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Eingeladener Vortrag
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Quantifizierung der Schädigung von DNA in wässriger Lösung unter direkter Elektronenbestrahlung
(2018)
To cure cancer radiation therapy is used to kill tumor cells.
It is based on radiation induced damage to biomolecules.
Especially DNA damage is of key interest due to its central role in apoptosis and mutation.
Because of the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the inelastic scattering of ionizing radiation and water.
A detailed understanding of the underlying molecular processes under physiological conditions is the prerequisite to develop more efficient therapies.
Goal of this work is to quantify the DNA damage caused by ionizing radiation in dependence of the inelastic scattering events and the energy deposit within the microscopic target volume of biological relevance.
The irradiations have to be performed in liquid, under consideration of the chemical environment.
Therefore, a new combination of experiment and Monte-Carlo simulations was developed and tested.
To make it possible to irradiate liquids with electrons within scanning electron microscopes a new sample holder was constructed incorporating an electron transparent nanomembrane.
It makes it possible to irradiate DNA, proteins or cells at different pH, salinity and in the presence of cosolutes.
%The most important results of this work are as follows:
The median lethal dose for a model system of plasmid DNA and water was determined by the combination of experimental data, particle scattering simulations (Geant4-DNA) and diffusion calculations as D0.5=(1.7+-0.3) Gy.
From the convolution of plasmid positions and the spatially resolved energy deposit, as determined by electron scattering simulations, the histogram of the energy deposit within the target volume of the plasmids and the microscopic median lethal energy deposit was calculated as E0.5=6+-4eV.
It could be deduced that on average less than two ionization events are sufficient to cause a single-strand-break.
The relation of single-strand-breaks (SSB) to double-strand-breaks (DSB), which is of importance for microdosimetric modeling, was determined as SSB:DSB = 12:1.
The presented method for the determination of microscopic dose-damage relations was further extended to be applicable for general irradiation experiments.
It becomes independent of the type of primary radiation used, the experimental geometry, and the diffusional properties of the molecules under investigation.
This way different experimental systems with varying, inhomogeneous energy deposit characteristics become comparable with each other, which is not possible when only macroscopic averaged values are taken into account.
In addition, the radiation protection properties of the compatible solute ectoine, as well as its influence on the water properties and biomolecules were investigated.
%In addition, the influence of the compatible solute ectoine on water, biomolecules and its radiation protection properties were investigated.
Raman spectroscopy revealed a concentration dependent increase of the collective water modes in the OH-stretching region, which was found to be independent of the sodium chloride concentration.
Molecular dynamic simulations showed that the zwitterionic properties of ectoine lead to its half-chair conformation.
The hydrogen bonds in the first hydration shell are more stable and have an increased lifetime compared to the bulk water.
Irradiation experiments with DNA in the presence of 1M ectoine revealed an increase of the survival rate by a factor of 1.41 as compared to the absence of ectoine.
The protective properties of ectoine result from the increase of the inelastic scattering probabilities of low energy electrons at the acoustic vibrational modes of water and its properties as OH-radical scavenger.
This was shown by Raman spectroscopy and electron paramagnetic resonance measurements (EPR).
Meso-Lactide was polymerized in bulk at 60, 80, and 100 °C by means of three different types of catalysts: dibutyltinsulfides (2,2-dibutyl-2-stanna-1,3-dithiolane and 2,20-dibutyl-2-stanna-1,3-dithiane), dibutyltin derivatives of substituted cate-chols (BuCa, CyCa, and BzCa), and dibutyltin derivatives of2,2 dihydroxybiphenyl (SnBi) and 2,2-dihydroxy-1,10-binaphthyl(SnNa. Only the latter two catalysts were active at 60 °C. The architecture of the resulting polylactides depends very much on the structure of the catalyst and on the temperature. At the lowest temperature (60 °C), SnBi and SnNa mainly yielded even-numbered linear chains, but SnNa also yielded even-numbered cycles at 100 °C and short reaction times. In contrast,BuCa, CyCa, and BzCa mainly yielded odd-numbered cycles, although the same catalysts yielded even-numbered linear chains when benzylalcohol was added.
An artificial digestion of silver nitrate is reported. It is shown that AgSCN nanoparticles emerge from ionic silver in saliva and remain present during the entire digestion process. The particles were characterized by infrared spectroscopy and small- and wide-angle X-ray scattering (SAXS/WAXS) regarding their composition and size distribution.
We found cascade IR generation in Al laser induced plasma. This generation includes doublet transitions 3s25s 2S1∕2→ 3s24p 2P1∕2,3∕2 → 3s24s 2S1∕2; corresponding to strong lines at 2110 and 2117 nm, and much weaker lines at 1312–1315 nm. The 3s25s2S 1∕2 starting IR generation level is directly pumped from the 3s23p 2P3∕2 ground level. The starting level for UV generation at 396.2 nm (transitions 3s24s 2S1∕2 → 4p 2P3∕2) is populated due to the fast collisional processes in the plasma plume. These differences led to different time and special dependences on the lasing in the IR and UV spectral range within the aluminum laser induced plasma.
Bei der Fertigung dickwandiger Bauteile durch Schweißverfahren mit großen Abschmelzleistungen kommt es zu einer Wasserstoffversprödung. Diese ist abhängig von den Grundwerkstoff-Zusatzwerkstoff-Kombinationen, welche zu unterschiedlichen Ausscheidungen führen und das Diffusions- und Trappingverhalten des Wasserstoffes im Gefüge beeinflussen. Die metallurgischen Einflüsse sind bisher unbekannt. Es werden Empfehlungen zur Wärmeführung beim Schweißen abgeleitet. Hierzu ist es notwendig, die metallurgie- und mikrostrukturspezifische Wasserstoffdiffusion und -freisetzungstemperatur zu bestimmen. Die Konzepte zur Vermeidung der Kaltrissanfälligkeit werden an UP/MSG-Bauteilschweißungen entwickelt. Ziel ist die Identifikation von metallurgisch günstigen GW-Zusatz-Kombinationen zur a-priori Vermeidung zeitverzögerter wasserstoffunterstützter Kaltrissbildung geschweißter Komponenten aus modernen Stählen.
A three-dimensional multi-physics numerical model was developed for the calculation of an appropriate equivalent volumetric heat source and the prediction of the transient thermal cycle during and after fusion welding. Thus the modelling process was separated into two studies. First, the stationary process simulation of full-penetration keyhole laser beam welding of a 15 mm low-alloyed steel thick plate in flat position at a welding speed of 2 m/min and a laser power of 18 kW was performed. A fixed keyhole with a right circular cone shape was used to consider the energy absorbed by the workpiece and to calibrate the model. In the calculation of the weld pool geometry and the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature were taken into account. The obtained local temperature field was then used in a subsequent study as an equivalent heat source for the computation of the transient thermal field during the laser welding process and the cooling stage of the part. The system of partial differential equations, describing the stationary heat transfer and the fluid dynamics, were strongly coupled and solved with the commercial finite element software COMSOL Multiphysics 5.0. The energy input in the transient heat transfer simulation was realised by prescription of the nodes temperature. The prescribed nodes reproduced the calculated local temperature field defining the equivalent volumetric heat source. Their translational motion through the part was modelled by a moving mesh approach. An additional remeshing condition and helper lines were used to avoid highly distorted elements. The positions of the elements of the polygonal mesh were calculated with the Laplace’s smoothing approach. Good correlation between the numerically calculated and the experimentally observed weld bead shapes and transient temperature distributions was found.
In an increasing number of modern steel applications, high-strength structural steel grades are demanded to meet specifications regarding a high load-bearing capacity and a low operating weight. Lightweight design rules enhance the safety requirements, especially for welded joints. Besides a higher cracking risk for high-strength steel welds, the formation of tensile residual stresses might lead to fracture due to overloading or premature failure if not adequately considered. In this study, a stress-strain analysis was conducted at component-related structures from S960QL using digital image correlation while preheating, welding and cooling adjacent to the weld seam. X-ray diffraction analysis of the local residual stresses in the weld seam showed a good comparability with global analyses using either a DIC system or a special testing facility, which allowed in situ measurements of welding loads. By analysing two different seam geometries, it could be shown that lower multi-axial stresses arise if a narrower weld groove is used. Comparative analyses revealed a direct correlation of the local residual stresses in the weld with transverse shrinkage restraint, whereas the residual stress level in the HAZ is significantly affected by the bending restraint of the weld construction and the occurring bending stresses, respectively.
In this article the question of the certification of calibration samples for the characterisation of advanced thin film materials is addressed within the framework of reliable process control or quality management purposes. Reference measurement techniques can be used in order to address the gap in appropriate certified reference materials (CRMs) for thin film analyses. They allow for qualifying out-of-production samples originating from an operating production line as calibration samples. As a template for this procedure, CIGS [Cu(In,Ga)Se2] layers, that are absorber layers for high efficiency thin-film solar cells, have been used for establishing and validating reference-free X-ray fluorescence (XRF) analysis and Auger-electron spectroscopy (AES) as reference measurement techniques. The focus was on determining the average mole fractions in the CIGS layers obtaining results traceable to the SI unit system. Reference-free XRF is physically traceable and is based upon radiometrically calibrated instrumentation and knowledge of atomic fundamental data. Sputter-assisted AES can be established as a chemically traceable method after careful calibration using a certified reference material (CRM) based on a total number counting method.
For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and – 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process.
The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures.
Dynamics and ionic conductivity of ionic liquid crystals forming a hexagonal columnar mesophase
(2018)
For the first time, the molecular mobility of two linear-shaped tetramethylated guanidinium triflate ionic liquid crystals (ILCs) having different length of alkyl chains were investigated by a combination of broadband dielectric spectroscopy (BDS) and specific heat spectroscopy (SHS). By self-assembly, these ILCs can form a hexagonal ordered mesophase besides plastic crystalline phases and the isotropic state. Three dielectric active processes were found by BDS for both samples. At low temperatures, a γ-process in the plastic crystalline state is observed which is assigned to localized fluctuations of methyl groups including nitrogen atoms in the guanidinium head. At higher temperatures but still in the plastic crystalline state, an α1-process takes place. An α2 process was detected by SHS but with a completely different temperature dependence of the relaxation times than that of the α1-relaxation. This result is discussed in detail, and different molecular assignments of the processes are suggested. At even higher temperatures, electrical conductivity is detected and an increase in the DC conductivity by four orders of magnitude at the phase transition from the plastic crystalline to the hexagonal columnar mesophase is found. This result is traced to a change in the charge transport mechanism from a delocalized electron hopping in the stacked aromatic systems (in the plastic phase) to one dominated by an ionic conduction in the quasi-1D ion channels formed along the supermolecular columns in the ILCs hexagonal mesophases.
Beim Schweißen höherfester Stähle mit LTT-Zusatzwerkstoffen im Wurzelbereich der Schweißverbindung wird eine Erhöhung der Kaltrisssicherheit durch die Erzeugung von Druckeigenspannungen erreicht.
Es sind mechanische Gütewerte und Eigenspannungen in Abhängigkeit der Randbedingungen, insbesondere der Wärmeführung und des Nahtaufbaus im Wurzelbereich, systematisch zu ermitteln. Durch das Ableiten von Verarbeitungsempfehlungen wird eine sichere und optimale Handhabung der LTT-Zusätze ermöglicht.
Ziel ist die Entwicklung eines Maßnahmenkatalogs für die schweißtechnische Verarbeitung von LTT-Zusatzwerkstoffen zur Kaltrissvermeidung im Wurzelbereich höherfester Schweißverbindungen speziell für den Offshore-Bereich.
The in situ analysis of the damage evolution in a metal Matrix composite (MMC) using synchrotron X-ray refraction radiography (SXRR) is presented. The investigated material is an Al alloy (6061)/10 vol% Al2O3 MMC after T6 heat treatment.
In an interrupted tensile test the gauge section of dog bone-shaped specimens is imaged in different states of tensile loading. On the basis of the SXRR images, the relative change of the specific surface (proportional to the amount of damage) in the course of tensile loading was analyzed. It could be shown that the damage can be detected by SXRR already at a stage of tensile loading, in which no Observation of damage is possible with radiographic absorption-based imaging methods.
Moreover, the quantitative analysis of the SXRR images reveals that the amount of damage increases homogeneously by an average of 25% with respect to the Initial state. To corroborate the experimental findings, the damage distribution was imaged in 3D after the final tensile loading by synchrotron X-ray refraction computed tomography (SXRCT) and absorption-based synchrotron X-ray computed tomography (SXCT). It could be evidenced that defects and damages cause pronounced indications in the SXRCT images.
Virologists. You might know a couple of them, but unless you are a virologist yourself, the probability that you have collaborated with one in the past is low. The community is relatively small, but they pack a heavy punch and are expected to play a leading role in the research into pathogens that lies ahead. You may ask why we think virologists are our future. Suffice it to say that it is not just because they have invented technologies that belong to the space age, including use of viruses as vehicles to shuttle genes into cells[1], organic nanoparticles with specific tools attached to their surfaces to get inside target cells[2], and using genetically modified viruses as therapies to fight against cancer[3]. Did you know that virologists currently only know of about 3,200 viral species but that more than 320,000 mammal-associated viruses[4] are thought to await discovery? Just think about the viruses hidden in the Arctic ice[5] or in the insects and other animals from once cut-off regions in the world, which now face ever-increasing human exposure[6]. But a heroic (as well as an apocalyptic) role for virologists may also be on the horizon, as the adoption of phage therapy may, in the future, be used to control harmful bacteria when antibiotics fail
Beim Bau einer Salzgrotte für eine Wellnesslandschaft im Keller eines Wohnhauses kam es zu einer folgenschweren Explosion: Die bei der Verwendung des Bauschaums freigesetzten Gase und Dämpfe sammelten sich im Keller und entzündeten sich schließlich. Durch die Explosion starben zwei Arbeiter, ein weiterer Arbeiter sowie die Käuferin der Salzgrotte erlitten massive Verbrennungen.
Dieser Aufsatz stellt das Gerichtsurteil gegen die Geschäftsführer der ausführenden GmbH vor, bereitet die wesentlichen Aussagen zu Gefährdungsbeurteilung, Schutzmaßnahmen, Betriebsanweisung, Unterweisung und Aufsichtsführung auf, erläutert sie und ergänzt Bezüge zur heute einschlägigen Gefahrstoffverordnung (GefStoffV).
Analytical flaw assessment
(2018)
The paper provides a review on analytical flaw assessment methods with the focus on fracture under monotonic loading and fatigue crack propagation. The first topic comprises linear elastic as well as elastic-plastic fracture mechanics approaches. It essentially follows their historical development. Topics which are separately discussed are reference/Limit loads, the treatment of secondary stresses, strength mismatch, constraint, unstable crack propagation (monotonic R-curve analyses) and statistical aspects. With respect to fatigue crack propagation the analytical treatment of crack closure and constraint and the Determination of the cyclic elastic-plastic crack driving force is discussed. Finally, cyclic Rcurve analyses are briefly addressed.
Im Bauwesen werden häufig Polymerbeschichtungen auf Beton eingesetzt um zum einen ein bestimmtes Aussehen zu schaffen und zum anderen das Bauteil vor Alterung, Verschleiß und Schädigung zu schützen. Für die Erfüllung aller genannten Ziele ist das Erreichen einer vom Hersteller festgelegten Sollschichtdicke essentiell. Daher wird die Dicke der Beschichtung nach erfolgtem Schichtauftrag überprüft. Für den in diesem Zusammenhang anspruchsvollen mineralischen Untergrund Beton stehen bislang allerdings nur zerstörende Prüfverfahren zur Verfügung. Aus diesem Grund wurden im Rahmen des Projektes IRKUTSK in Kollaboration mit der IBOS GmbH ein auf aktiver Thermografie basierendes Verfahren sowie ein Gerät für den vor-Ort-Einsatz entwickelt, mit dessen Hilfe eine zerstörungsfreie Schichtdickenbestimmung möglich ist.
Das Poster erläutert das Messverfahren und die Umsetzung in der Praxis. Es werden Messergebnisse sowie der Vergleich mit zerstörend ermittelten Schichtdicken gezeigt. Hierbei konnte eine sehr gute Übereinstimmung nachgewiesen werden. Die notwendigen Erweiterungen des zugrundeliegenden Modells in Bezug auf die einzelnen Parameter werden erläutert und diskutiert.
Die hier vorgestellte Arbeit ist Teil des ZIM-Projektes IRKUTSK mit dem Förderkennzeichen KF2201089AT4 und ist gefördert durch das Bundesministerium für Wirtschaft und Energie aufgrund eines Beschlusses des Deutschen Bundestages.
ZfPStatik bezeichnet die Verwendung von statistisch bewerteten Messergebnissen, die mit zerstörungsfreien Prüfverfahren im Bauwesen (ZfPBau) gewonnen werden und in statischen Berechnungen zum Nachweis der Tragfähigkeit verwendet werden. Dazu ist die Ermittlung der Messunsicherheit der Versuchsdaten auf der Basis des GUM (Guide to the Expression of Uncertainty in Measurement) der erste Schritt. Der statische Nachweis erfolgt durch Grenzzustandsgleichungen, die im Bauwesen angewandt werden. Diese müssen modifiziert werden, so dass jede Messgröße als Zufallsvariable in der Grenzzustandsgleichung vorhanden ist. Der statische Nachweis erfolgt mit probabilistischen Berechnungsmethoden aus der Zuverlässigkeitstheorie. Diese Vorgehensweise wird exemplarisch für den Standsicherheitsnachweis eines Plattenbalkenquerschnitts einer Stahlbetonbrücke auf Biegung angewandt. Auf die möglichen Schlussfolgerungen aus den probabilistischen Berechnungen wird abschließend kurz eingegangen.
Steigende Anforderungen an Brückenbauwerke in Deutschland gehen mit der Alterung und dem sich zunehmend verschlechternden Zustand bestehender Bausubstanz einher. In der aktuellen Entwicklung wurde die Notwendigkeit von Nachrechnungen der Standsicherheit erkannt. Die Zuverlässigkeitstheorie bietet für das Bauwesen geeignete probabilistische Methoden zur Beurteilung von Tragwerken auf Basis der tatsächlichen Bauwerkseigenschaften.
Die Verfahren der zerstörungsfreien Prüfung im Bauwesen ermöglichen die Messung quantitativer Kenngrößen, die den Zustand eines Bestandsbauwerks realitätsnah widerspiegeln. Um die Objektivität einer Messung zu wahren, wurden Methoden zur Gütebewertung von Messergebnissen zerstörungsfreier Prüfverfahren entwickelt und das Konzept der Validierung eingeführt. Damit sind die Voraussetzungen geschaffen, um statistisch abgesicherte und statisch relevante Informationen über die innere Konstruktion eines Tragwerks (ohne signifikante Zerstörung des Bauwerks) zu erheben.
Der vorliegende Beitrag fasst die Beantwortung grundlegender Fragestellungen zusammen, um den Lückenschluss zwischen der statischen Nachrechnung von Brücken und der zerstörungsfreien Prüfung im Bauwesen herzustellen. Das Ziel ist die Verwendung von Messdaten der zerstörungsfreien Prüfverfahren als stochastische Eingangsgrößen in statischen Berechnungen. (...)
The aim of the study presented in this paper is to highlight the potential of niobium carbide cutting tool inserts for machining and to compare their performance to commercially available tungsten carbide inserts. In this work, a comparison between a conventional Wc-Co insert and NbC-Co inserts was carried out under hard machining conditions on specimens made of 100Cr6 bearing steel grade (SAE 52100).
Full densification of Fe, Co and Ni bonded NbC based cermet’s was achieved by pressure less liquid phase sintering in vacuum for one hour at 1420°C. The hardness and toughness of the NbC matrix cermet’s can be mainly tailored by the binder composition and secondary carbide additions. Ni binder based NbC cermet’s allow the combination of high hardness and improved toughness. The addition of lesser amounts of VC/Cr3C2 in a NbC partially substituted WC-Co cemented carbide increased significantly the hardness in combination with a moderate fracture toughness.
The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks as a sign for genotoxicity3. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays.
Heizöllagerbehälter aus Kunststoffen (z.B. Polyethylen) sind für einen sicheren Betrieb von 30 Jahren, dem Zeitraum der Produkthaftung, ausgelegt. Die Tankhersteller empfehlen zur Gewährleistung der Sicherheit nach Ablauf von 30 Jahren den Ersatz dieser Behälter. Kunststoffe unterliegen im Laufe ihrer Nutzungsdauer der Alterung durch die Veränderung ihrer Eigenschaften. Das Ausmaß der Alterung und die Art des Abbauvorganges hängen im Wesentlichen vom chemischen Abbau des Kunststoffes, der Wanddicke des Behälters und den Umgebungsbedingungen ab. Aufgrund der Komplexität der Alterungsvorgänge sind Aussagen zum Langzeitverhalten bzw. zur Lebensdauer der Heizöllagerbehälter ohne geeignete Langzeitprüfungen problematisch. Bisher liegen keine Untersuchungen zum Langzeitverhalten der Kunststoffe vor, insbesondere nach einer Nutzungsdauer über 20 Jahre. In der BDH-Broschüre: Effiziente Systeme und erneuerbare Energien wird darauf hingewiesen, dass ca. 45 % der Heizöllagerbehälter aus Kunststoffen in Deutschland 26 Jahre und älter sind. Viele dieser Tankanlagen sind zudem noch nie von einem Sachverständigen überprüft worden. Schätzungen gehen davon aus, dass mehr als 10.000.000 Tankanlagen aus Kunststoffen in Deutschland vor 1987 errichtet wurden.
Ziel der Untersuchungen ist, den Schädigungsgrad der Kunststoffe im Vergleich zu den unbelasteten Werkstoffen zu ermitteln. Da die BAM bis Ende der 80-iger Jahre für die Zulassung dieser Behälter zuständig war, sind die Daten über den eingesetzten Werkstoff für den Vergleich noch vorhanden. Der Bundesverband Lagerbehälter e.V. und das Institut für Wärme und Oeltechnik (IWO) befürworten diese Untersuchungen, um eine Überalterung der Tankanlagen zu vermeiden. Diese Überalterung könnte die zukünftige Gefahr für die Heizöltankanlage sein, nicht der Wettbewerb mit anderen Energieformen.
A frequently studied environmental contaminant is the active substance diclofenac, which is removed insufficiently in sewage treatment plants. Since its inclusion in the watch list of the EU Water Framework Directive, the concentrations in surface waters will be determined throughout Europe. For this, still, more precise analytical methods are needed. As a reference, HPLC-MS is frequently employed. One of the major metabolites is 4’-hydroxydiclofenac (4’-OH-DCF). Also, diclofenac lactam is important for assessing degradation and transformation. Aceclofenac (ACF), the glycolic acid ester of diclofenac is used as a drug, too, and could potentially be cleaved to yield diclofenac again. In various sewage treatment plant influent samples, diclofenac, 4’-OH-DCF, DCF lactam and ACF could be determined with detection limits of 3 µg/L, 0.2 µg/L, 0.17 µg/L and 10 ng/L, respectively.
The possibility to produce dense monolithic ceramic parts with additive manufacturing is at the moment restricted to small parts with low wall thickness. Up to now, the additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
PTFE/PS core-shell-nanoparticles were characterised by STXM, T-SEM, and ToF-SIMS. Shell-thicknesses were calculated and compared. Preliminary results from ToF-SIMS showed the capabilities of this method.
Parameter study for CFD in the bottle – grid resolution plays an important role on the temperature at the specific positions, 2D axi-symetrical calculation is a sufficient solution strategy in regards to the examined particular Problem. The intensity of filling process can be controlled by pressure “User defined function” provided by experiments. Numerical simulation demonstrated feasibility to predict temperature progress during the filling process successfully validated by experiments. The turbulent model k-w SST is the best strategy for the turbulent property calculations. The most intensive turbulent kinetic energy appeared in the middle region of the pressure bottle, the impact of the eddy viscosity on the wall was mostly in the wall region.
Zukünftig werden vermehrt P-Recyclate auf den Düngemittelmarkt kommen. Diese müssen ausreichend charakterisiert werden, um Sicherheit und Wirksamkeit beurteilen zu können. Mit dem Vortrag wurde der wissenschaftliche Beirat für Düngungsfragen des Bundesministeriums für Ernährung und Landwirtschaft beraten.
Influence of support configurations on the characteristics of selective laser-melted Inconel 718
(2018)
Samples fabricated using two different support configurations by following identical scan strategies during selective laser melting of superalloy Inconel 718 were characterized in this study. Characterization methods included optical microscopy, electron back-scattered diffraction and x-ray diffraction residual stress measurement. For the scan strategy considered, microstructure and residual stress development in the samples were influenced by the support structures. However, crystallographic texture intensity and the texture components formed within the core part of the samples were almost independent of the support. The formation of finer grains closer to the support as well as within the columnar grain boundaries resulted in randomization and texture intensity reduction by nearly half for the sample built on a lattice support. Heat transfer rates dictated by the support configurations in addition to the scan strategy influenced the microstructure and residual stress development in selective laser-melted Inconel 718 samples.
Assessment of quality management for transport packages not requiring authority design approval
(2018)
The majority of transports of radioactive materials are carried out in packages which don’t need a package design approval of a competent authority. Low active radioactive materials are transported in such kind of packages e.g. in the medical and pharmaceutical industry and in the nuclear industry as well.
In Germany the decision to phase out nuclear energy leads to a strong demand for packages to transport low and middle active radioactive waste due to the dismantling and decommissioning of nuclear power plants. According to IAEA regulations the “non-competent authority approved package types” are the excepted packages and the industrial packages of Type IP-1, IP-2 and IP-3 and of Type A.
For the packages of Type IP-2, IP-3 and Type A an assessment by the German competent authority is required for the quality management for the design, manufacture, testing, documentation, use, maintenance and inspection. In general a compliance audit of the manufacturer of the packaging is required during this assessment procedure.
Im Gegensatz zu den zulassungspflichtigen Versandstücken für die gemäß der gefahrgutrechtlichen Regelwerksanforderungen eine behördlich ausgestellte Zulassung erforderlich ist, ist für die prüfpflichtigen Versandstücke lediglich eine behördliche Anerkennung und Überwachung des Managementsystems für die Auslegung, Herstellung, Prüfung, Dokumentation, den Gebrauch, die Wartung und Inspektion erforderlich.
In der Bundesrepublik Deutschland ist gemäß den Festlegungen in der Gefahrgutverordnung Straße, Eisenbahn und Binnenschifffahrt die Bundesanstalt für Materialforschung und -prüfung (BAM) zuständig für die Anerkennung und Überwachung von Managementsystemen.
Research and development of WC grades is 90 years ahead of niobium carbide-based hard materials, which showed already as light-weight and unexplored material a very high potential for many technical applications, especially for wear protection and machining. NbC evoluted recently from lab scale to pilot scale, especially in areas where established WC-based materials are causing economic, environmental or technical concerns. Benchmark trials of NbC-based hard metals indicated already a favorable performance in machining of steel components.
Dynamic characterisation of historic bell-tower using a sensitivity-based technique for model tuning
(2018)
The most relevant results of the vibration-based investigations performed on a historic masonry tower in Italy namely the Santa Maria a Vico bell-tower is here presented. The first part of the study involves preliminary full-scale ambient vibration measurements in operational conditions and dynamics-based finite element (FE) modelling. At first, a manual tuning of the uncertain parameters of the model was carried out to adjust material properties, soil-structure interaction and constraining effect of the neighbouring structures. Then, based on the sensitivity analysis, only the most sensitive parameters were chosen as updating parameters. Finally, a model updating technique based on a sensitivity-based method was used to minimise the error between experimental vibration data and numerical response values. To this aim, a residual vector defined as the weighted difference between the measured quantities and calculated quantities was used. The uncertain structural parameters of the FE model were identified by minimising a robust penalty function. The calibrated model was used as an important tool for the seismic assessment of the structure using pushover analysis. Since the assumed value of the masonry compressive strength is the most sensitive parameter of non-linear behaviour, a sensitivity analysis was performed considering reference values in the range of interest. The seismic safety corresponding to increasing levels of the seismic hazard was finally investigated.
Severe fires at the Friedrichshain flak bunker in May 1945 destroyed or severely damaged an important part of the collection of the Kaiser-Friedrich-Museum, Berlin, today’s Bode Museum. Fragments of two marble sculptures by Tullio Lombardo, sculptor of the Italian renaissance, have survived and are now stored in the Bode Museum. In preparation for restoration, the condition of the sculptures has been documented in detail in 2010. The study revealed that the fragments are not stable enough to exhibit them in a horizontal nor in an upright position. The intention of a further study in 2012 was to find a correlation between ultrasonic velocity and mechanical properties of burned Carrara marble as a basis for stabilization measures. The results and numerous supplementary experiments show that the current condition of the sculptural fragments can not only be explained by the exposure to fire.
Sand erosion of solar glass: Specific energy uptake, total transmittance, and module efficiency
(2018)
Surface roughness, R Z , normal transmittance, Τ N , total transmittance, Τ T , and photovoltaic (PV) module efficiency, η S , were measured for commercial solar glass plates and PV test modules identically sandblasted with different loads of quartz sand (200 – 400 μ m), impact inclination angles, and sand particle speed. Measured data are presented versus the specific energy uptake during sand blasting, E (J/m2). Cracks, adhering particles, and scratch ‐ like textures probably caused by plastic flow phenomena could be observed after sand blasting. Their characteristic size was much smaller than that of sand particles.
After blasting and subsequent cleaning, the glass surface was still covered with adhering glass particles. These particles, cracks, and scratch ‐ like textures could not be removed by cleaning. For sand blasting with α = 30° inclination angle and E = 30 000 J/m2, normal transmittance, total transmittance, and relative module efficiency decreased by 29%, 2% and ∽ 2%, respectively. This finding indicates that diffusive transmission of light substantially contributes to PV module efficiency and that the module efficiency decrease caused by sand erosion can be better estimated from total than by normal transmittance measurements.
One of the holy grails in chemistry is to reconstruct some of life’s functions within synthetic materials. In this contribution, we demonstrate that “simple” macromolecular architectures such as dendritic amphiphiles, Janus dendrimers, thermoresponsive and hybrid organic-inorganic (co)polymers enable to mimic some of the functions of proteins for biomineralization, natural bactericides, biological membranes or the stimuli-responsive cytoskeleton.
Mixing and curing of geopolymers and related alkali-activated materials without storage and handling of highly alkaline solutions possesses advantages regarding safety and economic viability; one possible approach is to produce these materials from solid silica feedstocks and solid sodium aluminate, and subsequent mixing with water. We present a comparison between geopolymers and geopolymer-zeolite composites synthesized by this route from different silica feedstocks (by-product silica from chlorosilane production, microsilica, rice husk ash) and with different SiO2/Al2O3 ratios, using results from XRD, NMR, SEM, thermal analysis, mechanical and acid resistance testing. The use of rice husk ash favors formation of a fully amorphous geopolymer with high strength. Utilization of the other silica feedstocks leads to formation of geopolymer-zeolite composites, the amount and kind of zeolites depending on the feedstock and the SiO2/Al2O3 ratio. These composites show beneficial dehydration behavior, viz. no distinct dehydration step of thermal strain, with the phase assemblage after heating to 1000 °C controlled by the starting composition. Mortars produced from both, the geopolymers as well as the compo¬sites, exhibit high resistance to sulfuric acid attack, making them promising materials for the construction and the repair of industrial and sewer structures.
From simple molar mass disperse homopolymers over copolymers to functionalized, 3-dimensional structures containing various distributions, the complexity of polymeric materials has become more and more sophisticated in recent years. With applications in medicine, pharmacy, smart materials or for the semiconductor industry the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Instead of a complicated, time consuming and/or expensive 2d-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, here a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization mass spectrometry (ESI) is proposed. We used SEC for the separation because unlike other separation modes the separation in this mode solely should occur due to the hydrodynamic volume with no interference of other interactions. This simplifies the interpretation and the above mentioned heterogeneities should show a slight difference in hydrodynamic volume. ESI mass spectrometry can offer more than an access to mass dependent information like MMD, end group masses or CCD in polymer analysis. The online coupling to SEC allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible or accessible only by time consuming or expensive methods. Because these heterogeneities might vary with the molar mass, analysis of the whole MMD-Peak (here the total ion current (TIC)) would not lead to the desired information. The broadening of the chromatographic peaks in this case does not origin from the already well known band broadening factors in chromatography from diffusion. This band broadening is attributed to the nature and composition of the analyte itself. Surprisingly there is very little investigation into the peak width or peak shape due to analyte structure itself found in literature. It is also shown, that with proper calibration even quantitative information could be obtained. This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples we demonstrate the possibilities and limitations of this approach.
Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite
(2018)
Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus.
Development and market introduction of new nanomaterials trigger the need for an adequate risk assessment of such products alongside suitable risk communication measures. Current application of classical and new nanomaterials is analyzed in context of regulatory requirements and standardization for chemicals, food and consumer products. The challenges of nanomaterial characterization as the main bottleneck of risk assessment and regulation are presented. In some areas, e.g., quantification of nanomaterials within complex matrices, the establishment and adaptation of analytical techniques such as laser ablation inductively coupled plasma mass spectrometry and others are potentially suited to meet the requirements. As an example, we here provide an approach for the reliable characterization of human exposure to nanomaterials resulting from food packaging. Furthermore, results of nanomaterial toxicity and ecotoxicity testing are discussed, with concluding key criteria such as solubility and fiber rigidity as important parameters to be considered in material development and regulation. Although an analysis of the public opinion has revealed a distinguished rating depending on the particular field of application, a rather positive perception of nanotechnology could be ascertained for the German public in general. An improvement of material characterization in both toxicological testing as well as end-product control was concluded as being the main obstacle to ensure not only safe use of materials, but also wide acceptance of this and any novel technology in the general public.
Pollution through emission of toxic gases is an increasing problem for the environment. It affects similarly agricultural, industrial and urban areas. In future, environmental emissions in ambient air must be monitored at even lower concentrations as nowadays. One environmental relevant compound is ammonia and its conversion product ammonium that have strong negative impact on human health and ecosystems. Most ammonia measurements in ambient air are performed in the range below 1000 nmol·mol 1 and thus there is a need for reliable traceable ammonia gas standards and in addition in situ analytical procedures for monitoring (in ambient air to avoid that thresholds are exceeded). Therefore, the use of reference materials is necessary for development accompanying test or for calibration, e. g. of structure-integrated sensors and mobile multi-gas sensors.
The developed gas standard generator produces gas mixtures that comply with the metrological traceability for ammonia gas standards in the desired environmentally relevant measurement range. The method is based on the permeation of ammonia through a membrane at constant temperature and pressure. The resulting ammonia penetrant gas flow is then mixed with a carrier gas flow to generate a gas standard flow of known concentration. The dynamic rage is enlarged by using a two dilution steps. Depending on the permeation rate, generable molar fractions are possible in the range nmol·mol-1 to a few µmol·mol-1. We present the design of an ammonia gas standard generator and first results of the characterisation of its individual components supporting the uncertainty assessment according to GUM for stable gas concentrations in this range. The relative uncertainty of the generated ammonia gas standard is smaller than 4 % (k = 2).
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining importance for bioimaging cytometry to answer analytical, biological and biomedical questions. High sensitivity and spatial resolution make it an excellent tool for imaging of metal and heteroelement distribution in single cells. Comparable to CyTOF imaging mass cytometry, metal coded antibodies can be used for multiparametric analysis as well as quantification.
In this project, nanocrystals are investigated as new highly sensitive metal tags for identification and quantification of biomarkers, like Alzheimer’s or breast cancer, in clinical cell assays and tissue samples. Of high significance is the simultaneous analysis of several biomarkers at once, which is possible by special coding of lanthanide tags on the biomarker associated antibody. Nanocrystals show potential for sensitive measurement in MS due to high stability and signal amplification compared to tags with fewer metal atoms. For proof of principle, synthesis and characterization of lanthanide doped nanocrystals was performed by a nanoPET pharma GmbH with great reproducibility and homogenous size. In A549 cell cultures, the uptake and distribution of these nanocrystals within the monolayered cells was investigated by LA-ICP-MS measurements using subcellular resolution. The nanocrystals showed high sensitivity and the possibility of multiparametric analysis by doting different lanthanides. Additionally, stability of the bioconjugation of the nanocrystals and target antibodies was investigated using Dot Blot experiments and LA-ICP-MS.
Solution doping of commercial polymethyl methacrylate (PMMA) polymer optical fibers (POFs) is presented as a novel approach for preparation of custom cladding-doped POFs (CD-POFs). The presented method is based on a solution-mediated diffusion of dopant molecules into the fiber cladding upon soaking of POFs in a methanol-dopant solution. The method was tested on three different commercial POFs using Rhodamine B as a fluorescent dopant. The dynamics of the diffusion process was studied in order to optimize the doping procedure in terms of selection of the most suitable POF, doping time and conditions. Using the optimized procedure, longer segment of fluorescent CD-POF was prepared and its performance was characterized. Fiber’s potential for sensing and illumination applications was demonstrated and discussed. The proposed method represents a simple and cheap way for fabrication of custom, short to medium length CD-POFs with various dopants.