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Eingeladener Vortrag
- nein (1102)
Diffraction-based experimental determination of Residual Stress in AM parts: A critical discussion
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, not always paralleled by the knowledge about the materials properties and performance. In particular, residual stress (RS) has been soon recognized as an issue in AM parts, so that parts are always post-heat-treated. Moreover, much effort has been spent on simulating RS, especially using finite element methods.
The experimental determination of RS has thereby become increasingly important, and even simple data constitute (to date) a piece of knowledge to fill the above-mentioned gap. In particular, diffraction methods, which are basically non-destructive, offer enormous possibilities to gain knowledge on real components, since neutrons and synchrotron radiation can penetrate even heavy metals up to several millimeters (or even centimeters). Indeed, some success has been obtained, and the knowledge about the origins of the RS fields, as well as their variation as a consequence of heat or mechanical treatments, has been greatly expanded.
In this talk, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with focus on those produced by laser powder bed fusion) has even allowed showing that process parameters that were considered unimportant play a major role in the onset of stress.
However, while RS is starting to be considered in the part design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigated about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even to date unclear will also be discussed, such as the determination of the reference unstrained samples and of the principal axes of stress. All these aspects will draw the path towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Verwertung von Bodenmaterialien - Ergebnisse aus dem UFOPLAN-Vorhaben und Transfer der Ergebnisse
(2019)
Dem Fachbeirat Bodenuntersuchungen des BMBF/UBA wurden Ergebnisse zum UFOPLAN-Forschungsvorhaben „Monitoring zur Verwertung von Bodenmaterial“ vorgestellt. Die potentielle Auswirkung der neuen Regularien in der geplanten Novelle der BBodSchV (4. Referentenentwurf der Mantelverordnung) auf die Erweiterung der Verwertungsmöglichkeiten von Bodenmaterialien wird aufgezeigt. Probleme des Umgangs mit der analytischen Messunsicherheit im Grenzwertbereich und mit der Vergleichbarkeit der zugelassenen Elutionsverfahren werden diskutiert.
The second edition of this textbook on physical electrochemistry, written by two experienced teachers of physical chemistry, corrosion engineering and materials science and engineering, covers the current knowledge which should be transferred to students of these fields.
In 20 chapters the fundamentals of electrochemistry, the most important electrochemical measurement techniques and applications of electrochemistry are covered.
It can be concluded that this study fulfills its intension of “serving as a key textbook in undergraduate courses” dealing with electrochemistry and being “a reference source for graduated students, researchers and engineers” interested in this field. Teachers will find sufficient content for preparing lectures on this topic. Even self‐learning is well supported by the clear structure, presented content and provided sources for further reading.
Dieser umfangreiche Leitfaden gibt Auskunft zur thermisch‐mechanischen Beständigkeit von 199 Eisen‐, 77 Nickelbasis‐ und 23 Kobaltbasislegierungen und ist ein sehr gutes und bestimmt erweiterbares Nachschlagewerk für Konstrukteure und Praktiker, die über den Einsatz geeigneter Werkstoffe in hohen Temperaturen entscheiden müssen.
Die zerstörungsfreien Methoden zur Untersuchung und Charakterisierung von Materialien sowie zur Detektion von betriebsbedingten und herstellungsbedingten Fehlern mit akustischen und elektrischen Methoden werden vorgestellt. Schwerpunkt bilden die Ultraschall-, die Wirbelstrom- und die Streuflussprüfung. Die Verfahren werden anhand des Aufgabenspektrums des Fachbereiches 8.4 der BAM dargestellt.
Die Schwerpunktthemen für die Forschung der BAM im Bereich der zerstörungsfreien Prüfung werden vorgestellt. Es stehen die aktuellen Forschungsprojekte der Fachbereiche 8.1 bis 8.7 der Abteilung 8 und des Arbeitsgebietes Probabilistische Sicherheits- und Zuverlässigkeitsanalysen von Frau Dr. Bertovic sowie der Nachwuchsgruppe von Frau JProf. Dr. Kruschwitz im Vordergrund.
The presentation introduces the BAM as well as the experimental possibilites at the BAM TTS in the first part. The general possibilities regarding Power2Gas with respect to hydrogen production by electrolysis are preseneted. Furthermore the Hydrogen Strategy of Germany and the status quo regarding grenn energy solutions in the transport sector are given. In the last part of the presentation a short overview of relevant investigations in the field of hydrogen safety and alternative fuels for cars as well as perspectively planned investigations of the BAM in this area are presented.
Avoiding road crashes has been the purpose behind many specialized software and hardware systems, involving both active and passive safety principles. Global Positioning technologies were incorporated into the transportation systems with the main purpose of acquiring the position of the vehicle under a continuous basis, for security and economy purposes. However, the GPS data can also be used for assessing the level of safety at which the vehicle is driven. On the basis of the essential data available from commercial GPS devices, in this paper we propose a combined performance measurement to assess the road safety level at which the vehicle is being driven. Such performance measure uses GPS data of the vehicle displacement, including the speed and the acceleration, as well as the course (latitude and longitude coordinates), in an integral driving assessment formulation that can run in real time. Results from the experimental use of this formulation suggest that the level of safety in the driving is time dependent, and that there are risky situations when different factors converge.
Multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) has evolved significantly since its introduction in 1992. The second and third generation instruments now allow isotope ratio measurements at unprecedented precisions, 0.001 % or better. However, precision alone is not enough for producing accurate and reliable isotope ratio measurements. Metrological considerations such as the selection of suitable calibration strategies, proper assessment of instrumental biases, and the estimation of overall measurement uncertainty remain critical to the measurement process. Properly assessed, measurement uncertainty then provides the interval within which a result can be considered both accurate and precise.
All mass spectrometric measurements are affected by instrumental mass discrimination and produce isotope ratios that are biased relative to their “true” ratio. To produce accurate and traceable isotope ratio measurements, it is imperative that certified isotope reference materials (iCRMs) be used for calibration and validation purposes. iCRMs reporting absolute isotope ratios are an analyst’s first choice, particularly when its uncertainty is sufficient for the intended use. However, when smaller uncertainties are required to resolve subtle differences between samples, delta-scale measurements become important. Here, the difference between an isotope ratio measured in a sample and in an internationally accepted isotope reference material (iRM) is determined. This deviation can be positive or negative relative to the iRM, is called a delta value, and is often expressed in per mil units.
This presentation will highlight the potential for MC-ICP-MS to produce isotope ratio measurements with minimal uncertainties by examining three applications involving Mg isotopes: 1) the certification of a set of iCRMs for their absolute isotope ratio using a gravimetric isotope mixture approach; 2) the comparison of these iCRMs with currently accepted Mg delta-scale reference materials through intercalibration, and 3) the determination of isotope fractionation exponents for geochemical applications.
The laser-based direct energy deposition (DED) as a technology for additive manufacturing allows the production of near net shape components. Industrial applications require a stable process to ensure reproducible quality. Instabilities in the manufacturing process can lead to faulty components which do not meet the required properties.
The DED process is adjusted by various parameters such as laser power, velocity, powder mass flow and spot diameter, which interact with each other. A frequently used comparative parameter in welding is the energy per unit length and is calculated from the laser power and the velocity in laser welding. The powder per unit length comparative parameter in the DED process has also be taken into account, because this filler material absorbs energy in addition to the base material.
This paper deals with the influence of mass energy as a comparative parameter for determining the properties of additively manufactured parts. The same energy per unit length of 60 J/mm as well as the same powder per unit length of 7.2 mg/mm can be adjusted with different parameter sets. The energy per unit length and the powder per unit length determine the mass energy. The laser power is varied within the experiments between 400 W and 900 W. Energy per unit length and powder per unit length are kept constant by adjusting velocity and powder mass flow. Using the example of Inconel 718, experiments are carried out with the determined parameter sets. In a first step, individual tracks are produced and analyzed by means of micro section. The geometry of the tracks shows differences in height and width. In addition, the increasing laser power leads to a higher dilution of the base material. To determine the suitability of the parameters for additive manufacturing use, the individual tracks are used to build up parts with a square base area of 20x20 mm². An investigation by Archimedean principle shows a higher porosity with lower laser power. By further analysis of the micro sections, it can be seen that at low laser power, connection errors occur between the tracks.
The results show that laser power, velocity and powder mass flow have to be considered in particular, because a constant mass energy can lead to different geometric as well as microscopic properties.
Die zunehmenden Nachweise von Kunststoffen in verschiedenen Umweltmedien erfahren in den letzten Jahren weltweit ein zunehmendes wissenschaftliches, gesellschaftliches und politisches Interesse. Besondere Aufmerksamkeit erfahren Kunststoffpartikel von 1-1.000 µm sogenanntes Mikroplastik. Es wurde mittlerweile in Wasser, Böden, Luft und Biota nachgewiesen. Obwohl die Wirkungen auf die natürlichen Umweltfunktionen noch unklar sind und kontrovers diskutiert werden, ist allein durch die ubiquitäre Präsenz eine systematische Erfassung von Eintragsquellen und Verbleib der Partikel über alle Umweltmedien notwendig, um Maßnahmen zur Reduktion der Einträge zu veranlassen.
Für eine zuverlässige Erfassung sind medienübergreifende Verfahren zu entwickeln, welche die drei analytischen Schritte, Probennahme, Probenaufbereitung und Detektion beinhalten. Die Verfahren adressieren unterschiedliche Zielgruppen, welche verschiedene analytische Informationen fordern. Für die akademische Bewertung werden Verfahren mit hohem analytischen Aufwand favorisiert, welche möglichst detaillierte Information über Partikelsorte, -größe, -zahl und -oberflächenbeschaffenheit geben. Im Gegensatz dazu, fordern Anwender aus der Praxis schnelle und einfache Monitoring Verfahren, welche die Bestimmung eines Massengehaltes, bzw. eines Grenzwertes zulassen. Allen ist gemeinsam, dass ein hoher interdisziplinärer Anspruch besteht, der sowohl technische Voraussetzungen zur repräsentativen Probennahme und die Limitationen von Detektionsverfahren berücksichtigt, als auch die Fachkompetenz von Biologen, Umweltwissenschaften, Analytiker und Polymerwissenschaftler einschließt.
Verfahren zum Mikroplastiknachweis müssen auch verschieden Proben mit sehr unterschiedlichen Gehalten an natürlicher Matrix gerecht werden. So müssen allein für Wasser Verfahren entwickelt werden, die Mikroplastik verschiedener Form (sphärische Partikel, komplexe Bruchstücke, Fasern) aus Medien mit sehr variablen Partikelanteil (u.a. Trinkwasser, Oberflächenwasser, Abwasser) repräsentativ erfassen sowie schnell und kostengünstig sind – einschließlich der notwendigen Probenaufbereitung. Die jeweiligen Detektionsverfahren müssen z.B. einzelne Partikel oder integrale Gehalte über drei Dekadenklassen für thermoplastische und insbesondere auch elastomere Partikelsorten erfassen können.
One of the most important goals in civil engineering is to guaranty the safety of constructions. National standards prescribe a required failure probability in the order of 10-6 (e.g. DIN EN 199:2010-12). The estimation of these failure probabilities is the key point of structural reliability analysis. Generally, it is not possible to compute the failure probability analytically. Therefore, simulation-based methods as well as methods based on surrogate modelling or response surface methods have been developed. Nevertheless, these methods still require a few thousand evaluations of the structure, usually with finite element (FE) simulations, making reliability analysis computationally expensive for relevant applications.
The aim of this contribution is to increase the efficiency of structural reliability analysis by using the advantages of model reduction techniques. Model reduction is a popular concept to decrease the computational effort of complex numerical simulations while maintaining a reasonable accuracy. Coupling a reduced model with an efficient variance reducing sampling algorithm significantly reduces the computational cost of the reliability analysis without a relevant loss of accuracy.
Casks for storage and transportation of used fuel rods of radioactive material are equipped with polyethylene (PE) for improved neutron flux shielding. The embedded PE structures are additionally exposed to gamma radiation and heat flow due to the specific high activity of the fission products. 60Co γ-radiation and heat load experiments at 125°C has been performed to evaluate PE degradation during the ageing process. FAR-FTIR-experiments were subsequently performed at differently aged PE test samples to characterize the oxidation process and morphological changes in the samples during the ageing at 125°C.
Im Vortrag werden Ergebnisse eines Forschungsvorhabens des DVS vorgestellt, in dem ein Verfahren zur Vermeidung von Schweißimperfektionen im Überlappbereich einer laserstrahlhybridgeschweißten Rundnaht entwickelt wird. Die Strategie der Prozessführung beim Schließen der Rundnaht sieht hervor, dass ein fehlerfreier Überlappbereich durch die Kontrolle der Erstarrungsbedingungen am Schweißnahtende erreicht wird. Die kontrollierte Wärmeführung wird durch eine Anpassung der Parameter von beiden beteiligten Schweißprozessen, dem Laserstrahl- sowie MSG-Schweißprozess realisiert. Es konnte gezeigt werden, dass eine Defokussierung des Laserstrahls von bis zu 40 mm über den Weg von max. 15 mm während der Bewegung des Schweißkopfes zu einer deutlich besseren Nahtausbildung im Überlappbereich führt. Es konnte eine günstige kelchförmige Schweißnahtform ohne eine Tendenz zur Rissbildung erzielt werden.
Elastomere werden vielfach in Produkten eingesetzt, die bei verschiedenen Temperaturen verwendet werden. O-Ringe sind kostengünstige Dichtelemente, die allerdings für die Funktionsfähigkeit und Sicherheit eines Produkts entscheidend sein können. Die untere Temperatur-einsatzgrenze ist dabei relevant und aus wissenschaftlicher Sicht nicht allgemein gültig zu definieren, da diese einerseits durch die Änderungen der Materialeigenschaften im Zuge des Gummi-Glas-Übergangs definiert werden, die Temperaturlage dieses Übergangs jedoch sehr stark von den jeweiligen Einsatzbedingungen (z.B. Frequenz) abhängt. Dadurch ergeben sich große Unterschiede zwischen statischen und dynamischen Anwendungen.
Verschieden Untersuchungen sollen vorgestellt und interpretiert werden, um das Auditorium auf verschiedene Herausforderungen aufmerksam zu machen und Lösungsansätze vorzustellen.
For many sealing applications rubber O-rings are applied due to their special properties and easy use. In many applications as e.g. in aviation, traffic or process technology the material can be exposed to a variety of conditions during operation as e.g. low temperatures, elevated temperatures and different media. Therefore, it is important to know the material behaviour and the seal performance under those conditions. Additionally ageing of seals is an important factor which has an influence on the long term reliability.
In this contribution we would like to discuss different aspects affecting the seal performance, lifetime estimation and address open questions which should be addressed to come to a deeper understanding of these seals commonly understood as typical machine elements.
Results of running investigations at the Bundesanstalt für Materialforschung und -prüfung (BAM), Division 3.4 “Safety of Storage Containers” are presented and discussed.
Humidity is one of principal environmental parameters that plays an important role in various application areas. Distributed humidity/water sensing is sought after in wide range of applications including concrete condition monitoring in civil engineering, SHM of large structures such as dykes or dams, soil moisture measurement in agriculture or leak detection in pipeline or sewage industry. Using humidity-induced strain of specialty hygroscopic coating materials, such as polyimide (PI) seems as the most promising approach so far. In this work, relative humidity and temperature response of different commercial PI-coated and tight-buffer fibers is investigated for the development of distributed humidity sensor.
Das Teilprojekt zielt auf die Entwicklung integrierbarer verteilter faseroptischer Sensoren (u. a. verteilte Brillouin-Sensorik, verteilte akustische Sensorik) für die Langzeitüberwachung von Betriebsparametern in Hoch- und Mittelspannungskabelanlagen. Mit Hilfe der Sensoren sollen unzulässige Dehnungen, Übertemperaturen und das Eindringen von Feuchte, z. B. in Unterseekabeln, detektiert werden. Das Teilprojekt beinhaltet ebenfalls die Entwicklung integrierfähiger Sensoren für verteiltes (vibro-)akustisches Monitoring an Unterseekabeln, vor allem zur Lokalisierung und zur Abwendung von Störfällen und Schäden durch äußere mechanische Einflüsse (z. B. Ankerwurf).
Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe (polybromierte Flammschutzmittel) in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden.
Recent facade fires worldwide have driven change in regulations for façade fire safety in different parts of the world. The Grenfell Tower fire 2017 in London triggered a thorough investigation of many aspects of the fire. One investigation was about the UK building regulations from Dame Judith Hackett. This investigation compares the UK with the situation other parts of the world. Key findings of the review of building regulations by Judith Hackett are:
Warfarin als ein Vertreter der NSO-Hetereozyklen, ist seit den 1950er Jahren einer der bekanntesten Gerinnungshemmer. Beim Menschen wird es bis heute zur Vorbeugung von Thrombose und der Behandlung von Vorhofflimmern und Arrhythmie eingesetzt. Doch schon einige Jahre vor der FDA Zulassung als Medikament wurde es zur Bekämpfung von Nagetieren eingesetzt. Bis heute wurde es nur teilweise durch weitaus wirksamere antikoagulante Rodentizide (ARs) der zweiten Generation, sogenannte Superwarfarine, ersetzt. In der Fachliteratur finden sich zahlreiche Beispiele für sekundäre und tertiäre Vergiftung mit ARs bei Wildtieren und anderen Nichtzieltieren. Bisher ist relativ wenig über die Bioakkumulation, Persistenz und Toxizität von ARs und deren Transformationsprodukten (TPs) in der terrestrischen und aquatischen Umwelt, sowie der Nahrungskette bekannt.
Um Einblicke in mögliche Transformations- und Abbauprozesse von Warfarin zu erhalten und um Umwelteinflüsse zu simulieren, wurde es in einer elektrochemischen Reaktorzelle oxidativ umgesetzt und mittels Massenspektrometrie analysiert. Hinsichtlich der Wasseraufbereitung in Kläranlagen wurden technisch relevante Simulationsverfahren wie Chlorung, UV-Bestrahlung und Ozonung angewendet um potentielle Eliminierungswege aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt, massenspektrometrisch analysiert und verglichen.
We report the synthesis and characterization of carbon nanodots (CDs) with high quantum yield (>50%) and tailored optical absorption as well as emission properties. A well-described protocol with polyethyleneimine (PEI) as amine precursor is used as a reference to a new CD system which is stabilized by aromatic 2,3-diaminopyridine (DAP) molecules instead. The DAP stabilizer is installed in order to red-shift the absorption peak of the n-π* electron transition allowing efficient radiative recombination and light emission. Size, shape, and chemical composition of the samples are determined by (HR)TEM, EDX and FTIR-spectroscopy. Optical parameters are investigated using UV-VIS, PL and QY measurements. Several parameters such as concentration, excitation wavelength and pH are studied. Zeta-potential analysis indicate that pH-induced (de-)protonation processes of functional moieties directly affect the n-π* energy bands. This results in unique pH-dependent absorption and emission characteristics which are discussed on the specific chemical composition of each CD system.
Our aim is to develop a new simple and inexpensive method for full field X-ray fluorescence imaging. We combine an energy-dispersive array detector with a coded aperture. To obtain the information from the recorded image, a reconstruction step is necessary. First tests were carried out at the BAMline at BESSY II. This method enables the simultaneous detection of multiple elements, which is important e.g. in the field of catalysis.
We developed a new method for full field X-ray fluorescence imaging at the BAMline @ BESSY II. We combined an energy dispersive array detector for X-rays with a coded aperture to get high resolution images.
In coded aperture imaging, an object is projected through a mask, producing many overlapping images on the detector. To get the information about the investigated object out of the projected image, a decoding step is necessary.
The first part of our project was to develop the decoding algorithms. We tested the reported reconstruction with an antimask and compared the results with the performance of self-written reconstruction programs based on an iterative and a genetic algorithm. First tests were performed with raytracing simulations.
The next step was the collection of experimental data at the BAMline @ BESSY II (HZB). A test objects could be successfully reconstructed with our newly developed algorithm.
Extensometer sind seit Jahrzehnten im Einsatz und bilden die Basis für eine präzise Dehnungsmessung in werkstoffmechanischen Versuchen. Jedoch ist die Temperaturstabilität von Extensometern häufig noch nicht ausreichend beachtet worden, um Fehler verursacht durch Temperaturschwankungen zu minimieren. Dieses wird derzeit nicht nur in Deutschland, sondern auch international zunehmend diskutiert. Datenblätter von Extensometern sind teils unvollständig besonders hinsichtlich von Temperatureinflüssen. Extensometer für den Einsatz bei höheren Temperaturen sollen z.B. laut Normen für dehnungsgeregelte Ermüdungsversuche mit Luft oder Wasser aktiv gekühlt werden. Jedoch schreiben die Normen keine Temperatur-Toleranzen für Extensometer vor. Dehnungsfehler verursacht durch Temperaturschwankungen am Extensometer bleiben meist verborgen, da die Temperatur des Extensometers standardmäßig gar nicht gemessen wird. Die Ursache von Einflüssen zur Temperaturstabilität von Extensometern wird erläutert. Ein einfaches Rechenbeispiel zeigt die Empfindlichkeit von Extensometern gegenüber Temperaturschwankungen und die Auswirkungen auf den Dehnungsfehler. Lösungsmöglichkeiten zur Optimierung werden aufgezeigt. Der Anwender von Extensometern soll sensibilisiert werden, um der Temperaturstabilität von Extensometern sowohl hinsichtlich Herstellerspezifikationen als auch bei der Anwendung von Extensometern im Prüflabor mehr Aufmerksamkeit zu schenken, um letztlich die Qualität von Versuchsergebnissen zu verbessern. Empfehlungen an Extensometerhersteller werden formuliert. Dieses Thema wird zukünftig auch in Prüfnormen mehr Aufmerksamkeit geschenkt werden. Es werden Maßnahmen zur Verbesserung der Temperaturstabilität von Extensometern Einzug in Prüfnomen finden, um letztlich verlässlichere Versuchsergebnisse zu erhalten. Es ist beabsichtigt, eine Verbesserung der Temperaturstabilität von Extensometern z.B. bei der nächsten Revision der Prüfnormen ISO 12106 und ISO 12111 für dehnungsgeregelte LCF- und TMF-Versuche zu berücksichtigen.
Localized laser surface treatments are able to produce tailor-made surface properties to fulfill requirements of a variety of technical applications. Especially micrometric surface topologies can be beneficial for optimizing tribological contact situations. Structures with lowered surface features are already utilized for bearings or cylinders of combustion engines. There are also other fields of application, where the potential of protruding surface features is known, e. g. for metal forming tools.
A promising approach for a tailored surface treatment working in the microsecond range is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This technique is able to produce micrometric surface structures and to improve simultaneously the wear resistance by creating metal matrix composites.
In this talk, the laser implantation technique is described and compared to the state of the art. The potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces is demonstrated by means of microstructural and topographical investigations of different ceramic materials and steel substrates. Finally, results of research projects are presented aiming on the application of such structured surfaces. Their capability to change and optimize friction and wear are demonstrated for fully lubricated contacts, tools for hot sheet metal forming and tools for cold rolling of sheets for automotive applications.
Das Prozessmonitoring stellt einen wichtigen Baustein für eine Qualitätssicherung additiv gefertigter Bauteile dar, insbesondere bei kleinen Losgrößen. Der Vortrag zeigt einen Überblick aktueller Entwicklungen der BAM im Bereich des Prozessmonitorings für das Laserstrahlschmelzen (laser powder bed fusion) metallischer Werkstoffe. Durch Vergleich mit der Referenzmethode Computertomografie wird am Beispiel der thermografischen Verfahren gezeigt, wie relevante Defekte in Bauteilen detektiert werden können und Einsatzpotenziale sowie Limitierungen aufgezeigt.
Polymers of intrinsic microporosity (PIMs) have recently emerged as novel materials for a broad range of high-performance applications from gas separation to electronic devices. The very rigid, contorted polymer chains show only limited molecular mobility and therefore pack inefficiently giving rise to intrinsic microporosity with pore sizes generally smaller than 1 nm resulting in BET surface areas larger than 700 m2/g. Using conventional thermal analysis techniques, no glass transition temperature (Tg) of PIMs could be unambiguously detected up to now. Employing fast scanning calorimetry (FSC) based on a one chip sensor, decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this limitation. The FSC device is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. Evidence of a glass transition is obtained for a series of PIMs with different chain rigidities. Local small-scale fluctuations are held responsible for the glass transition of highly rigid PIMs rather than segmental motions as in conventional polymers.
In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert.
Demonstrationsexperimente
(2019)
Korrosionsprüfung
(2019)
Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)-
Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement.
The European Commission's recommendation on the definition of nanomaterial [2011/696/EU] is broadly applicable across different regulatory sectors and requires the quantitative size Determination of constituent particles in samples down to 1 nm. A material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The implementation of the definition in a regulatory context challenges measurement methods to reliably identify nanomaterials and ideally also nonnanomaterials as substance or product ingredient as well as in various matrices.
The EU FP7 NanoDefine project [www.nanodefine.eu] addressed these challenges by developing a robust, readily implementable and cost-effective measurement strategy to decide for the widest possible range of materials whether it is a nanomaterial or not. It is based on existing and emerging particle measurement techniques evaluated against harmonized, material-dependent performance criteria and by intra- and inter-lab comparisons. Procedures were established to reliably measure the size of particles within 1-100 nm, and beyond, taking into account different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics.
A main outcome is the establishment of an integrated tiered approach including rapid screening (Tier 1) and confirmatory methods (tier 2), a decision support flow scheme and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool which implements the flow scheme in a user-friendly software and guides the user in a semi-automated way through the entire decision procedure. It allows a cost-effective selection of appropriate methods for material classification according to the EC's nanomaterial definition and provides a comprehensive report with extensive explanation of all decision steps to arrive at a transparent identification of nanomaterials as well as non-nanomaterials for regulatory
purposes.
Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with Errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs.
An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal, has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. In the TEM micrograph the particles tracked manually according to the measurement protocol. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy.
Bei der Explosion in einer Herstellungsstätte für ein Pulver zur Reinigung industrieller Feuerungsanlagen in Deutschland ist eine Person tödlich verunglückt. Die BAM wurde gebeten, beschlagnahmte Muster des Reinigungspulver zu bewerten. Dafür wurden verschiedene Untersuchungen durchgeführt. Diese sollten klären, ob die stoffliche Einstufung des Reinigungspulvers in die Stoffklasse 5.1 für die sichergestellten Pulverproben zutreffend ist. Es konnte nachgewiesen werden, dass die untersuchten Pulverproben explosionsgefährliche Eigenschaften aufweisen. Die von explosionsgefährlichen Stoffen ausgehenden Gefährdungen müssen ermittelt und bei der Herstellung und Verwendung berücksichtigt werden. Die Gefährdungen sind entsprechend neu eingeführter sicherheitstechnischer Kennzahlen ermittelt und anschließend klassifiziert worden. Die Klassifizierung erfolgte durch die Zuordnung zu einer s.g. Gefahrgruppe.
GPS-data based calculation scheme for assessing, in real-time, the level of safety exerted during driving, has been described and used. The several variables involved considered the main factors that lead to road mishaps, including the speed, the acceleration and the effects that these variables have on the vehicle when it is negotiating a turn. The performance measure combines three individual performance outputs: speed, acceleration and a hybrid performance measure considering the speed, the acceleration and the change in latitude/longitude. The measures are designed in such a way that weighting factors can be calibrated in order to establish certain critical parameters. On the other hand, the terms in the equations preclude any division by zero of the involved ratios. On the other hand, the simplicity of the equations makes it possible to carry out the assessment in real time. The use of the resultant performance measure to a relatively long path, together with its current average value, indicates that the safe performance of the driving changes with time, and that, for the selected values of the calibration constants, the traveling speed dominates the overall safety performance of the driving. Furthermore, the different calibration constants provide the possibility of considering different types of hazmat carrying vehicles. While many other formulation components could be integrated into the performance measure, this three-component performance measure could be used to assess the driving of a hazmat-carrying vehicle, in order to detect and to prevent dangerous conditions, such as driver fatigue.
Finally, the implementation of the different performance measure formulations in a system such as the one described in the introduction of this paper, could be straightforward.
A testing methodology has been proposed in this paper, to compare the load transfer derived from solid and liquid cargoes when the carrying vehicle is subjected to a lateral acceleration in a tilt table. Besides the type of cargo, the other factors
(a) One-quarter fill level
(b) One-half fill level
(c) Three-quarter fill level
(d) Fast input
considered are the fill level and the rate at which the considered are the fill level and the rate at which the acceleration input is acceleration input is exerted on the vehicleexerted on the vehicle. The acceleration The acceleration input can represent the entering of the carrying vehicle into a input can represent the entering of the carrying vehicle into a curved portion curved portion of of aa road.
The testing device integrates the needed components to measure the fourmeasure the four--wheel loads of the wheel loads of the carrying vehicle, while carrying vehicle, while providing different times to attain providing different times to attain aa 10°10° angle angle for the tilt table. for the tilt table.
The performance measure selected is significant to assess the rollover trend of a vehicle, on the basis of the wheel loads at both sides of the vehicle. both sides of the vehicle.
The outputs from the experiments suggest that the sloshing suggest that the sloshing cargo transfercargo transferss the greater loads, the greater loads, regardless of the fill level and regardless of the fill level and acceleration rate inputacceleration rate input, as a result , as a result of the shifting of the center of of the shifting of the center of gravitygravity of the liquidof the liquid, and of of the the dynamic vibration at the end of dynamic vibration at the end of the perturbation input. In this respect, while the solid cargo the perturbation input. In this respect, while the solid cargo exhibits an initial peak and decay, the exhibits an initial peak and decay, the sloshing cargo exhibits sloshing cargo exhibits several oscillations of the saseveral oscillations of the same magnitude, which is attributed me magnitude, which is attributed to the to the liquid inertia and liquid inertia and to the to the reflection of the surface waves. reflection of the surface waves.
A further analysis could supplement this research, to assess supplement this research, to assess the effect of some other factors on the dynamic the effect of some other factors on the dynamic behavior of the behavior of the liquid cargoliquid cargo-vehicle system. Fvehicle system. For example, to analyze the effect or example, to analyze the effect of longitudinal baffles, and to validate theoretical models.of longitudinal baffles, and to validate theoretical models.
Extensometer werden seit langer Zeit erfolgreich für die Ermittlung von werkstoffmecha-nischen Kennwerten eingesetzt. Allerdings wurden in den letzten Jahren immer wieder durch Temperaturschwankungen bedingte Drift an Extensometern festgestellt, die be-sonders in Langzeitversuchen zu Problemen führen können. Es wurden Ursachen für die thermische Drift von Extensometern aufgezeigt. Anhand von einem Beispiel wurde gezeigt, wie sich Temperaturschwankungen an einem Extensometer auf die Ergebnisse von werkstoffmechanischen Ermüdungsversuchen auswirken können. An einem weiteren Beispiel wurde beschrieben, dass der durch Temperaturschwankungen verursachte Dehnungsfehler eines Extensometers stark von der Höhe der Temperaturschwankung und von der Dehnungsschwingbreite abhängt und, je nach Anwendungsfall größer als 1% werden kann. Es wurde verdeutlicht, dass bisherige nach Norm vorgeschriebene Maß-nahmen oft nicht ausreichen, um Einflüsse von Temperaturschwankungen am Extenso-meter zuverlässig zu unterbinden. Vorschläge wurden aufgezeigt, um die Temperatursta-bilität von Extensometern zu verbessern. Das gesamte Temperaturmanagement von Raumtemperatur, Kühlwassertemperatur, Temperaturmessung am Extensometer etc. sollte von Grund auf neu betrachtet werden, um Verbesserungen bei der Temperatur-konstanz von Extensometern zu erlangen. Ferner wurde vorgeschlagen, Extensometer in temperaturkompensierter Ausführung zu entwickeln und zu verkaufen. Dieses sollte Ret-rofits für existierende Extensometer miteinschließen. Konkrete Maßnahmen zur Imple-mentierung in Materialprüfungsnormen müssen weiter diskutiert werden.
In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert.
Die Wettbewerbsfähigkeit der Prozessindustrie basiert auf der Sicherung der geforderten Produktqualität bei einer optimalen Nutzung von Anlagen, Rohstoffen und Energie. Ein Weg zur wissensbasierten Produktion führt über die Betrachtung der wesentlichen Apparate-, Prozess- und Freigabedaten aus Betrieben und Labors. Das Potenzial dieser Daten wird heute vielfach noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt.
Neben Fragen zur Datenerfassung, Datenkonnektivität und Datenintegrität müssen solche Daten für eine ganzheitliche Prozessanalyse zunächst mit Kontextinformationen zusammengebracht werden. Datenquellen enthalten Zeitwertpaare, aber auch diskrete Daten aus LIMS (Laboratory Information Management Systems) oder ELN (Electronic Laboratory Notebooks) und werden zunehmend durch 2D- und 3D-Daten aus der Chromatographie-Massenspektrometrie oder bildbasierter Analytik ergänzt.
Für die automatisierte Merkmalsextraktion, etwa zur Extraktion chemischer Informationen aus den oben genannten Datenquellen werden multivariate Werkzeuge und Algorithmen genutzt. Multivariate Statistiken wie PCA (Principle Component Analysis), PLS (Partial Least Squares) und LDA (Latent Discriminant Analysis) bilden die erste Grundlage für die Datenanalyse. Für diese Verfahren sind heute Datenvorbehandlungsschritte nötig. Die Modellbildung geschieht manuell und ist sehr aufwendig.
Können diese Daten im Zeitalter von ML (Machine Learning) und KI (Artificial Intelligence) anderweitig sinnvoll genutzt werden und ohne klassische Modellbildung? Die Bezeichnung „Big Data“ als Voraussetzung für datengetriebene Auswerteverfahren ist für die Prozessindustrie allerdings unpassend, denn auch bei mengenmäßig großen Datensätzen liegen für Kampagnen typischerweise nur Informationen über einige Batches mit einer Serie von Messdaten vor, die genügend Varianz für eine datengetriebene Auswertung aufweisen – nicht vergleichbar mit den Datenmengen im WWW oder von großen Internet-Konzernen.
Ein Weg zur wissensbasierten Produktion führt über die Betrachtung der wesentlichen Apparate-, Prozess- und Freigabedaten aus Betrieben und Labors. Das Potenzial dieser Daten wird heute vielfach noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt.
Neben Fragen zur Datenerfassung, Datenkonnektivität und Datenintegrität müssen solche Daten für eine ganzheitliche Prozessanalyse zunächst mit Kontextinformationen zusammengebracht werden. Datenquellen enthalten vor allem Zeitwertpaare, die numerisch vorbehandelt und möglichst vollautomatisch ausgewertet werden müssen. Am Beispiel NMR-spektroskopischer Daten wird der Stand der Auswertung mit physikalisch motivierten Modellen, wie z. B. dem IHM erläutert.
Die thermografische ZfP basiert auf der Wechselwirkung von thermischen Wellen mit Inhomogenitäten. Diese Inhomogenitäten hängen mit der Probengeometrie oder der Materialzusammensetzung zusammen. Obwohl die Thermografie für ein breites Spektrum von Inhomogenitäten und Materialien geeignet ist, ist die grundlegende Einschränkung die diffuse Natur der thermischen Wellen und die Notwendigkeit, ihre Wirkung lediglich an der Probenoberfläche radiometrisch messen zu können. Die Ausbreitung der thermischen Wellen von der Wärmequelle über die Inhomogenität zur Detektionsoberfläche führt zu einer Verschlechterung des räumlichen Auflösungsvermögens der thermografischen Technik. Ein neuer konzertierter Ansatz auf Basis einer räumlich strukturierten Erwärmung und einer Joint Sparsity des Signalensembles ermöglicht eine verbesserte Rekonstruktion von Inhomogenitäten.
Im Beitrag wird die Implementierung dieses Ansatzes auf Basis einer strukturierten Beleuchtung mit einem 1D-Laser-Array vorgestellt. Die einzelnen Emitterzellen des Laser-Arrays werden durch ein pseudozufälliges Binärmuster gesteuert und zusätzlich leicht verschoben. Die wiederholte Messung dieser verschiedenen Konfigurationen bei gleichzeitig konstanter Inhomogenität ermöglicht eine Rekonstruktion der Inhomogenität unter Ausnutzung der Joint Sparsity.
Im Vortrag werden die für den Betrieb der Erdgasnetze relevanten Kenngrößen des Explosionsschutzes erläutert. Der Einfluss von Wasserstoffeinspeisung auf diese Kenngrößen wird dargestellt und diskutiert. Die Stoffdaten der Erdgas-Wasserstoff-Gemische sind im Rahmen eines von der BG-ETEM geförderten Vorhabens in der BAM gemessen worden. Basis dieser Messungen waren in Europa harmonisierte Normen.
Zudem sind mit Hilfe von numerischen Methoden berechnete explosionsgefährdete Bereiche von Erdgas-Wasserstoff-Gemischen im Vergleich zum reinen Erdgas betrachtet worden. Der Vortrag gibt weiterhin Hinweise auf Auswirkungen von Wasserstoffzusätzen auf Gaswarngeräte.
Explosion and decomposition limits of flammable and chemically unstable gases were determined experimentally in a closed autoclave with an ignition energy higher than the standard 10 J a 20 J. The ignition source was a lightning arc caused by an exploding wire igniter as described in EN 1839 B. With a newly developed ignition system a graded ignition energy between 3 J and 1000 J was generated. Different types of gases were studied with this ignition system: methane as a typical fuel gas and reference gas for some standards for explosion limit determination, the refrigerant R32 (difluoromethane) as a mildly flammable gas with low burning velocity and high minimum ignition energy compared with methane as well as the chemical unstable gases acetylene, nitrous oxide and ethylene oxide, which can decompose explosively in the absence of air or other oxidizers. It was found that the influence of strong ignition sources on explosion and decomposition limits can be very different for different systems. In case of methane only the upper explosion limit was influenced significantly by the ignition energy, whereas the lower explosion limit was constant. In a standard test vessel with an inner volume of 14 dm3 it was difficult to quantify the upper explosion limit of methane exactly with the strong ignition source, because the explosion pressure did not increase abruptly near the explosion limit, but steadily over a large concentration range. Probably a larger explosion vessel is more appropriate in this case. In case of R32 however, it was the lower explosion limit that was influenced significantly by the ignition energy and not the upper explosion limit. A particularly strong dependency from the ignition energy was found for the decomposition limits of the chemically unstable gases in nitrogen. Here special regard is necessary in practical applications, if uncommonly strong ignition sources cannot be excluded.
Im Vortrag werden die sicherheitstechnischen Kenngrößen des Explosionsschutzes von Erdgas-Wasserstoff-Gemischen erläutert. Der Einfluss von Wasserstoffeinspeisung in Erdgasnetze wird dargestellt und diskutiert. Die Stoffdaten der Erdgas-Wasserstoff-Gemische sind im Rahmen eines von der BG-ETEM geförderten Vorhabens in der BAM gemessen worden. Basis dieser Messungen waren in Europa harmonisierte Normen.
Mit Hilfe von numerischen Methoden sind explosionsgefährdete Bereiche um Abblasvorrichtungen bei Erdgas-Wasserstoff-Gemischen im Vergleich zum reinen Erdgas betrachtet worden. Der Vortrag gibt weiterhin Hinweise auf Auswirkungen von Wasserstoffzusätzen auf Gaswarngeräte.
The exploration of metal phosphonates has gained great interest during the last decades, because of their structural diversity. They are promising candidates for a variety of applications ranging from adsorbance to electrocatalysis. The knowledge of the Crystal structure is significant for assigning a coordination polymer for a specific function. We investigated the influence of the fluorination degree of the organic linker on the Crystal packing, the interlayer distance, and the hydrophobicity of the resulting compounds. With fluorinated and nonfluorinated benzylphosphonic acids as starting materials in mechanochemical synthesis, four novel cadmium benzylphosphonates were obtained. Their structures were solved from powder X-ray diffraction.
Separation and detection of antioxidants using a graphene based electrochemical sensor platform
(2019)
CVD-Graphene is ideally suited as an active element for electrical and electrochemical sensing platforms, since it provides for high sensitivity and low detection limit. Electrochemical sensors provide a simple way to measure analytes in fluids with high sensitivity without the need for complex instrumentation. Due to These aspects, graphene sensors are interesting for a wide range of applications in bio analytics. Antioxidants are natural or synthetic compounds, which inhibit oxidation processes and hence often find use as preservatives.
It has been suggested that the long-term consumption of diets rich in antioxidants is associated with a lower risk of developing diseases linked to oxidative stress. Gallic acid and ascorbic acid are representatives of antioxidants. We have developed a graphene-based sensor platform to separate and subsequently detect antioxidants. Graphene exhibits low detection limits for ascorbic acid and polyphenols. In this study, the sensing of gallic acid and ascorbic acid on bare CVD graphene in various solvents was investigated by Square Wave Voltammetry. Furthermore, the separation and detection of the bioanalytes by deploying different membranes were evaluated.
Background. Aflatoxin B1 (AFB1) is a toxic low-molecular-weight secondary fungal metabolite produced mainly by Aspergillus flavus and Aspergillus parasiticus not only at pre-harvest time but also at post-harvest stages including storage. AFB1 was classified as a Group I carcinogen by the World Health Organization for Research on Cancer in 1993. AFB1 is able to naturally contaminate medicinal plants and therefore causing serious health issues for humans consuming the related medicine. This study aimed to develop an efficient fluorescence polarization immunoassay (FPIA) and for the first time a rapid (5-10 min), low-cost, and simple membrane-based flow-through immunoassay (MBA) for determination of AFB1 in medical herbs based on a monoclonal antibody.
Methods. Two different techniques for AFB1detection in medical herbs (Herba Orígani vulgáris, Folia Urticae, Fructus Rubi idaei) were developed and compared, namely an easy-to-use semi-quantitative flow-through membrane-based enzyme immunoassay (MBA), and a homogeneous method which needs no separation or washing steps (assay time 10 min), a quantitative fluorescence polarization immunoassay (FPIA).
Results. A cut-off level of the developed MBA can vary wide from 0.8 ppb to 1 ppb. The FPIA method showed a linear working range of 8.6 ppb to 64 ppb, IC50 of FPIA is 24 ppb. The results were in good correlation with the ELISA results (IC50 = 0.1 ppb). LC–MS/MS was used to confirm the results, too.
Conclusion. MBA can be used for a quick on-site AFB1 detection in medical herbs (Herba Orígani vulgáris (Oríganum vulgáre), Folia Urticae (Urtíca dióica), Fructus Rubi idaei (Rúbus idáeus)), the developed test does not require special equipment and is not time-consuming (5-10min), includes several simple steps and can be performed directly on-site. The major advantages of the developed FPIA are its simplicity and suitability for a rapid screening of a large number of samples.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Finally, I will show that BAM is very active in standardization and certification, including production of Reference Materials and Methods.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Kaltrissprüfung hochfester Feinkornbaustähle beim Schweißen mit modifiziertem Sprühlichtbogen
(2019)
Sind in Stahlkonstruktionen hohe Tragfähigkeiten bei geringem Eigengewicht gefordert, finden hochfeste Feinkornbaustähle mit Streckgrenzen ≥ 960 MPa Anwendung. In der Vergangenheit wurde der konventionelle Übergangslichtbogen (Konv. LB) zur schweißtechnischen Fertigung von hochfesten Stählen eingesetzt. In den letzten Jahren wurde der modifizierte Sprühlichtbogen (Mod. SLB) entwickelt, welcher reduzierte Nahtöffnungswinkel bei erhöhter Abschmelzleistung ermöglicht. Jedoch treten höhere Wasserstoffkonzentrationen verbunden mit Mikro-(Kalt-)rissen unter reduziertem Nahtöffnungswinkel mit Mod. SLB auf. In diesem Beitrag wird die Kaltrissempfindlichkeit des hochfesten Feinkornbaustahles S960QL mit artgleichem Schweißzusatzwerkstoff untersucht.
Es besteht die grundsätzliche Anforderung, dass alle nichtmetallischen und metallischen Materialien nur dann in Sauerstoffanwendungen eingesetzt werden dürfen, wenn sie sicherheitstechnisch auch für die entsprechenden Betriebsbedingungen geeignet sind. Der Vortrag stellt nicht nur die gängigen Prüfverfahren und Beurteilungskriterien. Es werden auch die folgenden Fragen beantwortet, die häufig von Wirtschaftsunternehmen und Verbänden gestellt werden:
- Welchen praktischen Anwendungsfall bilden die Prüfungen ab?
- Welche Untersuchungsmethoden führt die BAM durch?
- Warum verwendet die BAM ergänzende Beurteilungskriterien bei der sicherheitstechnischen Interpretation von Prüfergebnissen?
- Warum empfiehlt die BAM chargenbezogene Materialprüfungen?
- Worin unterscheiden sich die zwei von der BAM verwendeten Methoden zur Beurteilung der Ausbrennsicherheit von Armaturen und Anlagenteilen und welche Vor- und Nachteile bietet jede dieser Methoden?
Grundsätzlich dürfen alle nichtmetallischen und metallischen Materialien nur dann in Sauerstoffanwendungen eingesetzt werden, wenn sie sicherheitstechnisch für die Betriebsbedingungen geeignet sind. Neben allgemeinen Sauerstoff-spezifischen Anforderungen stellt der Vortrag die standardisierten Prüfverfahren und die Untersuchungsmöglichkeiten der BAM vor. Die Beurteilungskriterien für die Prüfverfahren werden kritisch betrachtet und es wird erklärt, in welchen Fällen und aus welchen Gründen die BAM ergänzende Beurteilungskriterien verwendet. Um den tatsächlichen, praktischen Anwendungsfall abzubilden, ist unter gewissen Umständen die Anpassung des Prüfumfangs möglich. Außerdem wird dargestellt, warum die BAM chargenbezogene Materialprüfungen empfiehlt.
Auch Sauerstoff- Armaturen und Anlagenteile müssen sicherheitstechnisch für die Betriebsbedingungen geeignet sein. Zur Beurteilung der Ausbrennsicherheit werden die zwei an der BAM praktizierten Vorgehensweisen mit ihren jeweiligen Vor- und Nachteilen vorgestellt: Untersuchung der Armatur als komplette Funktionseinheit bzw. Beurteilung der Armatur auf Basis der Untersuchungen der eingesetzten Materialien. Neben den Anforderungen aus produktspezifischen Normen wird auch für diesen Fall kurz erklärt, in welchen Fällen und aus welchen Gründen die BAM ergänzende Beurteilungskriterien verwendet bzw. den Prüfumfang anwendungsfallbezogen anpasst.
Kaltrissprüfung hochfester Feinkornbaustähle beim Schweißen mit modifiziertem Sprühlichtbogen
(2019)
Der konstruktive Leichtbau erfordert den zunehmenden Einsatz hochfester Feinkornbaustähle mit Streckgrenzen bis zu 1300 MPa. Um darüber hinaus Schweißzeit, Schweißnahtvolumina und Schweißkosten zu minimieren, kam es zur Entwicklung moderner Lichtbogenprozesse mit erhöhter Abschmelzleistung, wie bspw. dem modifizierten Sprühlichtbogen (mod. SLB). Dieser Beitrag zeigt Kaltrissuntersuchungen beim Einsatz des mod. SLB unter reduziertem Nahtöffnungswinkel eines Hochfesten S960QL. Mit Hilfe des fremdbeanspruchten Implant-Tests konnte dargelegt werden, dass durch die erhöhte Abschmelzleistung ein tieferes Einbrandprofil entsteht und es dadurch zu einer zeitverzögerten Rissbildung kommt. Ergebnisse des selbstbeanspruchenden TEKKEN-Tests zeigen eine deutliche Rissbildung im Schweißgut unter reduziertem Nahtöffnungswinkel. Durch eine Nachwärmung unmittelbar nach dem Schweißen kann diese Rissbildung minimiert werden.
Force-distance curves have been recorded on thin films of lubricants. The lubricants wet the AFM tip, which causes a capillary force. This force depends on the shape of the tip, as well as on physical properties like viscosity and surface tension, which have been determined additionally with other methods. This way, their influence on the shape of the curves could be analyzed.
Photothermal radiometry with an infrared camera allows the contactless temperature measurement of multiple surface pixels simultaneously. A short light pulse heats the sample. The heat propagates through the sample by diffusion and the corresponding temperature increase is measured at the samples surface by an infrared camera. The main drawback in radiometric imaging is the loss of the spatial resolution with increasing depth due to heat diffusion, which results in blurred images for deeper lying structures. We circumvent this information loss due to the diffusion process by using blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm.
Der Vortrag zeigt aktuelle Entwicklungen und Betätigungsfelder des Fachbereichs Prozessanalytik zum Thema Automation in der Analytik. Dies Umfasst die Laborautomation am Beispiel der Probenpräparation für die Röntgenfluoreszenzanalyse und moderne Synthesekonzepte in der organischen Chemie. Außerdem wird die Rolle der Prozessanalytik in der kontinuierlichen Produktion thematisier. Als Anschauungsgegenstand dienen die Überwachung einer Hydroformylierung mittels Raman- und NMR-Spektroskopie und der Einsatz eines NMR-Sensors in einer modularen Produktionsanlage im Pilotmaßstab.
At BAM, which is a federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes assessment of elastomeric seals applied in the casks. One of the aims is to identify a suitable method for estimating the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to five years. In order to assess sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings were aged as well. In order to understand the underlying ageing mechanisms in each material, material properties such as hardness, density and tensile properties were examined. Additionally, compression set (CS), which represents the recovery behaviour of a seal after release from compression, is measured. For obtaining results closely related to practical conditions, O-rings with a full-scale cord diameter of 10 mm were aged. However, this set-up can lead to heterogeneous ageing caused by diffusion-limited oxidation (DLO) effects especially for HNBR, resulting in distorted bulk properties such as compression set. However, if DLO-affected data is excluded, extrapolations of CS data are possible using time-temperature shifts.
For selecting an appropriate end-of-lifetime criterion, leakage rate measurements were performed, since leakage rate is the only characteristic directly correlated to the performance of the sealing system. A significant increase in leakage rate was considered as the end of the lifetime. However, the O-rings remained leak tight under static conditions even though material properties had already degraded strongly. For this reason, a modified, more demanding leakage test involving a fast small decompression of the seal was developed that allowed determining a more conservative end-of-lifetime criterion with a safety margin for EPDM seals. FKM, which is a very heat and oxidation resistant material, exhibited only little degradation, even though it had the smallest activation energy.
Seit dem 1. Januar 2019 müssen Hersteller alle ihre energieverbrauchrelevanten Produkte in der Europäischen Produktdatenbank für die Energieverbrauchskennzeichnung EPREL registrieren, bevor sie auf dem EU-Markt verkauft werden können. Nutzung, Aufbau und Admin-Struktur der Datenbank werden vorgestellt.
At the Stakeholder meeting of the EMPIR project “Multifunctional ultrafast microprobes for on-the-machine measurements”, details about two measurement modes were presented. Force distance curves and contact resonance measurements are compared. The basic principles are explained and exemplary measurements concerning mechanical properties of polymers are shown.
The motivation and the measurement setup for large fast-scanning piezoresistive cantilevers are presented. The theory behind the measurements of mechanical properties through contact resonance is explained. Results of such measurements on two kinds of polymer are compared to results from force distance curves. Noise, time-dependency and dependency of the results on the vibration mode are identified as challenges of contact resonance.
The geometry of the melt pool in laser beam welding plays a major role to understand the dynamics of the melt and its solidification behavior. In this study, a butt configuration of 20 mm thick structural steel and transparent quartz glass was used to observe the weld pool geometry in the partial penetration mode by means of a high-speed camera. The observations show that the dimensions of the weld pool vary depending on the depth. The areas close to the weld pool surface take a teardrop-shape. A bulge-region and its temporal evolution were observed approximately in the weld pool root. Additionally, a 3D transient thermal-fluid numerical simulation was performed to obtain the weld pool shape and to understand the formation mechanism of the observed bulging effect. The model considers the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties. The numerical results showed good accordance and were furthermore used to improve the understanding of the experimentally observed bulging effect.
High heat input leads to grain coarsening and softening in WM and HAZ; the tensile strength is reduced. Low heat input leads to inadmissible hardening in the WM; the impact strength is reduced.
The proposed t8/5-time of 3 s to 15 s could be achieved through the reduced welding velocity.
The concept of electromagnetic weld pool support system allowed single-pass welds in flat position without gravity drop-outs even for reduced welding speeds; in this way the heat input can be controlled.
The adaptation of the electromagnetic weld pool support system to laser and laser hybrid welding process can dramatically increase the potential field of application of these technologies for real industrial implementation.
Schwerpunkte:
Strategie zur Vermeidung von Schweißimperfektionen im Überlappbereich beilaserhybridgeschweißten Rundnähten für 9.5 mm dicke Rohre.
Anpassung der Laserleistung in Kombination mit der Defokussierung des
Laserstrahls sowie einer Endkraterfüllung am Ende der Schweißnaht führte zu einer besseren Nahtausbildung.
Herausrampung der Energie des Schweißprozesses, sodass ein Übergang von Durchschweißung zu einer Einschweißung mit gewünschter kelchförmiger Nahtgeometrie stattfand.
Einstellung eines Wärmestaus durch Defokussierung und Verschiebung des
Laserstrahls führt zu einem gut ausgebildeten Überlappbereich ohne Poren, Risse.
Schweißungen an Rohrabschnitten mit einer max. Wandstärke von 15 mm, bei gegebenenfalls weiteren Parameteranpassungen.
Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis
(2019)
The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis.
First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface.
Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios.
Zusammenfassung
Die vorliegende Arbeit befasst sich mit zwei zentralen Aspekten der High-Resolution-Continuum-Source-Molekülabsorptionsspektrometrie mit Graphitrohrtechnik (HR-CS-GFMAS), einer Analysetechnik für elementare Spurenanalyse.
Der erste Teil der Arbeit umfasst eine mechanistische Studie zur Molekülbildung auf Graphitoberflächen. Dies ist ein wichtiger Schritt, um analytische Signale zu entdecken. Dazu wurde die Molekülbildung von CaF analysiert, welches für die indirekte, analytische Bestimmung von Fluor in HR-CS-GFMAS genutzt wird. Die CaF Bildung wurde mittels einer Beschichtung aus Zirconium katalysiert und deren Struktur analysiert. Die Kinetik dieser Reaktion wurde durch Beobachtung des jeweiligen Molekülspektrums bei verschiedenen Atomisierungstemperaturen beobachtet. Ein Arrheniusplot zeigte für Fluor (n = 1) eine Reaktion Pseudo-erster Ordnung. Ein Übergangszustand wurde über die mit Zirconium überzogene Grafitoberfläche isoliert und seine Struktur mittels spektroskopischer Methoden Energiedispersive Rasterelektronenmikroskopie / Röntgenspektroskopie (REM-EDX), Röntgenphoto¬elektronenspektroskopie (XPS), Röntgenabsorptionsspektroskopie (XAS) und Raman Spektroskopie untersucht. Auf Grundlage dieser Ergebnisse wird ein Mechanismus vorgeschlagen, bei dem ZrO2 als heterogener Katalysator fungiert; in Folge einer Pyrolysestufe wird ein Übergangszustand des ZrO(OCaF) aktiviert, welcher bei höheren Temperaturen CaF(g) an der Zirconium-Graphitoberfläche freisetzt.
Im zweiten Teil der Arbeit werden Analysemethoden entwickelt, in dem HR-CS-MAS als Detektor für Nichtmetalle und Isotopanalyse angewandt wird. Hierfür wurde organisch gebundenes Chlor im Wasser bestimmt, der Fluorgehalt in Pflegeprodukten mit perfluorierten Inhaltsstoffen quantifiziert und der Schwefelgehalt in Erdöl untersucht. Weiterhin ermöglicht die hohe Auflösung der Messgeräte eine präzise Bestimmung der Isotopenverschiebung einiger untersuchter Molekülspektren. Daher wurden die Molekülspektren angereicherter Bor- und Magnesiumisotope untersucht. Auf diese Weise wurde das Potential von HR-CS-MAS für die akkurate und präzise Bestimmung von Isotop-Mengenverhältnissen nachgewiesen.
Magnesium is a major element in the hydrosphere and biosphere, and it is direct correlated with the carbon cycle. Therefore, the study of its isotopic fractionation in sediments and sea water helps to understand the earth’s climate and global warming. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg, and traditionally isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS).
For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix extraction. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰. This accuracy and precision discriminate the isotope fractionation in geological samples, and it is suitable for earth’s climate studies.
Residual stresses are crucial when assessing the performance of welded components. The present work deals with the possibilities of transferring the real-life boundary conditions of welding, which influence the residual stress, into the laboratory. The possibilities of a test system with a load capacity of 2 MN specifically developed for online monitoring of stress formation and cracking are shown. Due to the structural design, global process, geometry and material-dependent stresses are induced, which can be quantified in-situ during welding and post weld heat treatment. Examples are presented how the conditions to be found during production are simulated in the laboratory. It is shown how welding residual stresses in high-strength steels are affected by the heat control. Elevated working temperatures significantly increase the tensile residual stresses in the heat affected zone (HAZ). The effect of mechanical stresses resulting from welding on stress relief cracking is demonstrated by the example of a creep resistant steel. Reheat cracks were monitored online during post weld heat treatment.
Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice.
All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis.
Microstructure ageing of stainless steel AISI 316L manufactured by selective laser melting (SLM)
(2019)
Additive manufacturing (AM) processes, such as SLM, offer a variety of advantages compared to conventional manufacturing. Today AM parts are still comparatively less cost-effective if they are manufactured in large quantities. To make the AM parts more cost-efficient, the AM process has to be improved. It requires a good understanding of microstructure formation, microstructure-property-relations and ageing processes affected by different loads.
In this work the ageing behavior of SLM manufactured AISI 316L stainless steel is evaluated. The microstructure effected by mechanical, thermal and corrosive loads are investigated and compared to as-built microstructure. Tensile tests are used for mechanical ageing. For thermal and corrosive loads the typical application conditions of 316L apply. The methods of microstructure investigation include SEM, TEM, CT and EBSD. The main object of this work is the description of microstructure and ageing processes of AM parts.
Simultaneous multielemental analysis of crude oils by high-resolutions absorption spectrometry
(2019)
When crude oil arrives at a refinery it needs a lot of processing before it is suitable for cracking into lighter fractions. Sulfur has to be extracted to meet ultra-low sulfur legislation for most of the fuel grades, and desalination is a crucial process as chlorine within salts is corrosive to refinery equipment. Measuring the amounts of sulfur and chlorine within crude oil is the first step in a complex clean-up process.
Heavy metals, such as vanadium, nickel and iron need to be removed too. These metals can poison the catalyst used to crack the oil into lighter fractions. This is costly as it reduces the useful life of the catalyst. Like chlorine, heavy metals also have a corrosive effect on the plant. There is some evidence that the presence of some metals in the final product can reduce performance.
A fast determination of elements and size of suspended particles is vital for diagnosis and safeguard of refinery equipment. However, sample preparation for current analytical methods consumes precious time and lost particle size information.
High-resolution continuum source graphite furnace absorption spectrometry (HR-CS-GFAS) is proposed as a fast analytical method for elemental determination in crude oils and potentially for simultaneous multielement and particle size analysis. This HR-CS-GFAS instrumentation is coupled to a modular simultaneous echelle spectrometer (MOSES) and provides a full optical window with high resolution (from 180 to 900 nm with bandwidth λ/170,000). By using this set-up, it is possible to generate a multiparameter 3D spectral image (atomic and molecular lines, isotopic shift, atomization delay, and intensities). The generated spectral images can be analyzed by multivariate regressions for the elemental and particle size analysis. Additionally, if several atomic and molecular lines are simultaneously measured, they may be used in multi-energy calibration (MEC), a method based on the use of many wavelengths of the same absorbing/emitting entity to improve the accuracy in analytical atomic spectrometry. This MEC approach combined with multivariate image analysis allows the quantification of selected elements (Si, Al, Ni, Fe, V, S, and Cl) and overcomes matrix effects.
We present our research on the development of a Brillouin optical frequency-domain analysis (BOFDA) using a perfluorinated graded-index polymer optical fiber (PFGI-POF) as a sensing fiber. The described works include investigations both on the selection of the setup components with respect to mode coupling effects and on the impact of the humidity cross-sensitivity. The suitability of the developed POF-based BOFDA is proved by a distributed measurement on an 86 m long PFGI-POF recorded with the spatial resolution of 6 m.
Society for Applied Spectroscopy (SAS) Atomic Section Student Award.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation.
Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS), and laser ablation molecular isotopic spectrometry (LAMIS).
For the determination of Mg isotope ratios in selected rock reference materials, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied and their results compared with MC-ICP-MS. By HR-CS-MAS, samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi, and X 2Σ → B 2Σ+. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A 2Πi → X 2Σ, as well as direct analysis by the MgO molecule for the electronic transition A 1Π+ → X 1Σ. The MgF and MgO spectra are described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Results were accurate with precisions ranging between 0.2 ‰ and 0.8 ‰ (2 SD, n= 10) for HR-CS-GFMAS. No statistically significant differences were observed for samples w/o matrix extraction. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of direct analysis, however the precision is lower due the lack of solid isotopic calibration standards.
Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice.
All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis.
The separation of two closely located defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used.
The measured thermal waves can be transformed to virtual (ultrasound) waves that can be processed by applying ultrasound reconstruction algorithms and finally the super resolution algorithm. Otherwise, it is also possible to make use of a Fourier transform with a subsequent super resolution routine.
These super resolution thermographic image reconstruction techniques in post-processing are discussed and evaluated regarding performance, accuracy and repeatability.
Magnesium (Mg) is a major element in a range of silicate and carbonate minerals, the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg with natural abundances of 79 %, 10 %, and 11 %, respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight variations of isotope amount ratios n(26Mg)/n(24Mg) in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods and isotope ratios are expressed as deviation from an internationally agreed upon material, i.e. the zero-point of the δ-value scale. Drawbacks of this method include the high costs for instruments and their operation, experienced operators and elaborate, time-consuming chromatographic sample preparation.
Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high- resolution continuum source graphite furnace molecular absorption spectrometry (HR- CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS).
For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X2Σ → A2Πi and X 2Σ → B2Σ+ around wavelengths 358 nm and 268 nm, respectively. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A2Πi → X2Σ as well as the MgO molecule for the electronic transition A1Π+ → X1Σ around 500 nm. The MgF and MgO spectra are described by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Isotope amount ratios in rock samples with and without matrix separation were analyzed. Calculated δ-values were accurate and obtained with precisions ranging between 0.2 ‰ and 0.5 ‰ (1 SD, n = 10). On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared to MC-ICP-MS.
Additive manufacturing (AM) offers diverse advantages compared to conventional manufacturing. In this work the microstructure of austenitic steel 316L, manufactured with Selective Laser Melting (SLM), was analyzed and compared to microstructure of 316L hot rolled material. Methods used for analysis are microprobe, optical microscopy and electron backscatter diffraction.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS).
For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰.
Boron and Magnesium present two and three stable isotopes respectevely. It is due to their relatively large mass difference (~ 10%) that isotope fractionation leads to considerable isotope amount ratio variations in the nature. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Traditionally, isotope ratio variations have been determined by mass spectroscopic methods.
Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) for boron and Magnesium monofluoride (MgF) for magnesium in a graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) were evaluated. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements
Magnesium is a naturally occurring element that can be found in several mineral forms in the earth crust. This element presents three stable isotopes 24Mg, 25Mg and 26Mg with a natural abundance of 79%, 10%, and 11% respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight isotope amount ratio variations n(26Mg)/n(24Mg) in biological and geological samples. Traditionally, isotope amount ratios have been measured by mass spectrometric methods. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time-consuming. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi and X 2Σ → B 2Σ+ around wavelengths 358 nm and 268 nm respectively. In the case of LAMIS, it was studied the MgF molecule for the electronic transitions A 2Πi → X 2Σ as well as the MgO molecule for the electronic transition A 1Π+ → X 1Σ around 500 nm. The MgF and MgO spectra are composed by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by a partial least square regression (PLS) calibrated with enriched isotope spikes. The isotope amount ratios in rock samples with and without matrix separation were analyzed. Resulting delta values were obtained with precisions ranging between 0.2-0.5 ‰. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared with MC-ICP-MS.
Crystalline molecular materials with mechanical flexibility are promising for technological development. This is particularly true for the development of advanced materials with optoelectronic and biomedical applications. While a growing number of mechanically flexible crystalline molecular materials are being reported,1 they remain scarce. At present, most discoveries are serendipitous, as limited design strategies are currently known. Amongst these strategies Desiraju et. al. suggested that elastic materials must contain herringbone structures.2 For plastic crystals, the so-called ‘shape-synthon’ strategy has been developed, in which weak non-covalent interactions are introduced into structures to facilitate mobility of molecules.3 This includes formation of slip planes. Generally, these models have performed very well at predicting and rationalizing the mechanical properties of new materials. Recently, however, a family of one-dimensional covalent networks (coordination polymers; CPs) has been described, which show mechanical elasticity. With drastically different structural chemistry, these systems do not seem to adhere to the currently established rules. Herein, we present the first such system: a plastically bendable crystal of a 1D CP, [Zn(-Cl)2(3,5-Cl2Py)2]n (where 3,5-Cl2Py = 3,5-dichloro pyridine). This CP crystallizes in a tetragonal, and can therefore be bent over two major faces to acute angles without fracturing. We conducted bending and indentation experiments to quantify the mechanical properties of the CP crystal. This was complimented by Vibrational (Raman and Terahertz) spectroscopy and theoretical calculations for deeper understanding of molecular level structural deformation.