Filtern
Erscheinungsjahr
- 2016 (2193) (entfernen)
Dokumenttyp
- Vortrag (910)
- Zeitschriftenartikel (520)
- Beitrag zu einem Tagungsband (326)
- Posterpräsentation (322)
- Sonstiges (25)
- Dissertation (21)
- Buchkapitel (19)
- Forschungsbericht (15)
- Beitrag zu einem Sammelband (13)
- Tagungsband (Herausgeberschaft für den kompletten Band) (7)
Sprache
- Englisch (1621)
- Deutsch (564)
- Mehrsprachig (6)
- Italienisch (1)
- Russisch (1)
Schlagworte
- Concrete (42)
- NDT (39)
- Korrosion (33)
- Simulation (29)
- Fluorescence (28)
- XPS (28)
- Gefahrgut (26)
- Reliability (25)
- Zerstörungsfreie Prüfung (25)
- Corrosion (23)
Eingeladener Vortrag
- nein (910)
Gas chromatography using atmospheric pressure chemical ionization coupled to mass spectrometry (GC/APCI-MS) is an emerging metabolomics platform, providing much-enhanced capabilities for structural mass spectrometry as compared to traditional electron ionization (EI)-based techniques. To exploit the potential of GC/APCI-MS for more comprehensive metabolite annotation, a major bottleneck in metabolomics, we here present the novel R-based tool InterpretMSSpectrum assisting in the common task of annotating and evaluating in-source mass spectra as obtained from typical full-scan experiments. After passing a list of mass-intensity pairs, InterpretMSSpectrum locates the molecular ion (M0), fragment, and adduct peaks, calculates their most likely sum formula combination, and graphically summarizes results as an annotated mass spectrum. Using (modifiable) filter rules for the commonly used methoximated-trimethylsilylated (MeOx-TMS) derivatives, covering elemental composition, typical substructures, neutral losses, and adducts, InterpretMSSpectrum significantly reduces the number of sum formula candidates, minimizing manual effort for postprocessing candidate lists. We demonstrate the utility of InterpretMSSpectrum for 86 in-source spectra of derivatized standard compounds, in which rank-1 sum formula assignments were achieved in 84% of the cases, compared to only 63% when using mass and isotope information on the M0 alone. We further use, for the first time, automated annotation to evaluate the purity of pseudospectra generated by different metabolomics preprocessing tools, showing that automated annotation can serve as an integrative quality measure for peak picking/deconvolution methods. As an R package, InterpretMSSpectrum integrates flexibly into existing metabolomics pipelines and is freely available from CRAN (https://cran.r-project.org/).
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.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
The objective of the present work was the investigation and demonstration of the potential of sol-gel alumina layers as corrosion protection of commercial power plant steels under oxyfuel conditions. The starting points of this work were modified Yoldas-sols which were developed in the BAM-department 5.6. These sols were suitable for the spin-coating method only. The application of coatings on tubes by spin-coating is impossible. Therefore, the chemical composition of the modified Yoldas-sol had to be adapted to the dip- and spray-coating techniques.
Exclusively the sol with the composition s-0.52-6-1.5 with a nitrate/aluminium ratio of 0.52; a solid content of 6 wt.% and a PVP (binder) content of 1.5 wt.% could fulfill the necessary criteria: long-term stability; formation of a dense, crack-free and well adhered layer on polished metal surfaces; as well as high protective abilities against corrosion in H2O-CO2-O2-SO2.
The commercial power plant steel X20CrMoV12-1 (X20) and the steel X12Cr13 were successfully coated with the sol s-0.52-6-1.5 by means of the dip-coating method. An at least 400 nm thick alumina layer (δ-Al2O3) is necessary to ensure the corrosion protection of these steels. The corrosion of the coated samples compared to that of the uncoated ones was significantly reduced, even after 1000 h of exposure in a H2O-CO2-O2-SO2 atmosphere at 600°C. Sulfur and carbon were not detected at the substrate surface or beneath the coating. Hence the transport of the flue gas components SO2 and CO2 into as well as through the alumina layer could be hindered. The diffusion of the alloying elements (Cr, Mn, Si) into the alumina layer resulted in the formation of mixed oxides like δ-(Al,Cr)2O3. Formation of such phases considerably contributed to the corrosion protection.
The long-term stability of the sol s-0.52-6-1.5 and the high protective abilities of the alumina layer on commercial power plant steels provide a good basis for an industrial application.
Various methods have been used for introducing fire retardant additives into polymers. Deposition of thick fire retardant coatings directly onto polymer substrates is an alternative technique. An important Advantage of the coating technique is the preservation of the physical and chemical integrity of the polymer material. Moreover, the fire retardancy of the polymer materials can be achieved following their production. Suitable coating materials are inorganics, intumescent, char-forming, oxygendiluting, and cooling or radical quenching layers. The most important problem is to achieve sufficient coating thickness to withstand the direct attack of flame and to protect the polymer bulk from pyrolysis, otherwise blistering of coating, caused by emitted pyrolysis gases, is often observed.
To avoid blistering of coating, the adhesion between polyolefin Substrate and fire retardant coating has to be extraordinarily high.
In order to achieve such a high level of adhesion, the polymer surface has to be modified with adhesion-promoting functional groups. The deposition of thin plasma polymers as adhesion-promoting layers with NH2, OH or COOH groups has been the most suited method. These functional groups are able to form covalent bonds and other interactions between the fire-resistant coating and the plasma-modified polyolefin substrate.
Additionally, the plasma polymer counteracts the strong mechanical stresses in the laminate on exposure to high temperatures by its flexibility. The thick fire retardant coatings were chosen based on “green” ecological aspects to avoid flame-initiated emission of toxic or corrosive gases and remains of toxic char.
Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces
(2016)
Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned.
The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers.
The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces.
Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces
(2016)
Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned.
The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers.
The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces.
Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces
(2016)
Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned.
The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers.
The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces.
Currently available separation channels for asymmetric flow
field-flow fractionation (AF4), which results in long analysis
time and solvent consumption, limits the application of AF4 in
[1} the field of nanoparticle analysis .
A miniaturized AF4 channel was introduced for the rapid
analysis of different nanoparticle samples. UV-Vis-MALS
provides the possibility to measure the particle size and molar
mass and offers a powerful tool for the investigation of
[2] separation performances of different AF4 channels .
Our objective was to develop fast and reliable separation
methods for both channels and enable a direct comparison by
the corresponding chromatographic parameters.
The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP) using Asymmetrical Flow Field-Flow Fractionation (AF4) was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized. Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD) and limit of quantification (LOQ) obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis.
Das Recycling von Gipsabfällen wird schon seit einigen Jahren in unterschiedlichem Umfang in mehreren europäischen Ländern betrieben.Für die Verwertung der aufbereiteten RC-Gipse in der Gipsproduktion sind Qualitätsanforderungen festgelegt. Gipskartonplatten sind für die Herstellung von qualitativ hochwertigen RC-Gipsen besonders geeignet. Ein Forschungsprojekt im UFOPLAN des Umweltbundesamtes untersucht den aktuellen Stand des Gipsrecyclings in Deutschland und anderen europäischen Ländern und beleuchtet Hemmnisse und Maßnahmen zur Förderung des Gipsrecyclings in Deutschland. In einer umfassenden Ökobilanz wurden verschiedene Szenarien zur Gewinnung von RC-Gipsen bewertet. In dem Beitrag werden erste Ergebnisse dieses Projektes aufgezeigt.
In impact simulations, the instantaneous change of velocity in the contact area can lead to artificial oscillations. These oscillations might significantly influence the results, especially when nonlinear and rate dependent constitutive formulations are used.
In this work, a nonlinear penalty formulation similar to a soft contact formulation is presented.
Derzeitiger Stand von Wissenschaft und Technik:
Die Inspektion der Rotorblätter von Windenergieanlagen (WEA) erfolgt derzeit durch Sichtinspektion von außen und wenn möglich auch von innen. Das die Wartung ausführende Personal muss sich hierfür von der Gondel aus abseilen oder die Inspektion von einer speziellen Plattform aus durchführen. Dazu muss die WEA für die Dauer der Inspektion außer Betrieb gesetzt werden. Kleinere Schäden am Rotorblatt können sofort ausgebessert werden. In Deutschland ist ein zweijähriges Wartungsintervall vorgeschrieben.
Begründung/Zielsetzung der Untersuchung:
Das bisher angewandte Verfahren der individuellen Nahinspektion aller Rotorblätter lässt nicht ohne weiteres auf den Offshore-Bereich übertragen. Allein der notwendige Umstieg von einem Boot auf eine fest stehende Plattform bei geringem Wellengang von 1 m Wellenhöhe veranschaulicht die Schwierigkeiten. Weitere typische Probleme sind eingeschränkte Zugänglichkeit bei Schlechtwetterlagen, lange Anfahrtswege und das schlecht kalkulierbare Risiko der Seekrankheit. Es besteht daher Bedarf an neuen Inspektionsmethoden, bei denen die WEA nicht direkt begangen werden muss. Ein entsprechendes Verfahren könnte auch im onshore-Bereich eingesetzt werden, um Wartungsintervalle zu optimieren und Stillstandszeiten zu minimieren.
Methode:
Thermografische Verfahren sind berührungslos und werden bereits zur Rotorblattinspektion eingesetzt, allerdings nur während der Fertigung und dicht am Rotorblatt. Weiterhin ist bekannt, dass Thermografiekameras auch auf Hubschraubern eingesetzt werden, z.B. zur Personensuche. Im Rahmen des Projektes soll untersucht und evaluiert werden, ob Thermografie auf größere Entfernungen zur Untersuchung von Rotorblättern geeignet ist. Gemäß Projektplan sind vor allem Laboruntersuchungen an geeigneten Probekörpern sowie Außenmessungen an WEA geplant. Damit soll das Potenzial der thermografischen Ferninspektion von Rotorblättern evaluiert werden.
Ergebnis:
1. Die Untersuchungen an Rotorblattausschnitten mit verschiedenartigen Fehlern im Labormaßstab belegten die Eignung der Thermografie als zerstörungsfreie Prüfmethode für Rotorblätter.
2. Langzeituntersuchungen an einem Teilbereich eines Rotorblatts in einer Freiluftanordnung zeigten, dass messbare thermische Kontraste an inneren Strukturen oder an inneren Fehlern unter verschiedenartigen Wetterbedingungen entstehen können.
3. Bei Messungen an Rotorblättern im montierten Zustand, d.h. an einer intakten WEA, treten entsprechende thermische Kontraste ebenfalls auf. Allerdings ist die Nachweisbarkeit erschwert durch Reflexionen aus der Umwelt sowie durch Wind, der zu charakteristischen thermischen Streifenmustern auf den Rotorblättern führt. Bei Messungen an ruhenden Rotorblättern dominiert der erste Effekt, während der Wind kaum stört. Bei sich drehenden Rotorblättern ist die Situation umgekehrt, störende Reflexionen können korrigiert werden, aber der Wind beeinflusst die thermischen Kontraste beträchtlich, vor allem in nabenfernen Bereichen der Rotorblätter.
Schlussfolgerung/Anwendungsmöglichkeit:
Eine abschließende Evaluierung der Eignung der Thermografie als Ferninspektionsmethode für WEA-Rotorblätter konnte nicht vorgenommen werden. Ursache hierfür sind sowohl die vielfältigen Störfaktoren bei einer Freiluftmessung als auch das Fehlen einer geeigneten Referenzanlage, an der typische Rotorblattfehler und –defekte während des Betriebs systematisch beobachtet werden können. Die Schlussfolgerung ist daher, dass weitere Forschungsarbeit notwendig ist, um Möglichkeiten und Einsatzgrenzen einer thermografischen Ferninspektion angeben zu können.
Eine thermografische Rotorblattinspektion ist unter günstigen Witterungsbedingungen anwendbar und kann wahrscheinlich innere Defekte aufdecken, auch wenn der direkte Nachweis innerhalb des Projektes nicht geführt werden konnte. Wenn ein Rotorblatt-Thermogramm Auffälligkeiten aufweist, vor allem im Vergleich zu den beiden anderen Rotorblättern der gleichen Anlage, ist eine nähere Untersuchung der entsprechenden Stelle zu empfehlen. Das Auftreten solcher Kontraste, deren räumliche Ausdehnung und Ausprägung hängen jedoch von vielfältigen Faktoren ab und sind gemäß jetzigem Kenntnisstand noch nicht voll verstanden.
Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers.
Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories.
This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.
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 design concept, which is the state-of-the-art in European standards.
A solid database is needed for the determination of the partial safety factor on the resistance side. 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.
Mineralische Baustoffe werden aus Baurestmassen, industriellen Rückständen und Verbrennungsrückständen zurückgewonnen. Die Bundesanstalt für Materialforschung und -prüfung (BAM) und ihr Fachbereich Schadstofftransfer und Umwelttechnologien haben mit verschiedenen Partnern den Feinkornbereich fokussiert.
Multi residential buildings, developed as highly energy-efficient and airtight are nowadays often fitted with mechanical Ventilation Systems as a way to overcome shortcomings and even defects tinked to indoor climate. The presented study investigates the potential of low-emitting. natural building materials with hygroscopic properties to contribute to a healthy and comfortable indoor environment, while reducing the need for mechanical Ventilation.
A selection of natural building materials suitable for application as internal partition walls has been investigated with regards to their water vapour adsorption capacity.
Special emphasis was placed on the investigation of modified earth plasters as well as wood-based materials, used as wall lining to provide increased adsorption capacities.
In addition, tests on materials emissions (formaldehyde, VOCs, SVOCs and radon) as well as adsorption tests of airborne pollutants have been conducted in specially-designed fest chambers. All tests were performed at either the material or the component tevel.
Overall results to date suggest that natural materials contribute to an improved indoor environment quality through an increased moisture-buffering capacity, low emissions and the potential to adsorb airborne pollutants, therefore reducing the need for mechanical Ventilation.
Zinnober (HgS) ist neben Eisenoxiden (Fe2O3 oder FeOOH) das am häufigsten verwendete mineralische Rotpigment. Die relativ seltenen Vorkommen in der Natur wurden schon in der Vorgeschichte abgebaut und in Gräbern und auf Felsmalerei als rote Farbe verwendet. In Asien spielt Zinnoberrot als Schreibtusche eine wichtige Rolle. Besonders zur Zeit des Buddhismus findet sich das Rot verstärkt auch auf Wandmalerei und Statuen. Schon früh beherrschte man die synthetische Herstellung und Optimierung des Pigments mit Zusatzstoffen, so dass von einer regional unterschiedlichen Verarbeitung auszugehen ist. Auf Grund seiner physikalisch-chemischen Eigenschaften (gute Eindringtiefe, konservierende Wirkung) wurde das leuchtend rote Farbpigment auch als Handelsware genutzt.
Die Pigmentanalyse gibt Auskunft über
- kulturelle Vorkommen, die Nutzung von Zinnober als Rotpigment in einem bestimmten Kontext.
- natürliche Vorkommen, die Herkunft des Minerals entsprechend der regionalen Bildungsbedingungen.
- Werkstätten, die Herstellung als Farbpigment mit unterschiedlichen Techniken.
Vorgestellt werden rote Tinten und Tuschen auf Schriftstücken der Seidenstraßenkulturen mit Zinnober als charakteristisch für eine bestimmte Tradition in der Verwendung und möglicher Indikator für kulturellen Austausch. Die in unterschiedlichen Schriften und Sprachen erhaltenen Manuskriptfragmente gelangten Anfang des letzten Jahrhunderts von der Oasenstadt Turfan nach Berlin, wo sie entziffert und kulturhistorisch erforscht werden. Die chemische Zusammensetzung ihrer Rottöne wird differenziert und in Rückkopplung mit der historischen Klassifikation der untersuchten Objekte verglichen. Eine solche Identifizierung von Farbtypen kann zur Einordnung von Kulturobjekten fragwürdiger Herkunft herangezogen werden.
The objective of this study is to find out how far geochemical characteristics of the blue mineral pigment can be confirmed in respect to its provenance. In dependence of the quantity of samples analysed from a special geological region and the methods applied, a range of variation is taken into consideration. To provide clues, a multi-technique analytical approach with µXRF and ESEM is applied to samples from the most famous deposits.
Special elements determined as fingerprint are related to the textural features corresponding directly to the geological conditions of forming. The results and the statistical output allow a differentiation that enables an optimized local classification of the blue stone. To be aware of the limits of analysis is an absolute requirement for each geo-tracing implemented on blue coloured cultural objects of unknown provenance. For testing the possible sources of lapis lazuli, the blue pigment used as paint on murals and as ink on manuscripts from the Silk Road is analysed in an exemplary way.
Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials
(2016)
One current and much-debated topic in the characterization of nanomaterials (NM) is the implementation of the recently introduced recommendation on a definition of a nanomaterial by the European Commission.
All currently available sizing techniques able to address nanoparticles were systematically evaluated. It was demonstrated that particle sizing techniques like: analytical centrifugation, particle tracking analysis, single-particle inductively coupled plasma mass-spectrometry, differential electrical mobility analysis, dynamic light scattering, small angle X-ray scattering, ultrasonic attenuation spectrometry, but also gas Adsorption analysis based on the BET-method can be applied for a screening classification. However, the quality of the results depends on the individual material to be classified. For well-dispersed, nearly spherical (nano)particles most of the sizing techniques can be applied in a quick and reliable way. In contrast, the classification of most real-world materials is a challenging task, mainly due to non-spherical particle shape, large polydispersity or strong agglomeration/ aggregation of the particles. In the present study it was shown that these issues can be resolved in most cases by electron microscopy as a confirmatory classification technique.
Electron microscopy techniques such as TEM, STEM, SEM or TSEM transmission in SEM) are capable of assessing the size of individual nanoparticles accurately (see Figures 1 and 2). Nevertheless the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after its simple, dry preparation. The consequences of additional typical issues like loss of information due to Screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed.
Aluminium is still one of the most important contact metallisations for power electronic chips like MOSFETs or IGBTs. With a large difference in thermal expansion coefficients (CTEs) between aluminium and silicon and the temperatures generated in hot-spots during high power transients, these layers are prone to failure due to thermo-mechanical fatigue. Usually lifetime assessment is done by subjecting dedicated test specimens to standardised stress tests as e.g. active or passive thermal cycling. This paper proposes a novel method for accelerated stress testing and lifetime modelling of thin aluminium films in the high-cycle fatigue regime by isothermal mechanical loading. The proposed novel test method is suggested to complement or replace resource-demanding thermal cycling tests and allow simple in-situ monitoring of failure.
Der vorliegende Fachartikel stellt die wichtigsten zerstörungsfreien Prüfmethoden zur Qualitätssicherung von dünnen Strukturklebungen vor. Auf diese Weise wird ersichtlich, welche Methoden neben der zerstörenden Prüfung von dünnen Strukturklebungen eingesetzt werden können, um einen Haftfestigkeitsverlust zu detektieren. Steigende Leichtbau- und Dämpfungsanforderungen an großflächige Blechbauteile sorgen trotz erhöhter Kosten für einen zunehmenden Einsatz von modernen hybriden Schichtverbundwerkstoffen in zahlreichen Konstruktionsanwendungen. In der Luft- und Raumfahrtindustrie gehören solche Werkstoffe seit geraumer Zeit zum aktuellen Stand der Technik, wohingegen diese Werkstoffkonzepte in der mobilen Großserie derzeit nur selten zum Einsatz kommen. Neben dem Materialversagen der einzelnen Schichten von Schichtverbundwerkstoffen spielt das interlaminare Versagen der Schichten untereinander eine entscheidende Rolle. In der Umformtechnik ist es möglich, dass die polymere Zwischenschicht und das Deckblech nach der Umformung noch in Kontakt stehen, obwohl die Scherfestigkeit bereits überschritten wurde. Dieser Kraftschluss der beiden Fügepartner resultiert aus den schwachen Van-der-Waals-Kräften, die eine eindeutige Detektion mit Hilfe von zerstörungsfreier Prüfung erschweren. Die vorliegende Publikation soll die Eignung diverser zerstörungsfreier Prüfverfahren auf die Detektion von sogenannten „kissing bonds“ (schwaches Anhaften der Schichten nach Versagen der Verbindung) überprüfen.
Focus of this work is the detection of vertical movements behind the casing of groundwater observation wells within the seal. A new multi-methodical and azimuthal logging tool, named Azimuthal-Annulus-Convection-Identification (AACI)-Log has been developed and tested. The measurement concept of this probe is based on the combination of three azimuthal measuring logs – contact temperature on the inside of the casing wall, backscattered gamma-rays (gamma-gamma density), and natural radioactivity (gamma ray). Consequently, a direction-oriented image of the annular space can be derived. Not only the reason (void, potential channel) but also the resulting effect (vertical movement of fluids) can be detected with the Azimuthal-Annulus-Convection (AACI) – Log at the same time.
Within the TF-project SiVi the BAM occupies itself interdisciplinary with the safety of traffic infrastructures considering extremely severe damage events. Therefore, a scenario of fire inside a traffic tunnel induced by a gas cloud explosion is chosen as representative. Additionally, a dangerous goods transporter shall be involved in the scenario.
As further aspect which shall be investigated is the use of liquefied natural gas (LNG) as fuel support in transport vehicle like trucks in future. The main component of LNG is methane as a flammable gas. To transport a sufficient amount of fuel the methane is cooled down at -161°C, its boiling point. In liquid phase LNG is compressed 600 times more than in gas phase.
The issue of department 2.4 is to identify the hazards for people and the tunnel structure located in the surrounding whilst a potential release of LNG out of a leaking tank occurs. Therefore, the temporal and spatial distribution of the gas cloud within the tunnel structure shall be recorded.
Basis for this will be experiments in 1:1 at BAM test rig TTS as well as numerical analysis within ANSYS CFX. On top ignition tests of the distributed gas cloud in a down scaled model allow statements on the emerging maximum pressure and temperature.
Influence of the of dealumination and porosity on the acid sites of natural zeolite clinoptilolite
(2016)
Heavy feedstock from crude and bio oil is a widely available and renewable resource for production of fuel and starting materials for other organic valuables by cracking or hydrocracking. Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent.
The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Clinoptilolite has a crystalline structure with a defined micropore system of medium size showing unique ion exchange and sorption properties. However, it is catalytically active only in the H-form. Also certain porosity is required for improvement of the accessibility of active sites.
This paper deals with the tuning of acid properties and of the mesoporosity of the clinoptilolite by variation of the Si/Al framework ratio, extra-framework aluminum and modification of the porosity by specific acid and water vapor treatment. The preparation of hierarchical pore structures containing interconnected micro-meso-macropores is an important factor influencing the catalytic performance.
The obtained materials have been characterized by XRD, TEM, FTIR, Raman, TG/DSC. The chemical composition has been determined by ICP-AES. The porosity have been investigated by nitrogen adsorption desorption measurements. The acidity has been measured by Ammonia-TPD. The extent of dealumination, stability of the clinoptilolite against acid treatment and the change in the nature of acid sites and their local structure has been studied by solid state 29Si and 27Al MAS NMR spectroscopy in detail. The catalytic activity has been investigated in the acetalization of benzaldehyde with 1,3-butanediol. The impact of the porosity, change of the Si/Al ratio as well as present Al species on catalytic properties will be discussed.
Das Poster stellt ein Konzept zur Bewertung der strukturellen Integrität von havarierten Tankbehältern vor. Es wurde ein dehnungsbasiertes Konzept eingeführt, welches einen Brückenschlag zwischen duktiler Schädigung und dem Integritätszustand des Behälters herstellt. Diese Thematik entspringt aus einem Kooperationsvorhaben der Organisationseinheiten 5.2 und 3.2.
Multiply negatively charged DNA oligonucleotides of small sizes (n=15-40 bases) have been subjected to a comprehensive tandem mass spectrometric study (MS/MS). Collision induced dissociation (CID) mass spectrometry (MS) was applied as a tool to break down isolated DNA oligonucleotides with a defined number of charges. Various lenghts and sequences were analyzed unravelling a comparable direct correlation between the threshold collision energy for fragmentation and the charge-per-base density in the precusor ion. It was also revealed that the increase in charges and thus Coulomb repulsion results in the transition from a folded, compact form to an elongated structure of the precusor ions.
Multiply negatively charged DNA oligonucleotides of small sizes (n=15-40) have been subjected to a comprehensive tandem mass spectrometric study (MS/MS). Collision induced dissociation (CID) mass spectrometry (MS) was applied as a tool to break down isolated DNA oligonucleotides with a defined number of charges. Various lenghts and sequences were analyzed and all of them showed a comparable direct correlation regarding the threshold collision energy for fragmentation and dependence on number of charges on the precursor ions. It was also revealed that the increase in charges and thus Coulomb repulsion results in the transition from a folded, compact form to an elongated structure of the precursor ions.
Dark-field Transmission electron microscopy (DFTEM) results were obtained and presented. The results are discussed with regard to additional microstructural characterisation of the primyra Phase and creep experiments of alloy 2618A. Different methods to determine the volume fractions of precipitate phases are presented.
Dislocations, as carriers of plastic deformation, affect important properties in technical materials, e. g., plasticity. The realistic description of plastic deformation caused by dislocations demands the representative measurement of their features, e.g., line direction, slip plane, Burgers vector and density. Bulk deformation of structural and functional alloys requires reliable data from large regions. The filiform nature of dislocations interacting with complex microstructures additionally demands observation and analysis techniques that allow resolving the details of their interactions in space. The use of electron tomography for this purpose is bound to difficult and time consuming experimental setups, which are not always applicable to any material. In this contribution a new tool is presented, which enables the three-dimensional reconstruction, visualization and quantification of dislocation densities and directions from manual tracing of scanning transmission electron microscopy (STEM) stereo-pairs. Examples are shown from samples of a creep-deformed monocrystalline Ni-base superalloy.
Die Anwendung thermoanalytischer Methoden für die Polymercharakterisierung hat aufgrund der makromolekularen Struktur von Polymere Vorteile. Es wurden zwei neue thermoanalyti-sche Verfahren entwickelt und deren Einsatz anhand von Anendungsbeispielen demons-triert, sowie mit etablierten, thermoanalytischen Methoden verglichen.
Für die thermische- und thermo-oxidative Zersetzungsgasanalytik wurde die Thermogravi-metrie (TGA) gekoppelt mit der Thermodesoptions-Gaschromatographie-Massenspektrometrie (TDS-GC-MS). Die Zersetzungsgase der TGA wurden dafür über ei-nen Festphasenadsorber geleitet, auf dem eine repräsentative Auswahl von polymerspezifi-schen Analyten adsorbiert wurde. Die thermische Extraktion der Analyten erfolgte in der TDS-GC-MS. Dies ermöglichte die Trennung der Analyten sowie die eindeutige Identifizie-rung mittels charakteristischer Massenfragmentmuster. Sie wurde als TED-GC-MS bezeichnet. Es stellte sich heraus, dass sie sich besonders für die Analyse von komplexen Kohlen-wasserstoffgemischen mit Molmassen von mehr als 100 g/mol eignet. In Kombination mit anderen Kopplungstechniken wie beispielsweise die TGA-FTIR/MS, die speziell für die Ana-lyse von kleineren Molekülen verwendet wurde, konnten neue grundlegende Zersetzungs-mechanismen entwickelt werden. Es wurde beispielsweise sichtbar, dass sowohl bei der thermischen als auch bei der thermo-oxidativen Degradation von Polyamid 66 (PA 66) Kon-densationsreaktionen eine wichtige Rolle spielen. Die Methode erwies sich darüber hinaus als besonders geeignet für die Identifizierung und Quantifizierung von Polymeren in Umweltproben. Es entstand dazu eine erste grundlegende Arbeit für die quantitative Bestimmung von Polyethylen (PE) Mikroplastik in Umweltproben.
Im zweiten Teil der Arbeit wurde eine steuerbare beheizbare Zelle eingeführt. Mit ihr war es möglich, mit Hilfe der Nahinfrarotspektroskopie (NIR), sich verändernde Netzwerkstrukturen während der Härtung sichtbar zu machen. Vergleichend dazu wurden etablierte, kalorische Messungen durchgeführt. Somit konnten für verschiedene Epoxidsysteme die Aushärtegrade während der Härtung mit variablen Heizraten bestimmt werden. Dadurch konnten Aushär-tungskinetiken erstellt werden, die durch isotherme und komplexe Aushärtungsszenarien validiert wurden.
Evaluation of nano-sized internal oxidation in a Fe-13Cr alloy exposed to water vapor atmosphere
(2016)
The topotactic formation of nano-sized precipitates immediately under the internal oxide layer in a Fe-13Cr alloy exposed to oxidizing water vapor atmosphere was recently reported. The precipitates were identified as lath-shaped Fe-Cr spinel exhibiting a crystallographic orientation relationship with the ferritic matrix. The authors proposed that these precipitates could act as a precursor to the formation of the spinel layer observed in the adjacent part of the oxide scale.The occurrence of internal oxidation in Fe–Cr alloys subjected to similar conditions had been previously identified and directly correlated to the presence of water vapor. In the present work, we attempt to rationalize the processes occurring during the oxidation of this alloy through thermodynamic and kinetic analyses based on the CALPHAD approach, using the geometrical representation of phase equilibria and concepts developed to describe internal oxidation. The influence of water vapor on the mechanism and kinetics of formation of the nano-sized precipitates and its role in the overall oxidation process is also considered.
Visualization of surface modifications may be very challenging for coating/substrate systems of either almost identical optical constants, e.g. transparent films on substrates of the same material, or minor film thickness, substance quantity and affected area, e.g. ultra-thin or island films. Methods for visualization are optical microscopy (OM), imaging ellipsometry (IE), and referenced spectroscopic ellipsometry (RSE). Imaging ellipsometry operates at oblique incidence near Brewster angle of the bare, clean or unmodified substrate. In this configuration, reflected intensities are rather weak. However, the contrast to add-on and sub-off features may be superior. Referenced spectroscopic ellipsometry operates in a two-sample configuration but with much higher intensities. In many cases, both ellipsometric techniques reveal and visualize thin films, printed-pattern, laser-induced changes, and impurities better than optical microscopy. In particular for stratified homogeneous modifications, ellipsometric techniques give access to modelling and hence thickness determination. Modifications under investigation are polymer foil residue on silicon, laser-induced changes of ta-C:H coatings on 100Cr6 steel, imperfections of ta-C:H on thermal silicon oxide, degradation of glass, thin film tin oxide pattern on silicon, printed and dried pattern of liquids such as deionized water, cleaning agents, and dissolved silicone. © 2016 Elsevier B.V. All rights reserved.
On April 23rd 2013 at 2:07 a.m., a 1.3 kg meteorite fell in the Braunschweig suburb Melverode (52° 13′ 32.19″ N. 10° 31′ 11.60″ E). Its estimated velocity was 250 km/h and it formed an impact pit in the concrete fall site with a diameter of 7 cm and a depth of 3 cm. Radial dust striae are present around the impact pit. As a result of the impact, the meteorite disintegrated into several hundred fragments with masses up to 214 g. The meteorite is a typical L6 chondrite, moderately shocked (S4) – but with a remarkably high porosity (up to 20 vol%). The meteorite was ejected from its parent body as an object with a radius of about 10–15 cm (15–50 kg). The U,Th-He gas retention age of ∼550 Ma overlaps with the main impact event on the L-chondrite parent body ∼470 Ma ago that is recorded by many shocked L chondrites. The preferred cosmic-ray exposure age derived from production of radionuclides and noble gas isotopes is (6.0 ± 1.3) Ma.
The LEK94 is a Ni-base superalloy single crystal (SX) of the second generation, a materials class which is important for its high temperature creep resistance (>1000°C) in first stage blades of low-to-medium pressure gas turbines. Monocrystalline Ni-base superalloy SXs have a two-phase microstructure consisting of small cubes (' phase with the ordered L12 crystal structure, cube edge length: 500 nm), separated by thin channels (γ phase with fcc solid solution structure, channel width: 20 nm). The microstructural evolution during high temperature and low stress tensile creep has been thoroughly investigated previously, mainly for [001] loading, both in terms of dislocation activity (filling of γ channels, formation of dislocation networks, cutting of the γ’ phase) as well as phase coarsening (rafting, topological inversion). Other loading geometries have received less attention.
The present work studies high temperature and low stress creep deformation of the superalloy LEK 94 at temperatures around 1000°C, where rafting occurs. Differences between loading under different uniaxial, biaxial and triaxial stress states are discussed. Stereo-microscopy and g∙b analysis in the scanning transmission electron microscopy mode (STEM) are combined for microstructural analysis. The focus is set on the role of dislocation interactions with the aging microstructure. Both development in STEM characterization methods, as well as the roles of phase coarsening, γ channel filling, microstructural heterogeneity and γ’ phase cutting are discussed.
Entwicklung eines Verfahrens zur Untersuchung der Heißrissresistenz lasergeschweißter Verbindungen
(2016)
In den letzten Jahrzehnten hat sich die Strahlschweißtechnik signifikant weiterentwickelt und als effizientes und wirtschaftliches Werkzeug in der Industrie etabliert. Für die Untersuchung der Heißrissresistenz verschiedener Werkstoffe existieren zahlreiche eigen- und fremdbeanspruchende Tests. Diese wurden aber speziell für andere Schweißverfahren, insbesondere das Lichtbogenschweißen, konzipiert.
Daher besteht die Notwendigkeit eines geeigneten Heißrisstests, bei dem Werkstoffe realen Strahlschweißbedingungen ausgesetzt werden können. Die Entwicklung sowie die Standardisierung einer aussagekräftigen experimentellen Methode stellen einen wichtigen Schritt auf dem Weg zur Vermeidung von Heißrissen und damit für die Gewährleistung der Sicherheit von gefügten Bauteilen dar. Ziel der Forschungsarbeiten ist es, einen geeigneten Test zur effektiven Untersuchung der Heißrissanfälligkeit von lasergeschweißten Verbindungen zu konzipieren und zu entwickeln.
ISO 10156:2010 contains a test method and a calculation method for flammability of gases and gas mixtures for the selection of cylinder valve outlets. The calculation method is used also to classify gas mixtures according to the national and international dangerous goods and dangerous substances regulations, e.g. according to the UN Recommendations on the Transport of Dangerous Goods (UN TDG) and the Globally Harmonized System of Classification and Labelling of Chemicals (UN GHS). The calculation method for gas mixtures requires substance parameters of the single components. These are the coefficients for the fire potential (Tci) and for inerting ability, the so-called nitrogen equivalence (Kk), which have been estimated conservatively by means of flammability data.
BAM checked Tci and Kk values of ISO 10156:1996 using three-component diagrams (Flammable gas-Inert-Air) of the CHEMSAFE® database. The experimental fundamentals and the principles of the calculation method are summarized in this paper. The revised data for Tci and Kk values were adopted in the tables of ISO 10156:2010.
Furthermore, subcategorization of flammable gases has been proposed by a UN working group and shall be implemented in the GHS in the meantime. The subcategorization requires the lower flammability limit (LFL) as an additional indicator. Therefore, a test method and a calculation method for LFL were proposed by BAM and have been implemented in the new draft of ISO/CD 10156:2016.
The calculation method for gas mixtures is based on Le Chatelier’s rule and was extended by using the Kk values for inert components in the mixture. The calculated LFLs of methane-inert gas mixtures were compared with experimental values for different types of inert gases. It could be shown that calculated LFLs are in good agreement with experimental values if the Kk values derived from three-component flammability diagrams are used. Although using the Kk values of ISO 10156:2010 leads to higher deviations, the results are still on the safe side.
Complex materials (e.g., porous ceramics) need high resolution techniques at multi-scale levels. Microstructure is intimately linked to properties and performance. One technique (or even a few techniques) is not enough. X-ray refraction and CT are very powerful tools. Non-destructive characterisation and quantitative image analysis techniques (2D and 3D) are necessary to understand the anisotropy.
Projektbeschreibung:
Das übergeordnete Ziel des Projekts ist es, ein Werkzeug bereitzustellen, mit dem die Arbeitsweise von Akkreditierungsstellen auf objektiver Grundlage und kennzahlenbasiert analysiert werden kann. Durch Anwendung auf mehrere Akkreditierungsstellen soll zudem eine vergleichende Analyse verschiedener Akkreditierungsstellen ermöglicht werden, die zur Harmonisierung der Arbeitsweise der Akkreditierungsstellen in Europa beiträgt. Mit zunehmender Harmonisierung entsteht zusätzliches Vertrauen in das europäische Konformitätsbewertungssystem.
Das Projekt umfasst vier Phasen. In der ersten Phase des Projekts werden die Tätigkeiten von Akkreditierungsstellen und ihre auf gesetzlichen und normativen Anforderungen beruhenden Verpflichtungen systematisch analysiert. Es wird eine mit Kennzahlen unterlegte Prozesslandschaft entwickelt, die ein Modell bildet, dem die implementierten Abläufe und eingesetzten Ressourcen der Akkreditierungsstelle zugeordnet werden können.
In der zweiten Phase werden die Prozesse der Deutschen Akkreditierungsstelle DAkkS dem Modell zugeordnet. Dabei werden mit Hilfe der DAkkS internen Datenbank Kennzahlen und Indikatoren erhoben. Die Übertragbarkeit des so erstandenen Modells wird in einem dritten Schritt durch die Erweiterung auf weitere Akkreditierungsstellen im europäischen Raum untersucht. In der vierten Phase wird die Analyse auf weitere europäische Akkreditierungsstellen ausgeweitet.
Projektbeschreibung:
Das übergeordnete Ziel des Projekts ist es, ein Werkzeug bereitzustellen, mit dem die Arbeitsweise von Akkreditierungsstellen auf objektiver Grundlage und kennzahlenbasiert analysiert werden kann. Durch Anwendung auf mehrere Akkreditierungsstellen soll zudem eine vergleichende Analyse verschiedener Akkreditierungsstellen ermöglicht werden, die zur Harmonisierung der Arbeitsweise der Akkreditierungsstellen in Europa beiträgt. Mit zunehmender Harmonisierung entsteht zusätzliches Vertrauen in das europäische Konformitätsbewertungssystem.
Das Projekt umfasst vier Phasen. In der ersten Phase des Projekts werden die Tätigkeiten von Akkreditierungsstellen und ihre auf gesetzlichen und normativen Anforderungen beruhenden Verpflichtungen systematisch analysiert. Es wird eine mit Kennzahlen unterlegte Prozesslandschaft entwickelt, die ein Modell bildet, dem die implementierten Abläufe und eingesetzten Ressourcen der Akkreditierungsstelle zugeordnet werden können.
In der zweiten Phase werden die Prozesse der Deutschen Akkreditierungsstelle DAkkS dem Modell zugeordnet. Dabei werden mit Hilfe der DAkkS internen Datenbank Kennzahlen und Indikatoren erhoben. Die Übertragbarkeit des so erstandenen Modells wird in einem dritten Schritt durch die Erweiterung auf weitere Akkreditierungsstellen im europäischen Raum untersucht. In der vierten Phase wird die Analyse auf weitere europäische Akkreditierungsstellen ausgeweitet.
The manuscript of the History of Outremer by William of Tyre stored at the BNF (ms. fr. 9084) is believed to have been illustrated by two different hands. Indeed, the first five miniatures of this manuscript appear to be very different from the last seventeen, which were supposedly painted by an artist known as the "Hospitaller Master". This painter worked on at least two manuscripts in Paris between 1276 and 1280, and eight more in Saint Jean d'Acre before 1291. During his stay in the Latin Kingdom of Jerusalem, his palette changed and reached its most important development in the Manuscript of the History of Outremer, maybe influenced by the colourful crusader style of the first five miniatures. The present work aims at identifying the pigments used on both parts of the manuscripts and see whether they are the same for both artists or not. For that, portable XRF analysis was used directly at the Bibliothèque National de France in Paris, where the manuscript is stored. This allowed a quick, non destructive and non invasive study of the manuscript. Significant differences were observed in the compositions of some pigments indeed, in particular for the red and green, showing the use of different palettes. This could indicate that the Hospitaller Master not only brought his knowledge and style, but also probably part of his palette of pigments with him when moving to Saint Jean d'Acre.
Quantification of microbial load in diesel storage tanks using culture- and qPCR-based approaches
(2016)
Microbial contamination of fuels, associated with a wide variety of bacteria and fungi, leads to decreased product quality and can compromise equipment performance by biofouling and microbiologically influenced corrosion of pipelines and storage tanks. Detection and quantification of biomass are critical in monitoring fuel systems for an early detection of microbial outbreaks. The aims of this study are (i) to quantify bacterial and fungal contamination in samples from diesel storage tanks of petrol stations, using both culture dependent- and culture independent (qPCR) approaches, and (ii) to analyse the diversity of cultivable diesel-contaminating microorganisms with the purpose to create a strain collection for further use in biodeterioration experiments. Both methodological approaches revealed a high microbial contamination in all studied samples, with the bacterial load being much higher than the fungal load. The diversity of cultivable microorganisms was rather low. Based on criteria of abundance and fuel degradation potential, the most relevant microorganisms were identified as bacteria of genera Bacillus, Citrobacter, Burkholderia and Acetobacter, the filamentous fungi Paecilomyces variotii and Pseudallescheria boydii, and a Dipodascaceae yeast. Furthermore the validity and utility of qPCR-based methods are discussed.
The Bundesanstalt für Materialforschung und -prüfung (BAM) in Germany has gathered extensive expertise over decades in the fields of design testing and safety assessment of transport and storage containers for radioactive materials. On behalf of the German commission for the disposal of highly radioactive waste, BAM had been assigned the elucidation of requirements for high level waste disposal containers specifically in terms of their retrievability from deep geological formations during repository operation and recovery after its closure over a period of time between 500 to 1000 years. The output of the initial assessment is presented taking into account the frame of the current German repository site selection procedure together with the definition of repository conditions corresponding to the potential deep geological formations to be considered for disposal.
This presentation addresses the spectrum of relevant stress factors for disposal containers and reflects their relevance and consequences during the repository operation phase including the emplacement and their potential retrieval. In addition, further aspects and consequences for container recovery after repository closure are discussed taking into consideration potential repository conditions of different geological formations.
Finally, potential disposal container concepts are briefly addressed comparing the consequences of an improvement of existing dual purpose casks versus completely new disposal canister designs adjusted to the specific geological conditions of the host rock formation. Pros and cons of these two concepts are depicted in order to address major challenges. However, precise container design concepts cannot be consolidated before repository conditions and derived specific container requirements are designated.
The presentation explains the requirements, process and challenges of the container design testing procedures for the Konrad repository, where low and intermediate level radioactive waste is planned to be disposed of beginnung end of 2022. BAM performs container design testing for more than 30 years whether analytically or experimentally. The challenges of the complex Konrad requirements concerning their proper interpretation and application is discussed in this presentation.
In order to reduce CO2 emission in concrete and minimize the environmental impact, majority of research focuses on using supplementary cementitious materials (SCMs) such as Fly Ash (FA), blast furnace slag (GGBS) and Silica Fume (SF) or Microsilica as a replacement for ordinary Portland cement in concrete. However, in terms of sustainability, it is not economically feasible to use the above mentioned SCMs in countries where these materials are not readily available. In addition, when dealing with the carbon footprint of concrete, despite their positive influence in concrete, such SCMs cannot be said to be eco-friendly materials due to their high energy production process. In many developing countries in sub-Saharan Africa (SSA), agriculture is the leading economic sector. Generally, agricultural by-products are eco-friendly in terms of low energy in production, and they often have no further use for the environment. These by-products (baggase, cassava peels and rice husks) are mainly not the materials of discussion in this current day and age and especially in the northern hemisphere, where the majority of concrete technology originates. Hence, it is inevitable to consider other more sustainable resources in concrete for SSA. Nevertheless, optimization of these resources in concrete can only function with a clear understanding of the reactivity of the materials and its interaction and mechanism to adopt similar and workable properties as a normal performance cementitious system.
This paper addresses rice husk ash (RHA) as a main SCM in various cementitious systems with added limestone filler (LSF) and observes its performance in mortar. Superplasticizers such as polycarboxylate-ethers (PCEs) and lignosulphonates (LS) are incorporated in the cementitious systems to improve workability. The interaction of RHA with the superplasticizers was investigated by means of zeta potential (ZP). According to the results presented, it is shown that RHA powder has a positive compatibility with the chosen superplasticizers and its performance in mortar with LSF also shows increase in strength and workability.
The main objective of this project presentation was to evaluate the by-products of paddy farming (in Tanzania) into sustainable building materials optimised for construction of low-cost housing, and suitable to be adopted in rice-producing countries in Africa. In Tanzania, rice husks are seldom used as a fuel – if not burnt or dumped in landfills and there is lack of awareness or active research on optimising the by-product RHA in cement and concrete technology. Scientific research within this field of technology can advance development by obtaining suitable properties of the by-products that can provide an advantageous and alternative measure for their use as SCMs not only in its raw form i.e. husks for low-cost housing but also in its artificial form i.e. RHA as a high-tech as a substitute for cement in Africa.
There is a wide range of research worldwide on supplementary cementitious materials (SCMs) such as fly ash and slag for substituting Portland cement. Such materials are suitable to be considered in a cementitious system with ordinary Portland cement (OPC) due to their high pozzolanic properties. In addition, many of the SCMs are said to significantly improve concrete properties especially in terms of strength and durability. Unfortunately, the production of such SCMs is not entirely eco-friendly and also limited to certain parts of the world, hence one has to look at alternative options.
The issue of availability of resources is a strong concept that is ever-increasing, and the use of more eco-friendly SCMs in a cementitious system is furthermore attractive. Hence this paper addresses the use of eco-friendly SCMs in concrete such as rice husk ash (RHA). Despite the fact that extensive research has been done on this material, its application in a cementitious system to obtain sufficient concrete properties is still rather limited.
In a country like Tanzania, high strength concrete construction is applicable in special construction cases but certainly not a high priority. Majority of construction is still undertaken using normal strength concrete. In a ternary cementitious system consisting of OPC, RHA and other readily available resources such as limestone filler (LSF), normal strength concrete can still be produced having good performance and suitable for regular on-site construction. This paper explains a possible application of obtaining sufficient concrete properties from the available resources.
Control chart systems are used in quality management systems to keep production processes stable. In concrete production they are often applied for the control of the compressive strength. The most efficient control chart systems are cumulated sums (cusum), which help to observe deviations from a targeted value. Unlike alternative observation chart systems that focus on process data evaluation, cusum observations react very rapidly on systematic process changes in processes. Therefore, the cusum method is particularly suitable if immediate counteractions have to be taken, like in the case of fresh concrete properties of self-compacting concrete (SCC), which can have severe influences on the durability and mechanical strength of concrete. The rheology of SCC can be affected by an enormous variety of influencing factors, from raw material properties to handling or environmental temperature. The present study shows that regardless of the material based influencing parameter for a rheology change, a steady slump flow can be achieved only by adding supplementary superplasticizer in case of loss of flow and adding stabilising agent (ST) in case of increased flow if the respective V-mask indicates a systematic change. A reference SCC was artificially manipulated in order to achieve realistic experimental data for flowability and flowability changes due to changes in the raw material properties. The results point out that productions with applied cusum methods were capable of keeping the target slump flow deviation within approximately 1% only, while productions without applied cusum method deviated up to 14% and more from the target.
Today, concrete engineers can vary consistencies between very stiff and self-compacting. The possibility to tailor rheological properties of concrete eventually opened up the path to multiple new technologies, where design criteria are no longer limited to the Young’s modulus and the compressive strength, but often comprise additional added value. It can therefore be concluded that the capability to control the rheology of concrete systems can be considered as the catalyst for concrete innovations such as polymer modified cementitious composites (PCC) self-compacting concrete (SCC), high-performance concrete (HPC), ultra-high performance concrete (UHPC) or strain hardening cement based composites (SHCC). In the same way rheology modifying admixtures will become key parameters in mastering the challenges of the next decades such as:
- Additive manufacturing/3D-printing
- Overcoming pumping height limitations
- Casting at extreme temperatures
- Tailored rheology at delivery
In many regions in the Southern hemisphere, and particularly in Africa, the effective use of chemical admixtures for concrete could significantly contribute to solve problems induced by the challenging climatic conditions, but particularly in Africa it is difficult to use them, due to lacking local supply and supply infrastructure. For Africa, concrete admixtures are largely shipped or transported from Europe, the Arabian Peninsula, or Asia. The long distance transportation of chemicals is not very environmentally friendly and the economic consequences are dramatic: the agents are difficult to purchase, expensive, and there is not a large variety of products available in the market.
However, bio-based chemicals have been used in construction for ages effectively. Due to the enormous relevance of rheology modifying admixtures it is worthwhile to recollect that nature provides an enormous variety of chemicals that can be used readily or with low processing. Today, the use of petrol based polycarboxylate ether superplasticizers has become quite common in concrete technology due to their versatility, but their uncomplicated and cost efficient availability is limited in most countries in Africa. However, alternatives are available, which can be found in many regions.
Plant extracts have been used to modify the properties of concrete for long time. These plants are typically regionally abundantly available, cheap, and they are environmental friendly. They do not require special caring for seedlings, weeding or manuring to grow since they grow wildly.
The talk will present an overview of various options for rheology modifying admixtures, that can be found in nature, and that may become a real alternative, once their interaction within the complex cementitious system is well understood.
Why Africa can spearhead innovative and sustainable cement and concrete technologies globally
(2016)
The perception of concrete in the society as well as in the politics is rather negative. This becomes obvious in the fact that the phrase “concrete jungle” has become synonym for hapless living with no perspectives. In politics and research funding, it is also not easy to create a broader audience, since concrete is falsely considered as old-fashioned material that is sufficiently understood today and does not need further considerations, particularly compared to allegedly newer materials. However, particularly since the last two decades the technology has completely changed. Binders of today are no more the same binders as used before, and concrete mixture compositions of today diverge quite significantly from compositions in the past. There is little understanding world-wide about that. This causes that potentials the concrete technology bears are wasted.
In the broadly found opinion that concrete is old-fashioned and ugly, it is ignored that architectural sins are not inherent to the material, which actually is extremely versatile and CO2-friendly compared to all other construction materials available. It is also ignored that 98% of the outer Earth’s crust are made of the elements cement and concrete are made from, and therefore it will be an illusion to believe that the complementary 2% can create materials to develop regions and infrastructures in less developed areas in the world.
For betterment in Africa the infrastructural development should have highest priority, since poor connections between settlements are responsible for enormous Price increases [2], and urban traffic congestion is responsible for an incredible loss of productivity. It is not unrealistic to assume that earners that are dependent on a car get stuck in traffic about 3-4 hours per day in cities like Lagos, Nairobi or Dar es Salaam. However, the traffic congestions do not only affect the car owners negatively but the living of the entire urban population every day.
Besides infrastructure, housing should be the other priority, since a large part of the African population does not live in adequate condition. This is a societal problem, since unequal Distribution of wealth is a major driving force for instability in societies. The latter has a global impact, since 8 many phenomena that can be observed all over the world such as political radicalism, xenophobia, terrorism, and migration can often be linked to instable societies.
However, the importance of infrastructure has an even wider range. Most African countries go through a change process recently. In order to strengthen very positive perspectives, the focus in politics and research funding is put on issues such as agriculture, energy, and health, which are without doubt extremely important issues. However, it is typically overlooked that all enhancements in these areas can only become effective, when an infrastructure is created to support the implementation of better concepts. Mobility is the key to a prosperous future, and mobility can only be granted by infrastructural construction activities. Hence, compared to many other regions in the world, cement and concrete technologies have a significantly higher relevance in Africa.
Im Testgelände Technische Sicherheit (TTS) verfügt die BAM über eine umfangreiche prüftechnische Infrastruktur für die mechanische und thermische Behälterbauartprüfung unterschiedlicher Behälterdesigns und -komponenten. Berichtet wird über Erprobungsprogramme und prüfmethodische Untersuchungen mit originalgroßen Prüfmustern von Transportverpackungen und Lagercontainer sowie Komponentenuntersuchungen unter Impaktbelastung. Im Großkomponentenversuch werden mit einem Prüfmuster eines Transportbehälters charakteristische Unfallbeförderungsbedingungen simuliert, dabei die Verformungen der Stoßdämpferkomponenten sowie die resultierenden maximalen Starrkörper-Verzögerungen ermittelt und analysiert. Ferner wird über das mechanische und thermische Beanspruchungsverhalten einer Umverpackung für den Transport von UF6- Zylindern im Ergebnis umfangreicher Fallsequenzen sowie einer Brandprüfung berichtet. Im Rahmen der Behälterentwicklung für den Standort Sellafield wurden mit einem dickwandigen Container für radioaktive Abfälle Fallprüfungen auf das unnachgiebige Fundament und eine Brandprüfung durchgeführt. Detaillierte Belastungsanalysen erfolgten an stoßdämpfenden Bauteilen und Materialien im Rahmen der angewandten Sicherheitsforschung.
Most microorganisms live in environments where nutrients are limited and fluctuate over time. Cells respond to nutrient fluctuations by sensing and adapting their physiological state. Recent studies suggest phenotypic heterogeneity in isogenic populations as an alternative strategy in fluctuating environments, where a subpopulation of cells express a function that allows growth under conditions that might arise in the future. It is unknown how environmental factors such as nutrient limitation shape phenotypic heterogeneity in metabolism and whether this allows cells to respond to nutrient fluctuations. Here, we show that substrate limitation increases phenotypic heterogeneity in metabolism, and this heterogeneity allows cells to cope with substrate fluctuations. We subjected the N2-fixing bacterium Klebsiella oxytoca to different levels of substrate limitation and substrate shifts, and obtained time-resolved single-cell measurements of metabolic activities using nanometre-scale secondary ion mass spectrometry (NanoSIMS). We found that the level of NH4+ limitation shapes phenotypic heterogeneity in N2 fixation. In turn, the N2 fixation rate of single cells during NH4+ limitation correlates positively with their growth rate after a shift to NH4+ depletion, experimentally demonstrating the benefit of heterogeneity. The results indicate that phenotypic heterogeneity is a general solution to two important ecological challenges - nutrient limitation and fluctuations - that many microorganisms face. Currently, we use NanoSIMS to develop a new approach that defines functionally-relevant, phenotypic biodiversity in microbial systems. In the last part of my presentation, I will highlight why the concept of phenotypic diversity is relevant for the understanding of antimicrobial resistance.
Most microorganisms live in environments where nutrients are limited and fluctuate over time. Cells respond to nutrient fluctuations by sensing and adapting their physiological state. Recent studies suggest phenotypic heterogeneity in isogenic populations as an alternative strategy in fluctuating environments, where a subpopulation of cells express a function that allows growth under conditions that might arise in the future. It is unknown how environmental factors such as nutrient limitation shape phenotypic heterogeneity in metabolism and whether this allows cells to respond to nutrient fluctuations. Here, we show that substrate limitation increases phenotypic heterogeneity in metabolism, and this heterogeneity allows cells to cope with substrate fluctuations. We subjected the N2-fixing bacterium Klebsiella oxytoca to different levels of substrate limitation and substrate shifts, and obtained time-resolved single-cell measurements of metabolic activities using nanometre-scale secondary ion mass spectrometry (NanoSIMS). We found that the level of NH4+ limitation shapes phenotypic heterogeneity in N2 fixation. In turn, the N2 fixation rate of single cells during NH4+ limitation correlates positively with their growth rate after a shift to NH4+ depletion, experimentally demonstrating the benefit of heterogeneity. The results indicate that phenotypic heterogeneity is a general solution to two important ecological challenges - nutrient limitation and fluctuations - that many microorganisms face. Currently, we use NanoSIMS to develop a new approach that defines functionally-relevant, phenotypic biodiversity in microbial systems. In the last part of my presentation, I will highlight why the concept of phenotypic diversity is relevant for the understanding of antimicrobial resistance.
Die Weiterentwicklung der Verfahren und Techniken zur dauerhaften Überwachung von Bauwerken ist Gegenstand zahlreicher Forschungs- und Entwicklungsvorhaben. Der praktische Einsatz dieser Verfahren beschränkt sich bisher jedoch auf durchaus zahlreiche, jedes für sich jedoch sehr konkrete Einzelprobleme beschreibende Projekte. Einer flächendeckenden Anwendung stehen häufig – berechtigte oder unberechtigte – Bedenken zur Effizienz dieser Verfahren im Vergleich zu baupraktisch etablierten Verfahren wie z. B. regelmäßigen Bauwerksinspektionen entgegen. Weiterführende Aspekte wie optimierte Wartungskonzepte oder Lebensdauerprognosen zur begründeten Priorisierung von Ertüchtigungsmaßnahmen sind aufgrund des Fehlens zeitnah realisierbarer, monetärer Vorteile oftmals schwer vermittelbar. Dieser Beitrag soll einige grundlegende Ziele aktueller Monitoringkonzepte anhand von Projektbeispielen der BAM aufzeigen, um die Potentiale dieser Verfahren zu verdeutlichen und mögliche sinnvolle Anwendungsgebiete zu erschließen. Im Vordergrund dieses Übersichtsbeitrages stehen dabei die grundlegenden Ideen und Ziele dieser Projekte; bezüglich der Ergebnisse wird auf die entsprechenden Fachveröffentlichungen verwiesen.
Several restoration projects of stained-glass windows have been performed in Lower Silesia (Poland) since 2010. The aim of the projects was to protect stained-glass windows against environmental impact of industial pollutants and acid rain by installing a protective glazing. The usefulness of protective glazing has been proved by climate measurements and determination of environmental impact before and after installation.
LIBS matures to a quantitative method for elemental analysis rather than a qualitative diagnostic tool. Numerous real world applications for bulk and microanalysis profit from instrumental and methodical advances in the last decade. Today, recording of numerous spectra from samples can be done with low experimental efforts and low cost per spectrum. Not surprisingly, LIBS data, with a high spectral resolution and a broad spectral range, become “big data” and can be utilized in different ways beyond elemental analysis. But, what is the generic or best approach for quantitative LIBS analysis? What techniques can be employed to gain new insights into data? Emergent information can arise through data fusion of LIBS data with other data, i.e. orthogonal spectroscopic or other information related to the sample. But are fused data better than data from a single method?
This talk will provide an in-depth overview what chemometric tools can do for LIBS. For quantitative analysis, pre-processing tools are essential to improve precision, accuracy, and reproducibility but at the same time their application to data is still based on phenomenological criteria. Multivariate analysis seems to dominate LIBS, but are there drawbacks on using all information from spectra. For different data sets from real applications, the use of multivariate calibration and (un)supervised pattern recognition will be discussed in comparison with reference analytical methods and possible improvements through plasma diagnostics and modelling.
Der Vortrag gibt einen Überblick die deutsche Ressortforschung. Neben einer Einordnung in das deutsche Wissenschaftssystem werden in einem historischen Überblick die Besonderheiten der Ressortforschung diskutiert. Besonderes Augenmerk wird der Frage gewidmet „Was ist gute Ressortforschung“. Kritisch erscheint besonders die Vereinbarkeit von exzellenter Wissenschaft und seriöser und unabhängiger Politikberatung.
Photodegradation of the „novel“ brominated flame retardant Tris-(2,4,6-tribromophenoxy)-s-triazine
(2016)
Brominated flame retardants (BFRs) comprise a class of structurally diverse compounds that are functionally related and used in materials to reduce the flammability of polymers. Due to their global distribution, potential persistence, bioaccumulation and toxicity most of the BFRs of the first generation are banned or restricted, and replaced by new ones. However, based on similar properties these new compounds may also pose a serious risk by causing adverse effects to human health and the environment. These alternative BFRs were grouped into two classes: „novel” and „emerging” BFRs. Emerging BFRs are defined as compounds that have been identified in any environmental compartments whereas novel BFRs are only detected in materials and/or goods above 0.1 wt.-%.
The environmental fate of these alternative BFRs is partially unknown. Over the past years a multitude of studies on the photodegradation of BFRs in environmental matrices have been conducted to assess the photochemical behavior and fate in the environment. The photolytic debromination reaction is particularly induced among BFRs by UV exposure. The novel brominated triazine-based flame retardant tris-(2,4,6-tribromophenoxy)-s-triazine (TTBP-TAZ) is a BFR that is mainly used in acrylonitrile butadiene styrene and high impact polystyrene.
Ballesteros-Gómez et al. detected TTBP-TAZ in 8 of 13 plastic parts of consumer products and in 9 of 17 indoor dust samples but the photochemical behavior and fate is not known until now. The results of the present study, focused on photodegradation processes were performed for the first time for TTBP-TAZ to identify the photolysis intermediates and products to assess the environmental fate.
There is currently a debate within the SIP community about the characteristic textural length scale controlling relaxation time of consolidated porousmedia.One idea is that the relaxation time is dominated by the pore throat size distribution or more specifically the modal pore throat size as determined in mercury intrusion capillary pressure tests. Recently new studies on inverting pore size distributions from SIP data were published implying that the relaxation mechanisms and controlling length scale are well understood. In contrast new analytical model studies based on the Marshall-Madden membrane polarization theory suggested that two relaxation processes might compete: the one along the short narrow pore (the throat) with one across the wider pore in case the narrow pores become relatively long.
This paper presents a first systematically focused study into the relationship of pore throat sizes and SIP relaxation times. The generality of predicted trends is investigated across a wide range of materials differing considerably in chemical composition, specific surface and pore space characteristics. Three different groups of relaxation behaviors can be clearly distinguished. The different behaviors are related to clay content and type, carbonate content, size of the grains and the wide pores in the samples.
Radiation induced attenuation in perfluorinated polymer optical fibres for dosimetry applications
(2016)
Real-time measurement of radiation-induced attenuation (RIA) in a commercial perfluorinated polymer optical fibre (PF-POF) is performed with regard to on-line Radiation monitoring purposes. Spectral character and dose dependence of fibre’s RIA is measured in 450-900 nm spectral region. Fibre exhibited high radiation sensitivity in the visible region with strong increase towards the UV wavelengths. Good linearity and high sensitivity reaching up to 130 dBm-1/kGy was demonstrated in the VIS region for a low-dose range. This of-the-shelf PF-POF could be therefore interesting for on-line remote dosimetry applications.
Impact of gamma radiation on transmission of a commercial Cytop polymer optical fibre (Lucina, Asahi Glass Company) is investigated. Spectral dependence of radiation induced attenuation in the investigated fibre is measured in the VIS-NIR spectral region. Besides attenuation increase, radiation is found to increase fibre susceptibility to water as well. While pristine Cytop fibre is rather humidity insensitive, strong humidity related absorption in the NIR region is observed after fibre irradiation. Selective irradiation of separate fibre sections is proposed as a way of fibre humidity sensitization and quasi-distributed water detection is demonstrated using optical time domain reflectometry at 1310 nm.
This paper describes and discusses the major challenges of spent fuel management in Germany after the phase-out of nuclear electricity generation was decided in 2011 and a new repository siting procedure was implemented in 2013. Consequences from those decisions which were legally founded by amendments of the German Atomic Energy Act (AtG) result in the need to transfer all remaining spent fuel from limited reactor operation (last reactor shutdown until the end of 2022) into casks for subsequent dry interim storage on-site. Storage licenses are generally issued site-specific considering specific dual purpose casks (DPC) and their inventories and they are generally limited to 40 years so far. But the need for extending the interim storage period in the future has become obvious. Even though, this may not be an issue to be solved already today questions about additional safety demonstrations will arise as soon as licenses need to be extended. Certainly, these questions will ask for reliable data about the long term performance and safety of structures, systems, and components, e. g. the long term performance of cask components and materials like bolted closure systems including metal seals, or fuel rod behaviour concerning cladding materials under stress and temperature conditions. In case of dual purpose casks for storage and transportation this includes aspects on how to demonstrate transportability during or after several decades of interim storage. Long term investigations often require plenty of time and therefore need to be initiated timely.
This paper describes and discusses the major challenges of spent fuel management in Germany after the phase-out of nuclear electricity generation was decided in 2011 and a new repository siting procedure was implemented in 2013. Consequences from those decisions which were legally founded by amendments of the German Atomic Energy Act (AtG) result in the need to transfer all remaining spent fuel from limited reactor operation (last reactor shutdown until the end of 2022) into casks for subsequent dry interim storage on-site. Storage licenses are generally issued site-specific considering specific dual purpose casks (DPC) and their inventories and they are generally limited to 40 years so far. But the need for extending the interim storage period in the future has become obvious. Even though, this may not be an issue to be solved already today questions about additional safety demonstrations will arise as soon as licenses need to be extended. Certainly, these questions will ask for reliable data about the long term performance and safety of structures, systems, and components, e. g. the long term performance of cask components and materials like bolted closure systems including metal seals, or fuel rod behaviour concerning cladding materials under stress and temperature conditions. In case of dual purpose casks for storage and transportation this includes aspects on how to demonstrate transportability during or after several decades of interim storage. Long term investigations often require plenty of time and therefore need to be initiated timely.
The presentation shows how the three-dimensional quantification of dislocations and their characteristic features, e.g. Burgers vector, line direction, dislocation density, is carried out at the transmission electron microscope in scanning mode (STEM) at Division 5.1 at BAM. Exemplarily, the methods are shown for Ni-base superalloy single crystals, for which a short introduction is given using further TEM techniques. Additional examples on low angle grain boundaries, nucleation of oxides at dislocations and interaction of dislocations and carbides are shown.
The content of the presentation was addapted, aiming at scientists who work within the DFG Priority Programme 1713 "Strong coupling of thermo-chemical and thermo-mechanical states in applied materials".
Inductively coupled plasma mass spectrometry (ICP-MS) is a well-established analytical method for multi-elemental analysis in particular for elements at trace and ultra-trace levels. It has found acceptance in various application areas during the last decade. ICP-MS is also more and more applied for detection in the life sciences. For these applications, ICP-MS excels by a high sensitivity, which is independent of the molecular structure of the analyte, a wide linear dynamic range and by excellent multi-element capabilities. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional bioanalytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range.
In this chapter, we focus on new applications where the multi-element capability of ICP-MS is used for detection of lanthanoides or rare earth elements, which are applied as elemental stains or tags of biomolecules and in particular of antibodies.
In vielen Bereichen der Industrie und im verarbeitenden Gewerbe werden eine Vielzahl brennbarer Stäube gezielt oder ungewollt produziert, verarbeitet, transportiert oder anderweitig verwendet. Je nach Material- und Staubeigenschaften weisen diese eine teilweise sehr hohe Reaktivität auf. Es gilt weiterhin als allgemein bekannt, dass die Partikelgröße einen entscheidenden Einfluss auf das Brand- und Explosionsverhalten von Stäuben ausübt. Mit Abnahme der Partikelgröße nehmen die gefährlichen Auswirkungen im Falle einer Explosion und die Zündempfindlichkeit der Stäube zu. Aufgrund der veränderten Eigenschaften im Nanometerbereich hat die Produktion solcher Stäube mit sehr geringen Primärpartikelgrößen in den letzten Jahren zugenommen. Diese Entwicklung wird sich in den folgenden Jahren fortsetzen. Über das Brand- und Explosionsverhalten solcher Stäube war bis vor wenigen Jahren jedoch kaum bis wenig bekannt.
In vielen Bereichen der Industrie und im verarbeitenden Gewerbe werden eine Vielzahl brennbarer Stäube gezielt oder ungewollt produziert, verarbeitet, transportiert oder anderweitig verwendet. Je nach Material- und Staubeigenschaften weisen diese eine teilweise sehr hohe Reaktivität auf. Es gilt weiterhin als allgemein bekannt, dass die Partikelgröße einen entscheidenden Einfluss auf das Brand- und Explosionsverhalten von Stäuben ausübt. Mit Abnahme der Partikelgröße nehmen die gefährlichen Auswirkungen im Falle einer Explosion und die Zündempfindlichkeit der Stäube zu. Aufgrund der veränderten Eigenschaften im Nanometerbereich hat die Produktion solcher Stäube mit sehr geringen Primärpartikelgrößen in den letzten Jahren zugenommen. Diese Entwicklung wird sich in den folgenden Jahren fortsetzen. Über das Brand- und Explosionsverhalten solcher Stäube war bis vor wenigen Jahren jedoch kaum bis wenig bekannt.
Topic of the presentation is the predictability of safety characteristics like the Self Accelerating Decomposition Temperature (SADT) by means of simple correlations from DSC measurements or by models, which incorporate amongst others the molecular structure of the considered compound.
Already existing models of quantitative structure-property relationship (QSPR) for SADT determination suffer from test results, which are, on the majority, not comprehensible. The quality of the generated models is questionable.
One item within the Safera-project is the provision of reliable data to have a solid basis for the prediction.
Inductively coupled plasma mass spectrometry (ICP-MS) is based on formation of positively charged atomic ions in a high-frequency inductively coupled Argon plasma at atmospheric pressure. The ions are extracted and transferred from the plasma source into a mass analyzer operated at high vacuum via an interface equipped with a sampling and a skimmer cone. The ions are separated in the mass analyzer according to their charge to mass ratio. The ions are converted at a conversion dynode and are detected by use of a secondary electron multiplier or a Faraday cup.
From an analytical point of view, ICP-MS is a well-established method for multi-elemental analysis in particular for elements at trace- and ultra-trace levels. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional analytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range. For these applications, ICP-MS excels by a high sensitivity which is independent of the molecular structure and a wide linear dynamic range. It has found acceptance in various application areas and during the last decade ICP-MS is also more and more applied for detection of rare earth elements particularly in the life sciences.
Due to the fact that all molecules introduced into the high temperature of the plasma in the ion source were completely dissociated and broken down into atoms, which are subsequently ionized, all elemental species information is completely lost. However, if the different species are separated before they enter the plasma by using adequate fractionation or separation techniques, then ICP-MS can be used as a very sensitive element-specific detector. We will discuss this feature of ICP-MS in this chapter in more detail at hand of the speciation of gadolinium-containing contrast agents.
In Germany the damages on concrete motorways have increased during the past 15 years. This led often to a reduction of service life from 30 to 10 years. In spite of comprehensive research the reasons for these damages have not been clarified yet. But it is known that in this context the ASR plays a decisive role. Against this background ASR performance tests have been developed. However, these tests do not take into account the effects of mechanical loading due to cyclic traffic and climatic impact. Therefore in Germany the ASR research group 1498 was founded. The research group consists of three experimentally- and two multi-scale modelling oriented subprojects, which are working closely together. Selected findings of BAM’s experimental subproject SP4 are content of this contribution. The aim was to investigate the impact of a cyclic mechanical pre-damage on moisture transport. The pre-damaging was carried out on large-format beams using a cyclic four point bending test with a total number of 5 million load cycles. Thereby the damage process was monitored by using different NDT-techniques. After the mechanical pre-damaging, smallsized specimens were taken from loaded as well as unloaded areas of the large format beams. Absorption tests were carried out on these specimens using water and NaCl solution. Thereby moisture distribution was measured with Nuclear Magnetic Resonance (NMR) and Time Domain Reflectometry (TDR). Additionally, moisture suction was quantified integrally by means of gravimetric measurements. The analysis of the first test data shows that the mechanical loading influences the moisture transport.
Zur Vermeidung der schädigenden Alkali-Kieselsäure-Reaktion in Betonbauwerken wird die Alkalireaktivität von Gesteinskörnungen im Vorhinein getestet. Der 60°C-Betonversuch ermöglicht eine vergleichsweise schnelle Einschätzung nach fünf-monatiger Testzeit. Dazu wird die Dehnung von Betonprüfkörpern, die mit der zu testenden Gesteinskörnung hergestellt wurden, manuell alle 28 Tage gemessen. Ein alternatives, an der BAM in den vergangen Jahren entwickeltes Verfahren setzt Dehnungssensoren ein, um kontinuierlich und online zu messen. Die Dehnungskurven sind eine gute Grundlage sowohl für die Prognose vom Expansionsverhalten während des Tests als auch für die Validierung von Expansionsmodellen.
The concrete prism test at 60°C facilitates accelerated testing of alkali-silica reactivity of aggregates within five months. Manual measurement is usually conducted to determine expansion of test specimen every 28 days. This conventional procedure gives only limited insight to expansion behaviour of ASR-affected prisms. Due to the large time intervals, expansion exceeding the critical value of 0.3 mm/m is likely to be noticed late. Continuous recording applied in this work resolves this problem and delivers beneficial information on the shape of the expansion curve.
Different types of aggregate have been tested applying continuous and manual measurement to the concrete specimens.
Models of ASR-induced expansion, available in the open literature, so far are validated with discontinuous data hardly tracing the modelled curve. Continuous measurement improves validation and further model development.
The martensitic steels X30CrMoN15-1 and 100Cr6 did not show any hydrogen enhanced wear in sliding friction tests against alumina balls in hydrogen gas environment. However, depending on the purity of the environment, unexpected high wear occurred at the alumina ball. The results of a tests series with a broad variation of test parameters are presented.
Bio-diagnostic assays of high complexity rely on nanoscaled assay recognition elements that can provide unique selectivity and design-enhanced sensitivity features. High throughput performance requires the simultaneous detection of various analytes combined with appropriate bioassay components. Nanoparticle induced sensitivity enhancement, and subsequent multiplexed capability Surface-Enhanced InfraRed Absorption (SEIRA) assay formats are fitting well these purposes. SEIRA constitutes an ideal platform to isolate the vibrational signatures of targeted bioassay and active molecules. The potential of several targeted biolabels, here fluorophore-labeled antibody conjugates, chemisorbed onto low-cost biocompatible gold nano-aggregates substrates have been explored for their use in assay platforms. Dried films were analyzed by synchrotron radiation based FTIR/SEIRA spectro-microscopy and the resulting complex hyperspectral datasets were submitted to automated statistical analysis, namely Principal Components Analysis (PCA). The relationships between molecular fingerprints were put in evidence to highlight their spectral discrimination capabilities. We demonstrate that robust spectral encoding via SEIRA fingerprints opens up new opportunities for fast, reliable and multiplexed high-end screening not only in biodiagnostics but also in vitro biochemical imaging.
Sliding wear of martensitic steels in hydrogen – X30CrMoN15-1 and 100Cr6 – the role of water traces
(2016)
Initially the primary objective of the project has been the investigation of the influence of gaseous hydrogen on the wear of martensitic steels under heavy tribological stress. As a counter body an Al2O3 ball has been used because the material is inert and hard so that a low amount of wear was expected. If only the gas pressure is responsible for the absorption of hydrogen from the gas to pure α-iron it would require 15·105 MPa (~15 Mbar) to press 1 ppm into the material.
In the test series the Al2O3 balls showed in N2 and H2 atmosphere a higher wear compared to aerial experiments which showed a smaller wear track and a severer wear for the disc. Because of scattering and thereof following investigations it was shown that hydrogen has no noticeable influence but water traces in the gas are manipulating the outcome of the tests distinctly.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
Hydroxyapatite (HA) is a bioceramic material with excellent biological properties. However, these properties are strongly dependent of ist crystallinity degree, with high values of crystallinity associated to poor resorption rates and bioactivity. This work evaluates the properties of HA samples produced by two different free-forming conformation methods, CNC machining and 3D printing. In both cases, porous gypsum samples were produced and subsequently converted into HA in a reaction with di-ammonium hydrogen phosphate at 100°C and pH 8. A total conversion of the samples was achieved after 36 h independently of the conformation method used. The microstructure, however, before and after the conversion is showed to be dependent on the method used. After conversion the machined samples achieved a Maximum compressive strength of 3.5 MPaforporosities of circa 80%, while 3D printed samples achieved a tensile strength of 2.0 MPa by porosities of 61%.
The scope of our study was to prepare Fe-based highly active catalysts for water treatment processes. The reactive nanomaterials were
synthesized by chemical precipitation; the post-synthesis coating of the as obtained nanostructures was achieved by capping the magnetic cores with a
polymeric surfactant, polyethylene glycol (PEG). The resulted Fe3O4/PEG nanoparticles were further used to immobilize two types of reactive materials on
their surface, either ferrous oxalate (FO) or ferric citrate (FC), yielding the final products – two green Fenton-like heterogeneous nanocatalysts. The
sensitized catalysts were characterized by several microstructure characterization techniques such as X-ray diffraction (XRD), vibrating sample
magnetometry, BET, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). All experiments were performed on a
laboratory scale set-up. Important variables such as effect of hydrogen peroxide concentration, UV light, the amount of catalyst and contact time for the
catalytic wet peroxide oxidation (CWHPO) of BPA were examined. The results indicate that the oxidation rate increased under UV light in the presence of
low-concentration H2O2.
Metalloproteins, which represent about 30 % of the total proteome, are often important markers for distinguishing between healthy and diseased states of patients. As such markers have become increasingly important in clinical diagnostics, some of these proteins are routinely analysed in clinical laboratories. Reliable and comparable results are the basis for the investigation of changes in the proteome due to different health conditions. Nevertheless, for many proteins the results achieved with different routine measurement procedures or in different laboratories vary widely, thus hampering medical insights and the development of treatments. Reference measurement procedures with results traceable to the International System of Units (SI) will also help to greatly improve the performance of routine measurement procedures and, this way, they support the understanding of changes in the metallome.
Previously on sulfur determination in metal revealed a lack of traceability and inconsistent results. Solving the problems a reference procedure for sulfur measurement in metal are required to build up a reliable reference value. In this study a procedure was developed for quantification of total sulfur at low concentration (in sub ppm level) in metal using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The ion exchange method and complexing agent were applied in this procedure to avoid loading large amount of metal into the instrument. Adding ammonia as a complexing agent into sample solution to reduce sulfur-metal co-elute. The procedure shows high performance and it is expressed in % recovery of sulfur (> 90%) and % metal elimination (>99 %). Additionally, relative measurement uncertainties were calculated less than 1.5 % and the results are traceable directly to SI units. This study would establish as reference procedure for sulfur measurement in metal sample which fit for these purpose as follows; for certified reference material and assigned value for inter-laboratory comparison.
Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers.
Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories.
IDMS Training
(2016)
Based on its proven records especially in reference material certification, isotope dilution mass spectrometry (IDMS) is considered as one of the most powerful and most accurate methods for determining amounts of substance. Contrary to other calibration approaches, IDMS does not directly suffer from long-time changes or drifts in instrument sensitivity. Moreover, provided isotopic exchange between the sample and spike is ensured, losses of analyte do not affect the analytical result. Both advantages are based on the fact that IDMS only requires isotope ratio measurements and isotope ratios are largely unaffected by instrumental drift, setup or by matrix, unless an isobaric interference is present.
The Consultative Committee for Amount of Substance (CCQM), the world's highest institution for metrology in chemistry, considers IDMS as the most important “Primary Method of Measurement” for amount determination. The total combined uncertainty, according to ISO and EURACHEM guidelines, can easily be calculated via the IDMS equations. Applying it correctly, IDMS has the potential to be a primary method of measurement yielding SI traceable values in the most direct way with combined uncertainties significantly smaller than obtainable by other methods.
In general it can be stated that IDMS is the most important reference method for elemental and elemental species analysis, offering highest accuracy and precision or smallest measurement uncertainties, when properly applied. Thus IDMS represents by far the best suited reference method for RM characterisation. Due to its universal applicability IDMS offers sufficient potential to follow future needs in analytical chemistry as well as in the RM sector.
This presentation will demonstrate the basic principle of IDMS and will show its Pros and Cons as well as its pitfalls. Possible sources of errors and bias are mentioned and correction models will be discussed. Notice will be given to metrological aspects such as traceability and uncertainty. Differences in the application of thermal ionization mass spectrometry and inductively coupled plasma mass spectrometry are discussed as well as differences between different types of mass spectrometers. This will be illustrated by practical examples from various fields.