was investigated using 3D x-ray computed tomography at different resolutions. Applying both Fast Fourier Transform and a newly developed image analysis algorithm, we quantitatively evaluated porosity and pore orientation. The statistical approach allows extraction of spatially resolved or average values. Porosity values based on x-ray absorption agree with mercury intrusion measurements, while pore orientation factors agree with x-ray refraction data (Part 1 of this work), and with published crystallographic texture data.
Internal cask content collisions during drop test of transport casks for radioactive materials
(2013)
In transport casks for radioactive materials, significantly large axial and radial gaps between cask and internal content are often present because of certain specific geometrical dimensions of the content (e.g. spent fuel elements) or thermal reasons. The possibility of inner relative movement between content and cask will increase if the content is not fixed. During drop testing, these movements can lead to internal cask content collisions, causing significantly high loads on the cask components and the content itself. Especially in vertical drop test orientations onto a lid side of the cask, an internal collision induced by a delayed impact of the content onto the inner side of the lid can cause high stress peaks in the lid and the lid bolts with the risk of component failure as well as impairment of the leak tightness of the closure system. This paper reflects causes and effects of the phenomenon of internal impact on the basis of experimental results obtained from instrumented drop tests with transport casks and on the basis of analytical approaches. Furthermore, the paper concludes the importance of consideration of possible cask content collisions in the safety analysis of transport casks for radioactive materials under accident conditions of transport.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. We shall show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. We will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben.
Using the Modular Reliability Model the three different main influencing elements, i.e. intrinsic capability (IC), application parameters (AP) and the human factors (HF), are, in the first instance, investigated separately. The intrinsic capability stands for the pure physical-technological process of the signal detection caused by the waves or the rays from a material defect in the presence of noise (driven by the material and the devices). This intrinsic capability is the upper bound of the possible reliability. Already when measuring this intrinsic capability for thick walled components the original one-parameter POD must be extended to a multiparameter POD, where, in addition to the defect size, a number of additional physical parameters, such as the grain size distribution (or attenuation), defect depth, and angle or surface roughness, must be considered. For real life cycle assessments it is necessary to evaluate the signal response from real defects. The industrial application factors, e.g. coupling conditions, limited accessibility, heat and environmental vibrations, diminish the reliability. The amount of reduction can be determined quantitatively, if the underlying conditions are controlled. In case they are not controlled it is necessary to count for a fluctuation in the reliability in the field anyway. The third group of important influencing factors are the human factors, which do not only cover the individual performance capability of the inspectors but also the design of the working place,the procedure, the teamwork quality, interaction with systems, the organization, and finally, the relationship between the companies involved in the inspection process and to which extend the responsible parties are aware of it. When comparing an “ideal inspection” with a “real inspection” it is worth while to look how the existing practices, rules and standards support reliable testing and where the “delta” is. In the context of vigor, with respect to the industrial end user, it needs to be shown how the level of reliability of NDE, influenced by the different factors, has an impact on acceptance or rejection of safety critical parts.
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, whereby porosity and solid matter are intermingled. Mechanical, thermal, and filtration properties can only be precisely estimated if the morphology of both solid matter and porosity can be quantitatively determined. Using 3D computed tomography (CT) at different resolutions, and several X-ray refraction-based techniques, we quantitatively evaluated porosity and pore orientation in cordierite diesel particulate filter ceramics.Moreover, applying both Fast Fourier Transform (FFT) and a newly developed image analysis algorithm (directional interface variance analysis, DIVA), we quantitatively evaluated porosity and pore orientation. Both the experimental techniques and the statistical approach allow extraction of spatially resolved or average values.Porosity values from synchrotron computed tomography used turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data. This latter point also implies that the study of the pore/matter interface is sufficient to describe the morphological properties of these materials.
A management system based on international, national or other standards acceptable to the competent authority shall be established and implemented for all activities including design, manufacture, testing, documentation, use, maintenance, inspection in accordance with IAEA SSR-6. Hereby, quality assured testing and documentation can substantially contribute to the demonstration of package design compliance with the regulations. Nowadays, a drop test campaign within the approval process of packages for radioactive materials can be a very complex and extensive project including various test and measurement techniques. On this basis of procedures and documents the experimental tests of packages and containers are performed with quality proofed results and a high reliability. A complete traceability and direct transferability of package design test results can give particular importance to the type approval procedure.
In context with new cask designs and their approval procedure, the experimental testing of impact limiters under drop test conditions becomes more and more important in order to assess the damage mechanics behaviour and safety margins for validation reasons. In recent years, various designs of impact limiters have been tested by the Federal Institute for Materials Research and Testing within specific component testing and particularly with regard to type B package design approval procedures. The paper focuses on the experimental realisation of impact limiter tests and presents implemented measurement techniques to determine the amount of deformation and to explain the impact behaviour by means of photogrammetric metrology and three-dimensional fringe projection method, high speed motion analysis and adjusted deceleration measurements.
In context with new cask designs and their approval procedure the experimental testing of impact limiters under drop test conditions becomes more and more important in order to assess the damage mechanics behavior and safety margins for validation reasons.
In recent years various designs of impact limiters have been tested by the Federal Institute for Materials Research and Testing (BAM) within specific component testing and particularly with regard to type B package design approval procedures.
The paper focuses on the experimental realization of impact limiter tests and presents implemented measurement techniques to determine the amount of deformation and to explain the impact behavior by means of photogrammetric metrology and 3-d fringe projection method, high-speed motion analysis and adjusted deceleration measurements.
BAM safety related research of containers for radioactive material focuses on advanced mechanical safety assessment methods for verification of the structural integrity and leak tightness under normal conditions of transport and hypothetical accident conditions during transport and storage. An essentially unyielding target with a rigid surface is required for impact tests performed for package approval according to IAEA regulations. In addition to specification of a target, e.g. with a combined mass more than 10 times that of the specimen for drop tests, unyielding target characteristics have been investigated with various package designs and different impact tests. The unyielding target of the BAM drop test facility, a reinforced concrete block together with an embedded and anchored mild steel plate, provides relatively large mass and stiffness with respect to the packages being tested. For monitoring reasons accelerometers and strain gauges are embedded in the concrete block of the foundation at several positions. Additionally, dynamic impact responses like vibrations and rigid body motion can be measured by seismic accelerometers. The mechanical characterisation of the target's rigidity is based on experimental results from various drop tests. Test containers with weights of 181 000 kg, 127 000 kg and 8010 kg hit the target with velocities up to 13·5 m s-1 in the horizontal and vertical drop positions. The rigidity of the impact target can be demonstrated with experimental results confirmed by analytical approaches. Some conclusions can be drawn about experimental testing as well as analytical calculations in order to compare impact effects.
This paper presents a comparison between full scale prototype and reduced scale model drop test data in regard to similarity mechanics. Together with a current BAM research project, the paper contributes to the further development of mechanical evaluation methods for safety assessment of RAM transport and storage packages including the transferability of package impact response from reduced scale models to full scale packages.
This paper presents technical details of the drop test performance as well as some experimental results of tests carried out with the Japanese 'Yoyushindo-Disposal' waste container for intermediate depth disposal. The drop test program comprised three single 8 m drop tests at the specimen's corner edge orientation onto a concrete slab. The slab was connected to the unyielding IAEA target of the BAM's 200 t drop test facility. The three tested specimens had masses between 20 000 and 28 000 kg depending on their content mass. The tests were accompanied by various metrology, such as strain and deceleration measurements, optical three-dimensional deformation methods, leak tightness testing and test installation for potential particle release measurements to collect a set of data for establishing a basis for safety assessment.
Three drop test campaigns have been performed with DN 30 Protective Structural Packaging (PSP) developed by DAHER NUCLEAR TECHNOLOGIES GmbH for the transport of natural, enriched and reprocessed uranium hexafluoride (up to 5 wt%) in 30B cylinders.
The mechanical prototype testing is intended to demonstrate that the package DN30 complies with regulatory requirements under normal and hypothetical accident conditions of transport (NCT, ACT) relevant to IF, AF and B(U)F packages, respectively.
The paper includes the results of the latest test campaign carried out in 2015-2016 at the drop test facility of BAM, Germany with new full scale prototypes of the DN30 PSP and 30B cylinders. Repetition of drop test sequences became necessary after changing to Polyisocyanurate foam as shock absorbing material with variable foam densities. Furthermore, the mechanical behavior of the UF6 content of the 30B cylinder is now simulated by a mixture of cement and steel grid as modified surrogate material; instead of small steel balls. The behavior of this new content simulation is assumed to be more realistic with respect to the properties of real UF6.
In context with Japanese disposal and transport container safety assessment the German Federal Institute for Materials Research and Testing (Bundesanstalt für Materialforschung und -prüfung) per-formed extensive drop test series with prototypes of RAM packages in recent years.
The paper presents two cooperative projects focused on project management, testing performance and experimental results.
In the first project, a full-scale prototype of a package for transport and storage of spent fuel elements with a total mass of 127,000 kg and its reduced-scale model which was similar to the prototype in both geometry and design were drop tested in 9 m and 1 m puncture tests at various drop orientations under regulatory conditions. In context with a corresponding research project the test data was used in combination with numerical methods to investigate the phenomenon of internal cask- content collisions during drop tests. Here, technological gaps between basket or radioactive content and cask body or primary lid can be a reason for significant high dynamic loadings of cask components and its internals due to additional impact interactions in the cask cavity caused by inner relative movement between content and cask. Further investigations were carried out in the field of similarity mechanics comparing experimental drop test data of the full-scale prototype and reduced-scale model in regard to the transferability of package impact response from reduced-scale models to full-scale packages.
In the second project, drop tests with a waste container for intermediate depth disposal were per-formed being contracted by Kobe Steel, Ltd. and a consortium of Japanese electric power plant com-panies. The drop test program comprised three single 8-m drop tests in a specimen’s corner edge orientation. For drop tests according to legal regulations for interim storage or final disposal it is often necessary to use a target which represents the real ground of the storage facility. In such cases the container hits directly onto a well-defined concrete slab on top of the IAEA target. Here, the directly impact target for the drop tests were concrete slabs manufactured in Japan and connected by mortar to the impact pad of the unyielding IAEA target.
In context with new cask designs and their approval procedure, the experimental testing of impact limiters under drop test conditions becomes more and more important in order to assess the damage mechanics behaviour and safety margins for validation reasons. In recent years, various designs of impact limiters have been tested by the Federal Institute for Materials Research and Testing within specific component testing and particularly with regard to type B package design approval procedures. The paper focuses on the experimental realisation of impact limiter tests and presents implemented measurement techniques to determine the amount of deformation and to explain the impact behaviour by means of photogrammetric metrology and three-dimensional fringe projection method, high speed motion analysis and adjusted deceleration measurements.
Inhalt ist die zerstörungsfreie Detailuntersuchung von Holzbauteilen mit einem dreidimensional abbildenden Ultraschall-Echoverfahren. Das neu entwickelte 3D-Verfahren berücksichtigt den anisotropen Aufbau des Holzes. Die Bildschnitte und Projektionen werden aus flächigen Ultraschallaufnahmen berechnet. Die Messungen erfolgen an Probekörpern sowie an Bauteilen aus der Praxis. In dem Forschungsvorhaben wird die für Holz neue 3D-Rekonstruktionsrechnung verwendet und mit dem Ziel weiterentwickelt, unter Berücksichtigung der anisotropen Struktur des Holzes eine dreidimensional aufgelöste Abbildung von Reflektoren im Inneren der Holzbauteile zu ermöglichen. Damit werden die bisher für Holzbauteile zur Verfügung stehenden Verfahren entscheidend ergänzt, weil nun eine hochgenaue dreidimensionale Abbildung erreichbar ist (Auflösung: 20 mm und besser).
Der Beitrag konzentriert sich auf bildgebende Messverfahren, die der dreidimensionalen Bestimmung mechanischer, geometrischer und kinematischer Parameter von Materialien und Bauteilen dienen. Das sind hier insbesondere die Mehrbildfotogrammetrie sowie die Stereomessverfahren, die auf folgenden physikalisch-optischen Grundlagen beruhen: die zeit- und raumveränderliche Projektion von Lichtstreifensystemen, die Bildkorrelation mittels Grauwertmustern und die Verfolgung kontrastreich applizierter Punkttargets. Letztendlich werden aus den gemessenen Punktkoordinaten unterschiedlicher Dichte und Belastungszustände die gewünschten 3D-Parameter abgeleitet. Hierzu gehören z. B. die Oberflächengestalt und deren Verformung, approximierte 3D-Geometrielemente, veränderliche 6DoF-Starrkörperorientierungen, Vektorverschiebungsfelder, Oberflächendehnung, Koordinaten-Zeit-Funktionen, Geschwindigkeit und Beschleunigung. Diese Kenngrößen sind beispielsweise für die Ermittlung mechanischer Werkstoffeigenschaften und -kennwerte bis hin zur Form- und Verformungsmessung von Bauteilen in gezielt quasi-statisch oder dynamisch beanspruchenden Prüfeinrichtungen wichtig. Vorteilhaft für die praktische Anwendung dieser Verfahren ist insbesondere, dass sie berührungslos arbeiten, kombiniert werden können und skalierbar sind z. B. hinsichtlich Messvolumen, Auflösung, Genauigkeit und Koordinatensystemen der zu bestimmenden 3D-Punktkoordinaten an Materialoberflächen bzw. Komponenten.
Ausgehend von der Beschreibung der messtechnischen Prinzipien dieser Verfahren sollen zwei Anwendungsbeispiele aus dem Bereich der Gefahrgutbehäl-terprüfung im Rahmen von Bauartzulassungen und der normungsbegleitenden Mate-rialforschung den Stand in der Anwendungspraxis aufzeigen und einen Eindruck hinsichtlich der flexiblen Einsatzmöglichkeiten dieser optischen 3D-Verfahren verdeutlichen.
This report describes the progress in understanding and describing the detectability of the ultrasonic inspection technique developed by SKB for the inspection of copper tubes used for the final disposal of the Swedish spent nuclear fuel. In former research activities dedicated to the different parts of the canister, the probability of detection (POD) evaluation technique, as developed for thin aircraft components, was further developed for the application on complex hick-walled components. The result of this development was the introduction of a “multi-parameter” POD framework. In contrast to taking only the defect size into consideration (as for aircraft components) additional influencing factors, relevant for thick components, such as depth position, orientation and part geometry, were included. Furthermore, the variation of ultrasonic attenuation due to various material properties was included.
BAM is the German Federal Institute for Materials Research and Testing and the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste. In context with safety assessment of RAM packages BAM performed numerous drop tests in the last decades. The tests were mostly accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers. The procedure of drop testing and the resulting measurement analysis are the main methods to evaluate the safety against mechanical test conditions. Measurement techniques are dedicated to answer questions in regard to the structural integrity of a RAM package, the mechanical behavior of the prototype as well as of its content under impact conditions.
Test results like deceleration-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of numerical calculations. In this context the adequate selection of accelerometers and measurement systems for the performance of drop tests is important. Therefore it is not only necessary to find suitable positions for the accelerometers at the test specimens, but also to consider technical boundary conditions as e.g. temperature.
Drop testing of a container for the storage. transport and disposal of intermediate level waste
(2017)
Impact tests were performed, as part of a corresponding container’s substantiation, during design development of a shielded container. The container will be used for storage, transport, and disposal of intermediate level waste in the UK.
The mechanical test program comprised a 9m free drop test onto an unyielding target in a container long lid edge down orientation at ambient conditions. Further, a 0,5m free drop test onto a punch target was performed. Here, the container was orientated with the lid downwards in a way that the punch, a mild steel bar, impacts a filter lid.
The test specimen was instrumented with strain gauges and accelerometers for the drop tests. Transient strains at selected points of the inner and outer container walls, at the shielding lid, as well as at the lid bolts were measured during the container’s impact. Furthermore, decelerations of the container body, container lid, and the skip were measured. The complex geometrical changes of the container due to impact were determined by optical 3d- deformation measures using the projected fringes method in combination with multi-image photogrammetry.
This paper summarizes the performance of the drop tests and various drop test results in context with the design development as well as aspects regarding the associated Finite Element (FE) analyses and post-test evaluation.
BAM is the German Federal Institute for Materials Research and Testing and the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste. In context with safety assessment of RAM packages BAM performed numerous drop tests in the last decades. The tests were mostly accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers.
The procedure of drop testing and the resulting measurement analysis are the main methods to evaluate the safety against mechanical test conditions. Measurement techniques are dedicated to answer questions in regard to the structural integrity of a RAM package, the mechanical behavior of the prototype as well as of its content under impact conditions.
Test results like deceleration-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of numerical calculations. In this context the adequate selection of accelerometers and measurement systems for the performance of drop tests is important. Therefore it is not only necessary to find suitable positions for the accelerometers at the test specimens, but also to consider technical boundary conditions as e.g. temperature.
Fire testing is an essential part of the hypothetical, cumulative mechanical and thermal test conditions that shall guarantee package safety in severe accidents. Within regulatory approval of transport or storage packages for radioactive material, specific thermal load tests are required in accordance to licensing conditions and international standards, respectively. The specifications of these thermal tests are based on test conditions with equivalent heat input to that of a hydrocarbon fuel fire. In the past, light heating oil, diesel or kerosene was mostly used as the fuel to generate the pool fire. In accordance with IAEA regulations for a fire in an accident, the temperature of 800 °C over a period of 30 minutes must be fulfilled. Furthermore, the delivery acceptance criteria for containers in nuclear waste repositories could reach for example average temperatures of 800 °C during a period of one hour in combination with defined requirements on activity release. BAM as a scientific and technical German federal government institute operates an open air Technical Safety Test Site for experimental investigations of dangerous good and its containment. In this areal a large fire test facility is under operation. Liquid Propane is utilized as fuel which is pumped via pipelines from a central storage tank to the fire exposed test facility areas. In the ring burner system, the gas is released from nozzles, and ignited by ignition burners. The paper includes examples of fire test performance with prototypes of a transport package and a storage container, respectively. In preparation of the thermal load, calorimeter tests have been performed using test specimens of appropriate size and behavior. For the fire test scenario is demonstrated that the IAEA thermal test requirements are fulfilled.
Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale
(2020)
Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation.
The chemical composition of surfaces functionalized with self-assembled monolayers (SAMs) is an important parameter that determines their performance in a broad range of applications, from immobilizing molecular machines to initiation and growth control of MOFs (Metal-Organic Frameworks). In this article, a critical Survey of XPS (X-ray photoelectron spectroscopy) and NEXAFS (near edge X-ray absorption fine structure) spectroscopy data for pyridine-functionalized monolayers on gold surfaces is presented to compile correlations that have been indiscernible before. Monolayers with aromatic backbones are compared to monolayers with aliphatic backbones.
Monolayers with pyridine end-groups are compared to mixed monolayers formed terpyridine-functionalized by molecules end-groups and non-functionalized molecules. Thiol-oxidation during ageing of the SAMs in air is addressed. And finally, the addressability of the SAMs for the deposition of metal-ions and organic molecules is investigated and compared. This work consequently delivers a comprehensive set of spectroscopic data of (ter-)pyridine-terminated SAMs and their performance as template for the preparation of functional multilayers of macrocycles exhibiting a preferential orientation.
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.
Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads.
Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9).
Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies.
A series of twelve 3-piperazinyl propenylidene indolone merocyanines was synthesized in a one-pot fashion using a consecutive three-component insertion-coupling-Michael addition sequence. Physicalorganic treatment of the absorption data of a consanguineous series of this library allows semiquantitative Linear Free Energy Relationships (LFERs) to be established and confirmation of the positive Absorption solvatochromicity. All Boc-substituted piperazinyl merocyanines display aggregation induced Emission (AIE), which was corroborated for two solvent systems. In particular, crystallization-induced Emission enhancement (CIEE) induced by ultrasonication could be shown for a model chromophore by confocal laser scanning microscopy (CLSM).
3-Aminovinylquinoxalines are readily accessible from (hetero)aryl glyoxylic acids or heterocyclic π-nucleophiles by consecutive four- and fivecomponent syntheses in the sense of an activation-alkynylation-cyclocondensation-addition sequence or glyoxylation-alkynylation-cyclocondensation-addition sequence in good yields. The title compounds are highly fluorescent with pronounced emission solvatochromicity and protochromic fluorescence quenching. Time-resolved fluorescence spectroscopy furnishes radiative and nonradiative fluorescence decay rates in various solvent polarities. The electronic structure is corroborated by DFT and TD-DFT calculations rationalizing the observed spectroscopic effects.
Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.