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Highly unrelaxed structural states of metallic glasses have often advantageous mechanical properties. Since metallic glasses continuously relax with time (age) or inherently are well relaxed after processing, methods to uniformly rejuvenate the material are needed. One approach that has received attention is the so-called cryogenic-cycling method, during which a metallic glass is repeatedly immersed into liquid nitrogen. In some cases, cryogenic cycling is truly efficient in increasing the stored excess enthalpy of metallic glasses, but it does not seem to be universally applicable to all alloys and structural states. The origins for these differences remain unclear due to our limited understanding of the underlying structural evolution. In order to shed more light onto the fundamental structural processes of cryogenic cycling, we pursue in-situ x-ray photon correlation spectroscopy (XPCS) to trace the atomic-scale structural dynamics of a Zr-based metallic glass in two different structural states (ribbon and bulk metallic glass). This method allows calculating the relaxation times as a function of time throughout the thermal cycling. It is found that the investigated glasses exhibit heterogeneous structural dynamics at 300 K, which changes to monotonic aging at 78 K. Cryogenic cycling homogenizes the relaxation time distribution for both structural states. This effect is much more pronounced in the ribbon, which is the only structural state that rejuvenates upon cycling. We furthermore reveal how fast atomic-scale dynamics is correlated with long-time average structural relaxation times irrespective of the state, and that the ribbon exhibits unexpected additional fast atomic-scale relaxation in comparison to the plate material. Overall, a picture emerges that points towards heterogeneities in fictive temperature as a requirement for cryogenic energy storage.
The hydrogen permeation current increase was noticed for carbon steel in 0.5 mol/L NaCl solution under strong anodic potentials, which is contrary to the common understanding. Hydrogen permeation under cathodic potentials has been widely studied because of possible hydrogen embrittlement failures of high strength steels in seawater, but investigations of anodic polarization on hydrogen permeation are fairly rare, as the hydrogen evolution reaction shall be retarded. To corroborate the observed phenomenon, experiments were conducted using both as-received and vacuum-annealed sheet specimens. It was verified that the observed phenomena originated from the released hydrogen in traps by metal dissolution under anodic polarization.
The feasibility of microbial hydrogen consumption to mitigate the hydrogen embrittlement (HE) under different cathodic potentials was evaluated using the Devanathan-Stachurski electrochemical test and the hydrogen permeation efficiency h. The hydrogen permeation efficiency h in the presence of strain GA-1 was lower than that in sterile medium. The cathodic potential inhibited the adherence of strain GA-1 to AISI 4135 steel surface, thereby reducing the hydrogen consumption of strain GA-1. The adherent GA-1 cells were capable of consuming ‘cathodic hydrogen’ and reducing the proportions of absorbed hydrogen, indicating that it is theoretically possible to control HE by hydrogen-consuming microbes.
Polymers that help tailoring rheological properties during the casting process have become inevitable constituents for all kinds of high-performance concrete technologies. Due to lacking industries, these typically crude-oil based admixtures are not readily available in many parts of the world, which limits the implementation of more sustainable high-performance construction technologies in these regions. Alternative polymers, which often demand for less processing, can be derived from local plant-based resources. The paper provides experimental data of flow tests of cement pastes with polysaccharides from Triumfetta pendrata A. Rich, acacia gum and cassava without and in the presence of polycarboxylate ether superplasticizer. The flow tests are amended by observations of the zeta potentials and the hydrodynamic diameters in the presence of and without calcium ions in the dispersion medium. The results show that in the presence of and without calcium ions all polysaccharides provide negative zeta potentials, yet, they affect flowability and thixotropy in different ways. Cassava starch, acacia gum, and the gum of Triumfetta pendrata A. Rich qualified well for robustness improvement, strong stiffening, and additive manufacturing, respectively. The reason for the different effects can be found in their average sizes and size distribution. Due to the promising results, a flow chart for local value chains is derived on the example of yet unused cassava wastes, which can be converted in parallel.
Non-conventional densely packed concrete mixtures are proposed and evaluated in this paper using engineered recycled mineral admixtures and recycled aggregates obtained from steel slag, quartz mining tailings, and quartzite mining tailings. High fines content sand-concretes containing coarser- and finer-than-cement recycled powders were designed to obtain blends with broader particle-size ranges and improved packing density. As a result, compressive strength up to 99 MPa, cement intensity up to 2.33 kg/m³/MPa, and consumption of recycled material up to 95 vol% were obtained. Compressive strengths up to 66 MPa and cement intensity up to 2.34 kg/m³/MPa were also obtained with the addition of coarse aggregates to such sand-concrete mixtures, with consumption of recycled material up to 96.5%. The results launch new insights on the role of recycled admixtures and aggregates on the mixture design of cement-based composites regarding efficiency improvement and technological performance.
Design : and use of engineered recycled mineral admixtures obtained from industrial and mineral waste are promising strategies to increase the range of materials suitable for use in cement-based composites. In this work, Portland cement-blended pastes containing mineral admixtures designed for improving particle packing were evaluated in the presence of low- and high-charge polycarboxylate-based superplasticizers. The powders were obtained from basic oxygen furnace slag, iron ore tailings, quartz mining tailings, and quartzite mining tailings. The zeta-potentials of the particles were obtained via electrophoretic mobility. The flow properties were evaluated by rheological tests performed in a Couette type rheometer. The hydration kinetics was evaluated by isothermal calorimetry and an adapted method based on the Vicat needle test. The high-charge PCE and the finer mineral admixtures produced more stable blends. Coarser mineral admixtures led to increased flowability and delayed hydration compared to finer ones. Steel slag powders presented the most significant plasticizer effects, but also the largest setting delays and segregation tendency. Quartz-rich superfines reduced the setting delays caused by the superplasticizers. In summary, both superplasticizers were effective in improving flow properties, but the high-charge PCE was effective in preventing segregation in pastes containing mineral admixtures coarser and heavier than cement.
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
Der Einsatz von hochfesten Stählen im Karosseriebereich des Automobilbaus hat während der letzten Jahre stark zugenommen. Hierzu zählen Dual- und Komplexphasenstähle, welche durch Kombination unterschiedlicher Gefügebestandteile auch deren Vorteile kombinieren, sowie TRIP (TRansformation Induced Plasticity) und Mangan-Bor Stähle, welche sehr gute Umformeigenschaften mit hohen Festigkeiten durch Martensitbildung bei der Umformung kombinieren. TWIP (Twinning Induced Plasticity) Stähle erreichen ähnliche Effekte durch forcierte Zwillingsbildung.
Die Ursachen für den Einsatz dieser Stähle liegen in dem Potential dieser Materialien zur Gewichts- und Kostenreduzierung, bei gleichzeitiger Erhöhung der Fahrgastsicherheit. Auf Grund der prinzipiell gegebenen Schweißeignung dieser Stähle, werden die klassischen Fügeverfahren im Karosseriebau wie das kostengünstige und effektive Widerstandspunktschweißen, das Metall-Schutzgas (MSG)-Schweißen oder das Laserschweißen angewendet. Allerdings treten teilweise Herausforderungen, beispielsweise durch Gefügeveränderungen in den Fügestellen auf, die zu ungewollten Aufhärtungen oder Erweichungen führen.
In diesem Projekt wird ein Verfahren entwickelt, mit welchem die lokalen Werkstoffeigenschaften von im Automobilbau typischen Werkstoffen und deren Fügestellen bestimmt werden können. Relevante Kennwerte sind in erster Linie das SpannungsDehnungs-Verhalten der verschiedenen Zonen einer Schweißverbindung; relevante Zonen wiederum sind neben dem Grundwerkstoff die Wärmeeinflusszone und das Schweißgut. Zu diesem Zweck wird das Verfahren der instrumentierten Eindringprüfung für den Einsatz bei hochfesten Stählen weiterentwickelt. Zunächst werden hierzu Zugversuche an einfachen Grundwerkstoffgeometrien durchgeführt. Im Anschluss wird die optische Dehnungsfeldmessung an stark taillierten, geschweißten Zugversuchsproben durchgeführt.
Die Taillierung dient dem Zweck, die WEZ auch mittels WPS über den gesamten Querschnitt der Probe erzeugen zu können, bzw. im Versuch auch Dehnungen in den relevanten Bereichen herbeizuführen.
Das im Projekt angewendete Auswerteverfahren, welches auf nichtlinearen Regressionsmodellen in Form von künstlichen, neuronalen Netzwerken beruht, ermöglicht die Vorhersage des Festigkeitsverhaltens des Werkstoffes anhand der gemessenen Krafteindringwegdaten.
Based on recently published research on leaching control mechanisms in electric arc furnace (EAF) slags, it is assumed that a FeO/SiO2 ratio of around one leads to low leached V and Cr concentrations. This ratio influences the mineral phase composition of the slag toward higher amounts of spinel and a lower solubility of calcium silicate phases by suppressing the formation of magnesiowuestite and highly soluble calcium silicate phases. To evaluate this hypothesis, laboratory and scaled up tests in an EAF pilot plant were performed on slag samples characterized by elevated V and Cr leaching and a high FeO/SiO2 ratio. Prior to the melting experiments, the optimum FeO/SiO2 ratio was calculated via FactSageTM. In the melting experiments, the ratio was adjusted by adding quartz sand, which also decreased the basicity (CaO/SiO2) of the slag. As a reference, remelting experiments without quartz sand addition were conducted and additionally, the influence of the cooling rate of the slag was examined. The remelted (without quartz sand) and the remelted modified slags (with quartz sand) were analyzed chemically and mineralogically and the leaching behavior was investigated. The modification of the slags yielded a minimized release of V and Cr, supporting the hypothesis that the FeO/SiO2 ratio influences the mineralogy and the leaching behavior.
Etalon features in transmittance spectra of films arise due to the coherent superposition of waves caused by reflections multiple times at the inner film boundaries. The fringe maxima occur at i𝜆 = 2nd cos 𝜑 with i - being an integer, 𝜆 - the wavelength, d - the film thickness, 𝜑 - the angle of incidence in respect to the film normal and n - the refractive index of the film. It is obvious that such features can hinder the interpretation of absorption bands when fringe amplitude and period are in the same range as the expected bands.
This poster discusses the suitability of two optical methods for the THz spectral range applied to Fourier Transform Spectroscopy.
Etalon effects in THz transmittance spectra, either taken in time- domain or frequency-domain, often hamper or even hinder the interpretation of film properties. In this paper we discuss the transferability and applicability of spectroscopic methods typically employed in the near and mid infrared spectral range to eliminate the fringes in the transmittance spectra in the THz spectral range.
Mit der zurzeit laufenden Überarbeitung der VDI Richtlinie 3783 Blatt 1 und dem Modellwechsel auf ein Lagrange'sches Partikelmodell ist das Fahnenmodell PLURIS in den Fokus der Störfallauswirkungsberechnungen gelangt. PLURIS wird schon seit Längerem zur Berechnung der Abgasfahnenüberhöhung von Schornsteinen und Kühltürmen eingesetzt und ist Grundlage der neuen VDI Richtlinie 3782 Blatt 3 (Entwurf), lm Gegensatz zu den bekannten Freistrahlmodellen zur Berechnung der Ausbreitung unter Druck stehender Gase, wird bei PLURIS nicht vorausgesetzt, dass die Strahlgeschwindigkeit deutlich größer als die Windgeschwindigkeit ist. Mit steigender Rechnerleistung wird auch die Gasausbreitungsberechnung mittels CFD-Programmen für die Praxis interessanter. Für eine genauere Berechnung der Geschwindigkeits- und Konzentrationsverteilung im Freistrahl wird eine feine Gitterauflösung erforderlich, die aber zu langen Rechenzeiten führt, wenn die Ausbreitung eines toxischen Gases in Entfernungen von mehreren 100 m berechnet werden soll. Durch die Kopplung der CFD-Berechnung mit einem Fahnen- oder Freistrahlmodell kann der Rechenaufwand reduziert werden.
Two types of cements were selected as the reference cement in the priority program 2005 of the German Research Foundation (DFG SPP 2005). A thorough characterization of CEM I 42.5 R has been made in a recent publication. In this paper, the characterization data of the other reference cement CEM III/A 42.5 N are presented from the aspects of chemical and mineralogical compositions as well as physical and chemical properties. The characterization data of the slag, which is the second main constituent of this specific cement besides the clinker, are presented independently. For all data received, the mean values and the corresponding errors were calculated. The data shall be used for the ongoing research within the priority program. Also, researchers from outside this priority program can benefit from these data if the same materials are used.
Supplementary cementitious materials (SCM) can reduce the total amount of Portland cement clinker in concrete production. Rice husk ashes (RHA) can be converted from an agricultural by-product to a high-performance concrete constituent due to a high amount of reactive silica with pozzolanic properties if they are burnt under controlled conditions. The way and duration of combustion, the cooling process as well as the temperature have an effect on the silica form and thus, the chemical and physical performance of the RHA. Various studies on the best combustion technique have been published to investigate the ideal combustion techniques. Yet, the process mostly took place under laboratory conditions. Investigating the difference between the performance of RHA produced in a rural environment and laboratory conditions is useful for the assessment and future enhancement of RHA production, and its application both as building material, for example in rural areas where it is sourced in large quantities, and as additive for high performance concrete. Thus, the paper presents a comparison between RHA produced under rudimentary conditions in a self-made furnace in the rural Bagamoyo, Tanzania and under controlled laboratory conditions at the Technical University of Munich, Germany, with different combustion methods and temperatures. In a second step, RHA was ground to reach particle size distributions comparable to cement. In a third step, cement pastes were prepared with 10%, 20% and 40% of cement replacement, and compared to the performance of plain and fly ash blended cement pastes. The results show that controlled burning conditions around 650 °C lead to high reactivity of silica and, therefore, to good performance as SCM. However, also the RHA burnt under less controlled conditions in the field provided reasonably good properties, if the process took place with proper burning parameters and adequate grinding. The knowledge can be implemented in the field to improve the final RHA performance as SCM in concrete.
Die additive Verarbeitung hochfester Feinkornbaustähle mittels Wire Arc Additive Manufacturing (WAAM) ist ein komplexes, aber zugleich auch effizientes Verfahren, bei dem Werkstoff, Bauteilgeometrie und Schweißprozess gezielt aufeinander abgestimmt sein müssen. Ziel dieser Studie war es, einen Zusammenhang zwischen den Prozessparametern und der generierten Schichtgeometrie zu ermitteln. Dazu wurden definierte Referenzkörper mit einem robotergestützten Schweißsystem additiv gefertigt und hinsichtlich Schichthöhe, Wandstärke und Mikrostruktur analysiert. Fokus der Untersuchung waren sowohl konventionelle als auch für die WAAM-Fertigung speziell entwickelte hochfeste Schweißzusatzwerkstoffe. Die geometrischen Eigenschaften additiv gefertigter Bauteile lassen sich insbesondere durch die Faktoren Drahtvorschubgeschwindigkeit und Schweißgeschwindigkeit gezielt einstellen. Jedoch können diese Parameter nicht beliebig variiert werden, auch aufgrund der rheologischen Eigenschaften der Zusatzwerkstoffe. Zu hohe Streckenenergien führen zu lokalen Überhitzungen und Fehlstellen in der generierten Schicht. Undefinierte Fließ- und Erstarrungsvorgänge im überhitzten Bereich erschweren die maßhaltige Fertigung. Deshalb wird bei speziellen WAAM-Schweißdrähten das Fließverhalten gezielt modifiziert, sodass es über einen größeren Temperaturbereich hinweg konstant ist. Erst die Kenntnis über die komplexen Zusammenhänge zwischen den Prozessparametern und der Bauteilgeometrie ermöglicht die Erzeugung exakter Schichtmodelle für die additive Fertigung. Dies bildet die Grundlage für die Bearbeitung weiterer Fragestellungen auf dem Gebiet der additiven Fertigung mit hochfesten Zusatzwerkstoffen und insbesondere deren Anwendung in modernen hochfesten Bauteilen.
Scaled-down experimental facility: Can reproduce actual failures; can produce simulated data for identifying cracks in the substructure or other defects. The acceleration data can be converted into an equivalent deformation. The experimental facility can analyse dynamic loads. Equivalent force data: Facilitates the application to a health monitoring system; simplifies the development of predictive maintenance. These data is helpful in validating analytical or simulation models.
Die Kenntnis von Materialeigenschaften spielt bei der Entwicklung oder Optimierung von Betonen und Bauweisen für den Straßenbau sowie der Qualitätssicherung eine bedeutende Rolle. Gleichermaßen bilden physikalische Materialkennwerte die Grundlage für die rechnerische Dimensionierung und die Restsubstanzbewertung von Betonfahrbahndecken. Eine relevante Kenngröße bei der Untersuchung thermisch induzierter Spannungs- und Verformungszustände stellt der thermische Ausdehnungskoeffizient dar. Im Zuge der systematischen Weiterentwicklung der rechnerischen Dimensionierung, aber auch im Zusammenhang mit der gezielten Verbesserung der Gebrauchseigenschaften von Betonfahrbahndecken gilt es zu hinterfragen, ob lastunabhängige Formänderungseigenschaften der verwendeten Betone aktuell ausreichend Beachtung finden, ob allgemeine Literaturwerte für die heutigen Fahrbandeckenbetone stets Gültigkeit besitzen und ob deren Implementierung in numerische Modelle zu realitätsnahen Vorhersagen führt. Für eine empirische Herangehensweise ist die Verfügbarkeit adäquater Prüfverfahren von entscheidender Bedeutung. In Deutschland existiert aktuell jedoch kein standardisiertes oder genormtes Verfahren für die prüftechnische Bestimmung des thermischen Ausdehnungskoeffizienten von Beton. Daher wurden unter Beachtung straßenbauspezifischer Gesichtspunkte zwei Prüfansätze entwickelt, die in diesem Beitrag vorgestellt sowie hinsichtlich möglicher Messunsicherheiten und Messungenauigkeiten diskutiert werden. Außerdem werden ausgewählte Ergebnisse aus Analysen an Bestandsbetonen aus dem BAB-Netz dargestellt. Im Ergebnis sollen die Untersuchungen einen Beitrag zur Schaffung der prüftechnischen Voraussetzungen für eine abgesicherte Quantifzierung der thermischen Dehnung von Fahrbahndeckenbetonen leisten.
Das Element Phosphor ist für Pflanzen, Tiere und Menschen essenziell. Um die Phosphorversorgung für Pflanzen in der Landwirtschaft zu gewährleisten, werden Phosphordünger eingesetzt. Die Nährstoffe werden hauptsächlich durch Wirtschaftsdünger (Gülle, Jauche, Stallmist) zurückgeführt. Zusätzlich werden in der konventionellen Landwirtschaft mineralische Phosphordünger eingesetzt, die vorwiegend aus dem fossilen Rohstoff Phosphorit gewonnen werden. Um die Abhängigkeit von fossilen Rohstoffen zu reduzieren, sollen nährstoffhaltige Rest- und Abfallstoffe zur Phosphordünger aufbereitet werden. In Abwasserkläranlagen fällt phosphorreicher Klärschlamm als Abfallstoff an. Der größte Anteil des Klärschlammes wird in Steinkohlekraftwerken, Zementwerken oder in Monoklärschlammverbrennungsanlagen verbrannt. Die Klärschlammaschen aus den Monoverbrennungsanlagen enthalten bis zu 12 Gew.-% Phosphor und sind daher für die Düngerherstellung geeignet.
Ein geeignetes Verfahren zur Aufbereitung der Klärschlammaschen ist die thermochemische Behandlung im Drehrohrofen. Mit dem sogenannten AshDec®-Prozess, kann ein Phosphordünger hergestellt werden. Aktuell wird eine großtechnische Anlage in Altenstadt (Bayern) geplant, die im Jahr 2023 den Betrieb aufnehmen soll. Der zentrale Bestandteil ist die Phasenumwandlung von schlecht pflanzenverfügbaren Phosphaten in der Klärschlammasche (vorwiegend das Calciumphosphat Whitlockit und Aluminiumphosphat) zu gut pflanzenverfügbaren Calciumalkaliphosphaten im Produkt. Um dies zu erzielen, werden die Aschen mit Natrium- und/oder Kalium-Verbindungen gemischt und einer thermochemischen Behandlung bei 800-1000 °C zugeführt. Um die Pflanzenverfügbarkeit und Düngewirkung von Phosphaten abschätzen zu können, ist die chemische Extraktionsmethode mit neutraler Ammoniumcitratlösung geeignet.
In der Dissertation werden die (Phosphor-)Phasenreaktionen und die Prozessbedingungen des thermochemischen Verfahrens untersucht, um das Verfahren gezielt zu modifizieren und die Wirtschaftlichkeit zu steigern. Die Zielphasen der thermochemischen Behandlung sind die Calciumalkaliphosphate CaNaPO4 und CaKPO4, und deren Mischphasen Ca(Na,K)PO4, welche in der Publikation 3.1 synthetisiert wurden. Für diese Calciumalkaliphosphate wurden die thermodynamischen Daten der Standardbildungsenthalpie, Standardentropie, Wärmekapazität und die Wärmemenge der Phasenumwandlung bestimmt (Publikation 3.1).
Bei der thermochemischen Behandlung von Klärschlammaschen wurden als Additive Natrium- und Kaliumsulfat bei verschiedenen Temperaturen getestet. Der Einsatz von Kaliumadditiven ist erwünscht, um den Marktwert des Produktes durch die Produktion eines Phosphor-Kalium-Düngers zu erhöhen. Zusätzlich wird eine möglichst geringe Prozesstemperatur angestrebt, bei der die erwünschten Calciumalkaliphosphate gebildet werden.
In den Publikationen 3.2 und 3.3 wird gezeigt, dass für Klärschlammaschen eine komplette Phasenumwandlung zu Calciumnatriumphosphaten ab 875 °C in Laborversuchen (Korundtiegel) mit dem Additiv Natriumsulfat erzielt werden kann. Der Einsatz von Kaliumsulfat erforderte notwendige Reaktionstemperaturen von über 1100 °C. Diese
unterschiedlichen Reaktionstemperaturen hängen mit den Schmelzpunkten von Natriumsulfat (890 °C) und Kaliumsulfat (1070 °C) zusammen. Um Kaliumsulfat in den Prozess bei niedrigen Temperaturen zu integrieren, wurden Natriumsulfat und Kaliumsulfat vor der Behandlung gemischt. Dies führte zu einer Schmelzpunkterniedrigung und resultierte in Reaktionstemperaturen zwischen 900 °C bis 1000 °C für die untersuchten Mischungen von Natrium- und Kaliumsulfat (Publikation 3.3).
Die Zusammensetzung der Calciumalkaliphosphate Ca(Na,K)PO4 war anders als erwartet. Bei der Phasenanalytik stellte sich heraus, dass bei geringem und mittlerem Anteil von Kaliumsulfat im Alkali-Additiv nur Calciumnatriumphosphate mit sehr geringen Kaliumgehalten gebildet wurden. Erst bei einem hohen Anteil von Kaliumsulfat in der Mischung der Alkalisulfate konnten kaliumhaltige Calciumalkaliphosphate nachgewiesen werden (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4). Dieser geringere Einbau von Kalium in die Calciumalkaliphosphate hängt mit den zusätzlich stattfindenden Reaktionen zwischen den Alkalien und den Silikaten zusammen. Es ist bekannt, dass die zugegebenen Alkalisulfate zuerst mit Silikaten und anschließend mit den Phosphaten reagieren. Silikate bauen bevorzugt Kalium ein, deswegen konnten erst kaliumhaltige Phosphate gebildet werden, wenn die Reaktion mit den Silikaten abgeschlossen war. Dies führte zu einem geringeren Kaliumanteil in den gebildeten Phosphaten im Vergleich zum Kaliumanteil der verwendeten Alkaliadditive. Das in Silikaten gebundene Kalium ist wahrscheinlich schlecht für die Pflanzen verfügbar. Dies könnte den Einsatz der produzierten Phosphor-Kalium-Dünger einschränken. Der bevorzugte Kaliumeinbau in Silikaten konnte auch in Kalkulationen mit den thermodynamischen Daten aus der Publikation 3.1 gezeigt werden.
Mittels Phasenanalytik vor und nach der chemischen Extraktion, konnte die Zugehörigkeit zu verschiedenen Modifikationen der Calciumalkaliphosphaten sicher bestimmt werden und eine ungefähre Zusammensetzung dieser Calciumalkaliphosphate abgeschätzt werden. So konnte nachgewiesen werden, dass die Modifikation vom CaNaPO4 ungefähr 10 % Magnesium einbauen kann. Wenn mehr Magnesium eingebaut wird, bildet sich die Phase (Ca,Mg)NaPO4, die eine vergleichbare Struktur wie die bekannte Phase (Ca0.72Mg0.28)NaPO4 aufweist. Dieses magnesiumreiche Calciumnatriumphosphat entstand vermutlich, wenn entweder erhöhte Anteile an Kalium eingebaut wurden (Ca0.8Mg0.2)(Na0.85K0.15)PO4 (Publikation 3.3) oder die Phasenumwandlung vom Calciumphosphat Whitlockit zum Calciumalkaliphosphat CaNaPO4 noch nicht abgeschlossen war (Publikation 3.2). Wenn mehr Kalium eingebaut wird, dann entsteht eine Phase (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4) ähnlich zu den Mischphasen aus der Publikation 3.1.
In den Publikationen 3.4 und 3.5 wurden keine Klärschlammaschen untersucht, sondern Biokohlen aus Modellklärschlämmen (Publikation 3.5) und Biomasseaschen (Publikation 3.4) aus der Vergasung oder Verbrennung einer Mischung aus Zuckerrohrbagasse und Hühnertrockenkot. Die thermochemischen Produkte der Biokohlen bzw. Biomasseaschen enthielten das gewünschte CaNaPO4 und hatten eine hohe Düngewirkung in Pflanzenwachstumsversuchen mit Sojapflanzen bzw. Gräsern.
In 2019 the Bundesanstalt für Materialforschung und –prüfung (BAM) conducted a benchmarking to compare the operations of European accreditation bodies and to identify best practices, with the aim of improving key processes in accreditation. Ten European accreditation bodies attended the comparison, four of which had already taken part in the pilot phase of the benchmarking project, which was conducted in 2017 by the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) and BAM.
The study, designed to examine and compare the operation of accreditation bodies in Europe, used a management tool called Process Maturity Benchmarking Tool, which was especially elaborated and validated for this purpose in the pilot phase, in order to determine the values of indicators, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits, and others. The second source is derived from the self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturities were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The results of the analysis were presented to and discussed with representatives of the ten accreditation bodies at a Results-Workshop that took place at BAM on 21/22 January 2020.
Sulfate is abundant in the environment and, as a result, sulfate-containing minerals constitute a large and important focus of research. These minerals play an important role in many geochemical and industrial processes, including the sulfur cycle, the construction industry (e.g., plaster of Paris), fault tectonics, acid mine drainage, and even rare biominerals. Important to note are the abundant amounts of sulfate (minerals) located on the surface of Mars, and in meteorites, extending the relevance of this mineral group beyond the realm of our planet. In geological systems, sulfate minerals such as barite are also important for indicating certain sedimentation environments. In this regard, sulfate deposits can be used to evaluate the redox state of ancient oceans during early Earth time periods.
Es wurde im Rahmen dieser Arbeit eine neue Methode der Biokonjugation entwickelt, die es ermöglicht humane Antikörper ortspezifisch mit IgG-bindenden Peptiden zu konjugieren. Als Basis fungierte ein Peptid, welches für den Einsatz gezielt modifiziert wurde. So sollte am C-Terminus ein Biotin eingefügt werden, dass für die spätere Detektion der Biokonjugation genutzt werden kann, während am N-Terminus ein Cross-Linker für die kovalente Bindung zum Antikörper eingefügt wurde. Das Biotin wurde mittels Biotin-Lysin eingebaut. Dies hat den Vorteil, dass die modifizierte Aminosäure direkt in der SPPS genutzt werden kann. Auch der Cross-Linker soll schon während der SPPS in das Peptid integriert werden. Als Cross Linker wurden die zwei heterobifunktionellen Succinimidyl(3-bromoacetamid)propionate und Succinimidyl(4-iodacetyl)aminobenzoat untersucht. Die Aktivierung des Peptides mit dem SBAP-Cross-Linker erfolgte am besten im pH-Bereich zwischen 7,0 und 9,0. Die Modifizierung des Peptides mit dem Iodid-Cross-Linker SIAB unter den gleichen Bedingungen zeigte allerdings keine zufriedenstellenden Ergebnisse. Da das erste Peptid allerdings in den Folgeexperimenten sehr gute Ergebnisse zeigte, musste kein weiterer Linker getestet werden. Zusätzlich zu der Cross-Linker-Wahl sollte der Abstand zwischen dem Cross-Linker und dem Grundgerüst des Peptides auf den Einfluss der Bindung untersucht werden. Dazu wurden drei Kontrollpeptide synthetisiert, die entweder um zwei Aminosäuren zwischen dem ursprünglichen N-Terminus des Peptides und dem SBAP-Linker verlängert wurden, keinen SBAP-Linker beinhalten oder die Verlängerung ohne SBAP-Linker besaßen. Die erfolgreiche Synthese aller vier Peptide wurde mittels MALDI-TOF-MS bestätigt.
Flexible joint transition systems in the form of bituminous joint transitions, type 4.1a according to RTD1007-1, have been used in the Netherlands with varying success. The lifespan in practice was found to vary greatly: between 1 and 5 years. This is too short a lifespan in relation to the lifespan of the layers of asphalt pavement. Ideally, the replacement of these bituminous joint transitions should take place simultaneously as the maintenance of the asphalt layers.
In the meantime, research has been carried out nationally and internationally into improving the life span of bituminous joint transitions. In Germany and Switzerland, the regulations have been shown to lead to a life span of more than 10 years. On this basis, ETAG032-3 was established in the context of EOTA in 2013.
In a competition "Silent sustainable joint transitions" held by the Dutch Directorate-General for Public Works and Water Management in the period 2007-2012, three flexible bituminous joint transitions have already been tested, two of which were ultimately found to be suitable. These have been included in the multi-choice matrix (RTD 1007-1) as concept 4.1b (anchored bituminous joint transition) and 4.1c (unanchored bituminous joint transition with stretch-spreading inlay and poured asphalt edge beams). Monitoring these joint transitions in practice over the past 8 years has shown that the desired life span is achievable with these improved joint transitions.
It is expected that the improvement in life span achieved abroad can also be realised in the Netherlands if several aspects specific to the Netherlands are taken into account:
For large parts of the Dutch main road network, the traffic intensity of 500,000 heavy vehicles per year assumed in the ETAG032-3 is insufficient. This is a factor 4 to 5 higher on the busiest main roads in the Netherlands.
On 90% of the Dutch main road network, in contrast to countries such as Germany and Switzerland, an open layer (ZOAB (zeer open asfaltbeton [very open asphalt concrete])) is used.
In the Netherlands, in contrast to countries such as Germany and Switzerland, bridges and viaducts are made on a large scale of prefabricated beams and 'floating' support systems that consist entirely of rubber supports that can be deformed all-round. Such constructions have a less favourable, high-frequency deformation behaviour under traffic load.
In Germany and Switzerland, a minimum joint mass temperature of -20 °C is assumed to test bituminous joint transitions. For the Netherlands, -15 °C is assumed, which has a favourable effect.
The present second version of RTD 1007-4 is a guideline for the development and realisation of a new generation of more durable flexible joint transitions with a minimum design life of 10-15 years and is a guideline for contractors to demonstrate that a flexible joint transition system meets the requirements as set out in the Directorate-General for Public Works and Water Management guideline RTD 1007-2.
In 2019 over 30 000 people were killed or injured by explosions caused by explosives like TNT, PETN, HMX and RDX. Therefore, highly sensitive assays for the detection of TNT are needed. In this study we compared two commercially available TNT antibodies: A1.1.1 and EW75C with a highly optimized indirect competitive ELISA based on a BSA-TNA conjugate. As a result, a precision profile for both antibodies was determined with a LOD of 170 pmol L-1 for the clone A1.1.1 and a LOD of 3,2 nmol L-1 for the clone EW75C. The measurements showed that the clone A1.1.1 is a highly sensitive antibody for the detection of TNT while the clone EW75C does show medium performance at most.
In the cross-reactivity characterization of both antibodies many substances, closely related to the structure of TNT were tested. Both antibodies showed strong cross reactivity with trinitroaniline and trinitrobenzene. For the clone A1.1.1, which is known to originate from immunization of mice with an TNP-glycine-KLH conjugate, this has to be expected. Interestingly the clone EW75C, which was not characterized yet, showed similar behavior. This suggests a TNA-conjugate as immunogen for the EW75C antibody as well. None of both antibodies showed cross-reactions to the high explosives PETN, HMX and RDX. Also, the cross-reactions of nitro musks with the antibodies were investigated. Despite their prohibition, nitro musks are still used in Asia especially and are particularly popular in India. The overall superior clone A1.1.1 showed a significant cross-reactivity to musk ambrette. For practical reasons the influence of musk ambrette on this assay when used in natural environment should be investigated.
In further experiments, the highly sensitive TNT antibody A1.1.1 was digested with papain to obtain monovalent Fab-fragments. Due to its high stability against the digestion, a custom protocol for the IgG1 subclass of mice, to which the clone A1.1.1 belongs, was developed, resulting in a quantitative digestion of the intact antibody to Fab fragments. The success of the digestion was determined with MALDI-TOF-MS and SDS-PAGE. It was shown that this protocol worked for many different antibodies of IgG1 subclass as well.
Plant tissues are complex composite structures of organic and inorganic components whose function relies on molecular heterogeneity at the nanometer scale. Scattering-type near-field optical microscopy (s-SNOM) in the mid-infrared (IR) region is used here to collect IR nanospectra from both fixed and native plant samples. We compared structures of chemically extracted silica bodies (phytoliths) to silicified and nonsilicified cell walls prepared as a flat block of epoxy-embedded awns of wheat (Triticum turgidum), thin sections of native epidermis cells from sorghum (Sorghum bicolor) comprising silica phytoliths, and isolated cells from awns of oats (Avena sterilis). The correlation of the scanning-probe IR images and the mechanical phase image enables a combined probing of mechanical material properties together with the chemical composition and structure of both the cell walls and the phytolith structures. The data reveal a structural heterogeneity of the different silica bodies in situ, as well as different compositions and crystallinities of cell wall components. In conclusion, IR nanospectroscopy is suggested as an ideal tool for studies of native plant materials of varied origins and preparations and could be applied to other inorganic–organic hybrid materials.
This work presents a spectroscopic study of metallic pigments and metal foils used in reverse glass paintings that were created between 1912 and 1954. Metallic pigments induce a notable sparkling effect by means of the lateral incidence of light, whereas metal foils enhance the gloss and create a glittering effect when the painting is viewed in reflected light. Both effects were desired features especially in modern reverse paintings on glass and applied by artists in manifold creative manner. The paper gives an overview on the composition of the metalfoils and metal pigments in 14 works as determined in situ by X-ray spectrometry. Metal foils made of tin, brass, aluminium and silver were found in nine paintings. Gold imitating Cu-Zn pigments in different hues and with various Cu/Zn net intensity ratios were recorded for six paintings. Silvery pigments were identified mainly as Al pigments, but also as Cu-Zn-Ni alloy in one case. Other uncommon metallic pigments were detected in Arlequin vindicatif (c. 1925) by Floris Jespers, who used not only Cu-Zn and Al pigments, but also brownish Cu and Cu-Zn-Sn pigments. Non-invasive diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) was used to classify the binding media of the metallic pigments. Drying oil and natural resin probably mixed with oil were the most common binding media. A polysaccharide-based binder was found in the silvery Cu-Zn-Ni pigment of Ohne Titel (1954) by Marianne Uhlenhuth.
CHG is very different compared to other graphite degenerations or defects;
Filigree, multi-branched string-like, 3d interconnected structure;
Morphology and volumetric amount of CHG cannot be accessed by stereological interpretation of 2d section data;
Field-tested, technically established method to quantify CHG in components not available;
Fatigue: CHG causes substantial reduction in fatigue limit and significant increase in crack growth rate;
Therefore: Avoid or exclude CHG!
Quasi-static dispersion of dusts for the determination of lower explosion limits of hybrid mixtures
(2020)
Knowledge of explosion limiting concentration of explosible materials is necessary for the design of explosion protection measures. Currently employed methods of testing MEC of a dust cloud or LEL of a hybrid mixture are based on arbitrary assumptions and possess technical limitations that often lead to values of MEC/LEL, which are unrealistically low or poorly reproducible.
This contribution presents an improved method for experimental determination of MEC of a combustible dust cloud or LEL of a flammable gas or hybrid mixture. The new set-up operates under laminar conditions and allows a uniform suspension of dust particles in an open top acrylic glass tube. Dust concentration is measured with the help of infrared sensors installed a few centimeters above and below the ignition source.
In order to evaluate the dependence of MEC on flow front velocity, MEC of lycopodium was determined at four flow velocities. The results show that the flow field intensity does not significantly influence the MEC of lycopodium for the flow ranges tested in this work. Moreover, LEL of hybrid mixtures of lycopodium and methane was also tested at flow velocities of 4.7 cm/s, 5.8 cm/s, 7 cm/s and 11 cm/s and compared with the values obtained from other sources. The results suggest that the requirement of high energy pyrotechnical igniter may be relinquished, provided that a truly homogeneous suspension of dust particles could be achieved.
Moreover, the effect of relative amount of dust and gas, on the course of ignition and flame propagation in hybrid mixtures at their LEL, was studied by the help of high speed videos. For hybrid mixtures of carbonaceous dusts (like lycopodium) at their LEL, ignition occurs in the gas phase, however, flame propagation is only possible through a two-way interaction of dust and gas during the course of combustion.
The efficiency and safety of railway transportation depend both on numerous factors linked to the vehicle, the infrastructure, the operator and the environment. Curved tracks are subjected to demanding situations due to elevated stress levels, as a function of the operating conditions and vehicle/infrastructure design. In such segments, steering forces are superimposed to lateral load transfers. The steering forces depend on the condition and the design of the centre plate and bogies’ suspensions design. While the friction at the centre plate provides the needed damping to mitigate the hunting vibration of the bogie in straight track segments, such yaw resistance originates high steering forces and rail damage on curved tracks. A centre plate with low friction at turns and high friction at straight track segments would thus be highly advantageous. In this paper, a centre plate design is proposed which provides a yaw-rotation resistance torque that depends on the bogie-car relative position. Two different designs are considered for that purpose, one that combines a spring-acted centring mechanism with a lower pair kinematics, while the other one involves higher kinematic pairs which should incorporate lateral damping elements. As a result of using an engineering design approach, the higher kinematic pairs-based design is recommended however, the validation of such operational principles, including the introduction of the needed damping, should be configured on the basis of experimental models.
High-entropy alloys containing up to 6 platinum group metals can be prepared by thermal decomposition of single-source precursors non requiring high temperature. We prepare the first example of a single-phase hexagonal high-entropy alloy. Heat treat- ment up to 1500 K and compression up to 45 GPa do not result in phase changes, a record temperature and pres- sure stability for a single-phase high-entropy alloy. The alloys show pronounced electrocatalytic activity in methanol oxidation, which opens a route for the use of high-entropy alloys as materials for sustainable energy conversion.
With the advent of widely accessible and cost-effective next-generation sequencing technologies, it has become increasingly feasible to study insect immunity on a deep genomic or transcriptomic level. Here we introduce a protocol that is aimed at exploiting transcriptomic data to study immunity in non-model insect organisms. We provide instructions for an entire workflow, starting with successfiil extraction of insect RNA through to bioinformatic guidelines for the effective analysis of mRNA sequencing data. The RNA extraction procedure is based on TRIzol Reagent and a spin-column clean-up Step. The bioinformatic pipeline is intended to help users identify immune genes from de novo transcriptome data and includes guidelines for conducting differential gene expression analyses on transcriptomic data. The immune gene prediction method is based on inferring protein homologs with HMMERand Blastp and talces Advantage ofthe ImmunoDB database, which is a valuable resource for research on insect immune-related genes and gene families. The differential gene expression analysis procedure utilizes the DESeq2 package as implemented in R. We hope this protocol will serve as a usefi.il resource for researchers aiming to study immunity in non-model insect species.
The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians.
The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize some of our results on the mechanistical aspects of the observed high corrosion resistance.
In der Automobilindustrie stellt das Presshärteverfahren eine Schlüsseltechnologie zur ressourceneffizienten Herstellung sicherheitsrelevanter Karosserie-komponenten dar. Während der Umformoperation treten jedoch hohe Reibungs- und Verschleißerscheinungen an den interagierenden Werkzeug- und Werkstückwirkflächen auf, die sowohl die Bauteilqualität als auch die Maschinenstandzeit nachhaltig beeinträchtigen. Um die bestehenden Verfahrensgrenzen zu erweitern, wird daher eine Modifikation der Presshärtewerkzeuge mittels Laserimplantation angestrebt. Hierbei werden in die Werkzeugoberfläche keramische Hartstoffpartikel anhand eines gepulsten Laserstrahles eingebettet, infolgedessen kuppelförmige sowie höchstfeste Strukturen im Mikrometerbereich entstehen. Die Auswahl geeigneter Hartstoffmaterialien stellt jedoch ein entscheidendes und bisweilen limitierendes Kriterium dar, um defektfreie sowie verschleißresistente Oberflächenmodifikationen zu generieren. In diesem Zusammenhang wurden im Rahmen dieser Arbeit unterschiedliche titanbasierte Hartstoffpartikel auf presshärtespezifische Werkzeugstähle laserimplantiert und anschließend mittels modifizierten Pin-on-Disk-Tests hinsichtlich ihres tribologischen Einsatzverhaltens untersucht. Um die Wirksamkeit des Laserimplantationsverfahrens zu evaluieren, wurden zudem Verschleißuntersuchungen an unmodifizierten Werkzeugoberflächen durchgeführt und mit den erzielten Ergebnissen der lokal dispergierten Topographien verglichen.
Within the scope of this work, a laser implantation process has been used, in order to improve the tribological performance of hot stamping tools. This surface engineering Technology enables the generation of dome-shaped, elevated and highly wear resistant microfeatures on tool surfaces in consequence of a localized dispersing of hard ceramic particles via pulsed laser radiation.
As a result, the topography and material properties of the tool and thus the tribological interactions at the blank-die interface are locally influenced. However, a suitable selection of hard ceramic particles is imperative for generating defect-free surface features with a high share of homogenously disturbed particles. For this purpose, different niobium (NbB2 and NbC) as well as titanium-based (TiB2 and TiC) materials were embedded on hot working tool specimens and subsequently analyzed with regard to their resulting shape and mechanical properties. Afterwards, modified pin-on-disk tests were carried out by using conventional and laser-implanted tool surfaces, in order to evaluate the wear and friction behavior of both tooling systems.
Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration.
Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running.
Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle.
While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated.
While there is a permanent improvement of concrete pavement mixtures and pavement construction types over the last decades, the state-of-the-art joint sealing materials and joint constructions seem to stagnate on an antiquated empirical level. This status has been reaffirmed in the latest European standard. The consequences in the motorway network due to unsatisfying capability and durabilty of joint sealing systems are unacceptable. In addition, inadequate traffic performance (noise emissions, roll-over comfort) and traffic safety losses in the joint area of concrete pavements are existing challenges. These deficits and weaknesses reflect a demand for joint sealing materials and constructions whose approval requirements take functional aspects into account. Furthermore a sufficient analysis of decisive loads and a practice-oriented method to evaluate the requirements towards performance and durability is still missed. In this contribution decisive loads to German highways are analyzed. The design of test specimen for representative functional testing of joint sealing systems is discussed. The focus is on the geometry of the test specimens and the used concrete mixture. Finally, a new approach for a function-orientated test concept that considers representative load functions is presented. The potential of this approach to validate the durability and capability of various joint sealing systems is also presented using an example.
The article “Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS)” was originally published Online First without Open Access. After publication in volume 413, issue 1, page 103–115 of the journal “Analytical and bioanalytical chemistry”, the authors decided to opt for Open Choice and to make the article an Open Access publication. Therefore, the copyright of the article has been changed to © The Author(s) 2021 and the article is forthwith distributed under the terms of the Creative Commons Attribution 4.0 International License.
Der Bericht zum Arbeitspaket 3 baut auf den Ergebnissen der internationalen Recherche (AP1) sowie der Zusammenstellung der Randbedingungen und Beanspruchungsgrößen für die Endlagerbehälter (AP2) auf. Die Anforderungen an die Behälter – regulatorische, betriebliche sowie solche aus der Standortgeologie und den Einwirkungen und Prozessen, denen die Behälter ausgesetzt sind – werden hergeleitet und systematisch dargestellt.
Die für das Endlagersystem zu betrachtenden Nutzungsphasen werden aus den regulatorischen Anforderungen hergeleitet und charakterisiert. Die Einwirkungen auf die Behälter in den drei potenziellen Wirtsgesteinen sowie die sich für die Erfüllung der Sicherheitsfunktionen des Behälters als Teil des Endlagersystems ergebenden Behälterfunktionen werden ebenfalls wirtsgesteins- und zeitphasenabhängig betrachtet. Schließlich werden aus den Einwirkungen auf die Behälter und den Anforderungen an die Behälterfunktionen auch quantifizierbare Behälterfunktionen für alle drei potenziellen Wirtsgesteine abgeleitet.
Dieser Bericht untersucht die im ersten Arbeitspaket ermittelten vorhandenen bzw. entwickelten Behälterkonzepte dahingehend, inwieweit die jeweiligen Behälterfunktionen unter den im zweiten und dritten Arbeitspaket ermittelten Randbedingungen und Einwirkungen den im dritten Arbeitspaket ermittelten Anforderungen an endlagerfähige Behälter in einem deutschen Endlager genügen. Zum anderen sollen, basierend auf den im zweiten Arbeitspaket ermittelten Randbedingungen und den im dritten Arbeitspaket hergeleiteten und zusammengestellten Anforderungen an die Endlagerbehälter, Vorschläge für mögliche generische Endlagerbehälter in den drei potenziellen Wirtsgesteinen Steinsalz, Tonstein und Kristallingestein erarbeitet werden. Die im ersten Arbeitspaket recherchierten Behälterkonzepte, deren Entwicklungslinien und zugrundeliegende Behälteranforderungen bilden hier den Ausgangspunkt für weitergehende Überlegungen hinsichtlich ihrer potenziellen Eignung für ein zukünftiges deutsches Endlager und zur Skizzierung generischer Konzepte für zukünftige Endlagerbehälter.
Im hier vorliegenden Bericht wurde im Rahmen einer umfassenden Literaturrecherche der nationale und internationale Stand von Wissenschaft und Technik hinsichtlich Behälterkonzepten und Behälteranforderungen erfasst. Dabei wurde eine umfangreiche Dokumentensammlung zusammengestellt und sortiert, die als Quellenbasis für alle weiteren Arbeiten zur Verfügung steht. Die Auswertung der gesammelten Informationen resultiert in einem Überblick über internationale Behälterentwicklungen sowie einer detaillierten Übersicht über die Behälterkonzepte und die ihnen zugrundeliegenden Anforderungskataloge aus elf fortgeschrittenen Endlagerprogrammen.
The physical and chemical analysis of aerosols using reliable and physically traceable methods is important for the thorough investigation of airborne particles to support a better understanding of their origin as well as their health and climate impacts. Within the European Metrology Research AeroMet project,the aim of hysikalisch–Technische Bundesanstalt’s (PTB) X-ray spectrometry group is to develop and establish traceable and reliable X-ray methods to measure the elemental mass deposition per unit area, the elemental composition,and the chemical binding state of particulate matter supported by a flat substrate. This approach can substantially contribute to support quantitative analytical methods during on-site measurement campaigns where portable Instrumentation is employed by qualifying suitable calibration samples for commercial analytical X-ray instruments and by investigating samples collected during the field campaign.
A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity.
Die Bemessung von tragendem Lehmmauerwerk erfolgt in Deutschland auf Basis der Lehmbau Regeln. Das dort verankerte Nachweisverfahren beruht auf einem globalen Sicherheitskonzept, welches aus zuverlässigkeitstheoretischer Sicht nicht mehr dem Stand der Technik entspricht. Auf Grund dessen wird das Bemessungskonzept für Lehmmauerwerk vom Deutschen Institut für Bautechnik (DIBt) voraussichtlich 2023 außer Kraft gesetzt. Ein statischer Nachweis von tragenden Lehmbauten wäre in Deutschland dann ausschließlich mit einer Zustimmung im Einzelfall (ZiE) oder vorhabenbezogener Bauartgenehmigung (vBg) möglich. Beides ist mit erheblichem Mehraufwand und höheren Kosten verbunden, was für den Lehmmauerwerksbau einen entscheidenden Nachteil im Vergleich zum konventionellen Mauerwerksbau darstellt. Um eine unkomplizierte Praxisanwendung von Lehmmauerwerk zu ermöglichen, werden innerhalb eines Forschungsvorhabens, welches von der Bundesanstalt für Materialforschung und -prüfung (BAM), dem Institut für Massivbau der Technischen Universität Darmstadt sowie dem Ingenieurbüro ZRS durchgeführt wird, auf Basis der Produktnormen für Lehmsteine und Lehmmauermörtel Grundlagen für ein aktualisiertes Bemessungskonzept entwickelt. Im Rahmen des Projekts wird ebenfalls untersucht, inwiefern die Bemessungsregeln nach den vereinfachten Berechnungsmethoden für unbewehrtes Mauerwerk gemäß DIN EN 1996-3 / NA auf den Lehmmauerwerksbau übertragbar sind. Falls eine Anwendung des normativen Nachweisverfahrens bei Lehmmauerwerk möglich ist, wäre zukünftig eine Aufnahme von Lehmsteinen und Lehmmauermörtel in den nationalen Anhang des Eurocode 6 denkbar, was eine bedeutsame Erweiterung des Anwendungsbereichs von Lehmmauerwerk zur Folge hätte.
Diverse wissenschaftliche Untersuchungen konnten zeigen, dass bemessungsrelevante Festigkeits- und Verformungseigenschaften von Lehmmauerwerksbaustoffen stark von der vorherrschenden Materialfeuchte abhängen, welche im hygroskopischen Wassergehaltsbereich im Wesentlichen von der relativen Luftfeuchte (RLF) bestimmt wird. Auch die Zwischenergebnisse des laufenden Forschungsvorhabens zur Entwicklung eines Bemessungskonzepts für Lehmmauerwerk ergaben eine deutlich erkennbare Abhängigkeit zwischen der Materialfeuchte und den relevanten Festigkeits- und Verformungseigenschaften. Eine detaillierte Kenntnis des feuchteabhängigen Materialverhaltens von Lehmsteinen, -mörtel und -mauerwerk ist zwingend erforderlich, um ein konsistentes und zuverlässiges Bemessungskonzept für Lehmmauerwerk zu entwickeln. Im Rahmen des laufenden Forschungsprojektes werden deshalb umfangreiche Versuche zum Drucktragverhalten von Lehmsteinen und -mörtel sowie Lehmmauerwerk nach Konditionierung bei unterschiedlichen RLF durchgeführt und analysiert. Weiterhin werden auf Basis der experimentellen Ergebnisse numerische Modelle kalibriert, welche die detaillierte Analyse der Biegedrucktragfähigkeit von Lehmmauerwerk ermöglichen.
In diesem Beitrag werden zunächst die bisherigen Zwischenergebnisse bezüglich der experimentell ermittelten feuchteabhängigen Materialkennwerte von Lehmsteinen, -mörtel und -mauerwerk dargelegt. Darauf aufbauend werden numerische Untersuchungen zur Bestimmung der Systemtragfähigkeit von Lehmmauerwerk unter Feuchteeinflusses durchgeführt und erläutert.
The presentation reflects the questions that have been raised by member states and NGOs.
As background information details on the question how to choose a suitable salvage pressure receptacle (SPR) are provided. This leads to the need for deleting the volume limitation for SPRs and to the discussions in 2014 and 2016 on this issue.
As an adequate substitution for deleting the volume limit for SPRs it is proposed to limit the pressure receptacles to be stored in by a maximum pressure-volume-value of 1.5 Mio bar-litres.
After some explanations to standardisation projects currently also tackling this pV-limit, some risk-based safety criteria for a limitation are mentioned with the focus of the consequence level and the general avoidance of catastrophic worst case scenarios.
The presentation starts with some key figures about BAM. Then it introduces BAM's competence centre H2Safety@BAM and shows aspects of special competence of the centre. It closes with information about the engagement of BAM in European research projects on hydrogen and a reference to our bilingual paper about our hydrogen strategy.
Der Vortrag beginnt mit dem erwarteten Bedarf an Wasserstoff und der Frage der Risikosteuerung bei stattfindender Marktdurchsetzung. Dem gegenüber ist an einem Beispiel der Prozess der Regelsetzung gestellt, was die Notwendigkeit pro-aktiven Handelns zeigt.
Es wird über die risikobasierte Definition von Sicherheit gezeigt, welche Bedeutung die Erfassung der Fertigungsstreuung hat und wie die quantitative Erfassung und Bewertung aussehen könnte. Zuletzt wird über den Aspekt der Alterung auf das Potential probabilistischer Zulassungsansätze verwiesen und aufgezeigt, wie die Wirkung von Vorschriften nach dem probabilistischen Sicherheitskriterium bewertet und optimiert werden kann.
First the acceptance rates resulting from the analysis of different minimum burst ratios and standards are displayed and explained. Especially the problems resulting from a further reduction if the minimum burst ratio are shown.
For a better understanding of these results the process of analysing the acceptance rate is explained in detail. This contains the alleged contradiction between safety of samples due to its scatter while the rejected sample provides a higher mean strength.
Then the importance of batch testing is explained and leads to the recommendation to have a strong interaction between provided mean strength and requested maximum of production scatter.
The fracture mechanics-based IBESS approach is applied to the determination of FAT classes of butt welds with crack Initiation along the weld toe. The aim is an investigation of the effect of the geometrical parameters toe radius, flank angle, reinforcement and secondary notches such as roughness or undercuts. The influence of these parameters is discussed both individually and in combination; however, excluding statistical distributions of them and the material data. The results, when compared with conventional FAT classes for butt welds, are encouraging with respect to a potential contribution of IBESS to the discussion of more advanced quality criteria for welds. To that purpose, demands for further research are proposed.
Structural health monitoring systems have been widely implemented to provide real-time continuous data support and to ensure structural safety in the context of structural integrity management. However, the quantification of the potential benefits of structural health monitoring systems has not yet attracted widespread attention. At the same time, there is an urgent need to develop strategies, such as optimizing the monitoring period, monitoring variables, and other factors, to maximize the potential benefits of structural health monitoring systems. Considering the continuity of structural health monitoring information, a framework is developed in this article to support decision-making for structural Health monitoring systems arrangement in the context of structural integrity management, which integrates the concepts of value of information and risk-based inspection planning based on an approach which utilizes a conjugate prior probability distribution for updating of the probabilistic models of structural performances based on structural health Monitoring information. An example considering fatigue degradation of steel structures is investigated to illustrate the application of the proposed framework. The considered example shows that the choice of monitoring variables, the Monitoring period, and the monitoring quality may be consistently optimized by the application of the proposed framework and approach. Finally, discussions and conclusions are provided to clarify the potential benefits of the proposed Framework with a special view to practical applications of structural health monitoring systems.
The scribe of ‘Erfurt 7’, a thirteenth-century Torah scroll now kept in Berlin, initially left blank spaces for the divine appellations Elohim ( אלהים ) and YHWH Elohim ( ,(יהוה אלהים which were filled in during a second stage of writing. The appearance of the ink employed to write the appellations was significantly darker than that of the surrounding ink.
X-ray fluorescence analysis (XRF) has shown that the light and dark brown inks had similar elemental compositions, but contained different ratios of iron to potassium, which could be explained by the use of different batches of ink.
According to some medieval sources, the divine appellations were sometimes filled in during a second stage of writing in the presence of ten men from the Jewish community. In Erfurt 7, the two-stage procedure was only performed in the first 1.5 columns of the original sheets, suggesting it may have been part of a public ceremony inaugurating the writing of the divine names in the scroll. Erfurt 7 emerges from this study not only as a ritual object used for liturgy, but as a rallying point for the Jews of Erfurt to come together as a community to express their reverence for the written form of God’s name. The divine name YHWH ( יהוה ) was written in a smaller script than the surrounding text on three replacement sheets using the same two-stage procedure. The ink used on the replacement sheets contained zinc, which is characteristic of other Erfurt manuscripts as well. This suggests that Erfurt was the place where the scroll was used, cherished and eventually repaired.
Der Einsatz von Aluminiumlegierungen als Konstruktionswerkstoff hat in den letzten Jahrzehnten aufgrund seines überlegenen Festigkeits-/ Gewichtsverhältnisses zugenommen. Dabei spielen höherfeste aushärtbare Al-Mg-Si-Legierungen eine wichtige Rolle.
Dieser Beitrag konzentriert sich auf die additive Fertigung von Prinzipbauteilen aus einer Al-Mg-Si-Aluminiumlegierung mittels Wire + Arc Additive Manufacturing. Werkstoffe dieses Legierungssystems weisen eine ausgeprägte Heißrissanfälligkeit auf, weshalb das artgleiche Fügen dieser Materialien, mittels Metallschutzgasschweißen, heutzutage immer noch eine Herausforderung darstellt. Kommerzielle Al-Mg-Si-Schweißdrähte sind am Markt nicht verfügbar.
In dieser Arbeit wird die Anwendbarkeit eines neuartigen Al-Mg-Si-Schweißdrahtes mit zusätzlichen kornfeinenden Elementen für die additive Fertigung mittels MSG-Verfahren gezeigt. Dazu wird der Zusammenhang von verwendeten Prozessparametern und der resultierenden Bauteilqualität untersucht, wobei die Größe und Verteilung von Poren sowie die Kornmorphologie analysiert werden. Darüber hinaus wird der Einfluss einer T6 Wärmenachbehandlung auf die mechanischen Eigenschaften des Werkstoffes untersucht und ein Vergleich zum entsprechenden Referenzmaterial (Knetlegierung) gezogen.
There are viral, fungal, bacterial and trypanosomal pathogens that negatively impact the individual and superorganismal health of the western honey bee. One fungal pathogen, Ascosphaera apis , affects larvae and causes the disease chalkbrood. A previous genome analysis of As. apis revealed that its genome encodes for RNA interference genes, similar to other fungi and eukaryotes. Here, we examined whether As. apis -targeting double-stranded RNA species could disrupt the germination of As. apis.
We observed that when spores were co-incubated with As. apis -targeting dsRNA, fewer spores were activated for germination, suggesting an uptake of exogenous genetic material at the very onset of germination and consequent damage to essential transcripts needed for germination. Overall, these results indicate that the causative agent of chalkbrood disease, As. apis , can be successfully targeted using an RNAi-based strategy.
Network modifier ions can decisively influence properties and structure of low melting alkali-zinc-borate glasses and thus cause complex effects on the liquid phase sintering of silver-glass metallization pastes. This effect was studied for X2O-ZnO-B2O3 (X = Li, Na, Rb) glasses for silver-glass metallization pastes. Viscosity and the glass transition temperature, Tg, were measured with rotational viscometry and dilatometry. Dried model pastes with 30 vol% LZB, NZB or RZB glass were prepared for sintering studies by means of heating microscopy measuring the silhouette area shrinkage of uniaxially pressed powder compacts during heating at 5 K/min. For comparison, the silhouette area shrinkage of pure glass and silver powder compacts were determined. Glass-silver wetting was investigated during heating of bulk glass cylinders placed on silver substrates. Glass RZB turned out to have the lowest viscosity among the glasses under study. Its glass transformation temperature, Tg, was found at 444 °C and it caused the lowest sintering onset for its glass and paste powder compacts. Slightly increased values of Tg were found for NZB and LZB (468 °C and 466 °C, respectively) and a slightly retarded sintering was found for both paste powder compacts. These results indicate that liquid phase sintering of silver-glass pastes under air atmosphere is mainly influenced by glass viscosity.
The paper presents the results of the radiocarbon dating and ink analysis of a leather fragment bearing an important liturgical text in Hebrew from the early centuries of the common era. The work initiated by the scholarly interest in the text stresses the importance of the date and materiality of the manuscripts and closes with an appeal to the curators of manuscript collections.
Für die Bestimmung der Restlebensdauer zyklisch beanspruchter Bauteile kommt dem Schwellenwert für Ermüdungsrissausbreitung ∆Kth und dem sich anschließenden Schwellenwertbereich der da/dN-∆K-Kurve große Bedeutung zu. Dem stehen Unsicherheiten bei der Bestimmung und Analyse gegenüber. Der Aufsatz befasst sich mit der Ermittlung des sogenannten intrinsischen Schwellenwerts, der als robuster Eingangsparameter für eine „rissschließfreie“ Analyse der Restlebensdauer von entscheidender Bedeutung ist.
Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
For hazard Assessment purposes we need models to predict what would happen in case of an accident.
The challenge in hazard assessment consists not only in choosing the right model, but beforehand to define the correct scenario .If models can be found for the physical effect to be simulated, the validation of these models is the next challenge.
Even if experimental data can be found it should always be checked, if these data are correct, even if in general experimental data are considered as “failsafe” or “the absolute truth”.
Abdominal aortic aneurysm (AAA) is a life-threatening vascular disease with an up to 80% mortality in case of rupture. Current biomarkers fail to account for size-independent risk of rupture. By combining the information of different molecular probes, multi-target molecular MRI holds the potential to enable individual characterization of AAA. In this experimental study, we aimed to examine the feasibility of simultaneous imaging of extracellular collagen and inflammation for size-independent prediction of risk of rupture in murine AAA. The study design consisted of: (1) A outcome-based longitudinal study with imaging performed once after one week with follow-up and death as the end-point for assessment of rupture risk. (2) A week-by-week study for the characterization of AAA development with imaging after 1, 2, 3 and 4 weeks. For both studies, the animals were administered a type 1 collagen-targeted gadolinium-based probe (surrogate marker for extracellular matrix (ECM) remodeling) and an iron oxide-based probe (surrogate marker for inflammatory activity), in one imaging session. In vivo measurements of collagen and iron oxide probes showed a significant correlation with ex vivo histology (p < 0.001) and also corresponded well to inductively-coupled plasma-mass spectrometry and laser-ablation inductively-coupled plasma mass spectrometry. Combined evaluation of collagen-related ECM remodeling and inflammatory activity was the most accurate predictor for AAA rupture (sensitivity 80%, specificity 100%, area under the curve 0.85), being superior to information from the individual probes alone. Our study supports the feasibility of a simultaneous assessment of collagen-related extracellular matrix remodeling and inflammatory activity in a murine model of AAA.
Abdominal aortic aneurysm (AAA) remains a fatal disease. Its development encompasses a complex interplay between hemodynamic stimuli on and changes in the arterial wall. Currently available biomarkers fail to predict the risk of AAA rupture independent of aneurysm size. Therefore, novel biomarkers for AAA characterization are needed. In this study, we used a mouse model of AAA to investigate the potential of magnetic resonance imaging (MRI) with an albumin-binding probe to assess changes in vascular permeability at different stages of aneurysm growth. Two imaging studies were performed: a longitudinal study with follow-up and death as endpoint to predict rupture risk and a week-by-week study to characterize AAA development. AAAs, which eventually ruptured, demonstrated a significantly higher in vivo MR signal enhancement from the albumin-binding probe (p = 0.047) and a smaller non-enhancing thrombus area compared to intact AAAs (p = 0.001). The ratio of albumin-binding-probe enhancement of the aneurysm wall to size of non-enhancing-thrombus-area predicted AAA rupture with high sensitivity/specificity (100%/86%). More advanced aneurysms with higher vascular permeability demonstrated an increased uptake of the albumin-binding-probe. These results indicate that MRI with an albumin-binding probe may enable noninvasive assessment of vascular permeability in murine AAAs and prediction of rupture risk.
Learned block iterative shrinkage thresholding algorithm for photothermal super resolution imaging
(2020)
Block-sparse regularization is already well-known in active thermal imaging and is used for multiple measurement based inverse problems. The main bottleneck of this method is the choice of regularization parameters which differs for each experiment. To avoid time-consuming manually selected regularization parameters, we propose a learned block-sparse optimization approach using an iterative algorithm unfolded into a deep neural network. More precisely, we show the benefits of using a learned block iterative shrinkage thresholding algorithm that is able to learn the choice of regularization parameters. In addition, this algorithm enables the determination of a suitable weight matrix to solve the underlying inverse problem. Therefore, in this paper we present the algorithm and compare it with state of the art block iterative shrinkage thresholding using synthetically generated test data and experimental test data from active thermography for defect reconstruction. Our results show that the use of the learned block-sparse optimization approach provides smaller normalized mean square errors for a small fixed number of iterations than without learning. Thus, this new approach allows to improve the convergence speed and only needs a few iterations to generate accurate defect reconstruction in photothermal super resolution imaging.
Fault detection for linear parameter varying systems under changes in the process noise covariance
(2020)
Detecting changes in the eigenstructure of linear systems is a comprehensively investigated subject. In particular, change detection methods based on hypothesis testing using Gaussian residuals have been developed previously. In such residuals, a reference model is confronted to data from the current system. In this paper, linear output-only systems depending on a varying external physical parameter are considered. These systems are driven by process noise, whose covariance may also vary between measurements. To deal with the varying parameter, an interpolation approach is pursued, where a limited number of reference models – each estimated from data measured in a reference state – are interpolated to approximate an adequate reference model for the current parameter. The problem becomes more complex when the different points of interpolation correspond to different noise conditions. Then conflicts may arise between the detection of changes in the eigenstructure due to a fault and the detection of changes due to different noise conditions. For this case, a new change detection approach is developed based on the interpolation of the eigenstructure at the reference points. The resulting approach is capable of change detection when both the external physical parameter and the process noise conditions are varying. This approach is validated on a numerical simulation of a mechanical system.
The goal of this work is to identify the optimal operating input for a lithiation reaction that is performed in a highly innovative pilot scale continuous flow chemical plant in an industrial environment, taking into account the process and safety constraints. The main challenge is to identify the optimum operation in the absence of information about the reaction mechanism and the reaction kinetics. We employ an iterative real-time optimization scheme called modifier adaptation with quadratic approximation (MAWQA) to identify the plant optimum in the presence of plant-model mismatch and measurement noise. A novel NMR PAT-sensor is used to measure the concentration of the reactants and of the product at the reactor outlet. The experiment results demonstrate the capabilities of the iterative optimization using the MAWQA algorithm in driving a complex real plant to an economically optimal operating point in the presence of plant-model mismatch and of process and measurement uncertainties.
Zur Bestimmung der reaktionskinetischen Daten von Schüttgütern und iur Vorhersage des Selbstentzündungsverhaltens großer.Lager kommen verschiedene Analysemethoden zum Einsatz. Dabei handelt es sich .um thermische Verfahren wie die Differential-Scanning- Kalorimetrie OS(. die simultane Thermoanalyse STA sowie die Mikrokalorimetrie zur hochpräzisen Messung von Wärmeströmen. Für die oben genannten Methoden werden sehr kleine Probenmengen verwendet. In der Regel wird das Selbstentzündungsverhalten jedoch mit Hilfe von isoperibolen oder adiabatischen Warmlagerungsversuchen ermittelt: die Probenvolumina liegen hier meist im Bereich von ca. 100 cm3 bis zu mehreren Litern.
Die Extrapolation auf technisch relevante Volumina birgt jedoch erhebliche Unsicherheiten. Diese Unsicherheiten zu identifizieren und zu reduzieren ist das Hauptziel eines 2018 gestarteten Forschungsprojekts. Dies soll in erster Linie durch den Aufbau eines Versuchsstandes zur Untersuchung von Probengrößen von bis zu. 1000 dm 3 geschehen.
Sowohl Warmlagerungsversucl1e im Labormaßstab als auch thermoanalytische Verfahren. die mit Hilfe verschiedener Methoden ausgewertet werden. lassen, einzeln betrachtet. häufig nur bedingt zuverlässige Aussagen über das Selbstentzündungsverhalten von großen Schüttgütern zu. Es werden komplette Versuchsreihen mit allen genannten Prüfverfahren vorgestellt und Aussagen zur Anwendbarkeit der Extrapolationsmethoden diskutiert.
Abstract: Since it is unknown for many applications, which PFASs are used and how they enter the environment, target analysis-based methods reach their limits. The two most frequently used sum parameters are the adsorbable organically bound fluorine (AOF) and the extractable organically bound fluorine (EOF). Both can be quantified using either combustion ion chromatography (CIC) or high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Here we provide an insight on the advantageous and disadvantageous of both sum parameters and both detection methods. Our study is based on the analysis of surface water samples. Next to total fluorine (TF) analysis, AOF and EOF were determined as well as CIC and HR-CS-GFMAS are compared and results are comparatively discussed. Fluorine mass balancing revealed that, the AOF/TF proportion was higher than the EOF/TF proportion. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF. Although, organically bound fluorine represents only a small portion of TF, PFASs are of worldwide concern, because of their extreme persistence and their bioaccumulation potential. The EOF-HR-CS-GFMAS method turned out to be more precise and sensitive than the AOF-CIC method and is a promising tool for future monitoring studies/routine analysis of PFASs in the environment.
Up to now, different analytical methods for single cell analysis exist focusing on key features such as size, shape, morphology and elemental composition. The combination of the latest ICP-MS techniques - ICP-ToF-MS - together with the latest developments in the field of sample delivery - micro droplet generator (MDG) – will allow a Deep insight into the composition and size of cells.
Microbiologically influenced corrosion (MIC) is an oxidation of metals affected by the presence or activity (or both) of microorganisms e.g. Shewanella Putrefaciens in biofilms on the surface of the corroding material. As this can happen for example in the soil on iron pipes of water pipes, in oil tanks or on steel sheet piling, there is great interest in MIC research, not only from various industrial sectors, but also from the environmental aspect.
A new approach towards performance-related design and scientific evaluation of joint sealing systems
(2020)
While there is a permanent improvement of concrete pavement mixtures and pavement construction types over the last decades, the state-of-the-art joint sealing materials and joint constructions seem to stagnate on an antiquated empirical level. This status has been reaffirmed in the latest European standard.
The consequences in the motorway network due to unsatisfying capability and durability of joint sealing systems are unacceptable. In addition, inadequate traffic performance (noise emissions, roll-over comfort) and traffic safety losses in the joint area of concrete pavements are existing challenges. These deficits and weaknesses reflect a demand for joint sealing materials and constructions whose approval requirements take functional aspects into account. Furthermore a sufficient analysis of decisive loads and a practice-oriented method to evaluate the requirements towards performance and durability is still missed.
In this contribution decisive loads to German highways are analyzed. The design of test specimen for representative functional testing of joint sealing systems is discussed. The focus is on the geometry of the test specimens and the used concrete mixture. Finally, a new approach for a function-orientated test concept that considers representative load functions is presented. The potential of this approach to validate the durability and capability of various joint sealing systems is also presented using an example.
The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix.
As the most electronegative element, fluorine has a strong influence on material properties such as absorption behaviour or chemical and thermal stability. Fluorine can be easily integrated into coordination polymers (CPs) via a fluorinated acetate, here trifluoroacetate in Ba(CF3COO)2, or directly via a metal fluorine bond (BaF(CH3COO)). In the present study both possibilities of fluorine integration were tested and their effect on structure and properties of barium coordination polymers was investigated in comparison with the non-fluorinated barium acetate (Ba(CH3COO)2). In addition to the study of their thermal behaviour and their decomposition temperature, the CPs structures were tested for their application as possible anode materials in lithium ion batteries and for their sorption of water and ammonia. The properties of the CPs can be traced back to the individual structural motifs and could thus trigger new design ideas for CPs in LIBs and/or catalysis.
According to UN Test O.2, surprisingly, the polychlorosilanes hexachlorodisilane (HCDS), octachlorotrisilane (OCTS) and decachlorotetrasilane (DCTS) formally fulfill the criteria of the “test for oxidizing liquids”. This result is in contrast to the properties of polychlorosilanes that are described in the literature and those we have experienced in our own production.
By investigating the reaction products from the UN O.2 test reactor, using IR, Raman and XPS spectroscopy, it was shown that the results are not due to oxidizing properties of HCDS, OCTS or DCTS, but are caused by the specified test substance cellulose. To our knowledge, this is the very first substance class in which the reference substance oxidizes the test sample, instead of vice versa. This represents an important limitation of the internationally used UN Test O.2 for this substance class. The cause for this false-positive result is the known high degree of affinity of oxygen to silicon.
It is shown that the correctly executed UN Test O.2 produces false-positive results and that the polychlorosilanes do not have an oxidizing effect and, therefore, do not have to be classified as “oxidizing substances”.
Composition and microstructure stability of cement compound under cyclic hydrothermal condition
(2020)
There have been many researches focused on the performance improvement of ultra-high performance concrete (UHPC) by autoclaving treatment. The goal of autoclaving is to increase the pozzolanic reaction, and to densify the cement stone and the transition zone which originates from the incorporation of supplementary cementitious materials (SCMs), such as silica fume, fly ash and blast furnace slag. Due to the superior properties, UHPC can also be utilized under high mechanical load and aggressive condition, for example, the fabrication of water tanks for thermal storage which is of great significance for saving energy and reducing CO2 emission. It is known that mineral stability of the hydration products of an inorganic binder is highly related to the temperature and pressure of the environment. A certain stable composition at room temperature, however, may undergo a phase transformation at high temperature and the performance decrease under this severe condition will generally be more severe. In this way, the rationale behind this deterioration under long-term hydrothermal condition involving many cycles and long duration has to be clarified, and then appropriate optimizing methods will be performed in order to obtain a kind of construction with high durability under aggressive environment. For this purpose, different types and amounts of SCMs are introduced into the standard mixture of UHPC and the phase compositions after autoclaving at 200 °C and 15.5 bar are determined by combined X-ray diffraction and scanning electron microscope. Mercury intrusion porosimeter is used to characterise the microstructure of the samples. In order to establish the relationship between microstructure and macroscopic properties, compressive and flexural strength are also investigated.
Composition and microstructure stability of cement compound under cyclic hydrothermal condition
(2020)
There have been many researches focused on the performance improvement of ultra-high performance concrete (UHPC) by autoclaving treatment. The goal of autoclaving is to increase the pozzolanic reaction, and to densify the cement stone and the transition zone which originates from the incorporation of supplementary cementitious materials (SCMs), such as silica fume, fly ash and blast furnace slag. Due to the superior properties, UHPC can also be utilized under high mechanical load and aggressive condition, for example, the fabrication of water tanks for thermal storage which is of great significance for saving energy and reducing CO2 emission. It is known that mineral stability of the hydration products of an inorganic binder is highly related to the temperature and pressure of the environment. A certain stable composition at room temperature, however, may undergo a phase transformation at high temperature and the performance decrease under this severe condition will generally be more severe. In this way, the rationale behind this deterioration under long-term hydrothermal condition involving many cycles and long duration has to be clarified, and then appropriate optimizing methods will be performed in order to obtain a kind of construction with high durability under aggressive environment. For this purpose, different types and amounts of SCMs are introduced into the standard mixture of UHPC and the phase compositions after autoclaving at 200 °C and 15.5 bar are determined by combined X-ray diffraction and scanning electron microscope. Mercury intrusion porosimeter is used to characterise the microstructure of the samples. In order to establish the relationship between microstructure and macroscopic properties, compressive and flexural strength are also investigated.
Ultra high performance concrete (UHPC) is known for its high compressive strength of more than 150 MPa and its high durability. Thermal treatment at 90°C can accelerate the strength development so that the 28-days-strength can be achieved immediately after the treatment and an additional increase up to 30 % in some cases. The reason for the strength development is an accelerated hydration of the clinker minerals and an intensified pozzolanic reaction leading to a denser microstructure.
In previous research inhomogeneities in form of a zonation after unprotected thermal treatment were observed and analysed in respect to changes in the microstructure. This zonation is defined by a different microstructure in the core compared to the outer zone in the matter of porosity, mineral phase composition and a significant change in the potassium and sulphur concentration of the zones is measurable.
To isolate different transport mechanisms responsible for these element distributions UHPC samples were thermally treated at 90 °C and the microstructure was investigated under dry conditions and after immersion in water to investigate the influence of dehydration during and rehydration after the thermal treatment on the microstructure. Through durability testing via water absorption, water vapour diffusion, permeability testing and sulfuric acid resistance transport mechanisms like diffusion, migration, capillary suction are under investigation in correlation with the microstructure analysis. For the microstructure analysis measurements with µXRF, mercury intrusion porosity, XRD and SEM were conducted.
Ultra high performance concrete (UHPC) is known for its high compressive strength of more than 150 MPa and its high durability. Thermal treatment at 90°C can accelerate the strength development so that the 28-days-strength can be achieved immediately after the treatment and an additional increase up to 30 % in some cases. The reason for the strength development is an accelerated hydration of the clinker minerals and an intensified pozzolanic reaction leading to a denser microstructure.
In previous research inhomogeneities in form of a zonation after unprotected thermal treatment were observed and analysed in respect to changes in the microstructure. This zonation is defined by a different microstructure in the core compared to the outer zone in the matter of porosity, mineral phase composition and a significant change in the potassium and sulphur concentration of the zones is measurable.
To isolate different transport mechanisms responsible for these element distributions UHPC samples were thermally treated at 90 °C and the microstructure was investigated under dry conditions and after immersion in water to investigate the influence of dehydration during and rehydration after the thermal treatment on the microstructure. Through durability testing via water absorption, water vapour diffusion, permeability testing and sulfuric acid resistance transport mechanisms like diffusion, migration, capillary suction are under investigation in correlation with the microstructure analysis. For the microstructure analysis measurements with µXRF, mercury intrusion porosity, XRD and SEM were conducted.
Fault detection for linear parameter varying systems under changes in the process noise covariance
(2020)
Detecting changes in the eigenstructure of linear systems is a comprehensively investigated subject. In particular, change detection methods based on hypothesis testing using Gaussian residuals have been developed previously. In such residuals, a reference model is confronted to data from the current system. In this paper, linear output-only Systems depending on a varying external physical parameter are considered. These systems are driven by process noise, whose covariance may also vary between measurements. To deal with the varying parameter, an interpolation approach is pursued, where a limited number of reference models { each estimated from data measured in a reference state { are interpolated to approximate an adequate reference model for the current parameter. The problem becomes more complex when the different points of interpolation correspond to different noise conditions. Then con icts May arise between the detection of changes in the eigenstructure due to a fault and the detection of changes due to different noise conditions. For this case, a new change detection approach is developed based on the interpolation of the eigenstructure at the reference points. The resulting approach is capable of change detection when both the external physical parameter and the process noise conditions are varying. This approach is validated on a numerical simulation of a mechanical system.
Tetraethyl orthosilicate (TEOS) was used as a chemical precursor to deposit ultra-thin SiO x C y plasma polymer films onto mild steel surfaces for preventing the corrosion process. The structure–property relationships of the coatings were evaluated by X-ray Photo Spectroscopy (XPS), X-Ray Diffraction (XRD), Fourier Transform InfraRed spectroscopy (ATR-FTIR) and Energy Dispersive X-ray spectroscopy (EDX) completed with Scanning Electron Microscopy (SEM). The SEM micrographs confirmed a pinhole-free surface morphology of the low-pressure deposited plasma polymer films. The TEOS molecules become fragmented in the plasma by numerous collisions with energy-rich electrons and heavier particles. Recombination of fragments and condensation onto the steel substrate is responsible for the formation of organic SiO containing plasma polymer layers. Such thin layers consist of predominantly SiO x structures. Their properties are determined largely by the gap distance between the two samples used as electrodes in the plasma. The efficiency of the corrosion-protecting coating was compared with uncoated samples. The corrosion protection was determined by exposure of samples to 3.5% NaCl aqueous solutions. For this purpose, polarization and Electrochemical Impedance Spectroscopy (EIS) were used to monitor the corrosion. The optimal gap distance between the electrodes was determined for corrosion protection. The best protective efficiency reached more than 97% of the total protection as measured at room temperature.
The synthesis and optimization of superior and eco-friendly sorbents for Pb(II) pose a great challenge in the field of water treatment. The sorbent was developed by introducing graphene oxide (GO) into the matrix of polyvinyl formaldehyde (PVF) foam. The immobilization of GO in PVF results in significant increase in the maximum adsorption capacity (Qt) of GO powder for Pb(II), from ≈800 to ≈1730 mg g−1 in the case of GO/PVF foam. As compared with GO powder in Pb(II) aqueous solutions, PVF matrix keeps GO sheets stable without any agglomeration. The large surface area of GO sheet allows the abundant oxygenated functional groups on its surface to participate effectively in the Pb(II) adsorption process, leading to the huge increase of the Qt. Adsorption isotherms and kinetic studies indicated that the sorption process of Pb(II) on GO/PVF was done on heterogenous surface by ion-exchange reaction. The GO/PVF foam showed an excellent reusability for more than 10 cycles with almost the same efficiency and without any significant change in its physical properties.
Herein, two polyurethane oligomers were successfully synthesized using a prepolymer mixing process. The prepolymers were synthesized based on the step-growth addition polymerization of polypropylene glycol, Methylene diphenyl diisocyanate and 2-hydroxyethyl methacrylate or 2-hydroxyethyl acrylate. Isopropanol was functioned as the isocyanate blocking agent. Thereafter, different terpolymer emulsions were prepared by the emulsion graft copolymerization with the vinyl acetate monomer in presence of 2-ethylhexyl acrylate as a vinyl monomer. The chemical structures of the synthesized oligomeric monomers were probed by FTIR spectroscopy and found to vary with the content of acrylic monomer used in the oligomer synthesis phase (i.e.hydroxyethyl acrylate or hydroxyethyl methacrylate). The topography, thermal stability, and particle size of terpolymers were investigated by SEM, TGA, and zeta potential, respectively. The TGA results demonstrated marked enhancement in thermal stability of the synthesized terpolymers up to ca. 600°C, which was concurrent with enhanced surface homogeneity and film properties as evidenced by the SEM images. These terpolymers showed also property enhancement as binders for textile pigment printing in terms of rubbing resistance, color strength and fastness to washing when compared to the commercial binders.
These judgments would provide a new competent synthesis route by introducing polyurethane acetate vinyl acrylate as the binder for use in pigment printing of cotton fabrics.
We show how the combination of the spatial autocorrelation function and permeability calculations, applied to 3D X-ray computed tomography data, can yield quantitative information on the anisotropy of both meso-structure and fluid flow in Diesel Particulate Filter (DPF) materials, such as Cordierite and SiC. It was found that both the degree of anisotropy, and the orientation of the permeability and meso-structure are similar, but not identical. We confirm that the morphological anisotropy of cordierite materials is weak, and clearly influenced by the extrusion process that determines the main direction of anisotropy. Properties of the autocorrelation function are discussed and it is shown why estimating the characteristic length of real meso-structures (grain or ?pore? size) is not possible. Finally, we show that the autocorrelation function applied on grey-level images can give a good estimate of the degree of anisotropy even with limited resolution.
Im Forschungsvorhaben KoBrA werden Anforderungen an Endlagerbehälter für hochradioaktive Abfälle erstmals systematisch und unter Berücksichtigung des internationalen Standes von Wissenschaft und Technik hergeleitet. Parallel werden die behälterrelevanten Randbedingungen und Beanspruchungsgrößen für Endlagerbehälter in den drei potenziellen Wirtsgesteinen Steinsalz, Tonstein und Kristallingestein ermittelt. Darauf aufbauend werden die zur Erfüllung der Anforderungen unter den gegebenen Einwirkungen und Beanspruchungen notwendigen Behälterfunktionen bestimmt und erste Konzeptideen für zukünftige Endlagerbehälter diskutiert bzw. entwickelt.
Liebe Leserin, lieber Leser,
die Explosion war bis an den Stadtrand von Berlin zu hören, als am 25. Mai 1894 auf dem Tempelhofer Feld etwa 70 mit Wasserstoff gefüllte Gasflaschen der "königlich-preußischen Luftschiffer-Kompagnie" detonierten. Auch wenn zum Glück niemand verletzt wurde: Die Explosion führte schlagartig vor Augen, welche Gefahren eine neue Technologie mit sich bringen kann.
Um weitere Unfälle wie diesen zu vermeiden, beauftragte die Regierung Adolf Martens, den Leiter der "Mechanisch-Technischen Versuchsanstalt", mit einem Gutachten.
1871 - vor 150 Jahren - hatte die Einrichtung in Berlin ihre Arbeit aufgenommen. Anfangs war sie nicht mehr als ein bescheidenes Laboratorium zur Prüfung der "Festigkeit von Eisen und Stahl". Rasch entwickelte sie sich jedoch zu einer unverzichtbaren Begleiterin des Fortschritts.
Heute, anderthalb Jahrhunderte später, bestimmen nicht mehr nur Schadensanalysen, sondern Megatrends wie die Globalisierung, die Digitalisierung oder Nachhaltigkeit viele der Forschungsprojekte und hoheitlichen Aufgaben, mit denen sich die Bundesanstalt für Materialforschung und -prüfung (BAM) beschäftigt, die aus der "Mechanisch-Technischen Versuchsanstalt" hervorging und 1954 gegründet wurde. Um den globalen, wirtschaftlichen und technischen Herausforderungen unserer Zeit zu begegnen, forscht, prüft, bewertet und berät die BAM heute unter anderem zu nachhaltigen Baustoffen, zur Sicherheit von Lithiumbatterien oder zur effizienten Nutzung erneuerbarer Energien. Und nicht zufällig widmen wir uns wieder intensiv der sicheren Verwendung von Wasserstoff - dem Schüsselelement für eine emissionsfreie Zukunft.
All dies geht heute nur national und international vernetzt, mit Partner*innen in Wissenschaft, Wirtschaft und Verwaltung, denn unsere Aufgaben überschreiten oft Ländergrenzen und fast immer Fachdisziplinen. Und sie bedürfen der Verständigung mit der Gesellschaft und der Politik über Ziele und Standards.
Lassen Sie uns daher gemeinsam an den globalen Herausforderungen für die Sicherheit in unserer Zeit arbeiten. Lassen Sie uns Potenziale, die in Zukunftstechnologien stecken, gemeinsam heben. Und lassen Sie uns 150 Jahre BAM, also 150 Jahre Wissenschaft mit Wirkung, feiern. Mehr dazu erfahren Sie hier im BAM Report 2020/21 und auf unserer Jubiläums-Website www.150.BAM.de.
Kombinierte faseroptische Messungen in Bohrlöchern helfen bei der Detektion von Kleinstleckagen
(2020)
Seit November 2019 läuft ein breit angelegtes und vom BMWi gefördertes ZIM-Kooperationsprojekt zwischen der Bundesanstalt für Materialforschung und -prüfung (BAM), der IAB'Weimar gGmbH, der GKSO GmbH & Co. Projekt KG, der DEEP.KBB GmbH sowie der Rembe Consulting PartG mbB. Ziel des Forschungsvorhabens sind sowohl die Lokalisierung als auch die Quantifizierung insbesondere sehr kleiner Leckagen in einer Bohrlochverrohrung durch die Nutzung faseroptischer Messtechnik. Durch Messdatenkopplung und den Wegfall bewegungsbedingter Nachteile einer Messsonde werden wesentlich präzisere Ergebnisse zur Bewertung der Bohrlochintegrität als üblich
erwartet.
In den letzten Jahrzehnten ist die Nachfrage nach kostengünstigen und flächendeckenden Kartierungsmöglichkeiten im Hinblick auf eine ertragssteigernde und umweltfreundlichere Bewirtschaftung von landwirtschaftlichen Nutzflächen stark gestiegen. Hierfür eignen sich spektroskopische Methoden wie die Röntgenfluoreszenzanalyse (RFA), Raman- und Gammaspektroskopie sowie die laserinduzierte Plasmaspektroskopie (LIBS). In Abhängigkeit von der Funktionsweise der jeweiligen Methoden werden Informationen zu verschiedensten Bodeneigenschaften wie Nährelementgehalt, Textur und pH-Wert erhalten.
Ziel dieser Arbeit ist die Entwicklung eines Online-LIBS-Verfahrens zur Nährelementbestimmmung und Kartierung von Ackerflächen. Die LIBS ist eine schnelle und simultane Multielementanalyse bei der durch das Fokussieren eines hochenergetischen Laserpulses Probenmaterial von der Probenoberfläche ablatiert wird und in ein Plasma überführt wird. Beim Abkühlen des Plasmas wird Strahlung emittiert, welche Rückschlüsse über die elementare Zusammensetzung der Probe gibt. Diese Arbeit ist im Teilprojekt I4S (Intelligenz für Böden) im Forschungsprogramm BonaRes (Boden als nachhaltige Ressource für die Bioökonomie) des Bundesministerium für Bildung und Forschung (BMBF) entstanden. Es wurden insgesamt 651 Bodenproben von verschiedenen Test-Agrarflächen unterschiedlichster Standorte Deutschlands gemessen, ausgewertet und zu Validierungszwecken mit entsprechender Referenzanalytik wie die Optische Emissionsspektroskopie mittels induktiv gekoppeltem Plasma (ICP-OES) und die wellenlängendispersive Röntgenfluoreszenzanalyse (WDRFA) charakterisiert.
Für die Quantifizierung wurden zunächst die Messparameter des LIBS-Systems auf die Bodenmatrix optimiert und für die Elemente geeignete Linien ausgewählt sowie deren Nachweisgrenzen bestimmt. Es hat sich gezeigt, dass eine absolute Quantifizierung basierend auf einem univariaten Ansatz aufgrund der starken Matrixeffekte und der schlechten Reproduzierbarkeit des Plasmas nur eingeschränkt möglich ist. Bei Verwendung eines multivariaten Ansatz wie der Partial Least Squares Regression (PLSR) für die Kalibrierung konnten für die Nährelemente im Vergleich zur univariaten Variante Analyseergebnisse mit höherer Güte und geringeren Messunsicherheiten ermittelt werden. Die Untersuchungen haben gezeigt, dass das multivariate Modell weiter verbessert werden kann, indem mit einer Vielzahl von gut analysierten Böden verschiedener Standorte, Bodenarten und einem breiten Gehaltsbereich kalibriert wird. Mithilfe der Hauptkomponentenanalyse (PCA) wurde eine Klassifizierung der Böden nach der Textur realisiert. Weiterhin wurde auch eine Kalibrierung mit losem Bodenmaterial erstellt. Trotz der Signalabnahme konnten für die verschiedenen Nährelemente Kalibriergeraden mit ausreichender, analytischer Güte erstellt werden.
Für den Einsatz auf dem Acker wurde außerdem der Einfluss von Korngröße und Feuchtigkeit auf das LIBS-Signal untersucht. Die unterschiedlichen Korngrößen haben nur einen geringen Einfluss auf das LIBS-Signal und das Kalibriermodell lässt sich durch entsprechende Proben leicht anpassen. Dagegen ist der Einfluss der Feuchtigkeit deutlich stärker und hängt stark von der Bodenart ab, sodass für jede Bodenart ein separates Kalibriermodell für verschiedene Feuchtigkeitsgehalte erstellt werden muss. Mithilfe der PCA kann der Feuchtigkeitsgehalt im Boden grob abgeschätzt werden und die entsprechende Kalibrierung ausgewählt werden.
Diese Arbeit liefert essentielle Informationen für eine Echtzeit-Analyse von Nährelementen auf dem Acker mittels LIBS und leistet einen wichtigen Beitrag zu einer fortschrittlichen und zukunftsfähigen Nutzung von Ackerflächen.
Im Rahmen der vom Bundesministerium für Bildung und -forschung geförderten Forschungsinitiative „BonaRes – Boden als nachhaltige Ressource der Bioökonomie“ soll sich das Teilprojekt „I4S – integrated system for site-specific soil fertility management“ der Entwicklung eines integrierten Systems zum ortsspezifischen Management der Bodenfruchtbarkeit widmen. Hierfür ist eine Messplattform zur Bestimmung relevanter Bodeneigenschaften und der quantitativen Analyse ausgewählter Makro- und Mikronährstoffe geplant. In der ersten Phase dieses Projekts liegt das Hauptaugenmerk auf der Kalibrierung und Validierung der verschiedenen Sensoren auf die Matrix Boden, der Probennahme auf dem Acker und der Planung sowie dem Aufbau der Messplattform. Auf dieser Plattform sollen in der zweiten Phase des Projektes die verschiedenen Bodensensoren installiert, sowie Modelle und Entscheidungsalgorithmen zur Steuerung der Düngung und dementsprechend Verbesserung der Bodenfunktionen erstellt werden.
Ziel der vorliegenden Arbeit ist die Grundlagenuntersuchung und Entwicklung einer robusten Online-Analyse mittels Energie-dispersiver Röntgenfluoreszenzspektroskopie (EDRFA) zur Quantifizierung ausgewählter Makro- und Mikronährstoffe in Böden für eine kostengünstige und flächendeckende Kartierung von Ackerflächen. Für die Entwicklung eines Online-Verfahrens wurde ein dem Stand der Technik entsprechender Röntgenfluoreszenzmesskopf in Betrieb genommen und die dazugehörigen Geräteparameter auf die Matrix Boden optimiert. Die Bestimmung der analytischen Qualitäts-merkmale wie Präzision und Nachweisgrenzen fand für eine Auswahl an Nährelementen von Aluminium bis Zink statt. Um eine möglichst Matrix-angepasste Kalibrierung zu erhalten, wurde sowohl mit zertifizierten Referenzmaterialien (CRM), als auch mit Ackerböden kalibriert. Da einer der größten Nachteile der Röntgenfluoreszenzanalyse die Beeinflussung durch Matrixeffekte ist, wurde neben der klassischen univariaten Datenauswertung auch die chemometrische multivariate Methode der Partial Least Squares Regression (PLSR) eingesetzt. Die PLSR bietet dabei den Vorteil, Matrixeffekte auszugleichen, wodurch robustere Kalibriermodelle erhalten werden können. Zusätzlich wurde eine Hauptkomponentenanalyse (PCA) durchgeführt, um Gemeinsamkeiten und Ausreißer innerhalb des Probensets zu identifizieren. Es zeigte sich, dass eine Klassifizierung der Böden anhand ihrer Textur Sand, Schluff, Lehm und Ton möglich ist.
Aufbauend auf den Ergebnissen idealer Bodenproben (zu Tabletten gepresste luftgetrocknete Proben mit Korngrößen < 0,5 mm) wurde im Verlauf dieser Arbeit die Probenvorbereitung immer weiter reduziert und der Einfluss verschiedener Kenngrößen untersucht. Diese Einflussfaktoren können die Dichte und die Homogenität der Probe, sowie Korngrößeneffekte und die Feuchtigkeit sein. Anhand des RMSE (Wurzel der mittleren Fehlerquadratsumme) und unter Berücksichtigung der Residuen werden die jeweils erstellten Kalibriermodelle miteinander verglichen. Um die Güte der Modelle zu bewerten, wurden diese mit einem Testset validiert. Hierfür standen 662 Bodenproben von 15 verschiedenen Standorten in Deutschland zur Verfügung. Da die Ergebnisse an gepressten Tabletten für die Elemente Al, Si, K, Ca, Ti, Mn, Fe und Zn den Anforderungen für eine spätere Online-Analyse entsprechen, wurden im weiteren Verlauf dieser Arbeit Kalibriermodelle mit losen Bodenproben erstellt. Auch hier konnten gute Ergebnisse durch ausreichende Nachweisgrenzen und eine niedrige gemittelte Messabweichung bei der Vorhersage unbekannter Testproben erzielt werden. Es zeigte sich, dass die Vorhersagefähigkeit mit der multivariaten PLSR besser ist als mit der univariaten Datenauswertung, insbesondere für die Elemente Mn und Zn.
Der untersuchte Einfluss der Feuchtigkeit und der Korngrößen auf die Quantifizierung der Elementgehalte war vor allem bei leichteren Elementen deutlich zu sehen. Es konnte schließlich eine multivariate Kalibrierung unter Berücksichtigung dieser Faktoren für die Elemente Al bis Zn erstellt werden, so dass ein Einsatz an Böden auf dem Acker möglich sein sollte. Eine höhere Messunsicherheit muss dabei einkalkuliert werden. Für eine spätere Probennahme auf dem Feld wurde zudem der Unterschied zwischen statischen und dynamischen Messungen betrachtet, wobei sich zeigte, dass beide Varianten genutzt werden können. Zum Abschluss wurde der hier eingesetzte Sensor mit einem kommerziell erhältlichen Hand-Gerät auf sein Quantifizierungspotential hin verglichen. Der Sensor weist anhand seiner Ergebnisse ein großes Potential als Online-Sensor für die Messplattform auf. Die Ergebnisse unter Laborbedingungen zeigen, dass eine robuste Analyse Ackerböden unter Berücksichtigung der Einflussfaktoren möglich ist.
An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise.
Im Rahmen der Integritätsbewertung einer zementierten 13 3/8" Rohrtour einer Sole-Produktionsbohrung wurden erstmals 2018 zeitgleich faseroptische Temperaturmessungen (DTS, Distributed Temperature Sensing) und faseroptische Akustikmessungen (DAS, Distributed Acoustic Sensing) durchgeführt und ausgewertet. Dazu wurde die Bohrung zeitweise mit Stickstoff bespannt und wieder entlastet. Durch die Bespannung der Bohrung mit Stickstoff in Kombination mit dem Herunterdrücken des Stickstoff-Sole-Spiegels unter den Rohrschuh der 13 3/8" Rohrtour, konnte Stickstoff aus der Kavernenbohrung durch eine Leckagestelle in die Zementation übertreten und dort ein Stickstoff-Reservoir bilden.
Bei der anschließenden Stickstoffentlastung erfolgte der Wiederanstieg des Stickstoff-Sole-Spiegels deutlich schneller als die Entleerung des in der Zementation angelegten Stickstoff-Reservoirs. Der dadurch entstandene Druckgradient hatte zur Folge, dass an der Leckagestelle der Stickstoff aus der Zementation in die aufsteigende Sole in Form von Bläschen eingetreten und dort aufgestiegen ist. Dieser Übertritt der Stickstoffbläschen war sowohl mit der Entstehung eines akustischen Geräusches als auch mit einer Temperaturänderung verbunden, welche mit der DAS- und DTS-Technik nachgewiesen werden konnten.
Um die Ergebnisse bzgl. ihres physikalischen Hintergrundes zu überprüfen und basierend auf einer mathematisch-physikalischen Grundlage eine nachvollziehbare Interpretation der Messergebnisse zu ermöglichen, wurde ein numerisches Simulationsmodell der gekoppelten Festkörper- und Druckakustik für die Bohrung aufgebaut. Das Modell berücksichtigt die Geologie und die Komplettierung der Kavernenbohrung. Nach Identifikation der Schallquelle konnte mit dem Modell die Ausbreitung des Schalldrucks in der Bohrung erfolgreich nachgestellt werden.
Um dieses Verfahren einer simultanen DAS-DTS-Messung in eine feldtaugliche Version zu überführen, läuft seit November 2019 ein breit angelegtes und vom BMWi gefördertes ZIM-Kooperationsprojekt zwischen der Bundesanstalt für Materialforschung und -prüfung (BAM), der IAB Weimar gGmbH, der GESO GmbH & Co. Projekt KG, der DEEP.KBB GmbH sowie der Rembe Consulting PartG mbB.
Durch die Messdatenkopplung und den Wegfall der bewegungsbedingten Nachteile einer Messsonde werden präzisere Ergebnisse zur Bewertung der Bohrlochintegrität erwartet. Das Ziel ist, mit Hilfe der noch zu entwickelnden einfachen und robusten Technik, quantitative Aussagen über die Zustände im verrohrten Bohrloch direkt am Messplatz treffen zu können, wobei ein Fokus auf Detektierung und Quantifizierung von Kleinstleckagen liegt. Im Rahmen dieses Forschungsprojektes kommt neben numerischen Berechnungen auch ein geplanter Bohrlochsimulator zum Einsatz, mit dem umfangreiche Untersuchungen zur Ermittlung der Grenzparameter und Detektionsschwellen durchgeführt werden sollen.
Climate change, CO2 reduction, resource efficiency are only 3 current keywords that describe the current industrial-economic situation. In order to influence climate change effectively, the conversion of supply systems with technically usable forms of energy must succeed in the next decade. The international network founded in Baku in 2015 bundles research activities in the broad field of energy supply and energy efficiency.
Discuss current research approaches and results with scientists and experts from renowned universities and follow Azerbaijan's efforts to implement the energy revolution.
In the DECHEMA Virtual Talks, general aspects of the safety and acceptance of hydrogen technologies were presented. How can trust in new technologies be built when past accidents led to myths and fairy tales? The presentation does away with general prejudices and shows that handling hydrogen is neither more unsafe nor safer than handling other fuel gases. The basis for the safe handling of hydrogen is always a risk analysis.
Elastomer seals are used in many industrial applications due to their excellent mechanical properties at a wide range of temperatures. Their high versatility and recovery potential under several load conditions make them well suitable for the application in containers designed for transport, storage and/or disposal of radioactive materials. In containers for low and intermediate level radioactive waste, elastomer seals are used as barrier seals, and as auxiliary seals in storage and transportation casks (dual purpose casks) for heat generating radioactive waste, such as spent fuel and high-level waste. While a seal exchange at defined intervals is typical in many conventional applications, it is impossible or at least hard to perform when principles of minimization of radiation exposure have to be considered and prohibit an unnecessary cask handling. An extensive knowledge of the change of the elastomer’s properties during aging and the availability of reliable end-of-lifetime criteria to guarantee the permanent safe enclosure of the radioactive material is mandatory. As BAM is involved in most of the national cask licensing procedures and in the evaluation of cask-related long-term safety issues, great efforts have been already made and are still planned to scientifically support this task.
Compression stress relaxation and compression set were identified as key indicators of elastomer long-term performance and quantitatively investigated in comprehensive test programs. Among other representative types of elastomers, specimens made from ethylene propylene diene rubber (EPDM) were tested before, during and after aging to capture the most important of their complex mechanical properties.
In the presented study, exemplary results were used to simulate the compression stress relaxation and the compression set of elastomer O-rings during aging. Regarding the influence of temperature, the time temperature superposition principle is applied in the relaxation analysis of elastomer O-rings. The proposed model is implemented in the commercial finite element software ABAQUS/Standard® [1] with a sequential temperature displacement coupling. Numerical results match the experimental compression stress relaxation measurements well. The prediction of compression set values after long-term aging shows a relatively good agreement with the experimental results. Nevertheless, all input parameters derived from the specimen tests, additional assumptions concerning boundary conditions and modeling strategy are discussed with regard to the identified slight discrepancies.
The possibility to extend the finite element model to represent the O-ring seal’s ability to recover after a (fast) partial release is taken into account
Polycarboxylate ethers (PCEs) are widely used in construction, but the exact nature of their interaction with cement is still debated. Aiming at a better understanding of the role of tricalcium Aluminate (C3A) in cement hydration, we assessed the potential of optical spectroscopy in combination with a water-soluble fluorescent organic reporter dye (S0586) to monitor the early hydration of C3A in the presence of 26 wt% CaSO4.2H2O (C3A26G-S) with and without PCE. As optical methods, steady-state fluorescence and diffuse reflectance (UV–VisDR) spectroscopy were employed. Phase characterization and particle size distribution were performed with in-situ X-ray diffraction (in-situ XRD) and dynamic light scattering (DLS). Our results show that fluorescence and UV–VisDR spectroscopy can be used to monitor the formation of metastable phases by the disaggregation of the dye S0586 in a cement paste as well as changes in ettringite formation. Addition of PCE slowed down the disaggregation of the dye as reflected by the corresponding changes of the dyes absorption and fluorescence. This prolonged induction period is a well-known side effect of PCEs and agrees with previous reported calorimetric studies and the Inhibition of gypsum dissolution observed by in-situ XRD. This demonstrates that fluorescence and UV–VisDR spectroscopy together with a suitable optical probe can provide deeper insights into the influence of PCE on C3A-gypsum hydration which could be e.g., utilized as screening method for comparing the influences
of different types of PCEs.
The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone.
We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs.
Redox switches are applied in various fields of research, including molecular lifts, electronic devices and sensors. Switching the absorbance between UV and Vis/NIR by redox processes is of interest for applications in light harvesting or biomedicine.
Here, we present a series of push-pull benzothiadiazole derivatives with high fluorescence quantum yields in solution and in the crystalline solid state. Spectroelectrochemical analysis reveals the switching of UV-absorption in the neutral state to Vis/NIR absorption in the reduced state. We identify the partial irreversibility of the switching process, which appears to be reversible on the cyclic voltammetry timescale.