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Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion beim Schweißen höherfester Feinkornbaustähle mit modifiziertem Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion
beim Schweißen höherfester Feinkornbaustähle mit modifiziertem
Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
The NWRimage system is the first elemental imaging-specific laser ablation instrument, offering breakthrough sub-micron spatial resolution and ultra-fast signal response for high throughput rates.
Laser ablation (LA) systems are used in conjunction with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) systems to detect and analyze tiny amounts of material. As ICP-MS systems have become more sensitive, a need has emerged for LA imaging tools with < 1 micron spatial resolution - a capability not previously available on the market. The NWRimage is provided with a carefully designed aerosol path from point of ablation to injection into the ICP itself. This aerosol path combined with a novel Dual Concentric Injector (DCI) ICP torch, yields < 50ms signal response to accelerate the speed of analysis and enabling enhanced sample throughput. The LA system is used for bio imaging of single cells and medical tissue samples.
Rubber is widely used as sealing material in various applications. In many fields the function of seal materials at low temperatures is necessary. Therefore, the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance.
It is known that the material properties of rubbers are strongly temperature dependent. At low temperatures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cooling, due to the glass transition the material changes from rubber-like entropy-elastic behaviour to stiff energy-elastic behaviour, that allows nearly no strain or retraction. Hence, rubbers are normally used above their glass transition. But as the minimum working temperature limit of elastomers cannot be defined globally and precisely, the lower operation temperature limit of rubber seals should be determined in dependence of the application conditions and the most relevant material properties.
In this paper, wesummarize results of our temperature dependent investigation of seal material properties by classical thermal analysis as Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA), combined with measurements of standardized tests as compression set and the seal performance determined in component tests. To reduce the test time of compression set tests a faster technique was developed and applied.
To study the influence of dynamic events on the seal performance and to enhance the understanding of occurring seal failure, a setup for a fast partial seal release was designed.
The sensitivity of low loss perfluorinated polymer optical fiber (PF-POF) to gamma radiation is investigated for on line radiation monitoring purposes. The radiation induced attenuation (RIA) of a commercial PF-POF based on Cytop material is measured in the visible spectral region. The fiber RIA shows strong wavelength dependence with rapid increase towards the blue side of the spectrum. The wide range of radiation sensitivities is available via careful selection of appropriate monitoring wavelength. The accessible sensitivities span from 1.99 ± 0.01 dBm⁻¹/kGy measured at 890 nm to 140.9 ± 0.6 dBm⁻¹/kGy measured at 460 nm. The fairly high radiation sensitivity as well as its wide tunability makes the fiber a promising candidate for a broad range of applications.
Überblick über die Normung zur Konformitätsbewertung- (ISO CASCO Toolbox)
Revision der ISO/IEC 17025 – Anforderungen an Labors
Revision der ISO/IEC 17011 - Anforderungen an Akkreditierungsstellen
Revision des ISO Guide 34 (neu: ISO 17034) -Anforderungen an die Kompetenz von Herstellern von Referenzmaterialien
Die Entwicklung von Wasserstoffbarrieren aus Glas erfordert die genaue Messung geringster H2-Permeabililtäten. Bisherige Untersuchungen haben gezeigt, dass die VHE-Pulvermethode diesbezüglich eine besonders hohe Empfindlichkeit bietet. Hierbei wird die isotherme Gasabgabe aus sphärischen Partikeln im Rahmen klassischer Diffusionsmodelle gefittet und daraus der Diffusionskoeffizient bestimmt. Für die Untersuchung von Gläsern mit möglichst geringer H2-Permeabilität ist jedoch eine Validierung der Genauigkeit der Methode notwendig. Vor diesem Hintergrund erfolgte die numerische Modellierung der H2-Abgabe mit Hilfe des Programms COMSOL Multiphysics®. Im Poster wird der Einfluss der Korngrößenverteilung der Glaspulverpartikel, der Partikelform sowie der Effekt einer nichthomogenen H2-Startverteilung auf die mittels Pulvermethode ermittelten Diffusionskoeffizienten diskutiert.
Single wire Gas Metal Arc Welding (SGMAW) and high power Tandem GMAW (TGMAW) are evaluated with respect to energy efficiency. The key performance indicator Electrical Deposition Efficiency is applied to reflect the energy efficiency of GMAW in different material transfer modes. Additionally, the wall-plug efficiency of the equipment is determined in order to identify the overall energy consumption. The results show that energy efficiency as well as economic process performance can be significantly increased by application of tandem processes. A comparative Life Cycle Assessment of a 30 mm thick weld is conducted to investigate the influences of the energy efficiency on the environmental impacts. Environmental burdens in the categories Global Warming Potential, Acidification Potential, Eutrophication Potential and Photochemical Ozone Creation Potential can be reduced up to 11% using an energy efficient TGMAW process
Abstract: The dangerous goods regulations UN/ADR 6.1.5.5.4 a) prescribe a maximum filling degree for determining the test pressure for the hydraulic pressure test by real measurements. The assumption is that the maximum filling degree of the liquid phase is the worst case concerning the gauge pressure. Therefore the main objective of this study is to investigate the effect of the filling degree on the gauge pressure.
Gauge pressure measurements and calculations for different substances were carried out at different filling degrees for a steel drum and a steel jerrican (heating-up from 15 °C to 55 °C).
The assumption that the maximum filling degree is the most critical is only valid for relatively rigid packagings: If the relative expansion of the packaging is smaller than the volume increase of the liquid phase due to heating-up, the gauge pressure increases with increasing filling degree.
But the opposite is true for relatively flexible packagings: If the relative expansion of the packaging exceeds the relative volume expansion of the liquid, the gauge pressure increases for decreasing filling degrees. The current regulations for the hydraulic test pressure determination at a maximum filing degree do not lead to the intended safety level. For a lower level than the maximum filling degree, the prescribed safety factor of 1.5 is not respected. Under transport conditions it is possible that the inner gauge pressure exceeds the test pressure. This can result in a failure of the packaging. There is a need to reconsider the regulations.
Experimentelle Untersuchungen zu streifenden Schlägen mit verschiedenen Edelstahlsorten in explosionsfähigen Atmosphären, jeweils bestehend aus Wasserstoff, Acetylen, Ethylen bzw. Propan mit Luft, haben gezeigt, dass deren Zündwahrscheinlichkeit sowohl von der Art des Brenngas-Gemisches als auch der Höhe der kinetischen Schlagenergie abhängt. Ein Einfluss des Chromgehaltes im Edelstahl auf die Zündwahrscheinlichkeit durch mechanisch erzeugte Schlagvorgänge konnte in dem untersuchten Bereich des Chromgehaltes nicht nachgewiesen werden, obwohl ein steigender Chromgehalt die Oxidationsfähigkeit abgetrennter Partikel erhöhter Temperatur tatsächlich senkt. Ferner haben weitere Werkstoffeigenschaften wie die Wärmeleitfähigkeit, spezifische Wärmekapazität, Dichte und Härte einen Einfluss auf die Zündwahrscheinlichkeit mechanischer Edelstahl-Schlagvorgänge bei Wasserstoff/Luft-Gemischen. Mit steigender Wärmeleitfähigkeit des Edelstahls sinkt die Zündwahrscheinlichkeit. Für die spezifische Wärmekapazität, Dichte und Härte konnte kein Einfluss nachgewiesen werden.
Für Schlagvorgänge wurden in der Norm EN 13463-1:2009 (DIN, 2009) Grenzwerte für die maximale kinetische Schlagenergie festgelegt, unterhalb derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann. Dabei wurde zwischen Schlagvorgängen mit funkenarmen Metallen, wie z. B. Kupfer, Messing, und Schlagvorgängen mit sogenannten „sonstigen Werkstoffen“ unterschieden. Die Grenzwerte dieser sonstigen Werkstoffe resultieren aus Versuchen der BAM mit unlegiertem Baustahl. Bei solchen Schlagvorgängen wird von Oxidationsprozessen einzelner Partikel mit dem Luftsauerstoff ausgegangen, die das Gasgemisch aufgrund des hohen Temperaturanstiegs entzünden.
In industriellen Anwendungen wie zum Beispiel der chemischen Industrie wird jedoch statt ferritischem Stahl überwiegend Edelstahl verwendet. Im Allgemeinen gilt mit Chrom hochlegierter Edelstahl bei Schlagvorgängen gegenüber ferritischem Stahl als funkenärmer, da die Oxidationsfähigkeit von Edelstahlpartikeln mit steigendem Chromgehalt abnimmt.
Bei den Schlagversuchen der BAM konnte zwar eine sinkende Oxidationsfähigkeit der Partikel, aber keine abnehmende Zündwirksamkeit von Edelstählen mit steigendem Chromgehalt beobachtet werden.
In diesem Beitrag soll in Kürze darüber informiert werden, welche Themen und Fragestellun-gen den Fachbeirat der BAM, seine Arbeitsgruppen und die BAM beschäftigt haben. Bereits in den letzten Jahren wurde an dieser Stelle über die Anforderungen an Kunststoff Drän-elemente berichtet. Vor dem Hintergrund unserer Beiträge zu diesem Thema, kam eine in-tensive Fachdiskussion im Fachbeirat der BAM und in weiteren Fachgremien in Gang. So wurden die Bemessungsgrundsätze der DGGT (Deutsche Gesellschaft für Geotechnik), die GDA (Geotechnik der Deponien und Altlasten) E (Empfehlung) 2-20 (Entwässerungsschich-ten in Oberflächenabdichtungssystemen), in einigen Punkten angepasst. Eine Musterverle-geanleitung für Kunststoff Dränelemente wurde erarbeitet. Der aktuelle Bearbeitungsstand soll hier vorgestellt werden. In diesem Zusammenhang wurde ein Untersuchungsprogramm zum Einfluss von Überlappstößen auf das Wasserableitvermögen von Kunst-stoff Dränelementen angestoßen. Die Ergebnisse sollen hier in Kürze vorgestellt und die Bedeutung für die Abminderungsfaktoren und damit für die Bemessung erläutert werden. Zu welchem Zeitpunkt muss ein Kunststoff Dränelement überbaut werden und welche weiteren Regelungen müssen hier beachtet werden? Was steckt eigentlich hinter diesen strengen Regelungen? Diese Fragen sollen im Folgenden diskutiert werden.
Die Deponieverordnung (DepV) fordert eine Akkreditierung der fremdprüfenden Stellen nach verschiedenen Normen. Die fachlichen Anforderungen an den „Fremdprüfer-Kunststoff“ legt die Richtlinie Fremdprüfer der BAM fest. Um diese Anforderungen im Akkreditierungsprozess ausreichend berücksichtigen zu können, wurde nun eine sogenannte DAkkS Regel erarbeitet, die die Anforderungen der Richtlinie spiegelt. Über den aktuellen Bearbeitungsstand soll berichtet werden.
Auch über die aktuelle Arbeit in Zusammenhang mit den Kunststoffdichtungsbahnen (KDB) soll berichtet werden. Der Prüfhinweis B14 (Bestimmung der Maßhaltigkeit von geosyntheti-schen Dichtungsbahnen aus Polyethylen hoher Dichte (PEHD)) wurde überarbeitet. Voran-gegangen war eine intensive Entwicklung der Prüfeinrichtung sowie ausgiebige Ringversuche im AK GWS (Arbeitskreis Grundwasserschutz). In diesem Zusammenhang wurden neue Anforderungen an die Produkte gestellt. Die Hintergründe dazu sollen kurz vorgestellt werden. Die DVS (Deutscher Verband für Schweißen und verwandte Verfahren) Richtlinie 2225-4 regelt das Schweißen der KDB auf der Deponiebaustelle. Werden KDB im strukturierten Bereich miteinander verschweißt, werden die Strukturen in der Regel vorher abgetragen. Die DVS Richtlinie 2225-4 sieht unter bestimmten Voraussetzungen von einem Abtragen der Strukturen ab. Vor diesem Hintergrund wurde ein Untersuchungsprogramm initiiert, das die Auswirkungen aufzeigen soll. Der Bearbeitungsstand wird vorgestellt.
In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining in importance. Latest improvements regarding spatial resolution (down to 1 µm) and washout time make LA-ICP-MS particularly interesting for single cell analysis.
Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest.
LA-ICP-MS was used to study the NP pathway from uptake, via intracellular processing up to cell division. Fibroblast cells were incubated with different metallic NPs under varying experimental conditions. For LA analysis the cells were fixed with formaldehyde and dried.
Our results show that LA-ICP-MS is able to localise NP aggregates within cellular substructures. The NPs accumulate in the perinuclear region in the course of intracellular processing, e.g. multivesicular fusion and endosomal maturation, but do not enter the nucleus [1, 2]. A strong dependence of NP uptake on concentration and incubation time was found. Additionally, the number of NPs internalized by individual cells was determined and variations within the cell population became visible.
A new laser ablation system providing a short washout time (50 ms) together with small spot sizes (< 4 µm) and high repetition rates allows high spatial resolution applications. First results of cell imaging will be shown.
The findings demonstrate the potential of LA-ICP-MS enabling insight into NP uptake and intracellular distribution dependent on experimental parameters.
Advanced methods for 3D green density characterization like computed tomography and 3D FE sinter modeling can be utilized for increasing the reliability of sintered components. The experimental in situ observation of sin-tering, however, is currently restricted to silhouette methods, i.e. heating microscopy. For complex shaped sam-ples, in situ shape screening during shrinkage would allow better validation of 3D sinter simulation models. Further, by revealing temporary sinter warpage, 3D high-temperature shape screening would allow to locate potential defects of complex sintered components. Against this background, BAM developed a testing device for in situ 3D high-temperature shape screening for ceramic and glass-ceramic tapes up to 1000°C [1-3]. Current work is focused on dropping this restriction in sample shape and temperature. The poster illustrates the current state of this work and possible applications of the method e.g. in detecting sinter warpage of metallized glass-ceramic LTCC tapes.
The laser-induced breakdown spectroscopy (LIBS) is a fast method to provide multi-elemental analysis of any sample. At the Federal Institute for Materials Research and Testing (BAM) the LIBS technique is applied on building materials to measure ingress profiles of harmful species like chloride and alkalis. The ingress depth and the quantitative amount is important for the evaluation of the potential for damage processes like the alkali-silica reaction or chloride-induced corrosion. Concrete as an example is a highly heterogeneous material with 1/7 cement (major component CaO) and 6/7 aggregates (SiO2) with different grain sizes. Due to a scanning procedure a two dimensional element distribution of a concrete surface can be measured. In order to have an automated Separation method to evaluate heterogeneous materials, different cluster algorithm have been tested. Best results have been achieved with the Expectation-Maximization-Algorithm (EM-Algorithm).
Phosphor ist ein für alle Lebewesen essentielles Element und in seinen Funktionen nicht zu ersetzen. Der Bedarf wird aus der Nahrung gedeckt, daher wird Phosphor letztendlich durch Ackerbau den Böden entzogen. Der Nährstoff muss ersetzt werden, um dauerhafte Landwirtschaft zu ermöglichen. Das geschieht zum einen durch den Einsatz von Wirtschaftsdüngern, aber zu einem großen Teil auch durch Mineraldünger. Das hierfür benötigte Rohphosphat wird bergmännisch aus fossilen Lagerstätten gewonnen. Die entsprechende Reichweite wird auf über 300 Jahre geschätzt. Daher besteht zwar keine unmittelbare Gefahr, dass dieser lebenswichtige Nährstoff zu Neige geht, es bestehen jedoch erhebliche Versorgungsrisiken. Zum einen ist Europa nahezu vollständig von Importen abhängig und damit auch Schwankungen der Weltmarktpreise ausgesetzt. Darüber hinaus liegen Förderung und Reserven von Rohphosphaten entweder in Ländern mit hohem Eigenbedarf (USA, China) oder in politisch instabilen Regionen (Marokko, West Sahara). Außerdem sind viele Rohphosphate mit Schwermetallen wie Uran, Thorium und Cadmium belastet. Das Umweltbundesamt schätzt, dass jährlich mehr als 160 t Uran durch Mineraldünger auf deutsche Ackerflächen ausgebracht werden. Rückgewinnung von Phosphor könnte helfen, diese Probleme zu reduzieren. Ein bedeutendes Potential dafür stellt der Abwasserstrom dar. Die Menge an Phosphor darin wird deutschlandweit auf etwa 70.000 t jährlich geschätzt. Das entspricht etwa der Hälfte der Menge an Phosphor, die derzeit für Mineraldünger benötigt wird. Der Vortrag würde sich mit möglichen Prozessen der Rückgewinnung, deren Wirtschaftlichkeit und Herausforderungen der Analytik befassen:
- in den letzten Jahren wurden zahlreiche Verfahren zur Rückgewinnung von Phosphor aus verschiedensten Phasen der Abwasserreinigung entwickelt (wässrige Phase, Klärschlamm, Klärschlammasche). Ausgewählte Verfahren würden vorgestellt und bewertet.
- für einen Einsatz der so gewonnenen Recyclingphosphate als Düngemittel muss die Schadstofffreiheit und Pflanzenverfügbarkeit der Nährstoffe sichergestellt werden. Dazu ist zu prüfen, ob die zurzeit gängigen Verfahren der Probenvorbereitung und Analytik auch auf Recyclingphosphate anwendbar sind. Das gilt neben der Bioverfügbarkeit von Phosphor besonders für Schadstoffe, da die Recyclingdünger aus Abfallmaterialien gewonnen werden, die stark belastet sein können. Das gilt besonders für die speziesspezifische Analytik von Chrom (Chrom (VI) vs. Chrom (III)) in verschiedenen Matrices.
Polybromierte Flammschutzmittel (PBFSM) werden seit den 1960er Jahren zur Herabsetzung der Entflammbarkeit von Polymeren verwendet. Diese stehen auf Grund ihrer potentiell persistenten, bioakkumulierenden sowie toxischen Eigenschaften bis heute im Fokus der Wissenschaft und Gesetzgebung. In den letzten Jahren kam es verstärkt zum Einsatz neuer („emerging“) sowie neuartiger („novel“) PBFSM. Diese Verbindungen wurden bereits in der Umwelt bzw. oberhalb von 0,1 Gew.-% in Bedarfsgegenständen nachgewiesen. Zwei Vertreter, über deren Vorkommen, physikochemischen Eigenschaften und Umwelt-verhalten nur wenig bekannt ist, wurden daher ausgewählt, um das Abbau- und Transformationsverhalten näher zu untersuchen. Um eine Einschätzung über das Umweltverhalten bzw. die Metabolisierung dieser Verbindungen vornehmen zu können, werden sowohl Untersuchungen der cyto-chromabhängigen Biotransformation (Phase I/II) anhand mikrosomaler Ansätze als auch die Simulation oxidativer/reduktiver Abbauprozesse durch die Kopplung aus elektrochemischer Zelle (EC) und massenspektrometrischer Detektion (MS) herangezogen. Ziel der präsentierten Arbeit ist es, ein erstes Verständnis des Umweltverhaltens dieser neuartigen Kontaminanten zu entwickeln, um so eine Bewertung über die toxikologische Relevanz dieser Verbindungen bzw. deren Umwelt-/Bio-Transformationsprodukte geben zu können.
Excelling in brevity but lacking in applicability, the 2011 EU nanomaterial definition has become a source of anguish for scientists and industry alike. Repeated pleas and discussions with our own envoy have demonstrated the strength of their resolve: this definition is unlikely to change. Manufacturers of many materials (cosmetics, pigments, foodstuffs, etc.) will have to characterise and label all their products accordingly, a task still impossible for lack of a clear metrological approach towards this goal. Therefore, the onus has fallen on the scientists to come up with a practicable measurement technique allowing inexpensive classification covering large swathes of the material landscape. Small-angle X-ray Scattering (SAXS) probes the size range in question, and can - with due care - deliver a bulk-averaged volume-weighted size distribution. Like any other real-world measurement method, however, it is not (and can never be) a universal solution. This presentation will clarify the SAXS technique, provide several application examples for nanomaterial characterisation, and will detail the limitations and pitfalls that accompany its abilities. At the end of this presentation, you will have the information to judge whether the technique is amenable to your materials or not.
Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST) in a relevant temperature range, i.e. phase separate from solution upon cooling, have been reported so far. Moreover, the most studied UCST type polymers namely polybetaines are difficult to use under physiological conditions, which significantly restricts their potential applications. Therefore, UCST polymers with sharp and robust phase transition in physiological conditions (in the presence of salts, ions etc.) are highly needed in order to extend the range of applications of this class of polymers. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied. At temperature below the UCST, the copolymer chains were aggregated together. The aggregate size was found to be larger with increasing AN contents and became smaller upon dilution of the copolymer solutions. While above the UCST, the copolymer chains were expanded and weekly associated in solution. The association between the copolymer chains formed smaller aggregates with increasing the AN contents or the dilution of the solutions. A model is proposed to explain such aggregation-association behavior of the Fig. 1.
Figure 1. Schematic illustration of the proposed thermos-induced aggregation behavior of the poly(AAm-co-AN) in aqueous solution.
An approach to achieve “zero leakage” is discussed with respect to the experience in Germany, where strict regulations for landfill lining and capping systems have been developed and issued because of large environmental problems related to landfills that accumulated in the 1970’s and 1980’s. Using a thick, high quality HDPE geomembrane (GMB), which is installed free of residual waves and wrinkles in intimate contact with a compacted clay liner (CCL) or geosynthetic clay liner (GCL) of very low permeability, by a qualified, experienced, well equipped and properly third-party controlled installer and which are protected by heavy protection layers designed with respect to long-term performance of the GMB, may result in a liner or capping system of practically no leakage. This is demonstrated by analyzing results of measurements obtained from permanently installed leak detection systems in combination with HDPE GMBs. The survey is based on 32 German landfills with 1,276,500 m² of installed HDPE GMB.
The process window and range of functional properties of NbC is wide, because micro-hardness, hot hardness, sliding wear resistance, elastic modulus and toughness can be tailored by the C/Nb ratio, because Nb4C3, Nb6C5 and other short and long range ordered phases occur in the region of homogeneity of NbCx (0,75≤ x ≤1.0) in the binary Phase diagram, and by the type of binder. Further improvements enable the addition of secondary carbides. Supporting results from literature and different grades with varying C/Nb ratio or binder types were illuminated. Thus, the NbC system offers to producers a wider process window, than WC. The impact of these tailored properties on sliding wear and cutting performance was illuminated by tribological and machining results. NbC can be synthesized by carbothermal conversion of Nb2O5 or be metallurgically grown in melts and leached out as coarse NbC cubes. NbC provides comparably lower friction in many relevant tribo-contacts and displays low wear. NbC and Nb2O5 have so far no REACH classification related to human toxicology and are not listed as substances of very high concern contrary to WO3 and Co3O4.
In the course of miniaturizing modern technology down to the molecular scale, much remain unknown about the materials behavior and the deviations from the bulk that might arises from confinement effects. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of Poly (vinyl methyl ether) (PVME) and of blends PVME / Polystyrene (PS) 50:50 wt-%,, which are miscible in bulk (thicknesses: ca. 8 nm – 160 nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed, where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. For PVME films, two thickness independent processes were observed and interpreted to be the α-processes of a bulk-like layer and a process due to an absorbed layer to the substrate. This adsorbed layer further undergoes a confinement effect that results in the localization of the segmental dynamics, which results in an Arrhenius-like temperature dependence. A detailed analysis of the dielectric strengths of both processes reveals that the thickness of the adsorbed layer decreases with increasing temperature, while that of the bulk-like layer increases. For the blend system, by measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process. The dynamic Tg obtained from the SHS measurements decreased with decreasing film thickness. On the other hand, BDS measurements showed a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in detail in a comprehensive discussion.
Successful implementation of an optical polarimetry measurement setup. Due to wall anchoring interactions HAT6 embedded in an untreated alumina membrane exhibits a radial orientation for pore sizes in between 30 nm and 80 nm. Embedded in large membranes, pore size of 180 nm, HAT6 forms the favored hexagonal columnar phase along the pore axis.
This lecture is an introduction to ICP-MS with a double focusing magnetic sector mass analyzer. It offers fundamental background, a thorough discussion of analytical features, and state of the art information on applications. Different types of double focusing instruments also are considered. Specific topics include fundamental aspects of ICP-MS (physical properties of a double focusing instrument, operational characteristics in comparison with quadrupole instruments); analytical characteristics (spectral and non-spectral interferences, figures of merit in low and high resolution modes, blanks and memory effects, HPLC and GC interfaces), and applications (industrial including ultra-pure reagents and alloys, environmental, geological, and biomedical materials).
By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis approach (evaporation induced self assembly).
Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases.
While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies.
Carbon-based conductive coatings are complex composites, consisting of an organic or inorganic binder and conductive carbon components, for application as anodes in impressed current cathodic protection systems of reinforced concrete structures. The electrochemical properties of three coatings at different humidity and in saturated calcium hydroxide solution were studied by electrochemical methods, such as electrochemical impedance measurement, measuring of open circuit potential over time and galvanostatic polarization.
Advanced oxidation processes have become an important part of research due to their capacity to degrade many environmental pollutants during water treatment. Especially the heterogeneous photocatalysis is a promising method because it often results in a full mineralization of many hazardous compounds. Incomplete degradation reactions can result in transformation products due to oxidative conditions. The transformation products may have a higher toxicity than the precursor substances and are often only partly removed during water treatment. Since a lot of these compounds are still unknown, transformation products are not detected by target analysis used in sewage treatment plants and are often released into the aquatic ecosystems. Therefore, extensive and effective non-target analytical methods are necessary for the monitoring and identification of the transformation products which can be generated during waste water treatment.
Titanium dioxide (TiO2) is the most frequently used photocatalyst because of its inexpensiveness, non-toxicity, chemical stability and its high photocatalytic activity. If TiO2 is irradiated electron-hole pairs are generated on the surface of the TiO2, resulting in the formation of active oxidized species such as hydroxyl radicals which can react with environmental pollutants.
A model system has been developed to simulate photocatalytic reactions in a laboratory scale. The commonly used pharmaceuticals metformin and gabapentin were selected as model substances because of their high input in waste water and the little information about their fate during water treatment. Metformin is the drug of choice for treating type 2 diabetes. More than half of the total amount of pharmaceuticals in the environment are the antidiabetic agent metformin and its major transformation product guanylurea. Gabapentin is used as antiepileptic drug and for the treatment of neuropathic pain. It is found in waste water influent in the high ng/L range.
First results of the optimization of the photocatalyst and its application are shown.
Silicon surface passivation with atomic layer deposited (ALD) thin films has gained more and more interest in the PV community in recent years. With ALD good film quality, accurate thickness control and conformity are reached. Furthermore, ALD is capable of coating difficult substrates such as nanostructured surfaces with the same accuracy as flat surfaces. A variety of materials such as Al2O3, TiO2 and HfO2 demonstrate good surface passivation quality both for front and rear surface of silicon solar cells. In addition of providing good surface passivation, thin films with high refractive index e.g. HfO2, TiO2 and AlN can act simultaneously as antireflection coatings when applied on the front surface of the device. Hence, ALD thin films can reduce both electrical and reflective losses in solar cells.
Thorough investigation of the optical properties of these layers is crucial for several reasons related to their production and use. Optical measurements provide a fast, easy, non-destructive, and in situ capable approach to quality assurance for photovoltaic devices. As the function of the final device is optical, optimisation of the device performance relies strongly on the knowledge of the wide-range dielectric function of the thin layers. In this contribution, we determined the optical constants of ALD generated layers of AlN, Al2O3, TiO2, and HfO2 in a wide spectral range covering the near ultraviolet and the mid-infrared regions by means of spectroscopic ellipsometry. By combining data from a UV-Vis-NIR ellipsometer (Woollam M2000DI) and an FTIR ellipsometer (Sentech Sendira), we can determine the optical constants alongside with the layer thicknesses from one large set of spectroscopic measurements. We consider this a contribution to the metrological treatment of stratified and structured thin films in the optical range by polarisation-sensitive measurement methods.
In recent years, upconversion nanocrystals (UCNC) have shown great promise for biological and medical applications, mainly because of their excitation in the NIR region, which provides minimum fluorescence background and a rather deep penetration into biological samples, as opposed to excitation in the visible or UV region. Moreover, they show a multitude of characteristic narrow emission bands as basis for ratiometric measurements. Commonly, Yb is the sensitizer of choice, because of a comparatively high absorption cross section, simple energy scheme, and rather efficient energy transfer to the activator, mostly Er, Tm or Ho. A main disadvantage of the use of Yb as sensitizer for biological and medical applications is its absorption band at 976 nm and hence the use of an excitation wavelength at which water has a non-negligible absorption. This can lead to significant sample heating, especially at long illumination times or high excitation power densities, and thus, tissue damage or even cell death. A possible solution is the tri-doping of UCNC with Nd as sensitizer, which can be excited efficiently at around 800 nm, where water absorption is at minimum.
The use of Nd as a sensitizer and Yb as a bridge between Nd and the activator Er in NaYF₄ nanocrystals is a relatively new way to overcome the problems of heating of samples in an aqueous environment. Disadvantages can arise from the tri-doping, which can favor non-radiative relaxation due to the more complicated excitation process compared to e.g., simple Yb,Er-doped UCNC, which might lower the upconversion quantum yields in these tri-doped systems. In order to quantify clear advantages, NaYF₄:Yb,Er,Nd nanoparticles were synthesized and spectroscopically studied using an 8 W 804 nm laser diode and a custom-designed Edinburgh instruments FSP980 spectrometer. Wavelength-dependent studies of the emission intensities and the decay kinetics of these tri-doped UCNC at different excitation power densities and excitation pulse widths revealed the clear advantages of preventing water absorption on measurable luminescence signals.
We were able to show the influence of pulse width and excitation power density on the luminescence intensities and decay kinetics lifetimes at different emission wavelengths. Additionally, we can clearly discern power density-dependent and independent peaks in the emission spectra. In summary, we demonstrate that the tri-doping of NaYF₄:Yb,Er,Nd nanoparticles is a very promising approach to render UCNC more efficient and to make them better suitable for biological and medical applications requiring measurements in aqueous environment.
The presentation gave an overview of the topic, the aims and the task allocation of the M-ERA.NET founded project named “Nanohype”.
In this project four research teams working hand in hand on computational modeling, synthesis and experimental validation to design novel metal-shelled Upconversion-NP combining plasmonic interactions.
As Ph.D. student at the BAM I am responsible for the optical characterization (measurements of lifetimes, Quantum Yields and PL emissions ) of these promising novel systems.
Hazardous substances with a boiling point close to ambient temperatures will evaporate at higher vapour pressures, so that the evaporation takes places in the smooth transition between the evaporation at boiling point and below boiling point, representing the transition between two different physical phenomena. Whilst the evaporation at boiling point is driven by the available heat flux, the evaporation below boiling point is driven by the concentration gradient between the pool surface and the ambient air. Available evaporation models usually focused on the correct description of the mass transfer coefficient for temperatures below boiling point. A formulation of the correct equation for the mass flow is rarely documented. Whilst the mass transfer coefficient formulation is more or less equivalent in most models, the main difference occurs in the formulation of the mass flow equation. In Fact two types of models can be identified: the models with a linear pressure term and the models with a logarithmic pressure term. Whilst the logarithmic formulations result in an infinite mass flow near boiling point, which is not plausible, the linear formulations reach (different) finite values. Due to a lack of published experimental data it was not possible to determine whether the linear approach is conservative, under predicting or more or less accurate close to the boiling point.
To evaluate the accuracy of each type of formulation, test series on liquid pools have been carried out at BAM for substances like Water, Ethanol, Cyclohexane, and Acetone. The tests were done under ambient conditions with a heatable, 90 cm diameter pool, so that the vapour pressures investigated ranged from 0 to close to 1 bar. The experimental data showed that neither of the linear nor the logarithmic formulation of the evaporation models is able to predict correctly the mass flow close to the boiling point. The logarithmic approach heavily over predicts the mass flow, while the linear approach is not conservative anymore when the vapour pressure exceeds 0.7 bar.
In the beginning of the 1980s earth building has undergone a renaissance, which nowadays leads to an increasing use of load-bearing earth constructions and in particular, earth block masonry. At present there are no common structural standards according to the semi-probabilistic calculation concept, which is the state-of-the-art in European standards. A solid database is needed for the determination of the materials partial safety factor. Therefore, compressive strength tests were carried out with two types of earth blocks and two types of prefabricated earth mortar. The evaluation showed that the variation of the compressive strength was remarkably less than expected, which seems to indicate high quality standards of the components earth block and mortar with regard to industrial production. On the basis of these results and together with the reliability method, a partial safety factor for earth block masonry subjected to compression was determined. The main aim of the research was the development of a first valid database for material parameters of earth block masonry with particular regard to statistical characteristics. The results showed that a common calculation method for earth block masonry based on partial safety factors following the valid masonry construction standard is feasible.
RRT O.2/O.3 – Results of BAM
(2016)
During the last couple of years BAM took part in different Round Robin Tests for the determination of oxidative properties of liquid and solid substances. The obtained results from these tests are reviewed and discussed in this presentation. New findings from recent particle size distribution measurements were discussed as well.
Analytical methods require efficient and versatile strategies to measure an increasing number of analytes that can be used in conjunction with established platforms like flow cytometry. Spectral multiplexing suffers from problems such as spectral crosstalk and often requires different excitation light sources increasing instrumentation costs. Thus, the number of distinguishable reporters with intensity-based barcodes is limited. An alternative can be lifetime encoding for discrimination of fluorophores based on their fluorescence decay kinetics.
We report on the suitability of µm-sized polymer particles stained with organic dyes for lifetime encoding. These dyes are excitable at a standard laser diode wavelength and detectable within a single spectral window. For lifetime-based discrimination, these dyes display sufficiently different luminescence decay kinetics. We present the spectroscopic properties of these beads and address challenges like the limited number of detectable photons in a flow for the reliable discrimination. These studies are expected to pave the road to new applications of fluorescence lifetime multiplexing for time-domain flow cytometry.
The steadily increasing number of analytes, especially in bioanalytics and environmental contexts, requires the development of efficient and versatile methods for the simultaneous determination of different parameters within a single run. Additionally, these methods should be applicable in conjunction with established platform technologies like flow cytometry.
Fluorescence techniques have proven to fulfill these requirements. Commonly performed spectral multiplexing utilizing a color code suffers from several problems, such as the sensitivity of fluorescence intensity measurements to fluctuations in excitation light intensity and dye concentration and hence, photobleaching and spectral crosstalk limiting the achievable number of detection channels. Moreover, it typically requires different costly excitation light sources.
Die Zahl der zugelassenen Fahrzeuge auf deutschen Straßen, welche statt herkömmlichen Otto- und Dieselkraftstoffen alternative Treibstoffkonzepte (z.B. LPG, CNG, H2) für den Antrieb nutzen, ist in den vergangenen Jahren kontinuierlich gestiegen. Der dabei zunehmende Mix an Behältertypen und die große Anzahl an alternativen Treibstoffen macht in Unfallsituationen die Berücksichtigung zusätzlicher Risiken notwendig. Zum Beispiel kann es bei einem Unfall zum Austritt von gasförmigen Treibstoffen sowie infolge eines Brandes auch zu einem Behälterversagen kommen. Das Schadensausmaß in einem solchen Fall übersteigt dabei deutlich das zu erwartende Ausmaß infolge eines PKW-Brandes mit herkömmlichen Kraftstoffen.
Aus der Literatur ist bekannt, dass ein Hotspot innerhalb eines Mikroreaktors auf einer Katalysatoroberfläche entstehen und zur Zündung einer Detonation im Reaktorinneren führen kann.
Um die Sicherheit von Mikroreaktoren diesbezüglich genauer untersuchen zu können, wurde ein Verfahren entwickelt, um einen künstlichen Hotspot mit regelbarer Temperatur im Inneren eines hierfür konstruierten Hochdruck-Mikroreaktors zu erzeugen.
Die Ergebnisse der experimentellen Untersuchungen zeigen einen deutlichen Einfluss der Rohrleitungsverzweigungen auf die ablaufenden Deflagrationen (Explosionsdruck und Flammenausbreitungsgeschwindigkeit) in der Rohrleitung. Eine erste numerische Simulation der beobachteten Abläufe in der Verzweigung, zeigt bereits eine rechte gute Übereinstimmung mit den experimentellen Daten.
We introduce the optical frequency domain reflectometry (OFDR) technique based on intensity modulation frequency sweep measurement for distributed disturbance measurement in optical fibres. By evaluating interferometric Rayleigh scattering changes along the fibre, strain and temperature changes are detected with 100 n(epsilon) sensitivity and 10 mK resolution. The vibration frequencies for low frequencies and up to the kHz-range can be obtained from power change evaluation in the spatial domain. This novel OFDR approach is a low-cost alternative for distributed disturbance measurement up to distances of several kilometres.
One of the unique advantages of polymer optical fibres (POF) is that they can be used to measure very high strain values up to 100 % and beyond exceeding the strain limits of silica fibre-based sensor principles. In this paper the distributed strain measurement capabilities of POF based on backscatter change evaluation are summarized and distributed backscatter measurement technologies are intro-duced. Application examples in the structural health monitoring (SHM) field are presented: a promising approach is the integration into technical textiles for high-strain measurement in earthwork structures and crack detection in buildings. The potential of POF for future applications in SHM such as distributed relative humidity sensing is discussed.
The effects of hydrogen admixture to natural gas on explosion regions, explosion group classification, explosion severity and on areas with explosive mixtures in case of gas release was studied experimentally. With increasing hydrogen fractions the mixtures become mainly more "critical", but up to 10 mole% hydrogen the influence on the safety characteristics are very low. By using appropriate calculation methods some of the safety characteristics could be calculated with good accuracy.
Industrial piping systems are particularly relevant to public safety and the continuous availability of infrastructure. However, condition monitoring systems based on many discrete sensors are generally not well-suited for widespread piping systems due to considerable installation effort, while use of distributed fibre-optic sensors would reduce this effort to a minimum. Specifically distributed acoustic sensing (DAS) is employed for detection of third-party threats and leaks in oil and gas pipelines in recent years and can in principle also be applied to industrial plants. Further possible detection routes amenable by DAS that could identify damage prior to emission of medium are subject of a current project at BAM, which aims at qualifying distributed fibre optic methods such as DAS as a means for spatially continuous monitoring of industrial piping systems. Here, first tests on a short pipe are presented, where optical fibres were applied directly to the surface. An artificial signal was used to define suitable parameters of the measurement system and compare different ways of applying the sensor.
Spontaneous deflagrations are recurring causes for incidents compromising the safety of humans and environment. In order to test the deflagration capability of substances, standard test methods are used according to VDI 2263 or UN-Manual. The test methods have been improved most recently by using an autoclave instead of conducting tests in open systems. The concept of using autoclaves for deflagration tests has been developed further on by varying the autoclave’s size, the substances and the test conditions. New experimental results are presented. On the basis of experimental data, numerical calculations will be developed in order to simulate the propagation of deflagrations.
Spontan einsetzende Deflagrationen sind eine wiederkehrende Ursache für sicherheitstechnisch bedeutsame Vorfälle in der chemischen Industrie. Bei der Explosion eines Mixers während der Herstellung einer Azodicarbonamid-Zubereitung wurden erhebliche Schäden in der Produktionsanlage und an Gebäuden in der Umgebung verursacht. Diese Tatsachen dienen als Motivation, die Deflagration von Azodicarbonamid (ADCA) unter verschiedenen Bedingungen zu untersuchen.
The thermal decomposition of dicumyl peroxide dissolved in ethylbenzene has been studied in our laboratories using differential scanning calorimetry (DSC), calvet calorimetry (C80), adiabatic calorimetry, reaction calorimetry and micro calorimetry. Based on the DSC and C80 experiments a formal kinetics model has been derived, which was compared to the other applied techniques. Finally we used our model to predict the thermal response of 216.5 L steel drums to exposure to constant elevated temperatures, both using the stationary Semenov approach as well as time-resolved CFD simulations. The prediction was compared to one-to-one testing using the UN-Test H.1. The observed level of consistency between model and experiments is remarkably good. The comparison with the 216.5 L testing clearly demonstrates that reliable and conservative predictions for technically relevant scales are possible as long as a validated model is used.
Amuay accident 2012 is one of similar accidents happened in Buncefield (2005), Jaipur and Puerto Rico (2009), respectively. Since experimental reproduction of such accidents is not always possible numerical simulations help a lot to understand the scenarios on qualitative basis. In this work the accident is reproduced with a CFD model which takes into account the heaviness of the gas (LPG), wind and gravity driven spread. The leak was reported to be located near a number of spherical tanks. The ignition source was presumably the running vehicles on a nearby street. A part of the refinery containing the locations of leakage and ignition was considered as computational domain. The road is located at the eastern boarder. The area contains different tanks, whose height was estimated due to a lack of available data. The diameter was extrapolated from the available image data. Further, a grid of walls is located between a number of tanks. The total domain has a size of 750 m x 400 m x 50 m. An unstructured mesh was created using tetrahedral elements with prism layers at the ground to improve mesh quality in the boundary layer. The mesh has a total number of 775 686 cells.
The transport of peracetic acid (PAA) in intermediate bulk containers (IBC) and tanks is only possible if they have suitable pressure relief devices. To determine the dimension of the pressure relief devices the 10-l-model tank of annex 5 of the UN Manual of Tests and Criteria is used.
During the investigation of a PAA this model tank fragmented. To prevent such violent events in the future, the model tank should be provided with additional pressure relief devices.
Das Abbrandverhalten und die thermische Strahlung von Poolfeuern organischer Peroxide (OP) wurden bereits in der Vergangenheit ausführlich untersucht. Dabei ergaben sich zum Teil erhebliche Unterschiede hinsichtlich der Abbrandraten, Temperaturen, Strahlungsintensitäten und Flammenlängen im Vergleich zu flüssigen Kohlenwasserstoffen. Das größere Gefahrenpotenzial von OP führt zu strikteren Sicherheitsbestimmungen für Lagerung und Transport. Da das Gefahrenpotenzial maßgeblich von den tatsächlich auftretenden Szenarien abhängt, ist eine Bewertung solcher Ereignisse unumgänglich um nachhaltig die Gesundheit von Mensch und Umgebung zu sichern. Ein Metallfass, gefüllt mit 200 Litern DTBP (Di-tertiär-butylperoxid), wurde auf dem Testgelände Technische Sicherheit der BAM einem Außenfeuer ausgesetzt. Durch den starken Wärmeeintrag erhöht sich die Massenabbrandrate des Peroxids um ein Vielfaches und das Fass entleert sich schließlich unter Ausbildung mehrerer Feuerbälle. Die Flammengröße, Flammentemperatur und damit die thermische Strahlung überschreiten die der gewöhnlichen OP-Poolfeuer. Die resultierenden höheren Sicherheitsabstände sind abschließend berechnet.
Long-term completely embedded sensor systems offer innovative possibilities for structural health Monitoring of concrete structures. Measuring of relevant parameters, e.g., temperature, humidity, or indication of corrosion can be performed with low energy sensors.
This allows to implement passive RFID sensor systems without cable connection and battery, which are power supplied exclusively by the electromagnetic field from the external Reader device. To evaluate characteristics and conditions of this concept, a systematical Investigation of the transmission characteristics with variation of relevant parameters, as communication frequency, installation depth, type of concrete, moisture content, etc. is currently carried out in an interdisciplinary research project at BAM. First results are presented in this paper.
Besides measurement of VOC emissions also the evaluation of odour emissions and the perceived intensity of odours gains in importance. Due to difficulties detected in the measurement method of the perceived intensity described in (ISO 16000-28, 2012) the introduction of “reference” odours will be recommended for the training of panellists and as basis for interlaboratory comparisons. In order to generate the “reference” odours standard liquid substances were directly injected into the main gas flow provided to the panellists. One of the substances tested was ethyl acetate. A pre-evaluation was conducted with six untrained panellists and has shown that ethyl acetate is potentially suitable as reference odour. For further validation of those “reference” odours they additionally will be provided to and evaluated by trained panellists of well established-measurement institutes.
In the search for highly efficient, low-cost, non-toxic, transparent conductive oxides (TCOs) suitable for large area applications for photovoltaics, ZnO and ZnO-related materials have received considerable attention. In the present work, Al and Ga doped ZnO films on oxidized Si substrates are characterized using mainly variable angle spectroscopic ellipsometry; additional optical and non-optical techniques were employed to confirm and support the ellipsometric models considered. The samples were obtained by means of pulsed chemical vacuum deposition (CVD) and atomic layer deposition (ALD).
As known from previous studies the presence of dopants in ZnO thin films generally induce significant changes in the optical, electrical and morphological properties. We present our findings for a series of Al and Ga doped ZnO layers with different concentrations of the dopants, discussing their influence on the optical and electrical properties.
Microbial induced corrosion (MIC) is a crucial problem in many technical plants as well as fuel tanks, leading to considerable damage and huge financial losses. Successful prevention of MIC requires the localization of first signs of corrosion as well as the identification of factors influencing the corrosion process.1 Hence, there is a growing need for sensitive and preferably inexpensive tools that enable the early detection of MIC. Of high importance are methods, which provide spatially and time-resolved information and allow the study of changes on metal surfaces as prerequisites for a more detailed analysis of ongoing corrosion processes at a MIC-affected site.2 In this respect, also the determination of corrosion rates can be of interest for the possible prevention of MIC.
Microbial induced corrosion (MIC) is a crucial problem in many technical plants as well as fuel tanks, leading to considerable damage and huge financial losses. Successful prevention of MIC requires the localization of first signs of corrosion as well as the identification of factors influencing the corrosion process.1 Hence, there is a growing need for sensitive and preferably inexpensive tools that enable the early detection of MIC. Of high importance are methods, which provide spatially and time-resolved information and allow the study of changes on metal surfaces as prerequisites for a more detailed analysis of ongoing corrosion processes at a MIC-affected site.2 In this respect, also the determination of corrosion rates can be of interest for the possible prevention of MIC.
In respect of modern approaches in material sciences and highly increased requirements on materials on safety relevant components, quality management and non-destructive testing reclaims a steadily increased meaning. The destructive meaning of measuring the degree of purity is defined in DIN EN 10247 through metallurgical investigations, especially microsections. For and comparable, but non-destructive testing due ultrasonic testing, the material the SEP 1927 is a well-defined industry standard. A novel and alternative way of reference block construction was focused by this work. The proposed amendments, regarding the manufactoring and machining, are less time and cost consuming. Verified by measurements the presented reference block fits the same acoustical characteristics and the requirements of the guideline.
Thermal treatment improves the excellent properties of UHPC. Recent studies have shown that an increase in compressive strength of more than 30 % is possible. However, the accurate conditions of thermal treatment for a maximal strength are considered as yet undetermined. A multitude of parameters can be varied: temperature, pressure, water saturation, and duration of the process steps. These parameters influence the phase development and in consequence the macroscopic properties of UHPC. The primary objective of the presented study was the optimisation of the conditions for thermal treatment, concerning compressive strength. It focuses on pre-storage time and duration of the treatment at defined temperatures and pressures (90 °C and 185 °C/1.1MPa).
As expected, experimental results showed a fundamental change of phase composition in hydrothermally treated UHPC in comparison to standard cured UHPC: Ettringite decomposes at higher temperatures and is absent after thermal treatment; the amount of portlandite and clinker phases decreases. The change of phase composition is accompanied by increased compressive strength.
Experimental studies of calcium-silicate-systems at hydrothermal conditions predict the formation of the crystalline C-S-H phase tobermorite. In fact, this is a typical phase occurring in other hydrothermally treated calcium-silicate-systems like Autoclaved Aerated Concrete (AAC). Commonly, high strength is attributed to the presence of tobermorite; however, in the presented study tobermorite was not detected in the hydrothermally treated UHPC. Therefore, tobermorite cannot be responsible for the increased strength of hydrothermally treated UHPC.
In conclusion the development of phases and strength of UHPC at hydrothermal conditions differs fundamentally from AAC and the experimental studies with water saturation. Results of these systems cannot be transferred to UHPC. In thermally treated UHPC, the hydration of clinker is enhanced and the puzzolanic reaction is intensified. Hence, more C-S-H is formed that fills pores and cracks, leading to a denser structure and finally to higher strength.
Methoden der Bauartprüfung und –zulassung von Behältern für radioaktive Stoffe, Sicherheitsnachweis von RAM –Behältern;
Versuchstechnische Anlagen der BAM für Gefahrgutverpackungen im Originalmaßstab; Durchführung experimenteller Untersuchungen mit Transport- und Lagerbehältern für radioaktive Stoffe; Fallprüfungen mit Prüfmustern und Modellbehältern; Beanspruchungsanalyse von Behälterkomponenten und Sicherheitsbewertung der Behälterkonstruktion; Vorstellung der BAM und des Testgeländes Technische Sicherheit
Industrial quality control (QC) nowadays requires the visualization of surface modifications from the macro-scopic to the microscopic or even nanoscopic scale. This is a prerequisite to the evaluation of functionality and reliability, the detection of defects and their separation of artefacts. The diversity of applications ranges from low-E glazings and solar panels, micro- and optoelectronics, micro- and smart devices to sensor-on-chip and lab-on-chip systems [1]. Optical microcopy (light, confocal laser scanning, white light interference) as established QC-tool is operated at normal incidence, i.e. p- and s-polarization are undistinguishable. Either light-intensity in terms of grey scale and colour or intensity-correlated effects of phase shifts are used. In case of ellipsometry, operated at oblique incidence, p- and s-polarization matter, and amplitude ratios and phase shifts upon reflection are measured. Hence, information content must be much higher.
The visualization of surface modifications may be very challenging for coating/substrate systems of either al-most identical optical constants, e.g. transparent films on substrates of the same material, or minor film thick-ness, substance quantity and affected area, e.g. ultra-thin or island films. Ellipsometry gives access to the con-trast of intensity (I), amplitude ratio (Ψ), and phase shift (Δ) with nanometer-scaled vertical and micrometer-scaled lateral sensitivity, one is able to identify tiny changes within an unmodified surface. As both mapping ellipsometry (ME) and imaging ellipsometry (IE) are operated in the optical far-field, surface inspection is also possible on the macroscopic scale. Near the Brewster-angle of the bare, undamaged, clean, and fresh substrate, the contrast to add-on and sub-off features is superior.
Fig. 1 shows three examples of ellipsometric imaging, i.e. a thin SnO:Ni film on SiO2/Si (Fig. 1a), a dried stain of an anti-body solution on cyclo-olefin-polymer (COP) shown in Fig. 1b, and a polyimide film residue on SiO2/Si (Fig. 1c). For all of these examples, ellipsometry provides much better contrast between substrate and surface modification than optical microscopy, sometimes primarily caused by the oblique incidence (Figs. 1a and 1c), in other cases related to the phase sensitivity of ellipsometry (Fig. 1b). Other examples are laser surface modifications and the corrosion of glass. In these cases, optical microscopy and IE yield to similar results, how-ever only ellipsometry gives access to modelling.
Further investigated coating/substrate systems are 100Cr6 steel, native oxide on silicon, borosilicate glass, and the polymer polycarbonate with deposited films of graphene and ta-C:H, printed and dried pattern of liquids such as water, cleaning agents, and dissolved silicone. Besides imaging ellipsometry, referenced spectral ellipsometry (RSE) has been applied, combining the advantages of both optical microscopy (fast measurement) and ellipsometry (high sensitivity to tiny modifications).
Photoluminescence techniques are amongst the most widely used tools in the material and life sciences, with new and exciting applications continuously emerging, due to their many advantages like comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. Drawbacks are , however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are time-dependent due to the aging of instrument components, and difficulties to measure absolute fluorescence intensities. Thus, there is a considerable need for standards for intensity, spectral, and temporal fluorescence quantities to meet the increasing need for instrument performance validation and global trends to harmonize physicochemical measurements. In this respect, instrument calibration strategies together with different types of fluorescence standards are presented as well as design concepts for robust, easy-to-use, and format-adaptable fluorescence standards useable for the determination of different fluorescence parameters and a broad variety of fluorescence techniques.
Die Mindestwanddicken der Tankkörper sind nach RID/ADR zu bestimmen. Zusätzlich sind die Tanks nach einer Norm oder nach einem von der zuständigen Behörde anerkannten technischen Regelwerk zu berechnen. Dabei ist der Tank unter Prüf- und Betriebsbelastungen auszulegen. Zusätzlich ist ein gefahrgutabhängiger Berechnungsdruck, der mit der Gefährlichkeit des Stoffes zunimmt, zu berücksichtigen.
Welded plate girders are used in heavy steel construction, industrial buildings and bride construction. Residual stresses are present in all plate structures. They are mainly caused by welding. In addition, they influence the load bearing capacity of these welded components. However, Eurocode (EC) does not provide any specific residual stress patterns for consideration of residual stress impact on load capacity. Hence, the decision for a particular problem has to be made by the designer. Many codes, including EC 3, permit the use of non-linear finite element analysis (FEA) for the design of structures. This contribution gives an overview on recent research topics: modeling, experimental measuring and evaluation of residual stresses as well as welding simulation tools and simplified methodologies for assessment of weld residual stresses.
Welded plate girders are used in heavy steel construction, industrial buildings and bride construction. Residual stresses are present in all plate structures. They are mainly caused by welding. In addition, they influence the load bearing capacity of these welded components. However, Eurocode (EC) does not provide any specific residual stress patterns for consideration of residual stress impact on load capacity. Hence, the decision for a particular problem has to be made by the designer. Many codes, including EC 3, permit the use of non-linear finite element analysis (FEA) for the design of structures. For that purpose, the contribution gives an overview on recent results derived from welded I-girders made from mild steel S355 and high-strength steel S690QL. Weld residual stresses have been investigated by X-ray diffraction (XRD) on small-scale specimen. In addition, residual stresses of welded component-like I-girders have been studied using the sectioning technique. The results confirmed the beneficial effect of certain edge preparation of the plates by flame cutting prior to welding. High-strength steels like the S690 can contribute to both: increased load capacity and decreased influence of weld residual stresses.
Gas sensors are an important tool in various areas for example in industrial process control as well as Gas sensors are an important tool in various areas for example in industrial process control as well as safety applications or in research. A useful gas detector should be selective, precise, stable and cost-effective. In the present research a surface based gas detection technique is investigated using the SPR effect with ellipsometric readout. This technique is called surface plasmon resonance enhanced ellipsometry (SPREE).
The sensor consists of a gold layer (40 nm) top-coated with a doped metal-oxide (M:SnOₓ,
5 nm). The coating is added by magnetron sputtering with doped targets with different doping concentrations. It could be shown that, without the top-coating, these type of sensors can detect various gases, e.g. CO, H2, O2, O3, He, N2, with sensitivities down to the ppm range (in air).
The goal of the present study is to characterize the additional coating materials in dependence of the coating conditions. With the help of the doped-metal oxide, the sensitivity increases dramatically by a factor of 100. Additionally, a selectivity for specific gases is observed which depends on the doping conditions of the coating. Changing the properties of the plasma coating process and the doping metal gives access to a variety of different layers and enables us to find the best conditions.
A combined finite element boundary element method has been developed to calculate the dynamic interaction of the railway track and the underlying soil. The track-soil results are coupled with a simple vehicle model to establish the force transfer function of the vehicle-track-soil system. Mitigation measures at the track, namely three different tracks with under-sleeper pads, are analysed. The un-sprung vehicle and heavy track masses on soft track elements yield a lower vehicle-tracksoil resonant frequency and a better reduction of the excitation forces at higher frequencies. If the effectiveness of the mitigation is measured as a vibration ratio between the isolated and an un-isolated reference track, the vehicle-track-soil resonance of the reference track has an important influence on the mitigation effectiveness. Therefore, different un-isolated reference tracks are analysed. It is shown how the frequency and amplitude of the vehicle-track resonance are influenced by the stiffness of the rail pads (strongest), the ballast (medium) and the soil (weakest). The reference track models have been compared with shaker tests on two railway tracks with strong resonances. The damage detection and repair control have become important tasks for ballast and slab tracks. Measurements which compare the damaged and the repaired status of the same track section at different times, or which compare a damaged and an intact track section at the same time, have been successfully performed at some sites in Germany and compared with the theoretical behaviour of intact and damaged tracks.
We have studied the influence of gamma rays on physical properties of different commercially available silica optical fibers stepwise irradiated up to a total dose of 100 kGy. The detection of radiation-induced changes in silica glass offers the possibility of using selected optical fibers as distributed radiation sensors. The measurements performed by us were based on optical backscatter reflectometry and Brillouin distributed sensing. The measurement methods enable an analysis of radiation-induced modification of the group refractive index and density of the optical fibers. The most distinct physical effect observed by us concerns the increase of the optical attenuation with rising total radiation doses. Quantitative measurement results indicate a crucial impact of fiber dopants on radiation-induced physical and sensory characteristics of silica optical fibers affected by differences in fiber fabrication techniques. Based on the obtained results, the suitability of distributed Brillouin sensing for dosimetry applications seems to be improved by modifying the refractive index profile of the fiber core.
Long wooden floor beams above a ball room in an old historical palace have been analysed experimentally. The eleven beams are weakly coupled by three layers of floor boards. It has been investigated if the state (the stiffness) of the wooden beams can be determined by vibration measurements of global or preferably local modes. Hammer, heel-drop and ambient excitations have been used. The vibration modes of the structure show dominating local deformations if an impact excitation is applied. This is understood as the positive superposition of several modes which yield the maximum at the excitation point but a cancellation at more distant points. Natural modes have been estimated from these vibration modes by standard and special methods which were necessary for the high damping of the wooden floor. It has been found that all floor beams contribute to each natural mode even for a weak coupling of the beams. In addition to the modal discussion, the impact tests have also been analysed for the wave propagation and amplitude attenuation with distance. The coupling of floor beams has been studied theoretically by an analytic multiple-beam model where the coupling by translational or rotational springs and by a common support motion has been assumed.
Permeability estimation from spectral induced polarization (SIP) measurements is based on a fundamental premise that the characteristic relaxation time (t) is related to the effective hydraulic radius (reff) controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We examine the link between t and reff for an extensive database of sandstone sampleswhere mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen-Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of 1 or 2 distinct representative diffusion coefficients but instead demonstrates strong evidence for 6 orders of magnitude of variation in an apparent diffusion coefficient that is well correlated with both reff and the specific surface area per unit pore volume (Spor). Two scenarios can explain our findings: (1) the length-scale defined by t is not equal to reff and is likely much longer due to the control of pore surface roughness; (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g. silica, clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from SIP relaxation time.
Zur Bestimmung des Feuchtezustands und insbesondere der Belegereife von Estrichfußböden kommen in Deutschland zerstörende Prüfverfahren zum Einsatz, die eine punktuelle Probenahme erfordern. Hierbei ergeben sich immer wieder Fehlinterpretationen, da zum einen die Probenahme selbst zu einer Veränderung des Feuchtezustands führt und zum anderen, weil die Verfahren an sich mitunter ungenau sind (z.B. abhängig von der Estrichzusammensetzung). Zusammen mit vier Forschungsinstituten und dem Industriepartner Bosch wurden an der BAM zerstörungsfreie Prüfverfahren auf deren Tauglichkeit zur Estrichfeuchtemessung untersucht und mit den herkömmlichen zerstörenden Verfahren verglichen.
Für diesen Versuch kamen verschiedene geophysikalische Verfahren zum Einsatz, darunter Nuklear Magnetische Resonanz (NMR), elektrische Widerstandsmessungen und Impulsradar (GPR). Es wurden neun verschiedene Estrichsorten hergestellt und während der Trocknungsphase bei Konstant-Normklima gelagert. Diese wurden sowohl zerstörend als auch zerstörungsfrei mit den o. g. Verfahren untersucht. Gleichzeitig wurden die Masseänderungen der Proben zur Bestimmung des integralen Feuchtehalts aufgezeichnet.
Die Ergebnisse zeigen zum einen, dass das Abtrocknungsverhalten von zementgebundenen Estrichen grundsätzlich unterschiedlich von dem anhydritgebundener Estriche ist. Während sich bei ersteren zügig ein deutlicher Feuchtegradient über die Höhe der Proben einstellt, verläuft dieser bei der zweiten Probengruppe sehr flach. Dies lässt sich vor allem in den NMR Daten räumlich hochaufgelöst nachvollziehen - die Datenakquise erfolgte mit einer NMR MOUSE PM 25. Ein ähnliches Bild ergibt sich auch aus den elektrischen Widerstandsmessungen, die mittels sog. Multi-Ring-Elektroden (MRE) durchgeführt wurden. MRE bezeichnen als Vertikalprofil angeordnete Ringelektroden mit einem Abstand von ca. 1-2 mm, zwischen denen jeweils Zwei-Punkt Widerstandsmessungen durchgeführt werden. Bei sehr geringen Feuchtegehalten (z.T. auch um die Belegereife) waren mit dieser Methode jedoch wegen der zu hohen Übergangswiderstände nur bedingt Messungen möglich. Im Gegensatz zu NMR und MRE sind mit dem Radarverfahren (2 GHz Antenne) keine tiefenbezogenen Aussagen möglich. Jedoch lässt sich über eine Amplitudenauswertung von direkter und an der Rückwand reflektierter Welle teilweise eine Aussage über Restfeuchtigkeit im Volumen treffen. Ebenso zeigt die Laufzeitdifferenz der beiden Wellen eine starke Abhängigkeit vom Feuchtegehalt.
In Germany there is an existing built infrastructure worth about 50 trillion Euros. The expected lifetimes of individual structures are up to 100 years. Considerable costs (annually about 35 billion Euros, the trend continues upwards) are involved in order to maintain and rehabilitate both residential as well as transportation infrastructure buildings. Most damages we observe on our built infrastructure are moisture-induced processes. Consequently reliable moisture measurement tools a highly needed for meaningful building diagnosis investigations. The optimal moisture measuring technique would be non-destructive, fast, repeatable, reliable, independent of steel in the vicinity, the surface condition or possible salt loads of the material under test. Since this is unfortunately not the case for any non-destructive method, it is often very difficult to decide for users which method to use for the particular testing problem. The only standardized methods in Germany are the “direct” and destructive Darr- and the CM tests. Although they can be highly accurate (when handled with care during the sampling), they deliver only punctual information and cannot be used for monitoring. The other, non-destructive methods are based on the change in humidity-dependent physical material properties. The underlying physics, their particular advantages and disadvantages are discussed in this paper.
Fahrbahnübergänge sind das bautechnisch-konstruktive Verbindungsglied von der Fahrbahn der freien Strecke auf Ingenieurbauwerke und anschließend wieder zurück auf die freie Strecke. Sowohl aus ökonomischen (Baukosten), ökologischen (Lärmschutz) als auch aus verkehrssicherheitstechnischen Gründen wurden in jüngster Zeit sogenannte flexible belagsähnliche Übergangskonstruktionen entwickelt. Der Beitrag benennt die materialtechnischen und konstruktiven Anforderungen als notwendige Grundlage für den Nachweis der Funktionsfähigkeit unter höchsten Verkehrsbeanspruchungen. Gleichzeitig werden neuartige material- und leistungsidentifizierende Kennwerte vorgestellt und deren Einfluss auf Funktionsfähigkeit und Dauerhaftigkeit diskutiert. Als versuchstechnische Grundlagen kommen durch die BAM entwickelte bzw. adaptierte Untersuchungsmethoden zur Anwendung. Die Interpretation der Untersuchungsergebnisse und deren Beitrag und Bedeutung für qualitätssichere europäische bzw. nationale Bauprodukte werden der Zielgruppe Verkehrsplanern, Straßenbaubehörden, Ausführenden und Nutzern erläutert. Schlussfolgerungen aus den veränderten baurechtlichen Rahmenbedingungen und Erfahrungen der BAM bei der europäischen Zulassung von Übergangskonstruktionen werden vorgestellt.
Fungal secondary metabolites such as phomopsin A (PHO-A) produced by the fungus Diaporthe toxica are referred to as “emerging” mycotoxins. Recently, we developed a biosynthetic approach to gain access to 15N-isotopically labelled PHO-A as internal standard (IS) for PHO-A matrix independent quantification of PHO-A in various commodities. Aim of the present work was to elucidate the applicability of the new IS for accurate quantification and to investigate the phomopsin formation on various legume seeds as well as plant material. In summary, the applicability of the SIDA-HPLC-MS/MS method could be proven and the potential of D. toxica to produce high amounts of phomopsins under unfavorable conditions on lupins and other legume seeds could be shown. Moreover, a novel toxic methylated PHO-A derivative was unveiled in natural samples infested with D. toxica.
Neue Trends & Alte Probleme: Das Leguminosenmykotoxin Phomopsin A in einer "worst case"-Betrachtung
(2016)
Leguminosen wie z.B. Bohnen, Erbsen, Soja und zunehmend auch die Samen der Süßlupine liefern aufgrund ihres hohen Proteingehaltes einen wertvollen Beitrag zu einer veganen oder vegetarischen Ernährung. Jedoch sind Lupinen anfällig für Infektionen mit dem Pilz Diaporthe toxica, der u.a. Phomopsin A als hepatotoxischen Sekundärmetaboliten bildet. Ziel der Arbeiten waren die Gewinnung und Anwendung eines 15N-isotopenmarkierten internen Standards für die HPLC-MS/MS-Analyse dieses Toxins sowie die Quantifizierung der Toxinbildung in einem „worst case“-Szenario.
Leguminosen wie z.B. Bohnen, Erbsen, Soja und zunehmend auch die Samen der Süßlupine liefern aufgrund ihres hohen Proteingehaltes einen wertvollen Beitrag zu einer veganen oder vegetarischen Ernährung. Jedoch sind Lupinen anfällig für Infektionen mit dem Pilz Diaporthe toxica, der u.a. Phomopsin A als hepatotoxischen Sekundärmetaboliten bildet. Ziel der Arbeiten waren die Gewinnung und Anwendung eines 15N-isotopenmarkierten internen Standards für die HPLC-MS/MS-Analyse dieses Toxins sowie die Quantifizierung der Toxinbildung in einem „worst case“-Szenario.
UHPC-AAC/CLC composite panels with self-cleaning properties. Materials and production technology
(2016)
The aim of this study is to show the development of a façade composite panel combining either an autoclaved aerated concrete or a cellular lightweight concrete insulation layer with a box-type external ultra-high performance concrete (UHPC) supporting layer. The paper presents the materials characteristics of the different components and the production technology of the panel. The efficiency of surface modifications of the materials forming the external shell of the panel is reported. The activation of self-cleaning properties is described. The test results showed that the most efficient way to use the water-repellent agent is its application on the substrate before the concrete cast.
Concerning the production technology, the preliminary studies showed more advantages of a two-step manufacturing procedure of the UHPC boxes than a one-step procedure.
The goal of the present study is to assess the feasibility to develop a first reliable database of materials parameters for Earth Block Masonry (EBM). The database is crucial when defining the materials safety factors. In the first part an experimental campaign of compressive tests were carried out on two types of earth block and two types of earth mortar. The results showed that the mean variation of the compressive strength was remarkably less than expected. This low variation is related to a production with high quality standards of the materials employed. In the second part a partial safety factor for EBM under uniaxial compression was determined through the reliability method. The results proved the reliability of a common calculation method for EBM based on partial safety factors following the current standards.
Vielzahl unterschiedlicher VOC kann aus Bauprodukten freigesetzt werden. In den meisten Bauproduktgruppen gibt es sowohl emissionsarme als auch emissionsreiche Produkte. Manche VOC sind produktgruppenspezifisch, z.B. Siloxane/Silikon, andere VOC unspezifisch wie Formaldehyd und Essigsäure. VOC-Analytik und Gerüche zeigen im Allgemeinen keinen Zusammenhang. Schwerflüchter zeigen Langzeitemission und ausgeprägte Senken-/Memoryeffekte. Drucker/Kopierer emittieren neben VOC auch Fein- und Ultrafeinpartikel. Radon kann aus manchen Bauprodukten abgegeben werden und bei luftdichten Gebäuden in radonarmen Gebieten Haupt-Radonquelle sein. Radonexhalation kann grundsätzlich (statisch/dynamisch?) mit VOC-Kammern - ergänzt mit geeigneten Messgeräten - bestimmt werden. Es existiert eine Vielzahl von Labels für emissionsarme Bauprodukte. Gerade bei modernen, dichten Bauten mit geringem natürlichen Luftwechsel sind hohe Schadstoffkonzentrationen zu erwarten, wenn nicht emissionsarme Materialien und Produkte zum Einsatz kommen.
Evaluation of high spatial resolution imaging of magnetic stray fields for early damage detection
(2016)
Metal magnetic memory (MMM) technique with associated ISO 24497-1:3 is gaining considerable interest in the magnetic NDT community. In contrast to traditional Magnetic Flux Leakage (MFL) testing, the inspection objects are not intentionally magnetized by an external magnetic field. Due to the physical coupling between mechanical stress and magnetization of ferromagnetic materials, it is assumed that the distribution of the residual MFL correspond to the internal stress of the specimen, or in the most general sense, to a degradation of the material.
Usually, MMM measurements are performed by relatively bulky magnetic inspection sensors. The evaluation of local magnetic field distribution is limited thereby. Highprecision GMR (Giant Magneto Resistance) measurements in the micrometer regime can provide a higher degree of information due to better spatial resolution.
We present a concise summary of studies on the correlation of magnetic structure and microstructure of steels. In particular, we compare residual stress measurements in S235JRC steel welds by means of neutron diffraction with high resolution magnetic field mappings. Results indicate a qualitative correlation between residual stresses and local stray field variation. In addition, stray field measurements of plastically deformed specimens for quasi-static and cyclic loading cases are discussed. The present study concludes that GMR sensors can detect inhomogeneous plastic deformations of S235JR steel in a very early stage, without specific signal processing according to the ISO 24497-1:3.
In einem von der BG ETEM geförderten Vorhaben wurden sicherheitstechnische Kenngrößen für den Explosionsschutz von Erdgas-Wasserstoff-Gemischen nach den aktuellen europäischen Normen gemessen. Dabei können für Stoffmengenanteile bis zu 10% Wasserstoff folgende Aussagen getroffen werden: Die unteren Explosionsgrenzen und Sauerstoffgrenzkonzentrationen verändern sich nur wenig. Der Einfluss auf Explosionsdrücke und KG-Werte ist ebenfalls vernachlässigbar. Die Modellgase mit Wasserstoffanteilen von bis zu 10 Mol-% erfüllen weiterhin sicher die Voraussetzung für die Ex-Gruppe IIA. Höhere Wasserstoffanteile (> 30%) können einige Kenngrößen relevant beeinflussen (z. B. OEG, LOC, MESG, KG).
In einem Vorhaben wurden sicherheitstechnische Kenngrößen für den Explosionsschutz von Erdgas-Wasserstoff-Gemischen nach den aktuellen europäischen Normen gemessen. Dabei können für Stoffmengenanteile bis zu 10% Wasserstoff folgende Aussagen getroffen werden:
Die unteren Explosionsgrenzen und Sauerstoffgrenzkonzentrationen verändern sich nur wenig.
Der Einfluss auf Explosionsdrücke und KG-Werte ist ebenfalls vernachlässigbar.
Die Erdgase mit Wasserstoffanteilen von bis zu 10 Mol-% erfüllen weiterhin sicher die Voraussetzung für die Ex-Gruppe IIA.
Höhere Wasserstoffanteile (> 30%) können einige Kenngrößen relevant beeinflussen (z. B. OEG, LOC, MESG, KG).
Berechnungen zeigen nur geringen Einfluss von 10 % H2 auf die Gasausbreitung.
Gaswarngeräte müssen in der Regel neu kalibriert werden.
The surface chemistry / functionalization of nanomaterials and microparticles largely controls the stability of these materials as well as their solubility and subsequent biofunctionalization and their interactions with biological systems. Moreover, in the case of some nanomaterials like semiconductor quantum dots or lanthanide-based upconversion nanocrystals, the ligand shell strongly affects their optical properties, e.g., via passivation of surface states and traps that favor luminescence quenching or the protection of surface atoms from quenching water molecules. This renders analytical methods for the quantification of surface groups like functionalities very important. Targets of broad interest are here amino, carboxyl, alkine and maleimide groups used for common bioconjugation reactions and typical ligands like thiols and polyethylene glycol (PEG) molecules of varying length, used for the tuning of material hydrophilicity and biocompatibility, minimization of unspecific interactions, prevention of biofouling, and enhancement of blood circulation times as well as surface-bound biomolecules like streptavidin or other biomolecules relevant e.g., for diagnostic assays. Here, we focus on simple optical methods relying on standard laboratory instrumentation, validated by method comparison and/or mass balances and present examples for their use for the characterization of different types of nanomaterials and microparticles.
Luminescence-based detection methods, ranging from fluorescence spectroscopy for photophysical and mechanistic studies over sensing applications, chromatographic separation techniques and the microarray technology with fluorescence detection to fluorescence microscopy, flow cytometry, single molecule spectroscopy, and molecular imaging to integrating sphere spectroscopy, are among the most widely used methods in the life and material sciences. This is due to e.g., their unique sensitivity enabling the detection of single molecules, potential for multiplexing, ease of combination with spatial resolution, and suitability for remote sensing. Many of these advantages are closely linked to the choice of suitable molecular and nanoscale fluorescent reporters, typically required for signal generation. This includes organic dyes without and with sensor function, fluorophore-encoded polymeric and silica nanoparticles as well as nanocrystalline systems like semiconductor quantum dots and upconversion phosphors, emitting in the visible (vis), near-infrared (NIR), and IR (infrared). Current challenges present the environment sensitivity of most fluorophores, rendering fluorescence spectra, measured intensities/fluorescence quantum yields, and fluorescence decay kinetics matrix-dependent, and instrument-specific distortions of measured fluorescence signals that need to be considered for quantification and comparability of data, particularly fluorescence spectra.
Here, current applications of luminescence-based methods and different types of reporters will be presented. In this context, suitable spectroscopic tools for the characteri-zation of the optical properties of fluorescent reporters and fluorophore-encoded microparticles, analytical tools for the determination of the surface chemistry of different types of particles, and different multiplexing strategies will be discussed.
The reliability of wheel set axle testing is of high importance because small discontinuities caused during manufacturing or rock fall impacts during operation might cause growing cracks during the operation load cycles. While most of the axles are tested by automated UT-systems today, the basic education of railway NDT operators is still manual testing providing the basic understanding and skills for the operators. In Germany it is a common rule that NDT operators in the railway branch need to refresh their knowledge and skills every five years including a refresh examination. The testing results from these exercises and from a parallel round robin test have been sampled at the DGZfP Railway Education Centre in Wittenberge for a period of about 5 years. The results of the operators written in test record sheets were compared with the “true” test crack or notch position in the axles used for examination. In this way the testing results could be categorized into “hits” and “misses” and the “hits” were further evaluated due to correct position and adequate amplitude height. Considering some thousand indications documented by the operators during the refresh examination and comparing transition bow, shaft and seat it was a highlight to see that the operators reach their best detection rate in the transition bow of the wheel axle set while this is often the most difficult part concerning the UT-echoes. Fortunately this is due to their raised awareness in the transition bow region because this is the most dangerous region with respect to fracture mechanics.
For two selected axles the experimental set up of 45° and 70° inward and outward UT-testing were also simulated showing clearly the difficulties of the UT-echoes detection of some specific test defects.
In order to provide nutrition for a growing world population pesticides are a necessary tool. Crop protection agents may be considered safe, if handled correctly. Nevertheless, they are subject to transformation processes and metabolization in the environment and technical installations. Transformation products (TP) and metabolites may be more harmful than the mother substance and thereby pose a threat to environmental and human health.
With 19 % market share in 2014, triazole pesticides are the class of organic fungicides which are most commonly used in Germany. However, only little data is available concerning their TP and metabolites. In this study the fate of the triazole fungicides propiconazole and difenoconazole in soil and water using model reaction systems mimicking their pathway in the environment and the industrial water treatment is investigated.
During application the substances may directly contaminate soil as well as surface waters. In these compartments, transformation by global irradiation needs to be considered. Due to their moderate mobility both pesticides may also end up in ground water from which drinking water is produced. Owing to the vigorous conditions during drinking water production the formation of a variety of technical TP can be expected. Additionally, for all compartments the degradation by bacteria is a factor which needs to be taken into account. For this survey, the potential for metabolization by model organisms is investigated.
In this work degradation and transformation of the fungicides is monitored using quantitative target analysis. Major components in the reaction mixtures are identified by non-target analysis. GC-EI-MS-spectra, HR-MS-measurements, or the comparison with native standards are utilised for structural elucidation. For identification, products will be isolated and characterized by NMR. Toxicity assessment of these TP is essential to define threshold values in the environment.
The model reaction systems will be presented and possible TP will be shown.
Welded I-girders are used in many applications in steel construction, especially a tailored mixture of different plate thicknesses is difficult to manufacture by rolling. Residual stresses are mainly caused by
welding and it is in most cases impractical to anneal the structures. Eurocode 3 (EC 3) does not provide any
specific residual stress pattern. Hence,
the decision for a particular problem has to be taken by the designer. Stability failures are often decisive in the design of steel beam and column members. Many standards, including EC 3, permit the use of non-linear FEA for the design of structures. Load influencing imperfections are mainly geometric deviations from the
ideal shape and residual stresses(both due to assembly or weld manufacturing). Currently the residual stresses are considered by simplified “robust” procedures fixed in common standards(such as EC 3. Models mostly based on specimens from mild steel. Information about high-strength steels is less
available for realistic assessment of residual stresses in full-scale I-girders. Hence, the scope of this work is the measurement of residual welding stresses on component-like I-girders S355 and S690 by sectioning method and global structural welding simulation.
Welded plate girders are used in heavy steel construction, industrial buildings and bride construction. Residual stresses are present in all plate structures. They are mainly caused by welding. In addiiton, they influence the load bearing capacity of these welded components. However, Eurocode (EC) does not provide any specific residual stress patterns for consideration of residual stress impact on load capacity. Hence, the decision for a particular problem has to be made by the designer. Many codes, including EC 3, permit the use of non-linear finite element analysis (FEA) for the design of structures. Recent developments in the last years, enabled the use of computerized models instead of laboratory experiments. In this scope, the FE-model should include all relevant factors properly. This important if considering that weld residual stresses can be a critical assessment factor. In addition, measuring of residual stresses is difficult, time consuming and expensive, it is therefore common to use founded distribution functions (e.g. Swedish BSK 99). Welding simulation tools offer new possibilities for a realistic assessment of weld-induced stresses and deformations. However, the modeling and the computational effort for large structural components is still not in a practicable range and a simplified methodology is in needed. As a result, a new approach (suitable for capacity analysis) is presented and detailed in the present contribution.
Testing and numerical simulation of elastomeric seals under consideration of time dependent effects
(2016)
Due to delays in the siting procedure to establish a deep geological repository for spent nuclear fuel and high level waste and in construction of the already licensed Konrad repository for low and intermediate level waste, extended periods of interim storage will become more relevant in Germany. BAM is involved in most of the cask licensing procedures and is responsible for the evaluation of cask-related long-term safety issues. Elastomeric seals are widely used as barrier seals for containers for low and intermediate level radioactive waste. In addition they are also used as auxiliary seals in spent fuel storage and transportation casks (dual purpose casks (DPC)).
To address the complex requirements resulting from the described applications, BAM has initiated several test programs for investigating the behavior of elastomeric seals. These include experiments concerning the hyperelastic and viscoelastic behavior at different temperatures and strain rates, the low temperature performance down to -40°C, the influence of gamma irradiation and the aging behavior.
The first part of the paper gives an overview of these tests, their relevant results and their possible impact on BAM’s work as a consultant in the framework of approval and licensing procedures.
The second part presents an approach of the development of a finite element model using the finite element code ABAQUS®. The long-term goal is to simulate the complex elastomeric behavior in a complete lid closure system under specific operation and accident conditions.
In the last two decades automated ultrasonic inspection devices took over a lot of applications that prior have been carried out using manual inspection with the evaluation of A-scans only. In parallel phased array systems have been developed and brought to the market which offer detailed and fast control over the sound field. When applying automated inspection phased array systems for UT measurements imaging of the recorded data in combination with the probe positioning data is used for the evaluation of inspections. B-Scan, C-Scan and S-Scan images are typically used with this setup.
For more sophisticated applications with linear arrays echo tomography and syntethic aperture focusing technique (SAFT) are well known methods and often applied for high resolution image reconstruction. Since channel count of phased array systems is constantly rising, matrix arrays with up to 256 elements entered the market. Signal processing in the matrix domain became 3D. Since some years the Total Focusing Method (TFM) is an additional imaging tool for these type of application. It is based on the Full Matrix Capture (FMC) using the elements of phased array probes as separate transmitters and receivers.
In this contribution we discuss the common ground of SAFT and TFM as well as the differences between these imaging tools. The combined use of automated inspection, matrix arrays and signal processing for high resolution measurements is a challenging task where a very long parameter list has to be taken into account. Under which conditions which elements of the full matrix should be taken for the reconstruction for best results?
Based on examples taken from measured and simulated echo signals it will be shown how image resolution can be optimized in dependence of different parameters like the distance between transmitters and receivers and their directivity patterns, the depth of echo source and the specimen geometry.
Ray tracing boudary value problems: simulation and SAFT reconstruction for ultrasonic testing
(2016)
The application of advanced imaging techniques for the ultrasonic inspection of inhomogeneous anisotropic materials like austenitic and dissimilar welds requires information about acoustic wave propagation through the material, in particular travel times between two points in the material. Forward ray tracing is a popular approach to determine traveling paths and arrival times but is ill suited for inverse problems since a large number of rays have to be computed in order to arrive at prescribed end points. In this contribution we discuss boundary value problems for acoustic rays, where the ray path between two given points is determined by solving the eikonal equation. The implementation of such a two point boundary value ray tracer for sound field simulations through an austenitic weld is described and its efficiency as well as the obtained results are compared to those of a forward ray tracer. The results are validated by comparison with experimental results and commercially available UT simulation tools. As an application, we discuss an implementation of the method for SAFT (Synthetic Aperture Focusing Technique) reconstruction. The ray tracer calculates the required travel time through the anisotropic columnar grain structure of the austenitic weld. There, the formulation of ray tracing as a boundary value problem allows a straightforward derivation of the ray path from a given transducer position to any pixel in the reconstruction area and reduces the computational cost considerably.