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Paper des Monats
- ja (68)
The choice of a pure cohesive or a pure frictional viscoplastic model to represent the rheological behaviour of a flowslide is of paramount importance in order to obtain accurate results for real cases. The principal Goal of the present work is to clarify the influence of the type of viscous model—pure cohesive versus pure frictional—with the numerical reproduction of two different real flowslides that occurred in 1966: the Aberfan flowslide and the Gypsum tailings impoundment flowslide. In the present work, a depth-integrated model based on the v-pw Biot–Zienkiewicz formulation, enhanced with a diffusion-like equation to account for the pore pressure Evolution within the soil mass, is applied to both 1966 cases. For the Aberfan flowslide, a frictional viscous model based on Perzyna viscoplasticity is considered, while a pure cohesive viscous model (Bingham model) is considered for the case of the Gypsum flowslide. The numerical approach followed is the SPH method, which has been enriched by adding a 1D finite difference grid to each SPH node in order to improve the description of the pore water evolution in the propagating mixture. The results obtained by the performed simulations are in agreement with the documentation obtained through the UK National Archive (Aberfan flowslide) and the International Commission of large Dams (Gypsum flowslide).
Bees are considered to be threatened globally, with severe overwinter losses of the most important commercial pollinator, the Western honeybee, a major concern in the Northern Hemisphere. Emerging infectious diseases have risen to prominence due to their temporal correlation with colony losses. Among these is Deformed wing virus (DWV), which has been frequently linked to colony mortality. We now provide evidence of a strong statistical association between overwintering colony decline in the field and the presence of DWV genotype-B (DWV-B), a genetic variant of DWV that has recently been shown to be more virulent than the original DWV genotype-A. We link the prevalence of DWV-B directly to a quantitative measure of overwinter decline (workforce mortality) of honeybee colonies in the field. We demonstrate that increased prevalence of virus infection in individual bees is associated with higher overwinter mortality. We also observed a substantial reduction of infected colonies in the spring, suggesting that virus-infected individuals had died during the winter. Our findings demonstrate that DWV-B, plus possible A/B recombinants exhibiting DWV-B at PCR primer binding sites, may be a major cause of elevated overwinter honeybee loss. Its potential emergence in naïve populations of bees may have far-reaching ecological and economic impacts.
Unity in defence: honeybee workers exhibit conserved molecular responses to diverse pathogens
(2017)
Background: Organisms typically face infection by diverse pathogens, and hosts are thought to have developed specific responses to each type of pathogen they encounter. The advent of transcriptomics now makes it possible to test this hypothesis and compare host gene expression responses to multiple pathogens at a genome-wide scale. Here, we performed a meta-analysis of multiple published and new transcriptomes using a newly developed bioinformatics approach that filters genes based on their expression profile across datasets. Thereby, we identified common and unique molecular responses of a model host species, the honey bee (Apis mellifera), to its major pathogens and parasites: the Microsporidia Nosema apis and Nosema ceranae, RNA viruses, and the ectoparasitic mite Varroa destructor, which transmits viruses.
Results: We identified a common suite of genes and conserved molecular pathways that respond to all investigated pathogens, a result that suggests a commonality in response mechanisms to diverse pathogens. We found that genes differentially expressed after infection exhibit a higher evolutionary rate than non-differentially expressed genes. Using our new bioinformatics approach, we unveiled additional pathogen-specific responses of honey bees; we found that apoptosis appeared to be an important response following microsporidian infection, while genes from the immune signalling pathways, Toll and Imd, were differentially expressed after Varroa/virus infection. Finally, we applied our bioinformatics approach and generated a gene co-expression network to identify highly connected (hub) genes that may represent important mediators and regulators of anti-pathogen responses.
Conclusions: Our meta-analysis generated a comprehensive overview of the host metabolic and other biological processes that mediate interactions between insects and their pathogens. We identified key host genes and pathways that respond to phylogenetically diverse pathogens, representing an important source for future functional studies as well as offering new routes to identify or generate pathogen resilient honey bee stocks. The statistical and bioinformatics approaches that were developed for this study are broadly applicable to synthesize information across transcriptomic datasets. These approaches will likely have utility in addressing a variety of biological questions.
A complex measuring campaign has been performed including the simultaneous measurement of vehicle, track, and soil vibrations during train runs at 16, 25, 40, 63, 80, 100, 125, 140, 160 km/h, and impulse measurements of the passenger car, three track sections and the soil. A ballast track on the soil surface and on a concrete bridge have been investigated as well as a slab track in a tunnel. The evaluation and comparison of all these data shows a generally good agreement for all components if the strong low- and high-frequency cut-off characteristics of the layered and damped soil are incorporated. There is a strong causal correlation between the vehicle and the soil by the dynamic excitation forces and a weak relation between the track and the soil by the axle-sequence spectrum of the train. However, the similarity between the axle-impulse spectrum observed at the track and the spectra of the ground vibration lead to the special excitation component of “scattered axle impulses” which is pre-dominant at the far-field points of the soil.
The objective of this work is to report the improvement obtained in the discrimination of complex aroma and taste with subtle differences in odor and flavor, by the use of fast suitable procedures for the cases of measurements in the field demanding decision-making in real time. The proposed electronic sensing systems, formed by an E-nose and VE-tongue, were used to discriminate cumin cultivars from different geographical origins, as well as to quantify the cumin adulteration percentages by using unsupervised and supervised chemometric tools. Thus, the results obtained are sufficiently encouraging as a starting point for the development of new electronic sensing systems with more improvement such the reliability of the sensors’ performance as well as the chemometric tools in order to deal with a complex dataset.
The order Chaetothyriales (Pezizomycotina, Ascomycetes) harbours obligatorily melanised fungi and includes numerous etiologic agents of chromoblastomycosis, phaeohyphomycosis and other diseases of vertebrate hosts. Diseases range from mild cutaneous to fatal cerebral or disseminated infections and affect humans and cold-blooded animals globally. In addition, Chaetothyriales comprise species with aquatic, rock-inhabiting, ant-associated, and mycoparasitic life-styles, as well as species that tolerate toxic compounds, suggesting a high degree of versatile extremotolerance. To understand their biology and divergent niche occupation, we sequenced and annotated a set of 23 genomes of main the human opportunists within the Chaetothyriales as well as related environmental species. Our analyses included fungi with diverse life-styles, namely opportunistic pathogens and closely related saprobes, to identify genomic adaptations related to pathogenesis. Furthermore, ecological preferences of Chaetothyriales were analysed, in conjuncture with the order-level phylogeny based on conserved ribosomal genes. General characteristics, phylogenomic relationships, transposable elements, sex-related genes, protein family evolution, genes related to protein degradation (MEROPS), carbohydrate-active enzymes (CAZymes), melanin synthesis and secondary metabolism were investigated and compared between species. Genome assemblies varied from 25.81 Mb (Capronia coronata) to 43.03 Mb (Cladophialophora immunda). The bantiana-clade contained the highest number of predicted genes (12 817 on average) as well as larger genomes. We found a low content of mobile elements, with DNA transposons from Tc1/Mariner superfamily being the most abundant across analysed species. Additionally, we identified a reduction of carbohydrate degrading enzymes, specifically many of the Glycosyl Hydrolase (GH) class, while most of the Pectin Lyase (PL) genes were lost in etiological agents of chromoblastomycosis and phaeohyphomycosis. An expansion was found in protein degrading peptidase enzyme families S12 (serine-type D-Ala-D-Ala carboxypeptidases) and M38 (isoaspartyl dipeptidases). Based on genomic information, a wide range of abilities of melanin biosynthesis was revealed; genes related to metabolically distinct DHN, DOPA and pyomelanin pathways were identified. The MAT (MAting Type) locus and other sexrelated genes were recognized in all 23 black fungi. Members of the asexual genera Fonsecaea and Cladophialophora appear to be heterothallic with a single copy of either MAT-1-1 or MAT-1-2 in each individual. All Capronia species are homothallic as both MAT1-1 and MAT1-2 genes were found in each single genome. The genomic synteny of the MAT-locus flanking genes (SLA2-APN2-COX13) is not conserved in black fungi as is commonly observed in Eurotiomycetes, indicating a unique genomic context for MAT in those species. The heterokaryon (het) genes expansion associated with the low selective pressure at the MAT-locus suggests that a parasexual cycle may play an important role in generating diversity among those fungi.
Seabird excrements (guano) have been preserved in the arid climate of Northern Chile since at least the Pliocene. The deposits of marine organic material in coastal areas potentially open a window into the present and past composition of the coastal ocean and its food web. We use the stable isotope composition of nitrogen and carbon as well as element contents to compare the principal prey of the birds, the Peruvian anchovy, with the composition of modern guano. We also investigate the impact of diagenetic changes on the isotopic composition and elemental contents of the pure ornithogenic sediments, starting with modern stratified deposits and extending to fossil guano. Where possible, 14C systematics is used for age information. The nitrogen and carbon isotopic composition of the marine prey (Peruvian anchovy) of the birds is complex as it shows strong systematic variations with latitude. The detailed study of a modern profile that represents a few years of guano deposition up to present reveals systematic changes in nitrogen and carbon isotopic composition towards heavier values that increase with age, i.e. depth. Only the uppermost, youngest layers of modern guano show compositional affinity to the prey of the birds. In the profile, the simultaneous loss of nitrogen and carbon occurs by degassing, and non-volatile elements like phosphorous and calcium are passively enriched in the residual guano. Fossil guano deposits are very low in nitrogen and low in carbon contents, and show very heavy nitrogen isotopic compositions. One result of the study is that the use of guano for tracing nitrogen and carbon isotopic and elemental composition in the marine food web of the birds is restricted to fresh material. Despite systematic changes during diagenesis, there is little promise to retrieve reliable values of marine nitrogen and carbon signatures from older guano. However, the changes in isotopic composition from primary marine nitrogen isotopic signatures towards very heavy values generate a compositionally unique material. These compositions trace the presence of guano in natural ecosystems and its use as fertilizer in present and past agriculture.
Sowohl die 3D-Formbestimmung als auch die Thermografie sind Verfahren der Qualitätssicherung. Im vorgestellten Projekt wird versucht, die beiden Methoden zusammenzuführen.
Das Prinzip des für die Formbestimmung verwendeten 3D-Scanners beruht auf dem bereits bekannten Verfahren der Streifenlichtprojektion. Die Neuartigkeit des hier verwendeten 3D-Scanners besteht darin, dass nicht im sichtbaren, sondern im infraroten Spektralbereich gearbeitet wird. Dadurch wird es möglich, nicht die Reflexion, sondern die Wärmestrahlung des Prüfobjektes nach Absorption der eingebrachten Strahlung auszuwerten. Dies ermöglicht, auch optisch „nicht-kooperative“ Oberflächen zu erfassen. Die Anregung mit Wärmestrahlung stellt das Bindeglied zum Verfahren der aktiven Thermografie für die Detektion verdeckter Schäden dar. Bei letzterem Verfahren wird der Wärmestau über Defekten beim Eindringen der Wärme in die Tiefe des Materials gemessen. Dabei stellen Defekte eine Störung des 3D-Scan-Verfahrens dar, während umgekehrt unregelmäßig geformte Oberflächen das thermografische Verfahren erschweren, d.h. der Messeffekt eines der Verfahren ist ein Störeffekt für das jeweils andere Verfahren.
Es wird zum einen der Frage nachgegangen, inwieweit das 3D-Scan-Verfahren durch verdeckte thermische Defekte beeinträchtigt wird, und zum anderen die Möglichkeit untersucht, den vorhandenen 3D-Scanner auch für die aktive Thermografie einzusetzen. Es werden CFK-Proben mit künstlich eingebrachten thermischen Defekten untersucht und die Möglichkeiten und Grenzen der vorhandenen Messapparatur für die Defekterkennung aufgezeigt.
Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances.
Die Synchrotron-Refraktions-Topographie basiert auf der Brechung von Röntgenstrahlung an den Grenzflächen zwischen Materialien mit unterschiedlichem Brechungsindex. Refraktionseffekte verändern die Ausbreitungsrichtung der Röntgenstrahlung, welche mit Hilfe der Methode des Analyser-Based Imaging analysiert wird. Dabei wird ein Silizium-Einkristall im Strahlengang zwischen Probe und Detektor platziert. Dieser Analysator-Kristall filtert, innerhalb seiner Streuebene, die Röntgenstrahlung gemäß ihrer Ausbreitungsrichtung. Durch das Rastern verschiedener Winkelpositionen des Analysator-Kristalls erhält man das Winkelspektrum der von der Probe gebrochenen Strahlung. Aus dieser Rocking Curve lässt sich die spezifische innere Oberfläche der Probe bestimmen. Diese Information wird über einen 2D-Detektor mit einer nominellen Pixelgröße von 3,6 μm gewonnen. Die Installation einer Zugprüfmaschine ermöglicht es die Proben in verschiedenen Lastzuständen insitu zu untersuchen. Damit ist es möglich die spezifische innere Oberfläche in Abhängigkeit der Last darzustellen und so Schädigungsmechanismen abzuleiten. Der Vorteil bei der Ausnutzung des Refraktionseffekts gegenüber der einfachen Durchstrahlung ist die höhere Sensitivität gegenüber Defekten mit geringem Volumen aber großer Oberfläche. Somit werden auch Mikrorisse und, speziell bei Kompositen, die Enthaftung zwischen Matrix und Verstärkung (Partikel, Fasern) erfasst. In dieser Studie wurden Metall-Matrix-Komposite bestehend aus einer Aluminium-Matrix verstärkt mit Aluminiumoxid-Partikeln untersucht. Hierzu wurden knochenförmige Zugproben präpariert, deren Messlänge einen rechteckigen Querschnitt von 1,7 mm × 1,3 mm aufwies. Die Proben wurden einem Zugversuch unterzogen, welcher in Intervallen unterbrochen wurde. Bei jeder Unterbrechung wurde unter quasi-statischer Last die Rocking Curve gemessen und ein Radiogramm der spezifischen inneren Oberflächen berechnet. Dabei konnte ab dem Erreichen einer Last von ca. 600 N ein Anstieg der spezifischen inneren Oberfläche beobachtet werden. Demgegenüber zeigen die zum Vergleich durchgeführten Durchstrahlungsaufnahmen keinerlei Defekte. Daher belegt diese Untersuchung das Potential der Refraktion-Topographie zur frühzeitigen Erkennung von Schädigungen mit hoher Empfindlichkeit.
In unserer heutigen Zeit werden die Zwischenräume innerhalb der einzelnen Abteilungen eines Betriebs und zwischen einzelnen nationalen oder globalen Akteuren immer wichtiger: Produzierbarkeit vs. Wirtschaftlichkeit, Fortschritt vs. Nachhaltigkeit. Auch die zerstörungsfreie Prüfung (ZfP) – bisher hauptsächlich als Endkontrolle oder Wartungselement wahrgenommen – kann und sollte im Wandel der Digitalisierung und Industrie 4.0 einen neuen Stellenwert erhalten.
Die ZfP kann schon während der Konstruktion helfen, sichere und zuverlässige Produkte zu erstellen. Jedoch müssen dafür eine adäquate Informationskultur und die notwendigen Kennzahlen vorhanden sein. Objektive, probabilistische Kennzahlen (wie die POD - Auffindwahrscheinlichkeit) sind hierbei der Schlüssel. Diese müssen jedoch unbedingt an Prüfverfahren, Prüfgegenstand und Prüfbedingung angepasst werden, da sonst die gesamte Aussage in Frage zu stellen ist. Im Vortrag werden Beispiele aus der Anwendung gezeigt, die die Aussagekraft der Kennzahl aber auch die Sorgfalt, mit denen die einzelnen Aussagen genutzt werden, unterstrichen werden soll. Bewertung von Daten von realen Fehler, Anpassung an die Bruchfestigkeit und die Betrachtung von mehreren Prüfparametern am Beispiel der Bewertung von radiographischen, Ultraschall- und Wirbelstromprüfung werden in dem Vortrag gezeigt.
Dass die Zuverlässigkeit der ZfP eine sehr wichtige Rolle bei der Bewertung sicherheitsrelevanter Systeme spielt, ist bekannt. Laut dem modularen Zuverlässigkeitsmodell für zerstörungsfreie Prüfprozesse hängt die Zuverlässigkeit von der innewohnenden (physikalisch-technischen) Fähigkeit der Prüfsystems, den Anwendungsparametern, den menschlichen Faktoren und dem organisatorischen Kontext ab. Seit Einführung des Modells während des ersten Workshops zur Zuverlässigkeit der ZfP (European-American Workshop on Reliability of NDE) wurde das Modell in weiteren fünf Workshops stetig weiterentwickelt, diskutiert und an den Stand der Wissenschaft angepasst. Das Ziel dieser Publikation ist es, den aktuellen Stand der Diskussion und die neusten Fragestellungen der internationalen Zuverlässigkeitsgemeinschaft vorzustellen. Im Einzelnen werden die Entwicklung fortgeschrittener Modelle zur Bewertung der Probability of Detection (POD), Bewertungsansätze im Bereich Structural Health Monitoring und Fragestellungen zu den menschlichen Faktoren dargestellt. Besonderer Wert wurde sowohl auf die Entwicklung, als auch auf die Anwendung der Ansätze in der industriellen Praxis gelegt.
Im vergangenen Jahrzehnt sind gitterinterferometrische Röntgenabbildungen zunehmend in den Fokus des Interesses gerückt. Sie sind insbesondere dann Vorteil, wenn der in der Standardradiographie erreichbare Kontrast nicht genügt, schwach absorbierende Mikro- und Nanostrukturen abzubilden.
Auf Kosten mehrerer Aufnahmen gestattet die Talbot-Lau Gitterinterferometrie, die Beiträge aus Absorption, Refraktion und (refraktiver) Streuung zu trennen. Dazu werden die Störungen der Interferenzmuster von Phasengittern ausgewertet. Im Gegensatz zu einer Vielzahl anderer refraktionsbasierter Abbildungsmethoden kann diese Technik mit konventionellen Röntgenröhren (mit divergenter, polychromatischer Strahlung) angewendet werden. Damit ist die Technik geeignet, typische ZfP-Fragestellungen zu lösen.
Hier stellen wir Untersuchungen zur Effizienz von Phasengittern vor. Die Visibilität (d.h. die Höhe der Oszillation im Interferenzmuster) wird als Funktion verschiedener geometrischer Parameter verfolgt. Eine Rotation um die Achse parallel zu den Gitterstegen ändert die Form des Gitterprofils (d.h. die Verteilung der Phasenschiebungen). Die kontinuierliche Variation des Winkels und des Detektionsabstandes führt zur Identifikation von ausgezeichneten Kombinationen mit maximaler Visibilität, wobei die Abstände deutlich geringer sind als im Standardaufbau mit senkrechter Gitterbestrahlung.
Unsere Studie umfasst Simulationen für monochromatische Quelle und den Vergleich zu experimentellen Ergebnissen mit der Synchrotronstrahlung.
In der Literatur wurden die Vorteile der Talbot-Lau Interferometrie für die zerstörungsfreie Prüfung von Faserkompositen und Verbundwerkstoffen demonstriert. Hier werden als Beispiele Messungen an Aluminiumtitanat (Al2TiO5) Pulver gezeigt.
Recently, there has been a rise in freshwater harmful algal blooms (HABs) globally, as well as increasing aquaculture practices. HABs can produce cyanotoxins, many of which are hepatotoxins. An ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for nine cyanotoxins across three classes including six microcystins, nodularin, cylindrospermopsin and anatoxin-a. The method was used to analyse free cyanotoxin(s) in muscle (n = 34), liver (n = 17) and egg (n = 9) tissue samples of 34 fish sourced from aquaculture farms in Southeast Asia. Conjugated microcystin was analysed by Lemieux oxidation to ascertain the total amount of microcystin present in muscle. Some tilapia accumulated free microcystin-LR in the muscle tissue at a mean of 15.45 μg/kg dry weight (dw), with total microcystin levels detected at a mean level of 110.1 μg/kg dw, indicating that the amount of conjugated or masked microcystin present in the fish muscle accounted for 85% of the total. Higher levels of cyanotoxin were detected in the livers, with approximately 60% of those tested being positive for microcystin-LR and microcystin-LF, along with cylindrospermopsin. Two fish from one of the aquaculture farms contained cylindrospermopsin in the eggs; the first time this has been reported. The estimated daily intake for free and total microcystins in fish muscle tissue was 2 and 14 times higher, respectively, than the tolerable daily intake value. This survey presents the requirement for further monitoring of cyanotoxins, including masked microcystins, in aquaculture farming in these regions and beyond, along with the implementation of guidelines to safeguard human health.
Air pollution and climate change are potential drivers for the increasing burden of allergic diseases. The molecular mechanisms by which air pollutants and climate parameters may influence allergic diseases, however, are complex and elusive. This article provides an overview of physical, chemical and biological interactions between air pollution, climate change, allergens, adjuvants and the immune system, addressing how these interactions may promote the development of allergies. We reviewed and synthesized key findings from atmospheric, climate, and biomedical research. The current state of knowledge, open questions, and future research perspectives are outlined and discussed. The Anthropocene, as the present era of globally pervasive anthropogenic influence on planet Earth and, thus, on the human environment, is characterized by a strong increase of carbon dioxide, ozone, nitrogen oxides, and combustion- or traffic-related particulate matter in the atmosphere. These environmental factors can enhance the abundance and induce chemical modifications of allergens, increase oxidative stress in the human body, and skew the immune system toward allergic reactions. In particular, air pollutants can act as adjuvants and alter the immunogenicity of allergenic proteins, while climate change affects the atmospheric abundance and human exposure to bioaerosols and aeroallergens. To fully understand and effectively mitigate the adverse effects of air pollution and climate change on allergic diseases, several challenges remain to be resolved. Among these are the identification and quantification of immunochemical reaction pathways involving allergens and adjuvants under relevant environmental and physiological conditions.
Verbesserung und Qualifizierung der Ultraschallprüfung von Mischnähten im Primärkreis von KKW
(2017)
Die im Primärkreislauf von Kernkraftwerken anzutreffenden austenitischen Schweiß- und Mischnähte sind nicht nur extrem sicherheitsrelevant, sondern stellen auch sehr hohe Anforderungen an die Materialprüfung. Neben der eingeschränkten Zugänglichkeit ist das makroskopische Gefüge der Schweißnaht für die Prüfung mit Ultraschall von höchster Bedeutung.
Um Materialfehler zuverlässig in Position und Größe bestimmen zu können, müssen die Kornorientierungen und die elastischen Konstanten des anisotropen Schweißnahtgefüges bekannt sein. Für die bildgebende Darstellung möglicher Materialfehler kommen folgende Arbeitsschritte zum Einsatz: Zunächst wird die Schweißnaht durchschallt, um mit einem inversen Verfahren wichtige Schweißnahtparameter wie beispielsweise die Kornorientierung bestimmen zu können. Auf der Basis dieser Parameter werden im nächsten Schritt die Schallwege mittels Raytracing (RT) simuliert. Zuletzt werden dieser RT-Simulation die Messdaten (A-Scans) von verschiedenen Sender- und Empfängerpositionen zugeordnet und nach der SAFT-Methode (Synthetic Aperature Focusing Technique) zeitaufgelöst überlagert. Die Kombination aus inversem Verfahren, RT und SAFT gewährleistet auch in anisotropen Werkstoffen eine ortsrichtige Visualisierung der Fehler.
Wir erläutern diese drei Verfahren und stellen die Prüfanordnung von Prüfkörpern mit künstlichen Testfehlern vor. Messdaten sowie deren Auswertung werden mit den Ergebnissen einer CIVA-Simulation verglichen.
Da kohlenstofffaserverstärkte Kunststoffe (CFK) in anspruchsvollen sicherheitsrelevanten Einsatzgebieten wie im Automobilbau und in der Luftfahrt eingesetzt werden, besteht ein zunehmender Bedarf an zerstörungsfreien Prüfmethoden. Ziel ist die Gewährleistung der Sicherheit und Zuverlässigkeit der eingesetzten Bauteile. Aktive Thermografieverfahren ermöglichen die effiziente Prüfung großer Flächen mit hoher Auflösung in wenigen Arbeitsschritten. Ein wichtiges Teilgebiet der Prüfungen ist die Ortung und Charakterisierung von Delaminationen, die sowohl bereits in der Fertigung als auch während der Nutzung eines Bauteils auftreten können, und dessen strukturelle Integrität schwächen.
In diesem Beitrag werden CFK-Strukturen mit künstlichen und natürlichen Delaminationen mit Hilfe unterschiedlich zeitlich modulierter Strahlungsquellen experimentell untersucht. Verwendet werden dabei Anregungen mit Blitzlampen und mit frequenzmodulierten Halogenlampen. Mittels Filterfunktionen im Zeit- und Frequenzbereich wird das Kontrast-zu-Rausch-Verhältnis (CNR) der detektierten Fehlstellen optimiert. Verglichen werden anschließend die Nachweisempfindlichkeit, das CNR und die Ortsauflösung der zu charakterisierenden Delaminationen für die unterschiedlichen Anregungs- und Auswertungstechniken. Ergänzt werden die Experimente durch numerische Simulationen des dreidimensionalen Wärmetransportes.
The determination of the microscopic dose-damage relationship for DNA in an aqueous environment is of a fundamental interest for dosimetry and applications in radiation therapy and protection. We combine geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We juxtaposition these results to the experimentally determined damage to obtain the dose-damage relationship at a molecular level. This approach is tested for an experimentally challenging system concerning the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here a microscopic target model for the plasmid DNA based on the relation of lineal energy and radiation quality is used to calculate the effective target volume. It was found that on average fewer than two ionizations within a 7.5-nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E1/2=6±4 eV. The presented method is applicable for ionizing radiation (e.g., γ rays, x rays, and electrons) and a variety of targets, such as DNA, proteins, or cells.
The report on the results of an in vitro digestion study of silver nanoparticles in presence and absenceof food. The particles were poly(acrylic acid) stabilized ultra-small silver nanoparticles with a radius of 3.1 nm and a relative size distribution width of 0.2. As food components oil, starch, skimmed milk powderand a mixture thereof were chosen. Aggregation of the particles was quantified with small-angle X-rayscattering in terms of log-normal radii distributions. Complete aggregation of the primary particles wasdetermined in the absence of food. In contrast, the presence of oil and starch initiates a disaggregationin the intestine. Only small aggregates of 6 nm radii and aggregation numbers of 7 were found in thepresence of milk powder. It prevents primary particles from etching in the gastric and intestinal juice.Our results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form butundergo a strong and food-dependent transformation in their state of aggregation.
In vielen Bereichen der Technik haben Konstruktionen unter Einsatz von CFK-Bauteilen und Komponenten die klassischen Metalle abgelöst. Die zerstörungsfreie Prüfung solcher CFK-Bauteile gewinnt somit zunehmend an Bedeutung. Ein mögliches Prüfverfahren ist dabei die Wirbelstromprüfung. Aufgrund der relativ geringen elektrischen Leitfähigkeit von CFK-Komponenten kommt hierbei häufig die sogenannte HF-Wirbelstromprüfung zum Einsatz.
In verschiedenen Untersuchungen der BAM konnten jedoch auch mit Wirbelstromprüfsystemen in niedrigen Frequenzbereichen gute Ergebnisse erzielt werden. Um die Möglichkeiten und Grenzen dieser konventionellen Wirbelstromprüfung auszuloten, wurden Messungen an Versuchskörpern durchgeführt, welche bereits bei der Validierung der Blitz- und Lock-in-Thermografie für neue Verfahrensnormen erfolgreich eingesetzt wurden. Ein Typ dieser Versuchskörper sind Flachproben aus CFK von 6 mm Dicke. In diesen wurden Flachbodenbohrungen mit Durchmessern zwischen 4 mm und 24 mm eingebracht. Die Restwandstärken liegen zwischen 0,06 mm und 3,66 mm. Ein weiterer CFK-Versuchskörper hat die Geometrie eines Stufenkeiles. Bei verschiedenen Stufenkeilen sind Wanddicken zwischen 1,4 mm und 5,4 mm realisiert worden. In diesen wurden künstliche quadratische Delaminationen mit Kantenlängen zwischen 2 mm und 20 mm eingebracht. Die Ergebnisse der Wirbelstromprüfung werden denen der aktiven Thermografie gegenübergestellt.
Zur Nachbildung von Kompositwerkstoffen wurden die flachen Versuchskörper mit geeigneten Versuchskörpern aus Aluminium und Stahl kombiniert. Die Wirbelstromprüfungen wurden mit einem handelsüblichen Prüfgerät im Frequenzbereich zwischen 500 Hz und 3 MHz und entsprechend angepassten Sensoren durchgeführt.
Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wird in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes ist die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen (CFK) am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen.
Ein Schwerpunkt in diesem Projekt ist die Bereitstellung geeigneter ZfP-Methoden. Dabei geht es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In diesem Vortrag werden Prüfsysteme und Prüfergebnisse der „konventionellen“ Wirbelstromprüfung vorgestellt. In einem ersten Schritt wurden Versuche an bereits geschädigten Druckgefäßen durchgeführt. Dabei wurden Druckgefäße mit den Materialpaarungen Stahl-CFK, Aluminium-CFK und Kunststoff-CFK untersucht. Die Dicken der CFK-Schichten reichten hierbei von ca. 4 mm bis ca. 8 mm. Anfangs wurden die Gefäße mit verschiedenen Sensoren von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. In einem zweiten Schritt wurden die Gefäße von innen geprüft. Hierbei bestand die besondere Herausforderung in der Prüfung eines Zylinders von 150 mm Durchmesser durch einen Zugang von nur 15 mm Durchmesser.
Mit den bei diesen Vorversuchen optimierten Prüfsystemen wurden dann begleitende Prüfungen bei Alterungsversuchen durchgeführt. In den Alterungsversuchen wurden Druckbehälter mit einem ca. 4 mm dicken Aluminiumliner und ca. 3,5 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Flaschen sind Atemschutzgeräte bei der Feuerwehr. Die verschiedenen Prüfsysteme und die mit ihnen erzielten Ergebnisse werden vorgestellt.
Regelwerke zur zerstörungsfreien Bestimmung des Reinheitsgrades wie das SEP 1927 und die ASTM E588 erreichen ihre Vergleichbarkeit unter Anwendung von - vergleichsweise einfachen - Referenzfehlern. Hinsichtlich Realisierbarkeit wird somit der Kompromiss zwischen Herstellung des Referenzfehlers und der erreichbaren Nachweisgrenze gefunden. Zur Weiterentwicklung über die Grenzen der SEP1927 hinaus, wurde der Versuch unternommen Fehler kleiner 500 μm herzustellen - welche aufgrund der geringen geometrischen Ausdehnung fertigungsbedingt schwierig zu realisieren sind. Bei den vergleichenden Untersuchungen kristallisierten sich zwei Fertigungsverfahren, Funkenerosion (EDM: electrical discharge maching) und die Fertigung der Bohrungen unter Verwendung eines Hochleistungslasers, als vielversprechend heraus. Zunächst wurden die Fehler mit beiden Verfahren in unterschiedlichen Größen (100, 250 und 100 μm) und Tiefen (1, 1,5 und 2 mm) unter Anwendung von computertomographischen Verfahren der Röntgenprüfung, die Geometrie der eingebrachten Fehlstellen und anschließend durch hochauflösende Tauchtechnikmessungen das Reflektionsverhalten charakterisiert.
Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users.
The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively).
First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments.
Four materials were investigated in pH 13 solution for 14 days
- 3D-Printer-Polymer was completely resolved
- PVC has no noticeable decrease in weight
- (VitaPro) glass filter for the sensor protector, has weight loss 2.7 %
- The epoxy resin has increased by 1.8 % due to moisture expansion
Different concrete samples were prepared for the validation of the systems.
RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring.
The genome of the Halomonas elongata type strain DSM 2581, an industrial producer, was reevaluated using the Illumina HiSeq2500 technology. To resolve duplication-associated ambiguities, PCR products were generated and sequenced. Outside of duplications, 72 sequence corrections were required, of which 24 were point mutations and 48 were indels of one or few bases. Most of these were associated with polynucleotide stretches (poly-T stretch overestimated in 19 cases, poly-C underestimated in 15 cases). These problems may be attributed to using 454 technology for original Genome sequencing. On average, the original genome sequence had only one error in 56 kb. There were 23 frameshift error corrections in the 29 protein-coding genes affected by sequence revision. The genome has been subjected to major reannotation in order to substantially increase the annotation quality.
Radiation induced attenuation in perfluorinated polymer optical fibres for dosimetry applications
(2016)
Real-time measurement of radiation-induced attenuation (RIA) in a commercial perfluorinated polymer optical fibre (PF-POF) is performed with regard to on-line Radiation monitoring purposes. Spectral character and dose dependence of fibre’s RIA is measured in 450-900 nm spectral region. Fibre exhibited high radiation sensitivity in the visible region with strong increase towards the UV wavelengths. Good linearity and high sensitivity reaching up to 130 dBm-1/kGy was demonstrated in the VIS region for a low-dose range. This of-the-shelf PF-POF could be therefore interesting for on-line remote dosimetry applications.
Impact of gamma radiation on transmission of a commercial Cytop polymer optical fibre (Lucina, Asahi Glass Company) is investigated. Spectral dependence of radiation induced attenuation in the investigated fibre is measured in the VIS-NIR spectral region. Besides attenuation increase, radiation is found to increase fibre susceptibility to water as well. While pristine Cytop fibre is rather humidity insensitive, strong humidity related absorption in the NIR region is observed after fibre irradiation. Selective irradiation of separate fibre sections is proposed as a way of fibre humidity sensitization and quasi-distributed water detection is demonstrated using optical time domain reflectometry at 1310 nm.
Novel MnS nanoclusters were synthesized on nickel foam (NF) using a successive ionic layer adsorption and reaction (SILAR) method. MnS nanoclusters with different sizes were obtained by varying the number of deposition cycles. The crystal structure, chemical composition, and surface microstructure of the electrodes were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field Emission scanning electron microscopy, and high-resolution transmission electron microscopy. The electrochemical behavior of the MnS nanoclusters was examined by cyclic voltammetry, galvanostatic charge–discharge, cycling test, and electrochemical impedance spectroscopy. The MnS nanoclusters prepared with 90 SILAR cycles showed the best supercapacitance in a 6 M KOH aqueous electrolyte with a specific capacitance of 828 F/g at a scan rate of 5 mV/s and cycling stability of 85.2 % after 5000 charge–discharge cycles.
Moreover, an asymmetric supercapacitor (ASC) was assembled with the as-prepared MnS electrode on NF as the positive electrode, hydrothermally prepared reduced graphene oxide (rGO) on NF as the negative electrode, and PVA–KOH gel as the electrolyte. The MnS@NF//rGO@NF ASC showed excellent electrochemical performance with maximum energy and power densities of 34.1 Wh/kg and 12.8 kW/kg, respectively. The ASC also showed a capacitive retention of 86.5 % after 2000 charge–discharge cycles, highlighting its practical application for energy storage.
Photocatalysis is a promising technique to reduce volatile organic compounds indoors. Titanium dioxide (TiO2) is a frequently-used UV active photocatalyst. Because of the lack of UV light indoors, TiO2 has to be modified to get its working range shifted into the visible light spectrum. In this study, the photocatalytic degradation of toluene, butyl acetate and limonene was investigated under UV LED light and blue LED light in emission test chambers with catalysts either made of pure TiO2 or TiO2 modified with graphene oxide (GO). TiO2 coated with different GO amounts (0.75%–14%) were investigated to find an optimum ratio for the photocatalytic degradation of VOC in real indoor air concentrations. Most experiments were performed at a relative humidity of 0% in 20 L emission test chambers. Experiments at 40% relative humidity were done in a 1 m³ emission test chamber to determine potential byproducts. Degradation under UV LED light could be achieved for all three compounds with almost all tested catalyst samples up to more than 95%. Limonene had the highest degradation of the three selected volatile organic compounds under blue LED light with all investigated catalyst samples.
Methane dry reforming (DRM) was investigated over highly active Ni catalysts with low metal content (2.5wt%) supported on Mg-Al mixed oxide. The aim was to minimize carbon Deposition and metal sites agglomeration on the working catalyst which are known to cause catalyst deactivation.
The solids were characterized using N2 adsorption, X-ray diffraction, temperature-programmed reduction, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. The results showed that MgO-Al2O3 solid solution phases are obtained when calcining Mg-Al hydrotalcite precursor in the temperature range of 550–800 °C. Such phases contribute to the high activity of catalysts with low Ni content even at low temperature (500 °C). Modifying the catalyst preparation with citric acid significantly slows the coking rate and reduces the size of large octahedrally coordinated NiO-like domains, which may easily agglomerate on the surface during DRM. The most effective Ni catalyst shows a stable DRM course over 60 h at high weight hourly space velocity with very low coke deposition. This is a promising result for considering such catalyst systems for further development of an industrial DRM technology.
Phosphorus-based flame retardants were incorporated into different, easily preparable matrices, such as polymeric thermoset resins and paraffin as a proposed model for polyolefins and investigated for their flame retardancy performance. The favored mode of action of each flame retardant was identified in each respective system and at each respective concentration. Thermogravimetric analysis was used in combination with infrared spectroscopy of the evolved gas to determine the pyrolysis behavior, residue formation and the release of phosphorus species. Forced flaming tests in the cone calorimeter provided insight into burning behavior and macroscopic residue effects. The results were put into relation to the phosphorus content to reveal correlations between phosphorus concentration in the gas phase and flame inhibition performance, as well as phosphorus concentration in the residue and condensed phase activity. Total heat evolved (fire load) and peak heat release rate were calculated based on changes in the effective heat of combustion and residue, and then compared with the measured values to address the modes of action of the flame retardants quantitatively. The quantification of flame inhibition, charring, and the protective layer effect measure the non-linear flame retardancy effects as functions of the phosphorus concentration. Overall, this screening approach using easily preparable polymer systems provides great insight into the effect of phosphorus in different flame retarded polymers, with regard to polymer structure, phosphorus concentration, and phosphorus species.
A first pilot study on the sorption of environmental pollutants on various microplastic materials
(2017)
With the drastic increase in plastic production, the input of plastic particles into the environment has become a recognised problem.
Xenobiotics are able to sorb to polymer materials, and this process is further enhanced where they Encounter microplastics (plastic fragments <5 mm). In this work we studied the sorption of metformin, a type-2 diabetes drug, and difenoconazole, a fungicide, onto the virgin polymer materials polyamide (PA), polypropylene (PP), and polystyrene (PS). Additionally, PP was cryo-milled and PA was treated with acid to investigate the influence of an increase in surface area and chemical modification. The material properties were also studied by dynamic scanning calorimetry (DSC), gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FTIR). Sorption experiments were performed on the basis of a full factorial design examining the effect of agitation, pH value, and salinity. Experimental results showed that difenoconazole sorbs readily to all microplastics, whereas the more polar analyte metformin did not show any affinity to the materials used. For difenoconazole the governing factor in all cases is agitation, while both pH and salinity exhibited only a slight influence. The modification of polymers leads to enhanced sorption, indicating that an increase in surface area (cryo-milled PP) or inner volume (acid-treated PA) strongly favours adsorption. Moreover, long-term experiments demonstrated that the time until equilibrium is reached depends strongly on the particle size.
Vibration-based model updating and identification of multiple axial forces in truss structures
(2017)
Safety assessment of existing iron and steel truss structures requires the determination of the axial Forces and corresponding stresses in truss structural members. The results of the axial force determination can be integrated as part of a structural health Monitoring scheme for existing trusses. In this work, a methodology is proposed to identify multiple axial forces in members of a truss structure based on the modal parameters. Vibration test allows the identification of the natural frequencies and mode shapes, globally of the truss structure as well as locally of the individual bars. The method calibrates the numerical model of the truss structure using a genetic algorithm and strategic validation criteria. The validation criteria are based on the identified natural frequencies and global mode shapes of the truss structure as well as information of the axial forces in the individual bars of the truss, which are estimated from the natural frequencies and five amplitudes of the corresponding local mode shapes of the single bars based on an analytical-based algorithm. The calibration allows the identification of the axial forces in all bars of the truss structure. For mode pairing strategy, a technique makes use of the enhanced modal assurance criteria with the calculation of the modal strain energies.
Moreover, the modal strain energies are also used to select the relevant local mode shape of the individual bars. The feasibility and accuracy of the proposed methodology is verified by laboratory experiments on several truss structures. In situ tests on existing trusses are intended. The results from one of the laboratory tested structures, i.e. a two-bar system, are included in this paper.
Die Feuerverzinkung von Betonstahl stellt auf der Grundlage der im Stahlbetonbau geltenden Regelwerke eine zusätzliche Maßnahme zur Steigerung der Dauerhaftigkeit insbesondere bei Korrosionsbeanspruchung infolge Karbonatisierung und/oder Chlorideinwirkung dar. Anders als im Ausland ist die Anwendung von feuerverzinktem Betonstahl in Deutschland bisher kaum verbreitet.
Im Rahmen des AiF-Forschungsprojekts IGF 499 „Technologie- und Sicherheitszuwachs bei der Anwendung von feuerverzinktem Betonstahl zum Ausbau einer nachhaltigen Marktposition im Stahlbetonbau“ sollten die einem breiteren Einsatz feuerverzinkter Betonstähle in Deutschland bisher entgegenstehenden offenen Fragestellungen beantwortet werden.
Die interdisziplinäre Forschergruppe bestand aus dem Fachgebiet Werkstoffe im Bauwesen, Technische Universität Kaiserslautern (Forschungsstelle 1), mit dem Arbeitsschwerpunkt Fertigungstechnik, der staatlichen Materialprüfungsanstalt Darmstadt an der Technischen Universität Darmstadt (Forschungsstelle 2), mit dem Arbeitsschwerpunkt Werkstofftechnik, und der Bundesanstalt für Materialforschung und –prüfung, Berlin (Forschungsstelle 3), mit dem Arbeitsschwerpunkt Korrosionsschutz.
Rohrleitungssysteme sind aufgrund ihrer Funktion und Ausdehnung für den Betrieb, die Verfügbarkeit und die Sicherheit von Industrieanlagen von besonderer Bedeutung. Die bisher in definierten Intervallen durchgeführten, wiederkehrenden Prüfungen zur Sicherstellung leckagefreier Rohrleitungen sind kostenintensiv und mit einem erhöhten Aufwand verbunden.
Mit dem interdisziplinären Forschungsprojekt AGIFAMOR (Ageing Infrastructures – Akustisches Monitoring von Rohrleitungen) arbeitet die BAM an der Entwicklung und Erprobung einer örtlich und zeitlich kontinuierlichen Zustandsüberwachung von Rohrleitungen basierend auf einem faseroptischen akustischen Messsystem, welches einen vergleichsweise geringen Installationsaufwand der Sensoren erfordert. Mit diesem Verfahren sollen vor allem betriebsbedingte Schädigungen infolge von Korrosion sowie daraus entstehende Pittings oder Risse erkannt und damit Leckagen verhindert werden.
Im Rahmen einer Machbarkeitsstudie zum Teilaspekt „Detektion von Risswachstum“ wurde ein 2,5 m langes, definiert vorgekerbtes Stahlrohr mit der faseroptischen Sensorik (FOS) ausgestattet und quasistatisch unter 4-Punkt-Biegung belastet. Mit fortschreitender Belastung wächst, ausgehend vom vorhandenen Außenumfangskerb, ein Riss im Stahlrohr bis zum Erreichen der Leckage – in der Praxis ein gefährliches Schadensszenario.
Parallel zur FOS erfolgten Messungen mit Schallemissionssensoren, Beschleunigungssensoren und Potentialsonden, deren Ergebnisse die Interpretation der FOS-Messergebnisse unterstützen sollen.
The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions.
Hydroxyapatite (HA) is a bioceramic material with excellent biological properties. However, these properties are strongly dependent of ist crystallinity degree, with high values of crystallinity associated to poor resorption rates and bioactivity. This work evaluates the properties of HA samples produced by two different free-forming conformation methods, CNC machining and 3D printing. In both cases, porous gypsum samples were produced and subsequently converted into HA in a reaction with di-ammonium hydrogen phosphate at 100°C and pH 8. A total conversion of the samples was achieved after 36 h independently of the conformation method used. The microstructure, however, before and after the conversion is showed to be dependent on the method used. After conversion the machined samples achieved a Maximum compressive strength of 3.5 MPaforporosities of circa 80%, while 3D printed samples achieved a tensile strength of 2.0 MPa by porosities of 61%.
Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches.
The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation.
The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment.
Hydroxyl radical-induced oxidation of proteins and peptides can lead to the cleavage of the peptide, leading to a release of fragments. Here, we used high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) and pre-column online ortho-phthalaldehyde (OPA) derivatization-based amino acid analysis by HPLC with diode array detection and fluorescence detection to identify and quantify free amino acids released upon oxidation of proteins and peptides by hydroxyl radicals. Bovine serum albumin (BSA), ovalbumin (OVA) as model proteins, and synthetic tripeptides (comprised of varying compositions of the amino acids Gly, Ala, Ser, and Met) were used for reactions with hydroxyl radicals, which were generated by the Fenton reaction of iron ions and hydrogen peroxide. The molar yields of free glycine, aspartic acid, asparagine, and alanine per peptide or protein varied between 4 and 55%. For protein oxidation reactions, the molar yields of Gly (∼32-55% for BSA, ∼10-21% for OVA) were substantially higher than those for the other identified amino acids (∼5-12% for BSA, ∼4-6% for OVA). Upon oxidation of tripeptides with Gly in C-terminal, mid-chain, or N-terminal positions, Gly was preferentially released when it was located at the C-terminal site. Overall, we observe evidence for a site-selective formation of free amino acids in the OH radical-induced oxidation of peptides and proteins, which may be due to a reaction pathway involving nitrogen-centered radicals.
Magura Cave, north-western Bulgaria, possesses valuable rock-art paintings made with bat guano and dated from the period between the Eneolithic and Bronze Ages. Since 2008, the Art Gallery is closed to the general public in order to protect the paintings from vandalism, microclimatic changes caused by visitors and artificial illumination, and the consequent growth of fungi and phototrophs. Nevertheless, some tourist visits are allowed under the supervision of cave managers. This study provides the first scientific report on cultivable fungal assemblages dwelling different substrata in the Art Gallery. A total of 78 strains, belonging to 37 OTUs (Ascomycota 81%, Zygomycota 13%, Basidiomycota 5%), were isolated in the study. This fungal diversity was clearly dominated by Penicillium (50% of strains) and Aspergillus (13%). The most relevant visible fungal colonies were detected in sediments rich in bat guano, where, besides Penicillium, other guanophilic fungi such as Mucor, Mortierella, Trichosporon and Trichoderma were dominant. Conversely, scarce fungi were detected on rock surface of painted walls. Based on the biocide susceptibility assay, octylisothiazolinone (OIT) and benzalkonium chloride (BAC) were effective inhibiting the in vitro growth of dominant fungal species in Magura Cave, when applied at concentrations ranged from 100 to 1,000 mg/L. These data provide a valuable knowledge about Magura fungi, and exemplify a type of preliminary test that may be conducted before planning any biocide treatment. However, considering the irreversible effects of biocides on the ecological balance in caves, and the low fungal contamination in painted walls of Magura Cave, there is no reason to use conventional biocides in this cave. Further studies, monitoring microbial communities and microclimatic parameters, should be conducted to improve the knowledge on microbial ecology in Magura Cave and possible human impacts, as well as to allow the early detection of potential microbial outbreaks.
Mit dem KorroPad Verfahren ist es dem Anwender möglich den Zustand der Passivschicht nichtrostender Stähle auf sehr einfache und schnelle Weise einschätzen zu können. Das Verfahren eignet sich dazu, den Grad der Passivität in Abhängigkeit der Umgebungsbedingungen und der Zeit nachzuvollziehen. Dies ermöglicht dem Anwender und Verarbeiter von nichtrostenden Stählen, die Lagerungsbedingungen und -zeiten einer frisch bearbeiteten Stahloberfläche zu ermitteln, welche für die Ausbildung einer stabilen Passivschicht notwendig sind, bevor diese risikoarm eingesetzt werden kann. Wie die hier dargestellten Beispiele und auch weitere zahlreiche praktische Anwendungen gezeigt haben, eignet sich das KorroPad ebenfalls für die Identifikation kritischer Prozessparameter bei der Verarbeitung nichtrostender Stähle. Mit dem Verfahren lassen sich viele rozessbedingte Einflussfaktoren auf die Oberflächengüte wie auch auf den Werkstoff charakterisieren. Aufgrund der schnellen und einfachen Auswertung der Prüfergebnisse können positive wie auch negative Veränderungen hinsichtlich der Passivschichtstabilität zügig erkannt werden. Dies ermöglicht es dem Anwender schnell zu reagieren, um kritische Einflüsse zu korrigieren und um eine Optimierung von Inhouse-Prozessen durchzuführen. Weitere Einsatzgebiete sind im Bereich der Wareneingangs- und/oder Warenausgangskontrolle denkbar, überall wo es um die Frage der Passivschichtstabilität einer nichtrostenden Stahloberfläche geht.
A facile method to probe the vascular permeability of nanoparticles in nanomedicine applications
(2017)
The effectiveness of nanoparticles (NP) in nanomedicine depends on their ability to extravasate from vasculature towards the target tissue. This is determined by their permeability across the endothelial barrier. Unfortunately, a quantitative study of the diffusion permeability coefficients (Pd) of NPs is difficult with in vivo models. Here, we utilize a relevant model of vascular-tissue interface with tunable endothelial permeability in vitro based on microfluidics. Human umbilical vein endothelial cells (HUVECs) grown in microfluidic devices were treated with Angiopoietin 1 and cyclic adenosine monophosphate (cAMP) to vary the Pd of the HUVECs monolayer towards fluorescent polystyrene NPs (pNPs) of different sizes, which was determined from image analysis of their fluorescence intensity when diffusing across the monolayer. Using 70 kDa dextran as a probe, untreated HUVECs yielded a Pd that approximated tumor vasculature while HUVECs treated with 25 μg/mL cAMP had Pd that approximated healthy vasculature in vivo. As the size of pNPs increased, its Pd decreased in tumor vasculature, but remained largely unchanged in healthy vasculature, demonstrating a trend similar to tumor selectivity for smaller NPs. This microfluidic model of vascular-tissue interface can be used in any laboratory to perform quantitative assessment of the tumor selectivity of nanomedicine-based systems.
Obwohl THz-TDS-Systeme vielfältige Qualitätsparameter von Dielektrika ermitteln können, ist deren industrielle Nutzung im Bereich der zerstörungsfreien Bauteilprüfung noch nicht anerkannter Stand der Technik. Ein pragmatischer Weg, TDS-Systeme neben traditionellen Prüfverfahren zu etablieren, sind systematische Untersuchungen an Modellbauteilen, mit dem Ziel einer Methodenentwicklung zur zuverlässigen berührungslosen Prüfung von Dielektrika. Anhand von THz-TDS-Messungen an Polyethylen-Testkörpern mit künstlich eingebauten Fehlstellen werden anfänglich die Möglichkeiten der Laufzeitmessung zur Ermittlung von Tiefenlagen von Ungänzen in Testkörpern präsentiert. Im weitern Teil wird gezeigt, wie durch eine veränderte Versuchsdurchführung und Verwendung eines modifizierten SAFT-Rekonstruktions-Algorithmus Tomogramme berechnet werden können, in denen die künstlich eingebrachten Fehlstellen hinsichtlich ihrer Größe und Lage geometrisch richtig dargestellt werden.
Development of theranostic concepts that include inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) imaging can be hindered by the lack of a direct comparison to more standardly used methods for in vitro and in vivo evaluation; e.g. fluorescence or nuclear medicine. In this study a bimodal (or rather, hybrid) tracer that contains both a fluorescent dye and a chelate was used to evaluate the existence of a direct link between mass spectrometry (MS) and in vitro and in vivo molecular imaging findings using fluorescence and radioisotopes. At the same time, the hybrid label was used to determine whether the use of a single isotope label would allow for MS-based diagnostics.
The excitation of localized surface plasmons in noble metal nanoparticles (NPs) results in different nanoscale effects such as electric field enhancement, the generation of hot electrons and a temperature increase close to the NP surface. These effects are typically exploited in diverse fields such as surface-enhanced Raman scattering (SERS), NP catalysis and photothermal therapy (PTT). Halogenated nucleobases are applied as radiosensitizers in conventional radiation cancer therapy due to their high reactivity towards secondary electrons. Here, we use SERS to study the transformation of 8-bromoadenine (8BrA) into adenine on the surface of Au and AgNPs upon irradiation with a low-power continuous wave laser at 532, 633 and 785 nm, respectively. The dissociation of 8BrA is ascribed to a hot-electron transfer reaction and the underlying kinetics are carefully explored. The reaction proceeds within seconds or even milliseconds. Similar dissociation reactions might also occur with other electrophilic molecules, which must be considered in the interpretation of respective SERS spectra. Furthermore, we suggest that hot-electron transfer induced dissociation of radiosensitizers such as 8BrA can be applied in the future in PTT to enhance the damage of tumor tissue upon irradiation.
Distributed measurement of humidity is a sought-after capability for various fields of application, especially in the civil engineering and structural health monitoring sectors. This article presents a method for distributed humidity sensing along polymethyl methacrylate (PMMA) polymer optical fibers (POFs) by analyzing wavelength-dependent Rayleigh backscattering and attenuation characteristics at 500 nm and 650 nm wavelengths. Spatially resolved humidity sensing is obtained from backscatter traces of a dual-wavelength optical time domain reflectometer (OTDR). Backscatter dependence, attenuation dependence as well as the fiber length change are characterized as functions of relative humidity. Cross-sensitivity effects are discussed and quantified. The evaluation of the humidity-dependent backscatter effects at the two wavelength measurements allows for distributed and unambiguous measurement of relative humidity. The technique can be readily employed with low-cost standard polymer optical fibers and commercial OTDR devices.
This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy
Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment.
In granular soils, long-term cyclically loaded structures can lead to an accumulation of irreversible strain by forming closed convective cells in the upper layer of the bedding. The size of the convective cell, its formation and grain migration inside this closed volume have been studied with reference to different stiffness of the embedded structure and different maximum force amplitudes applied at the head of the structure.
This relation was experimentally investigated by applying a cyclic lateral force to a scaled flexible vertical element embedded in a dry granular soil. The model was monitored with a camera in order to derive the displacement field by means of the PIV technique. Furthermore, the ratcheting convective cell was also simulated with DEM with the aim of extracting some micromechanical information. The main results regarded the different development, shape and size of the convection cell and the surface settlements.
A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature.
This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures.
The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron backscatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications.
In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water.
An UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its temperature-induced phase transition and aggregation behaviour studied by turbidimetry, static and dynamic light scattering, small angle neutron scattering (SANS) and cryo-transmission electron microscopy (cryo-TEM) measurements. The phase transition temperature was found to increase with increasing AN content in the copolymer, concentration of the solutions and copolymer chain length. A significant effect was observed onto the phase transition temperature by addition of different electrolytes into the copolymer solution. The copolymer chains were aggregated below the phase transition temperature and disaggregated above it. The size of the aggregates increases with increasing AN contents and concentration of the copolymer solutions below the phase transition temperature. The copolymer chains were expanded and weekly associated in solution above the phase transition temperature. A model is proposed to explain such association–aggregation behaviour of poly(AAm-co-AN) copolymers depending on AN contents and concentration of the copolymer solutions as a function of temperature.
The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits.
The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). The National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories.
Results were submitted by 11 NMIs and DIs. The participants used different measurement methods, though most of them used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion.
The material was quite challenging and a number of questions were raised at the IAWG meeting. Concerning S, the variation in S results between participants, particularly those using IDMS methods was discussed at the IAWG meeting. BAM, NIST and NMIJ reviewed their experimental conditions, results and/or uncertainty calculations for IDMS. According to the additional evaluation and investigation, the variances between the revised results became smaller than the original one, the revised results were overlapping between IDMS measurements of S content at the k=2 level. It is not possible to calculate a KCRV with values being modified after submission. It was concluded that this KC does not support S measurements.
Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participating NMIs or DIs. It is expected that sodium, calcium, potassium, magnesium and phosphorus at mass fractions greater than approximately 0.1 mg/kg, 0.1 mg/kg, 0.05 mg/kg, 0.05 mg/kg and 0.1 mg/kg respectively in biodiesel fuel and similar matrices (fuels and oils etc.) can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilized along with the IAWG core capability approach.
Der durch Kräfte senkrecht zur Stabachse belastete Balken ist eines der Haupttragelemente des Stahlbetonbaus. Biegebalken finden unter anderem Anwendung in Form von Brückenträgern oder Unterzügen. Die bei maximaler Beanspruchung auftretenden Versagensformen unterteilen sich dabei in Biege- und Querkraftversagen (Schubversagen). Ein Versagen des Balkens kann je nach Versagensmechanismus mit oder ohne Vorankündigung erfolgen. Gebräuchliche Bemessungskonzepte der Baupraxis zur Dimensionierung entsprechender Tragelemente zielen auf ein Versagen mit ausreichender Vorankündigung (große Verformungen oder breite Risse) ab, wie es z.B. beim sekundären Biegedruckversagen entsteht. Für die Zustandsüberwachung von Bauwerken (z.B. Brücken) mittels zerstörungsfreier Prüftechniken sind fundierte Kenntnisse zu den bei Biegebeanspruchung auftretenden Schadensmechanismen erforderlich. Im Rahmen eines BAM-internen Projektes sollen durch praxisnahe Untersuchungen an einer brückenähnlichen Referenzstruktur unterschiedliche auf das Tragwerk einwirkende thermische und mechanische Belastungen untersucht werden und in die Entwicklung eines Monitoringsystems einfließen. Anhand der aus Biegeversuchen vorliegenden Ergebnisse wird der Einsatz unterschiedlicher Methoden der zerstörungsfreien Materialprüfung gezeigt und deren Anwendbarkeit für die Analyse des Verformungsverhaltens von Stahlbetonbalken diskutiert. Hierzu wurde das Verformungsverhalten eines Stahlbetonbalkens (L = 2,75 m) in einem Vierpunkt-Biegeversuch im Labormaßstab untersucht. Das Hauptaugenmerk liegt dabei auf der Charakterisierung der ausschlaggebenden Versagensmodi durch die einzelnen zerstörungsfreien Prüfverfahren und der Vergleich zu klassischen Messmethoden (z.B. Verformungsmessung mittels induktiver Wegaufnehmer (IWA)). Die Biegeversuche wurden dazu durch Schallemissionsanalyse (SEA) und optische Verformungsanalyse mittels Stereo-Fotogrammetrie (SF) und Bildkorrelationsverfahren (BKV) begleitet.
This work demonstrates that phase-segregated poly(ester urethane) (PEU) with switching segments of crystallizable poly(1,4-butylene adipate) (PBA) can be programmed to generate two separate stress recovery events upon heating under constant strain conditions. For programming, two elongations are applied at different temperatures, followed by unloading and cooling. During the adjacent heating, two-step stress recovery is triggered. The results indicate that the magnitude of the stress recovery signals corresponds to the recovery of the two deformation stresses in reverse order. As demonstrated by further experiments, twofold stress recovery can be detected as long as the elongation at higher temperature exceeds the strain level of the deformation at lower temperature. Another finding includes that varying the lower deformation temperature enables a control over the stress recovery temperature and thus the implementation of so-called “temperature-memory effects”. Moreover, exerting only one elongation during programming enables a heating-initiated one-step stress recovery close to the deformation temperature. Based on these findings, such polymers may offer new technological opportunities in the fields of active assembly when used as fastening elements and in functional clothing when utilized for compression stockings.
Referee Report 06 March 2017
(2017)
Driven mostly by the search for chemical syntheses under biocompatible conditions, so called "click" chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques possessing short set-up times. Here, we report on a fast and reliable calibration-free online NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement of 1H spectra with a time interval of 20 s per spectrum, and a robust, fully automated algorithm to interpret the obtained data. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in a variety of non-deuterated solvents while its time-resolved behaviour was characterized with step tracer experiments. Overlapping signals in online spectra during thiol-ene coupling could be deconvoluted with a spectral model using indirect hard modeling and were subsequently converted to either molar ratios (using a calibrationfree approach) or absolute concentrations (using 1-point calibration). For various solvents the kinetic constant k for pseudo-first order reaction was estimated to be 3.9 h-1 at 25 °C. The obtained results were compared with direct integration of non-overlapping signals and showed good agreement with the implemented mass balance.
Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility.
Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry.
This author interview is by Dr Michael G. Weller, Head of Division 1.5 Protein Analysis at Federal Institute for Materials Research and Testing (BAM). BAM (www.bam.de/en) is a senior scientific and technical institute with responsibility to the German Federal Ministry for Economic Affairs and Energy. Dr Weller's review paper, Quality issues of research antibodies is available for download in Analytical Chemistry Insights.
Immunoassays are suitable tools for high-throughput screenings. The prerequisite for accurate determinations by these methods is the selection of an excellent antibody. The production and selection of monoclonal antibodies is usually a tedious process. In this study, new strategies for improving antibody production and characterization were applied. This includes the monitoring of the immunization progress in mice through antibodies extracted from feces, which allows a time-resolved and animal-friendly monitoring of the immune response. Additionally, fluorescence polarization immunoassay (FPIA) could be successfully applied for fast and easy examination of cell culture supernatants and the investigation of antibody/antigen interactions including kinetics and fluorescence properties. These methods simplify the selection of the optimal antibody. As a target analyte, carbamazepine was chosen. This is a widely used antiepileptic drug which also frequently occurs in the environment. The new antibody enables CBZ determination in the concentration range 0.66–110 µg L-1 within 10 min using a high-throughput microtiter plate-based FPIA, and between 1.4 and 79 µg L-1 within 5 min applying an automated cuvette-based FPIA instrument, and from 0.05–36 µg L-1 using ELISA. The measurements were performed at a non-equilibrium state which improved the sensitivity and selectivity of the assays. Due to low cross-reactivity especially towards the main CBZ metabolite and other pharmaceuticals (<1%), this antibody gives the opportunity for application in medical and environmental analyses.
This article provides an impression on potentials in applying nowadays welding simulation tools in construction design. This is carried out exemplary on plate girders from two structural steel grades. The calculated residual stresses are compared with measurements by sectioning method. It has been repeatedly stated that present Eurocode models fail to approximate the residual stresses. Especially for high strength steel (HSS) only limited information is available on realistic occurring residual stresses in typical I-girders. The investigations are aimed to give further guidance on these values. A few proposals on advanced models are discussed.
In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.
Investigation of manuscripts found in sites along the Silk Road shows the history of communication and exchange between Asia and the Mediterranean over the centuries. Different scripts and languages preserved on paper in certain styles provide information about traditions and provenance.
To get an idea of the cultural background of the highly developed painting techniques obvious in some illuminated manuscripts, the material used for writing and painting is analyzed. Singular Sogdian and Tocharian manuscripts from Turfan show text on one side with a colorful painting on the other side of the document. In comparison with other productions of different periods or usages from the site, special features are worked out to characterize cultural roots or influence in the network of relationships. Details analyzed in the most elaborated documents Show various influences led to the colorful masterpieces.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
Reliable nanomaterial classification of powders using the volume-specific surface area method
(2017)
The volume-specific surface area (VSSA) of a particulate material is one of two apparently very different metrics recommended by the European Commission for a definition of "nanomaterial" for regulatory purposes: specifically, the VSSA metric may classify nanomaterials and non-nanomaterials differently than the median size in number metrics, depending on the chemical composition, size, polydispersity, shape, porosity, and aggregation of the particles in the powder.
Here we evaluate the extent of agreement between classification by electron microscopy (EM) and classification by VSSA on a large set of diverse particulate substances that represent all the anticipated challenges except mixtures of different substances. EM and VSSA are determined in multiple labs to assess also the level of reproducibility. Based on the results obtained on highly characterized benchmark materials from the
NanoDefine EU FP7 project, we derive a tiered screening strategy for the purpose of implementing the definition of nanomaterials. We finally apply the Screening strategy to further industrial materials, which were classified correctly and left only borderline cases for EM.
On platelet-shaped nanomaterials, VSSA is essential to prevent false-negative classification by EM. On porous materials, approaches involving extended Adsorption isotherms prevent false positive classification by VSSA. We find no false negatives by VSSA, neither in Tier 1 nor in Tier 2, despite real-world industrial polydispersity and diverse composition, shape, and coatings. The VSSA screening strategy is recommended for inclusion in a technical guidance for the implementation of the definition.
Die im Forschungsvorhaben erzielten Ergebnisse zeigen konkrete technische Lösungen für die automatisierte Anwendung des MSG Engspaltschweißen, sowohl mittels optischer als auch prozessorientierter Sensorik, und sprechen damit ein breites Spektrum möglicher Anwender, insbesondere KMU, an.
Die Seitenführung des Brenners auf Basis der optischen Messgrößen stellt eine robuste und einfach zu implementierende Möglichkeit zur Nahtverfolgung dar. Für die Höhenführung über der Schweißnaht wurde neben der Lösung mittels optischer Messverfahren zusätzlich eine direkt darauf aufbauende Möglichkeit zur Implementierung eines Lichtbogensensors abgeleitet. Das Vorgehen konnte sowohl für Sprühlichtbogenprozesse als auch bei Verwendung von Impulslichtbogenprozessen erfolgreich angewendet werden.
Die zur Sicherstellung eines gleichmäßigen Flankeneinbrandes entwickelte Pendelregelung ist ebenfalls für unterschiedliche Lichtbogenarten einsetzbar und muss vom Anwender auch beim Einsatz einer großen Bandbreite unterschiedlicher Prozessparameter nahezu nicht konfiguriert werden. Neben der im Rahmen der Verfahrensprüfung untersuchten Pendelraupentechnik konnte die Übertragbarkeit des Vorgehens auch auf die Strichraupentechnik anhand von gezielten Schweißversuchen aufgezeigt werden.
Die zunächst auf Basis der optischen Messwerte ausgelegte Füllgradregelung konnte die vorgesehenen Spaltvariationen von 18 bis 24 mm im Rahmen der durchgeführten Verfahrensprüfung ausgleichen. Die Ableitung eines äquivalenten Lichtbogensensors durch Kopplung beider Messprinzipien wurde am Laufzeitende des Vorhabens aufgezeigt, konnte jedoch durch zeitliche Beschränkung nicht für die Verfahrensprüfung berücksichtigt werden.
In Absprache mit dem projektbegleitenden Ausschuss wurde die Entwicklung der Prozessregelung für das Vorhaben auf Schweißungen in Wannenlage und Grundwerkstoffe der Güte S355J2 beschränkt.
Die Qualifizierung des Verfahrens unter Einsatz der beschriebenen Regelalgorithmen nach DIN EN ISO 15614-1 konnte für alle betrachteten Spaltbreiten zwischen 18 und 24 mm anhand einer 50 mm dicken Demonstratorprobe nachgewiesen werden.
Halophilic bacteria use a variety of osmoregulatory methods, such as the accumulation of one or more compatible solutes. The wide diversity of compounds that can act as compatible solute complicates the task of understanding the different strategies that halophilic bacteria use to cope with salt. This is specially challenging when attempting to go beyond the pathway that produces a certain compatible solute towards an understanding of how the metabolic network as a whole addresses the problem. Metabolic reconstruction based on genomic data together with Flux Balance Analysis (FBA) is a promising tool to gain insight into this problem. However, as more of these reconstructions become available, it becomes clear that processes predicted by genome annotation may not reflect the processes that are active in vivo. As a case in point, E. coli is unable to grow aerobically on citrate in spite of having all the necessary genes to do it. It has also been shown that the realization of this genetic potential into an actual capability to metabolize citrate is an extremely unlikely event under normal evolutionary conditions. Moreover, many marine bacteria seem to have the same pathways to metabolize glucose but each species uses a different one. In this work, a metabolic network inferred from genomic annotation of the halophilic bacterium Halomonas elongata and proteomic profiling experiments are used as a starting point to motivate targeted experiments in order to find out some of the defining features of the osmoregulatory strategies of this bacterium. This new information is then used to refine the network in order to describe the actual capabilities of H. elongata, rather than its genetic potential.
Electron Beam Melting (EBM) as a means of Additive Manufacturing (AM), is of interest for the fabrication of intricate geometries for cellular materials in areas where complex architectures are needed, e.g. biomedical implants. Most studies have focused on specific geometries and so the effect of the structure on mechanical performance is not well understood. Many kinds of micro- and macro-scale defects can arise in additively manufactured components, so assessment of their influence on properties is needed. In this work, lattices of Ti-6Al-4V having a cubic structure have been manufactured by EBM, and the effect of heat treatments above and below the β-transus temperature on microstructure and compression response have been investigated. The former modifies only slightly the α + β structure and mechanical performance whereas the latter leads to coarse alternating α and β lamellae packets and α at the prior grain boundaries with a 10% loss in yield strength. The variation in the compressive yield stress with strut diameter is in good accord with simple models based on compressive deformation rather than shearing or buckling. Internal pores for struts aligned with the build direction are found around the edges of the solid form, in regions which seem to be associated with the EB scan pattern. Struts normal to the build direction show more significant defects but their redundancy means that they do not compromise the compressive performance in the build direction. Using a particle size in the range 45–100 μm minimum weld-track sizes were experimentally and numerically identified to be 176 and 148 μm in depth respectively with a depth-to-width ratio of 0.55. This produced a beam pass of the order of 300 μm oversizing small features (struts of 0.4 and 0.6 mm nominal diameter) when a contour around the strut periphery was applied.
Für die Herstellung von Kupfer aus Primär- und Sekundärressourcen wurde eine Exergieanalyse der Aufbereitungs- und Gewinnungsverfahren durchgeführt. Für die Stoffgemische Kupfererz, Kupferkonzentrat und Hausmüllverbrennungsasche wurden die Exergien tabellarisch berechnet. Die Exergieaufwände der technischen Prozesse zur Kupferherstellung wurden mit den thermodynamisch minimal notwendigen Aufwänden verglichen. Die Nutzung von Sekundärrohstoffen aus Abfällen ist über weite Bereiche vorteilhaft, insb. wenn das Kupfer bereits in der metallischen Form vorliegt.
Experimental and phase field studies of age hardening response of a high purity Al‐4Cu‐1Li‐0.25Mn‐alloy (mass %) during isothermal aging are conducted. In the experiments, two hardening phases are identified: the tetragonal θ′ (Al₂Cu) phase and the hexagonal T1 (Al₂CuLi) phase. Both are plate shaped and of nm size. They are analyzed with respect to the development of their size, number density and volume fraction during aging by applying different analysis techniques in TEM in combination with quantitative microstructural analysis. 3D phase‐field simulations of formation and growth of θ′ phase are performed in which the full interfacial, chemical and elastic energy contributions are taken into account. 2D simulations of T1 phase are also investigated using multi‐component diffusion without elasticity. This is a first step toward a complex phase‐field study of T1 phase in the ternary alloy. The comparison between experimental and simulated data shows similar trends. The still unsaturated volume fraction indicates that the precipitates are in the growth stage and that the coarsening/ripening stage has not yet been reached.
Today’s efforts for lightweight design result in a growing application of high-strength structural steels from 960 MPa. In welded structures of these steels increased demands regarding component safety and a high elastic ratio should be considered. Hence, the prevention of an evolution of high weld-induced tensile residual stresses is required. Recent studies showed that component related restraint conditions of welds are able to elevate welding induced stresses to critical values, depending on material characteristics, the welding process and parameters. This work involves multi-axial welding loads as a consequence of the superposition of local residual stresses, global reaction stresses and moments, varying the welding parameters under different restraint conditions. The global welding loads are measured via GMA-weld tests in a special testing facility and via a DIC(Digital Image Correlation)-system in a slot weld. Local transverse residual stresses were analysed by means of X-ray diffraction. The application of a less amount of weld runs due to a modified welding parameters and welds seam configurations revealed as a beneficial approach to reduce welding loads in high-strength steels.
Welding is the most important joining technology. In the steel construction
industry, e.g. production of windmill sections, welding accounts for a
main part of the manufacturing costs and resource consumption. Moreover, social
issues attached to welding involve working in dangerous environments. This aspect
has unfortunately been neglected so far, in light of a predominant focus on economics
combined with a lack of suitable assessment methods. In this chapter,
exemplary welding processes are presented that reduce the environmental and
social impacts of thick metal plate welding. Social and environmental Life Cycle
Assessments for a thick metal plate joint are conducted for the purpose of
expressing and analysing the social and environmental impacts of welding.
Furthermore, it is shown that state-of-the-art technologies like Gas Metal Arc
Welding with modified spray arcs and Laser Arc-Hybrid Welding serve to increase
social and environmental performance in contrast to common technologies, and
therefore offer great potential for sustainable manufacturing.
We report on a study in which plasmid DNA in water was irradiated with 30 keV electrons generated by a scanning electron microscope and passed through a 100 nm thick Si3N4 membrane. The corresponding Monte Carlo simulations suggest that the kinetic energy spectrum of the electrons throughout the water is dominated by low energy electrons (<100 eV). The DNA radiation damage, single-strand breaks (SSB) and double-strand breaks (DSB), was determined by electrophoresis. The median lethal dose of D1/2 = 1.7 ± 0.3 Gy was found to be much smaller compared to partially or fully hydrated DNA irradiated under vacuum conditions. The ratio of DSB to SSB was found to be (1:12) as compared to 1:88) found for hydrated DNA. Our method enables quantitative measurements of radiation damage to biomolecules (DNA, proteins) in solutions under varying conditions (pH, salinity, cosolutes) for an electron energy range which is difficult to probe by standard methods.
We report on calibration standards of nanoparticles meeting the definition of a nanomaterial given by the European Commission (EU 2011) which are relevant for the characterisation methods applied in the NanoDefine project. We found that the Impact of nanoparticles is outstanding in the scientific literature. A number of 270.000 paper titles on nanoparticles are listed in the Web of Science data base. But surprisingly, the availability of suitable certified standard reference materials is scarce. Only a few sources were found. For example, BAM provides the database Nanoscaled Reference Materials at http://www.nano-refmat.bam.de/en/ in cooperation with the ISO/TC 229 Nanotechnologies. In addition, two publications from 2013 on nanoscale reference materials are available. Candidates of nano-(certified) reference materials from other ongoing or just finished FP6 and FP7 nano-metrology projects have been extracted from the Compendium of Projects in the European NanoSafety Cluster (Compendium NSC, 2013). Recommendations for selection of representative test materials and calibration standards for NanoDefine internal tasks, respectively, are also given.
The EU FP7 NanoDefine project was launched in November 2013 and will run until October 2017. The Project is dedicated to support the implementation of the EU Recommendation on the Definition of Nanomaterial
by the provision of the required analytical tools and respective guidance. Main goal is to develop a novel
tiered approach consisting of (i) rapid and cost-efficient screening methods and (ii) confirmatory measurement
methods. The "NanoDefiner" eTool will guide potential end-users, such as concerned industries and regulatory bodies as well as enforcement and contract laboratories, to reliably classify if a material is nano or not. To achieve this objective, a comprehensive inter-laboratory evaluation of the performance of current
characterisation techniques, instruments and software is performed. Instruments, software and methods are
further developed. Their capacity to reliably measure the size of particulates in the size range 1-100 nm and
above (according to the EU definition) is validated. Technical reports on project results are published to
reach out to relevant stakeholders, such as policy makers, regulators, industries and the wider scientific community, to present and discuss our goals and results, to ensure a continuous exchange of views,
needs and experiences obtained from different fields of expertise and application, and to finally integrate the resulting feedback into our ongoing work on the size-related classification of nanomaterials.
The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing.
It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions.
The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs.
The current paper presents residual stress analyses of large scale LTT (Low Transformation Temperature) welds. LTT filler materials are specially designed for residual stress engineering by means of an adjusted martensite phase transformation. Controlling the level of mostly detrimental residual stresses already during the welding process would be highly attractive as time and cost consuming post processing may be prevented. In large scale welds the residual stress state is influenced by the heat control (e.g. interpass temperature) during welding. Therefore, welding residual stresses are studied here putting the focus on the influence of welding process parameters while joining heavy steel sections with a thickness of 25 mm. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results show that control of the interpass temperature is vital for the residual stresses present in the joints. This accounts for the top surface but is most pronounced for the bulk of the welds. While high interpass temperatures are appropriate to induce compressive residual stresses in the weld metal, low interpass temperatures favor unwanted tensile residual stresses instead.
This report is the result of a comprehensive study on the available CMs which come potentially in question for the reliable analysis of the number based size distribution of a nanomaterial according to the EC recommendation for a definition of nanomaterial. Based on the performance criteria already established in NanoDefine the potential CMs are evaluated according to studies available in the literature as well as following the expertise of the NanoDefine consortium partners. The specific advantages and disadvantages of each method with respect to its applicability to the scope of NanoDefine are particularly highlighted. An CM evaluation table is produced so that the mostly suited CMs with respect to the EC definition can be grouped and recommended to the corresponding NanoDefine work packages for further specific development (improvement and adaption), or for direct validation and standardisation, respectively. The actual evaluation report including the recommended CMs will be revised and, if necessary, eventually updated at the mid time of the project. The update will be jointly discussed in the NanoDefine consortium on the basis of the results of testing the methods on the NanoDefine real world materials.
We propose the use of alternating pulse wavelengths in a direct-detection coherent optical time domain reflectometry (C-OTDR) setup not only to measure strain and temperature changes but also to determine the correct algebraic sign of the change. The sign information is essential for the intended use in distributed mode shape analysis of civil engineering structures. Correlating relative backscatter signal shifts in the temporal/signal domain allows for measuring with correct magnitude and sign. This novel approach is simulated, experimentally implemented and demonstrated for temperature change measurement at a spatial resolution of 1 m.
Carbon arc-air gouging is a common technology when repairing defects in welded structures. Often this technique is applied in repeated cycles even on the same location of the joint. Due to the multiple heat input by gouging and subsequent re-welding, the residual stresses are strongly influenced. This can become crucial when microstructure and mechanical properties are adversely affected by multiple weld reparations. Knowledge about the relation of gouging and residual stresses is scarce but important when high strength steels, which are sensitive to residual stresses, are processed. The present study shows the effect of repair welding on a high strength steel structural element. The weld and the heat affected zone were subjected to multiple thermal cycles by gouging and subsequent repair welding. The residual stresses were determined by X-ray diffraction at different positions along the joint. The results showed that the residual stress level has increased by the repair cycles. This is most pronounced for the heat affected zone. Adapted welding procedures may prevent detrimental residual stress distributions.
The nonlinear analysis became a common tool to precisely assess the load-bearing behavior of steel beam and column members. The failure level is significantly influenced by different types of imperfections, among geometric also structural imperfections (residual stresses). Here are still gaps in the knowledge. Nowadays, 3-D welding simulation developed to a level where it could provide reliable estimation of weld-induced distortion and residual stresses. Nevertheless, modelling and computational effort are still in a less practicable range. In this study a simplified procedure to implement residual welding stresses in continuous large scale members is proposed and the influence on the ultimate limit state of slender members in compression is evaluated for two common structural steel grades. The results showed significant improvements in the utilization of load bearing capacity compared with simplified design methods. The comparatively general approach in this study offers
potential for future optimization.
Residual stresses and distortions in welded I-girders for steel construction are relevant when evaluating the stability of steel beams and column members. The application of high strength steels allows smaller wall thicknesses compared to conventional steels. Therefore, the risk of buckling has to be considered carefully. Due to the lack of knowledge concerning the residual stresses present after welding in high strength steel components conservative assumptions of their level and distribution is typically applied. In this study I-girders made of steels showing strengths of 355 MPa and 690 MPa were welded with varying heat input. Due to the dimension of the I-girders and the complex geometry the accessibility for residual stress measurement using X-ray diffraction was limited. Therefore, saw cutting accompanied by strain gauge measurement has been used to produce smaller sections appropriate to apply X-ray diffraction. The stress relaxation measured by strain gauges has been added to residual stresses determined by X-ray diffraction to obtain the original stress level and distribution before sectioning. The combination of both techniques can produce robust residual stress values. From practical point of view afford for strain gauge application can be limited to a number of measuring positions solely to record the global amount of stress relaxation. X-ray diffraction can be applied after sectioning to determine the residual stresses with sufficient spatial resolution.
The detection and characterization of surface cracks in steel specimens prior to damage is a technologically and economically highly significant task and is of utmost importance when it comes to safety-relevant structures. In steel production where steel billets at high temperatures have to be inspected while moving a number of well-established NDT methods cannot be applied. Laser thermography however is a promising candidate to serve as a fast, non-contact and remote tool in this case. We present a study that shows that the crack detection capabilities of laser thermography can be extended also to specimens at high temperature. A combination of inductive and laser heating allows to systematically study the contrast formation as well as the optimization of the important measurement parameters. The experiments are accompanied by FEM simulations that provide a better insight of the physical correlations and support the experimental developments. The aim of these studies is to develop a system with high inspection speed and detection performance to be in-line operated under the hostile environment of steel production lines.
In this study, the feasibility of using non-contact Infrared thermography as a potential tool to monitor the CMT welding process is explored. The presence of internal defects such as porosity, lack of filler material deposition and formation of improper weld bead produce perturbations in the surface temperature which can be identified using an Infrared thermography technique. We present recent results obtained from online monitoring of the the dissimilar joining using CMT weld brazing of Aluminum and Steel using a transmission mode measurement approach. The effect of loss of zinc coating on the weldability of the cold metal transfer joining of aluminum to galvanised steel was investigated. A correlation between measured online thermal indications with the weld anomalies is successfully attempted and the results are compared with the conventional post-weld NDT inspection methods.
A permanent-magnet synchronous motor (PMSM) servo drive for lightweight robotic platforms that have a high torque demand at low rotational speeds has been developed. First, a current-independent torque controller is derived and cascaded with a speed and position controller, while merely an encoder is used as a sensor device in combination with a speed estimator. Finally, the speed estimator output is compared to gyroscope measurements and the overall functioning is verified on a real system.
A phosphaphenanthrene and triazinetrione group containing flame retardant (TAD) is combined with organically modified montmorillonite (OMMT) in epoxy resin thermosets (EP) to improve the performance of the flame-retardant system. When only 1 wt% OMMT/4 wt% TAD is introduced into the EP, the limited oxygen index (LOI) rises from 26% to 36.9% and a V-0 rating is achieved in a UL 94 test. The decomposition and pyrolysis products in the gas phase and condensed phase were characterized using thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR). The influence on the decomposition of EP, such as the increase in char yield, is limited with the incorporation of OMMT; a large amount of the phosphorus is released into the gas phase. The flame-retardant effect evaluation based on cone calorimeter data testified that OMMT improves the protective-barrier effect of the fire residue of OMMT/TAD/EP on the macroscopic scale, while TAD mainly causes flame inhibition. The fire residues showed a corresponding macroscopic appearance (digital photo) and microstructure (scanning electron microscope [SEM] results). The protective barrier effect of OMMT and the flame-inhibition effect of TAD combined to exert a superior flame-retardant effect, resulting in sufficient flame-retardant performance of OMMT/TAD/EP
A high-performance fiber Bragg grating-based (FBG) sensor device has been developed for the detection of small magnetic fields. Based on a smart multilayer jacket around the fibre over the physical length of the FBG, magnetic fields generated by rotating machine parts, power generators or power cable can be easily detected, analysed and evaluated. Consequently, this innovative, on-line and non-contact inspection method results in an increase in quality and reliability of high-performing machine parts, devices and cables. The basic physical principle is based on a magnetostrictive multilayer system that strains the high-resolution FBG element in presence of magnetic fields. Subsequently, a fixed relationship between induced magnetic field and wavelength change of the FBG element describes the characteristic sensitivity curve. Intensive tests regarding characterisation of this magnetic field FBG sensor have been carried out and its performance has been evaluated.
IND15 JRP SurfChem: Traceable quantitative surface chemical analysis for industrial applications
(2016)
The SurfChem project has made a significant contribution to traceable quantitative surface chemical analysis for industrial applications by delivering new certified reference materials and test samples for specific technical applications. Regular performance tests of instruments, metrological methodology for the detection of (bio)organic surface species, ambient and non-destructive surface chemical analysis for in-line process control and new in situ characterisation techniques of catalytically active surfaces have been achieved.
Materials and chemical producers require detailed knowledge of surface chemistry for research into new products. One way to understand a surface without damaging it is to bombard it with an electron beam, causing its atoms to emit characteristic X-rays enabling identification. The measurement of these must be precise as many elements emissions are close in energy – traceable reference materials will ensure instruments using this technique are stable and accurate.
Ultrasonic imaging systems usually require an array of ultrasonic transducers for data acquisition on a wide area on top of an object under investigation. The goal of an imaging algorithm is the use of reflected ultrasound data to form a recognizable image. Conventional algorithms like SAFT are based on an inverse Huygens' principle and need therefore a dense measurement grid. This requires a big effort in data capturing. For simple and inexpensive measurement different strategies of imaging with reduced amount of data and examples with a manual scanning device on concrete elements are presented.
Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectros-copy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical com-parison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory.
Rekonstruktion des Bestandsplans im Zuge der Nachrechnung der Brücke über die Leine bei Schwarmstedt
(2016)
Der aktuell im Rahmen der Nachrechnungsrichtlinie geforderte Nachweis von Tragfähigkeit, Gebrauchstauglichkeit und Ermüdung der Brückenbauwerke im Bestand der Länder und des Bundes stellt eine enorme Herausforderung dar. Insbesondere bei unvollständigen oder fehlenden Bestandsplänen der Bauwerke sind Maßnahmen erforderlich, um die erforderlichen Informationen zu beschaffen. Ein wirkungsvolles Instrument können hierfür die zerstörungsfreien Prüfverfahren des Bauwesens sein. In dem präsentierten Forschungsprojekt erfolgte die Rekonstruktion eines Bestandsplanes direkt auf die Anforderungen des mit der Nachrechnung beauftragten Ingenieurbüros. Darüber hinaus wurde der Entwurf eines Leitfadens erstellt, der im Falle von unvollständigen oder fehlenden Bestandsplänen die Grundlagen für die Beauftragung und Durchführung der Nachrechnung schafft.
Die zerstörungsfreien Prüfverfahren konnten ihre Fähigkeit bei der Untersuchung von Elementwänden in einzelnen Fallstudien erbringen. Aufbauend auf den Kenntnissen aus der Praxis und auf Testreihen im Rahmen von Laboruntersuchungen wurde ein erster Ringversuch geplant und durchgeführt. Im Rahmen dieses Ringversuchs wurden verschiedene Strukturdefekte und Einbauteile in Elementwände eingebaut. Die Messung der Wände erfolgte anschließend durch mehrere Messteams mit unterschiedlichen zerstörungsfreien Prüfverfahren. Zum Einsatz kamen hierbei das Ultraschall-Echo- und das Impact-Echo-Verfahren sowie das Impuls-Radar-Verfahren. Zur Verbesserung der Vergleichbarkeit zwischen den unterschiedlichen Prüfverfahren wurde auf die Elementwände ein einheitliches Messraster aufgebracht. Für eine möglichst objektive Messung der Wände erhielten die Messteams vor den Messungen keine Details zu den Strukturdefekten oder Einbauteilen. Die Prüfaufgabe bestand darin, die Wände mit dem jeweiligen Prüfverfahren zu untersuchen. Anschließend wurden die Ergebnisse der Messteams zentral gesammelt und ausgewertet. Anhand der zentralen Auswertung sollten Aussagen zu den eingebauten Inhomogenitäten ableitet werden. Hierdurch kann zum einen die Leistungsfähigkeit der Prüfverfahren an unterschiedlichsten Inhomogenitäten getestet werden, zum anderen können die Ergebnisse und somit die Prüfverfahren untereinander verglichen werden. Zu diesen in der Praxis immer häufiger vorkommenden Fragestellungen können grundsätzliche Aussagen zum Einsatz von zerstörungsfreien Prüfungen bei Elementwänden gewonnen werden. Über die Ergebnisse dieses Ringversuches wird nachfolgend berichtet.
In this work, fullerene has been functionalized with cyanuric Chloride at room temperature by a nitrene mediated [2 + 1] cycloaddition reaction. The adduct after functionalization is inherently in the form of azafulleroid and shows broad UV absorption in the wavelength range of 200–800 nm, as well as photothermal conversion and fluorescence with a high quantum yield.
A novel photoswitchable rotaxane was synthesised and its switching behaviour in solution was analysed with NMR and UV-Vis. A monolayer of rotaxanes was deposited on glass surfaces and the on-surface photoswitching was investigated. Angle-resolved NEXAFS spectra revealed a preferential orientation that reversibly changes upon switching.
Healable materials could play an important role in reducing the environmental footprint of our
modern technological society through extending the life cycles of consumer products and constructions. However, as most healing processes are carried out by heat alone, the ability to heal damage generally kills the parent material’s thermal and mechanical properties. Here we
present a dynamic covalent polymer network whose thermal healing ability can be switched ‘on’ and ‘off’ on demand by light, thereby providing local control over repair while retaining the advantageous macroscopic properties of static polymer networks. We employ a photoswitchable furan-based crosslinker, which reacts with short and mobile maleimidesubstituted poly(lauryl methacrylate) chains forming strong covalent bonds while simultaneously allowing the reversible, spatiotemporally resolved control over thermally induced de- and re-crosslinking. We reason that our system can be adapted to more complex materials and has the potential to impact applications in responsive coatings, photolithography and microfabrication.