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BAM Inside #1/2022
(2022)
BAM Update #5/2022
(2022)
The work on Tribology, digitalisation, and the harmonised procedures developed in i-TRIBOMAT Open Innovation Testbed was presented. The project develops procedures and shares ideas on how to deal with characterisation techniques and provide services to end users in different places and locations, which is realised by adopting a common and widely agreed procedures. i-TRIBOMAT is active also via YouTube platform to enhance communication and spread the word amongst the interested parties and society.
Mit dem stetigen weltweiten Anstieg der Nachfrage nach Polymerprodukten nimmt auch die potenzielle Menge an Kunststoffabfällen in der Umwelt zu. Problematisch ist, dass viele der wirtschaftlich relevantesten Kunststoffe sehr lange brauchen, um in der Umwelt abzubauen, sich dort akkumulieren und in kritisch betrachtetes Makro- und Mikroplastik zu zerfallen. Auf der Grundlage des Vorsorgeprinzips fordert die Europäische Kommission daher die Entwicklung neuer polymerer Materialien, die diesem Problem der Persistenz entgegenwirken und unter natürlichen Umweltbedingungen schneller abgebaut werden können. 1,2
Um dieses Problem anzusprechen, wurden mittels additiver Fertigung Polymerblends aus photooxidationsempfindlichem Polystyrol (PS) und hydrolyseempfindlicher Polymilchsäure (PLA) hergestellt. Die Hypothese war, dass sich die beiden Thermoplaste aufgrund ihrer unterschiedlichen Abbauprozesse gegenseitig in ihrem Abbau unterstützen, wenn sie unter moderaten, realitätsnahen Umweltalterungsbedingungen (45 °C) abwechselnd der Photooxidation und Hydrolyse ausgesetzt werden.
In der Praxis zeigten die Ergebnisse, dass die Degradation von PLA durch die Anwesenheit von PS deutlich beschleunigt worden ist – wohingegen die Degradation von PS gehemmt wurde. In diesem Vortrag werden die detaillierten Ergebnisse der Oberflächen- (ATR-FTIR, REM) und Bulk-Analysen (DSC, TGA, FTIR-Transmission, TED-GC/MS) der Blends sowie ergänzende Mikroplastik-Ergebnisse des umgebenden Wassermediums (TED-GC/MS) erörtert.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Gezeigt werden die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Beispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
Vortrag zum Kick-off des Projektes.
Ziel des Projektes ist es, die Eignung der Bestimmung eines oder mehrerer der genannten anthropogenen Marker im Abwasser zur Volumenkorrektur („Kalibration“) im SARS-CoV-2-Monitoring von Abwässern auf der Basis eines von der BAM zu erhebenden Messdatensatzes zu evaluieren.
Im Rahmen des Forschungsprojektes IGF 20470N wurden Untersuchungen zum Alterungsverhalten von reaktiven Brandschutzsystemen (RBS) auf Stahlbauteilen durchgeführt. Mithilfe der Ergebnisse einer umfangreichen Literaturrecherche sowie experimentellen und numerischen Untersuchungen sollte ein Vorschlag für ein Prüfkonzept zum Nachweis einer Nutzungsdauer von RBS von mehr als 10 Jahren auf Basis von Kurzzeitversuchen abgeleitet werden. Dabei setzt die Bewertung des Alterungsverhaltens von RBS voraus, dass die Mechanismen der Alterung hinreichend bekannt sind.
Dafür wurden zunächst systematisch Daten von Kurz- und Langzeitversuchen von nationalen Zulassungsprüfungen der letzten Jahrzehnte ausgewertet. Anschließend wurden umfangreiche experimentelle Untersuchungen an einer wasserbasierten sowie einer epoxidharzbasierten Richtrezeptur durchgeführt. Da aus der Literatur bekannt ist, dass die Einflüsse der Bewitterung zu einer Veränderung der Konzentration der Bestandteile innerhalb der Beschichtung führen können, wurden Untersuchungen mit Mangelrezepturen durchgeführt, wobei systematisch einzelne Bestandteile reduziert wurden. Neben optischen Untersuchungen wurden thermoanalytische Verfahren (DSC-TG-, ATR-FTIR-, Elementar-, Farbanalyse) angewandt sowie Brandversuche an beschichteten Stahlplatten durchgeführt. Des Weiteren wurden die Richtrezepturen den beschleunigten Kurzzeitversuchen gemäß EAD 350402-00-1106 (2017) unterzogen, welche die Zulassung von Produkten auf europäischer Ebene regelt. Für die wasserbasierte Richtrezeptur wurden die Bewitterung für den feuchten Innenraum (Typ Z1) mehrfach wiederholt (1x, 3x, 6x). Für die epoxidharzbasierte Richtrezeptur entsprach die Bewitterung dem Zyklus für die Außenanwendung (Typ X). In Brandversuchen sowie thermoanalytischen und optischen Untersuchungen wurde das Alterungsverhalten sowie die thermische Schutzwirkung analysiert.
Anschließend wurden numerische Simulationen von Stahlbauteilen mit gealterten RBS durchgeführt und anhand der experimentellen Untersuchungen validiert. Mithilfe der numerischen Modelle kann eine Bewertung der thermischen Schutzwirkung von Stahlbauteilen mit gealterten RBS vorgenommen werden.
Mithilfe der gesammelten Erkenntnisse wurde ein Vorschlag für ein Prüfkonzept für den Nachweis einer Nutzungsdauer von mehr als 10 Jahren abgeleitet. Das Prüfkonzept besteht dabei aus einem Katalog von Möglichkeiten, die aktuellen Zulassungsprüfungen auf europäischer Ebene für eine Nutzungsdauer von 10 Jahren auf einen längeren Zeitraum zu erweitern.
The development of the microbiologically influenced corrosion ( MIC ) -specific inductively coupled plasma-time of flight-mass spectrometry ( ICP-ToF-MS ) analytical method presented here, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis. For this, a MIC-specific staining procedure was developed, which ensures the analysis of intact cells. It allows the analysis of archaea at a single cell level, which is extremely scarce compared to other well-characterized organisms. The detection method revealed elemental selectivity for the corrosive methanogenic strain Methanobacterium -affiliated IM1. Hence, the possible uptake of individual elements from different steel samples was investigated and results showed the cells responded at a single-cell level to the different types of supplemented elements and displayed the abilities to uptake chromium, vanadium, titanium, cobalt, and molybdenum from solid metal surfaces. The methods developed and information obtained will be used in the future to elucidate underlying mechanisms, compliment well-developed methods, such as SEM-EDS, and develop novel material protection concepts.
The continuously increasing use of plastics is supposed to result in a rising exposure of MNPs to humans. Available data on human health risks of microplastics after oral uptake increased immensely in the past years and indicates very likely only low risks after oral consumption. Concerning nanoplastics, uptake, transport and potential adverse effects after oral uptake are less well understood. This study aims to investigate differences between microplastic particles and particles in the submicron- and nanoscaled size derived from food-relevant polymers with a particle size range consistent with higher potential for cellular uptake, fate, and effects when applied to human intestinal and liver cells. This work includes the development of cellular and subcellular detection methods for synthetic polymeric particles in the micro- and nanometer-range, using Scanning Electron Microscopy, Small-Angle X-ray and Dynamic Light Scattering methods, Asymmetric Flow Field Flow Fractionation, octanol-water fractionation, fluorescence microscopy and flow cytometry. Polylactic acid (250 nm and 2 μm (polydisperse)), melamine formaldehyde (366 nm) and polymethylmethacrylate (25 nm) were thoroughly characterized. The submicro- and nanoplastic test particles showed an increased uptake and transport quantity through intestinal cells. Both types of particles resulted in observed differences of uptake behavior, most likely influenced by different lipophilicity, which varied between the polymeric test materials. Toxic effects were detected after 24 h only in overload situations for the particles in the submicrometer range. This study provides further evidence for gastrointestinal uptake of submicro- and nanoplastics and points towards differences regarding bioavailability between microplastics and smaller plastic particles that may result following the ingestion of contaminated food and beverages. Furthermore, the results reinforce the importance for studying nanoplastics of different materials of varying size, surface properties, polymer composition and hydrophobicity.
Results:
- Four types of inks were measured iron gall (vitriolic and non vitriolic), carbonic, mixed and vegetable inks.
- We need to start analyzing systematically the organic part of the inks.
- Great variety in the composition of the inks.
- No correlation between the type of ink used and any other criteria apart from a personal preference.
- Inks purchased by (some) scribes.
- Reconstruction of the chronology of writing and signing of certain legal documents.
- Comparison with documents written by the Muslim court.
Antimicrobial resistance (AMR) is a global health problem with the environment being an important compartment for the evolution and transmission of AMR. Previous studies showed that de-novo mutagenesis and horizontal gene transfer (HGT) by conjugation or transformation – important processes underlying resistance evolution and spread - are affected by antibiotics, metals and pesticides. However, natural microbial communities are also frequently exposed to biocides used as material preservatives, but it is unknown if these substances induce mutagenesis and HGT. Here, we show that active substances used in material preservatives can increase rates of mutation and conjugation in a species- and substance-dependent manner, while rates of transformation are not increased. The bisbiguanide chlorhexidine digluconate, the quaternary ammonium compound didecyldimethylammonium chloride, the metal copper, the pyrethroid-insecticide permethrin, and the azole-fungicide propiconazole increase mutation rates in Escherichia coli, whereas no increases were identified for Bacillus subtilis and Acinetobacter baylyi.
Benzalkonium chloride, chlorhexidine and permethrin increased conjugation in E. coli. Moreover, our results show a connection between the RpoS-mediated general stress and the RecA-linked SOS response with increased rates of mutation and conjugation, but not for all biocides. Taken together, our data show the importance of assessing the contribution of material preservatives on AMR evolution and spread.
Clerodin was isolated from the medicinal plant Clerodendrum infortunatum, and CSD search showed the first crystal structure of clerodin by a single-crystal X-ray diffraction study. We checked its binding potential with target proteins by docking and conducted network pharmacology analysis, ADMET analysis, in silico pathway analysis, normal mode analysis (NMA), and cytotoxic activity studies to evaluate clerodin as a potential anticancer agent. The cell viability studies of clerodin on the human breast carcinoma cell line (MCF-7) showed toxicity on MCF-7 cells but no toxicity toward normal human lymphocyte cells (HLCs). The anticancer mechanism of clerodin was validated by its enhanced capacity to produce intracellular reactive oxygen species (ROS) and to lower the reduced glutathione content in MCF-7 cells.
Models for TOPAS/Geant4 to estimate the microscopic dose received by biomolecules during bioSAXS experiments.
The C++ classes in this repository extend the functionality of the TOPAS (http://www.topasmc.org/) Monte-Carlo program, which is itself a wrapper of the Geant4 MCS Toolkit (http://geant4.org).
Additive manufacturing (AM) processes are opening new design possibilities for large scale electrical devices such as power generators. Conventional manufacturing methods use copper rods which are wrapped, vacuum impregnated, bend and welded. These processes are labor-intensive and time-consuming. The introduction of AM methods for manufacturing the copper conductor and electrical insulation can reduce the size of the generator head, the most complex part of the generator.
In this study, the electrical and dielectrical properties of additively deposited ceramic layers are investigated and compared with the properties of conventionally fabricated bulk ceramics. The ceramic layers are thermally deposited by atmospheric plasma spraying of a commercially available alumina powder. Bulk ceramics are fabricated by dry pressing and sintering of the same powder. Microstructure and porosity were analyzed by scanning electron microscopy (SEM). Electrical and dielectrical properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards.
The microstructures of sprayed and sintered alumina show significant differences with respect to grain form and porosity. The density of the bulk ceramic is lower than the density of the sprayed layer due to the coarse particle size (d50 = 33 μm). Therefore, data from dense samples of the same chemical composition but lower particle size alumina powder were used for comparison.
Chromium(III) complexes can show phosphorescence from the spin-flip excited doublet states 2E/2T1 in the near-infrared with high photoluminescence quantum yields and extremely long lifetimes in the absence of dioxygen. The prototype molecular ruby, [Cr(ddpd)2]3+ (ddpd = N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine), has a photoluminescence quantum yield and a luminescence lifetime of 13.7% and 1.1 ms in deaerated acetonitrile, respectively. However, its luminescence is strongly quenched by 3O2 via an efficient Dexter-type energy transfer process. To enable luminescence applications of molecular rubies in solution under aerobic conditions, we explored the potential of sterically demanding ddpd ligands to shield the chromium(III) center from O2 using steady state and time-resolved photoluminescence spectroscopy. The structures of the novel complexes with sterically demanding ligands were investigated by single crystal X-ray diffraction and quantum chemically by density functional theory calculations. The O2 sensitivity of the photoluminescence was derived from absolutely measured photoluminescence quantum yields and excited state lifetimes under inert and aerobic conditions and by Stern–Volmer analyses of these data. Optimal sterically shielded chromium(III) complexes revealed photoluminescence quantum yields of up to 5.1% and excited state lifetimes of 518 μs in air-saturated acetonitrile, underlining the large potential of this ligand design approach to broaden the applicability of highly emissive chromium(III) complexes.
Calibration-free methods in laser-induced breakdown spectroscopy, CF LIBS, serve as an alternative to calibration-based LIBS techniques. Their major advantage is the ability for fast chemical analysis in situations where matrix-matched standards are not readily available (as, e.g., in the analysis of biological materials and remote analysis) or amount of samples are limited. Their main applications are in the industry, geology, biology, archeology, and even space exploration. This chapter overviews the principle of operation and performance of CF LIBS techniques.
Engineering grain boundaries demands a quantitative description of both their segregation and specific phase behavior. Recently I have proposed a density-based model for grain boundary thermodynamics that enables CALPHAD integrated derivation of grain boundary phase diagrams, broadly applied now in studying various alloys. Combining this model with experimental investigations, in this talk, new aspects of interfacial segregation and phase transformation revealed in polycrystalline alloys are discussed. The effect of elastic interaction on grain boundary phase behavior is incorporated. We consider Al alloys and novel high-entropy alloys and discuss a general strategy for grain boundary engineering.
Carbon nanomembranes are synthetic two-dimensional sheets with nanometer thickness, macroscopic lateral dimensions, and high structural homogeneity. They have great application potential in various branches of nanotechnology. Because of their full carbon structure, it is not clear whether macromolecules like poly(methyl methacrylate) (PMMA) can be irreversibly adsorbed on their surface. Here, irreversible adsorption means that the polymer chains cannot be removed by a leaching process, which is assumed in technological transfer processes. However, if polar defects are present on the carbon nanomembranes (CNMs), it may occur that polymers can be irreversibly adsorbed. To address this question, PMMA was spin-coated on top of CNMs, annealed for a specific time at different temperatures, and then tried to be removed by a acetone treatment in a leaching approach. The samples were investigated in detail by atomic force microscopy, X-ray photoelectron spectroscopy, and broadband dielectric spectroscopy, where the latter method has been applied to CNMs for the first time. Unambiguously, it was shown that PMMA can be adsorbed on the surface of CNMs after annealing the sample above the glasstransition temperature of PMMA. The general occurrence of polar defects on the surface of CNMs and the adsorption of polymers open opportunities for advanced innovative hybrid materials combining the properties of the CNM with those of the polymer.
Poly (ether ether ketone) (PEEK) has a high continuous service temperature, excellent mechanical properties, and good solvent and abrasion resistance, which can be further improved through the addition of carbon nanotubes (CNTs). CNT-PEEK nanocomposites are promising matrices for continuous carbon fibre composites; powder processing can mitigate the high melt viscosities in these systems. In this study, model single fibre (hierarchical) composites were produced by embedding sized and desized carbon fibres in nanocomposite CNTPEEK powders followed by single fibre pull-out tests to assess interfacial characteristics. Carbon fibre-PEEK interfacial shear strength is typically 40–45 MPa. Increasing CNT loadings increased fibre-matrix interfacial shear strength linearly up to ~70 MPa at 5.0 wt%, which was attributed to the CNT-based mechanical modification of the PEEK matrix. Apparent interfacial shear strength was inversely correlated with the embedded fibre length irrespective of carbon fibre sizing or CNT loading, indicating brittle fracture of the fibre-matrix interface.
Pulled out carbon fibres were still coated with the matrix, which indicated strong adhesion at the interface in all samples, likely related to a transcrystalline region. Adhesion was, however, negatively affected by the presence of epoxy sizings. Frictional shear strength was independent of embedded fibre length and CNT content for all samples.
The fabrication of nanostructures with ever-decreasing sizes has increased the demand of suitable characterization methods which allow to determine their shape and size at the true nanoscale, and similarly important, enable the investigation of their optical properties beyond the diffraction limit. Due to its high spectral and spatial resolution down to the (sub-) nanometer range, electron beam-based techniques, namely cathodoluminescence (CL) has become a powerful characterization tool, particularly to study plasmonic and dielectric nanostructures. However, the interpretation of the resulting spectral CL maps is not always unambiguously straightforward.
In this work, Mie resonances in single Si nanospheres of different sizes have been systematically studied, using experimental CL spectroscopy and an analytical CL model. For smaller spheres (r ~ 75 nm), the eigenmodes can be unequivocally identified, with relative changes in intensity of the electric and magnetic dipole depending on the electron beam position within the sphere. However, in larger spheres (r ~ 105 nm), the modal assignment becomes increasingly difficult due to a larger number of Mie modes in the visible spectral range. Additionally, penetrating electron beams generate two radiating dipoles at the two Si interfaces – due to the electron and its image charge collapsing at those interfaces – which can, depending on the electron beam’s velocity and its path length inside the particle, produce distinct resonances or dips (constructive or destructive interference of those two radiative dipoles). It is demonstrated that superimposed on the eigenmodes of the studied nanospheres, these resonances can distort the recorded spectrum and lead to potentially erroneous assignment of modal characters to the spectral features. An intuitive analogy is developed to unambiguously distinguish those resonance induced by transition radiation from the nanoparticle-specific Mie resonances.