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Paper des Monats
- ja (68)
For the application of the time-temperature superposition principle a suitable relation is needed to describe the time-temperature shift factor α. Therefore, the Arrhenius equation is widely used due to its simple form and often leads to suitable results. Where, the Arrhenius equation presents a linear relation for the temperature-dependent shift factor in logarithmic scale ln(α) with the absolute inverse temperature (1/ϑ). However, in cases with a large temperature range which eventually include more complex reaction processes, the functional relation between ln(α) and (1/ϑ) is nonlinear in the ‘Arrhenius plot’. In those cases, the monotone change of the nonlinear range in the ‘Arrhenius plot’ can be interpreted as a transient range between two approximately linear or constant regions. An extended application of the modified Arrhenius equation from Nakamura (1989) is presented in this study for this transient range. The introduced method was applied to describe the time-temperature equivalence in the relaxation analysis of restoring seal force of metal seals, which are used in lid-systems of transport and interim storage casks for radioactive materials. But, the method is widely valid and can be used for different objectives which are characterized by thermorheologically simple behavior with nonlinear sensitivity to inverse temperature.
High temperature oxidation of 9–12% Cr ferritic/martensitic steels under dual-environment conditions
(2017)
In normal operations, the opposite surfaces of the power plant components are exposed to two different environments, i.e. air/flue gas on the one side and steam on the other side. Exposure under such dual-environment can lead to accelerated corrosion of the components on the air side. The oxidation behaviour of ferritic/martensitic steel T92 was investigated under dual-environment in a specially designed test equipment. The samples were exposed to dry oxyfuel flue gas (CO2–27%N2–2%O2–1%SO2) on one side and to steam on the other side up to 1000 h at 650°C. The formation of oxide scales was characterised by optical microscopy and scanning electron microscopy with attached energy-dispersive spectroscopy. Oxidation rate of specimens under dual-Environment condition was almost three times higher than that in single-environment condition. This is explained based on hydrogen transport through the bulk alloy from the steam side to the flue gas side.
Die Feuerverzinkung von Betonstahl stellt auf der Grundlage der im Stahlbetonbau geltenden Regelwerke eine zusätzliche Maßnahme zur Steigerung der Dauerhaftigkeit insbesondere bei Korrosionsbeanspruchung infolge Karbonatisierung und/oder Chlorideinwirkung dar. Anders als im Ausland ist die Anwendung von feuerverzinktem Betonstahl in Deutschland bisher kaum verbreitet.
Im Rahmen des AiF-Forschungsprojekts IGF 499 „Technologie- und Sicherheitszuwachs bei der Anwendung von feuerverzinktem Betonstahl zum Ausbau einer nachhaltigen Marktposition im Stahlbetonbau“ sollten die einem breiteren Einsatz feuerverzinkter Betonstähle in Deutschland bisher entgegenstehenden offenen Fragestellungen beantwortet werden.
Die interdisziplinäre Forschergruppe bestand aus dem Fachgebiet Werkstoffe im Bauwesen, Technische Universität Kaiserslautern (Forschungsstelle 1), mit dem Arbeitsschwerpunkt Fertigungstechnik, der staatlichen Materialprüfungsanstalt Darmstadt an der Technischen Universität Darmstadt (Forschungsstelle 2), mit dem Arbeitsschwerpunkt Werkstofftechnik, und der Bundesanstalt für Materialforschung und –prüfung, Berlin (Forschungsstelle 3), mit dem Arbeitsschwerpunkt Korrosionsschutz.
Vibration-based model updating and identification of multiple axial forces in truss structures
(2017)
Safety assessment of existing iron and steel truss structures requires the determination of the axial Forces and corresponding stresses in truss structural members. The results of the axial force determination can be integrated as part of a structural health Monitoring scheme for existing trusses. In this work, a methodology is proposed to identify multiple axial forces in members of a truss structure based on the modal parameters. Vibration test allows the identification of the natural frequencies and mode shapes, globally of the truss structure as well as locally of the individual bars. The method calibrates the numerical model of the truss structure using a genetic algorithm and strategic validation criteria. The validation criteria are based on the identified natural frequencies and global mode shapes of the truss structure as well as information of the axial forces in the individual bars of the truss, which are estimated from the natural frequencies and five amplitudes of the corresponding local mode shapes of the single bars based on an analytical-based algorithm. The calibration allows the identification of the axial forces in all bars of the truss structure. For mode pairing strategy, a technique makes use of the enhanced modal assurance criteria with the calculation of the modal strain energies.
Moreover, the modal strain energies are also used to select the relevant local mode shape of the individual bars. The feasibility and accuracy of the proposed methodology is verified by laboratory experiments on several truss structures. In situ tests on existing trusses are intended. The results from one of the laboratory tested structures, i.e. a two-bar system, are included in this paper.
A first pilot study on the sorption of environmental pollutants on various microplastic materials
(2017)
With the drastic increase in plastic production, the input of plastic particles into the environment has become a recognised problem.
Xenobiotics are able to sorb to polymer materials, and this process is further enhanced where they Encounter microplastics (plastic fragments <5 mm). In this work we studied the sorption of metformin, a type-2 diabetes drug, and difenoconazole, a fungicide, onto the virgin polymer materials polyamide (PA), polypropylene (PP), and polystyrene (PS). Additionally, PP was cryo-milled and PA was treated with acid to investigate the influence of an increase in surface area and chemical modification. The material properties were also studied by dynamic scanning calorimetry (DSC), gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FTIR). Sorption experiments were performed on the basis of a full factorial design examining the effect of agitation, pH value, and salinity. Experimental results showed that difenoconazole sorbs readily to all microplastics, whereas the more polar analyte metformin did not show any affinity to the materials used. For difenoconazole the governing factor in all cases is agitation, while both pH and salinity exhibited only a slight influence. The modification of polymers leads to enhanced sorption, indicating that an increase in surface area (cryo-milled PP) or inner volume (acid-treated PA) strongly favours adsorption. Moreover, long-term experiments demonstrated that the time until equilibrium is reached depends strongly on the particle size.
Rohrleitungssysteme sind aufgrund ihrer Funktion und Ausdehnung für den Betrieb, die Verfügbarkeit und die Sicherheit von Industrieanlagen von besonderer Bedeutung. Die bisher in definierten Intervallen durchgeführten, wiederkehrenden Prüfungen zur Sicherstellung leckagefreier Rohrleitungen sind kostenintensiv und mit einem erhöhten Aufwand verbunden.
Mit dem interdisziplinären Forschungsprojekt AGIFAMOR (Ageing Infrastructures – Akustisches Monitoring von Rohrleitungen) arbeitet die BAM an der Entwicklung und Erprobung einer örtlich und zeitlich kontinuierlichen Zustandsüberwachung von Rohrleitungen basierend auf einem faseroptischen akustischen Messsystem, welches einen vergleichsweise geringen Installationsaufwand der Sensoren erfordert. Mit diesem Verfahren sollen vor allem betriebsbedingte Schädigungen infolge von Korrosion sowie daraus entstehende Pittings oder Risse erkannt und damit Leckagen verhindert werden.
Im Rahmen einer Machbarkeitsstudie zum Teilaspekt „Detektion von Risswachstum“ wurde ein 2,5 m langes, definiert vorgekerbtes Stahlrohr mit der faseroptischen Sensorik (FOS) ausgestattet und quasistatisch unter 4-Punkt-Biegung belastet. Mit fortschreitender Belastung wächst, ausgehend vom vorhandenen Außenumfangskerb, ein Riss im Stahlrohr bis zum Erreichen der Leckage – in der Praxis ein gefährliches Schadensszenario.
Parallel zur FOS erfolgten Messungen mit Schallemissionssensoren, Beschleunigungssensoren und Potentialsonden, deren Ergebnisse die Interpretation der FOS-Messergebnisse unterstützen sollen.
The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time Points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the Quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology.
Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L3 edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc.
The effectiveness of this mode of STXM operation is demonstrated for These nanoparticle clusters.
For in-service inspections on wheelset axles with a hollow drilling, mechanized ultrasound inspection systems with single element probes are typically used. The ultrasonic testing in the zones close to the external surface of the railway axles can be realized from the inside of the bore hole, without demounting the wheelset and without dismantling the wheels and the brake discs. The testing system must be able to find flaws in the external surface of the hollow shafts, whose surface lies in the radial-radial plane, these are called transversal flaw. Presently testing systems are used, where scanning is realized in the circumferential direction by mechanical rotation of the probe system in the actual drilling. The phased array probe system, which is presented here, can carry out the rotation scan electronically. The scan can be carried out by simply moving the system forward and backwards through the drilling without mechanical rotation. Manipulation becomes simpler and the inspection time can be shortened considerably. The ultrasonic beam can be inclined exactly and be focused in the plane vertical to the specimen axis.
The probe is designed with help of indispensable simulations using especially designed software developed by BAM. The feasibility and the alignment between the simulated and experimental results were shown in earlier projects reported by Boehm et al. (2006) and Völz et al. (2012). The main task here is to optimize a probe for bore holes with a diameter of 65 mm with an increase in sensitivity and a high spatial resolution. This development will be carried out by use of extensive simulations and result in certain changes of the relevant probe parameters.
Virulence determines the impact a pathogen has on the fitness of its host, yet current understanding of the evolutionary origins and causes of virulence of many pathogens is surprisingly incomplete. Here, we explore the evolution of Marek’s disease virus (MDV), a herpesvirus commonly afflicting chickens and rarely other avian species. The history of MDV in the 20th century represents an important case study in the evolution of virulence. The severity of MDV infection in chickens has been rising steadily since the adoption of intensive farming techniques and vaccination programs in the 1950s and 1970s, respectively. It has remained uncertain, however, which of these factors is causally more responsible for the observed increase in virulence of circulating viruses. We conducted a phylogenomic study to understand the evolution of MDV in the context of dramatic changes to poultry farming and disease control. Our analysis reveals evidence of geographical structuring of MDV strains, with reconstructions supporting the emergence of virulent viruses independently in North America and Eurasia. Of note, the emergence of virulent viruses appears to coincide approximately with the introduction of comprehensive vaccination on both continents. The time-dated phylogeny also indicated that MDV has a mean evolutionary rate of ~1.6 × 10−5 substitutions per site per year. An examination of gene-linked mutations did not identify a strong association between mutational variation and virulence phenotypes, indicating that MDV may evolve readily and rapidly under strong selective pressures and that multiple genotypic pathways may underlie virulence adaptation in MDV.
Classical film radiography is a well-established NDT technique and it is most commonly used for testing weld seams and corroded pipes e.g. in oil and gas industry or in nuclear power plants. In the course of digitization, digital detector arrays (DDA) are finding their way into industrial applications and are replacing film radiography step by step. This study deals with the latest generation of DDAs, the photon counting and energy resolving detectors (PCD), and their characteristics compared to charge integrating detectors (CID). No matter which technology to use, radiography still lacks a general issue: A three-dimensional object is projected onto a two dimensional image. Of course, advanced computed tomography (CT) algorithms exist since many years, but if the object to investigate is too large to fit into the manipulation system or its shape is not appropriate, CT is not feasible or sensible to be applied. To overcome this limitation, numerous laminographic algorithms have been developed in the past. In this study, photon counting detectors are used in combination with co-planar translational laminography to gain reconstructed three-dimensional volumes. Both laminographic testing and PCDs require a serious knowledge of many parameters that can influence the image quality in the resulting datasets. These are e.g. the detector efficiency and calibration procedure, setting of energy thresholds, exposure data, number of projections, beam length correction and spatial resolution. The use of PCDs yields more variables to be considered compared to CIDs. The most important parameters in laminographic testing and in the use of PCDs are described in this study and limits are discussed.
Non-destructive testing (NDT) helps to find material defects without having an influence on the material itself. It is applied as a method of quality control, for online structural health monitoring, and for inspection of safety related components. Due to the ability of automation and a simple test setup ultrasonic testing is one major NDT technique next to several existing options. Whereas contact technique allows the use of higher frequencies of some MHz and phased array focusing, air-coupled ultrasonic testing (ACUT) shows different advantages. Most significant for ACUT is the absence of any coupling fluid and an economical test procedure respective time and costs. Both contact technique and ACUT have been improved and enhanced during the past years. One important enhancement is the development of airborne transducers based on ferroelectrets, like charged cellular polypropylene (cpp), which makes the application of any matching layers being mandatory in conventional piezoelectric transducers unnecessary. In this contribution we show ultrasonic inspection results of specimens made of carbon- and glass-fibre-reinforced plastic. These specimens include defects represented by drill holes and artificial delaminations of various size and depth. We compare inspection results achieved by using contact technique to those achieved by ACUT. For ACUT, conventional piezoelectric transducers and transducers based on cpp were used, both focused as well as non-focused types. Contact inspections were performed with a multi-channel matrix array probe. Once the inspection data is recorded it can be analysed in order to detect and evaluate defects in the specimen. We present different analysing strategies and compare these regarding detection rate and sizing of defects.
A simple batch test leaching procedure is used in many countries, as a compliance test, to evaluate the leaching of mainly inorganic substances from soil. However, agitating certain types of soil and then passing the solution through a membrane filter with 0.45-µm pores yields filtrates that have been colored by the colloidal particles. These colloids might affect the results of the inorganic substances obtained in the batch tests. In this study, we evaluated the effects of colloidal particles on the results and the reproducibility of batch tests on contaminated soil using different agitation methods and membrane filters with different pore sizes. The leaching behaviors of As, Pb, Se, F and Cl from three types of soil were studied. The As and Pb concentrations in the leachates of some types of soil were clearly affected by the amount of colloidal particles with a diameter of 0.10–0.45 µm and by the agitation method used. This was probably because As and Pb were present mainly in the particulate form in the leachate that had been passed through a membrane filter with 0.45-µm pores. This is not the case for every type of soil. The results of batch leaching tests showed that not only dissolved but also colloidal forms with a diameter of 0.10–0.45 µm might be included and that the existence of colloidal particles in the leachate decreases the batch leaching test reproducibility.
Two novel species of the fungal genus Ochroconis, O. lascauxensis and O. anomala have been isolated from the walls of the Lascaux Cave, France. The interest in these fungi and their melanins lies in the formation of black stains on the walls and rock art which threatens the integrity of the paintings. Here we report solid-state cross polarization magic-angle spinning 13C and 15N nuclear magnetic resonance (NMR) spectroscopy and surface-enhanced Raman spectroscopy (SERS) of the melanins extracted from the mycelia of O. lascauxensis and O. anomala in order to known their chemical structure. The melanins from these two species were compared with those from other fungi. The melanins from the Ochroconis species have similar SERS and 13C and 15N NMR spectra. Their chemical structures as suggested by the data are not related to 3,4-dihydroxyphenylalanine, 5,6-dihydroxyindole or 1,8-dihydroxynaphthalene precursors and likely the building blocks from the melanins have to be based on other phenols that react with the N-terminal amino acid of proteins. The analytical pyrolysis of the acid hydrolysed melanin from O. lascauxensis supports this assumption.
As part of the Qumran project conducted at the Federal Institute for Materials Research and Testing (BAM) in Berlin between 2007 and 2010, my colleagues and I developed a new, integrated methodology for determining the original and acquired properties of highly heterogeneous Dead Sea Scrolls. The purpose of this methodology is to help scholars determine the provenance of fragments of the scrolls and sort and compare them more easily than in the past. Since our measurements allowed us to differentiate between the minerals originating from the production processes and the sediments accrued during storage in the caves in Qumran, we were able to reconstruct the treatment of hides and discovered that at least two distinct parchmentproduction techniques co-existed at the beginning of the common era.
The reconstruction of workmanship on animal hides in Antiquity raised doubts about the validity of the current definition of parchment, which is based on a production technique known from the Middle Ages. We hope that our current work will also help researchers understand the characteristic properties of gewil, qelaf and dukhsustos better.¹
The evolution and socio-geographic distribution of writing inks in late Antiquity and the early Middle Ages are the second focus of our investigative work at BAM.
We use X-ray fluorescence analysis (XRF) to determine the chemical composition of inks and NIR reflectography for their typology. We are amply assisted in our ambitious enterprise by codicologists and palaeographers who have adopted our methodology and conduct field studies of their own.
Our current projects focus on the material analysis of the writing materials
kept in the Taylor-Schechter Collection at Cambridge University Library,
which houses the largest collection of Cairo Geniza fragments, about 190,000.
Although Geniza manuscripts have attracted a great deal of scholarly attention,
the material aspects of these documents seem to have been largely neglected.
The current study aims to obtain information on the composition of the writing
supports and the inks that were used, the production of the original manuscripts
and the history of their degradation. The collected data should supplement the
description based on Hebrew palaeography and codicology. Moreover, a characterisation
of the writing materials would provide insights on trade, local production
techniques and social structures. The tabulated results have the potential to
be used as geo-chronological markers if sufficient data is collected.
For our study, we chose Hebrew legal documents and letters from three communities
that co-existed in Fustat (today Cairo) in the 11th century: the Jerusalemite
(or ‘Palestinian’) community, the Babylonian community and the Karaites, three
different communities with different scribal traditions. In addition to this, we
studied non-biblical scrolls attributed to the Palestinian and Babylonian communities.
The question we addressed was whether we can correlate the use of a
specific type of ink to an objective criterion.
For our analysis at Cambridge University Library, we used a number of protocols
developed at BAM (Bundesanstalt für Materialforschung und -prüfung) in
Berlin and at the Centre for Study of Manuscript Cultures, University of Hamburg
(CSMC). These include reflectographic examination followed by non-destructive
X-ray fluorescence (XRF) analysis using transportable instruments so that the
analysis can be carried out in situ.
We have illustrated our approach here by providing two examples. The first one
describes our investigation of the leather fragment containing a portion of the
Babylonian Talmud on its hair side (TS Misc.26.53.17). The second example illustrates
our ability to compare iron-gall inks using the XRF method. In this case,
we explored the question of the codicological attribution of three fragments (TS
F17.4, TS 12.755 and TS 12.756) to the same Talmud manuscript.
The development of alkali‐activated materials (AAMs) as an alternative to Portland cement (PC) has seen significant progress in the past decades. However, there still remains significant uncertainty regarding their long term performance when used in steel‐reinforced structures. The durability of AAMs in such applications depends strongly on the corrosion behaviour of the embedded steel reinforcement, and the experimental data in the literature are limited and in some cases inconsistent. This letter elucidates the role of the chemistry of AAMs on the mechanisms governing passivation and chloride‐induced corrosion of the steel reinforcement, to bring a better understanding of the durability of AAM structures exposed to chloride. The corrosion of the steel reinforcement in AAMs differs significantly from observations in PC; the onset of pitting (or the chloride ‘threshold’ value) depends strongly on the alkalinity, and the redox environment, of these binders. Classifications or standards used to assess the severity of steel corrosion in PC appear not to be directly applicable to AAMs due to important differences in pore solution chemistry and phase assemblage.
Proben mit einer Mittelkerbe aus Polyamid 66 mit 35% Gewichtsan-teil an Kurzglasfaser (PA-GF35) wurden im Spritzgießverfahren hergestellt und in einem ungeschädigten und durch Schwingbeanspruch geschädigten Zustand mittels Röntgenverfahren charakterisiert. Sowohl die Faserorientierungsverteilung als auch die Riss-/Mikrorissbildung wurden mit der Röntgenrefraktionstopographie in einem SAXS-Aufbau und dem Diffraction-Enhanced-Imaging am Synchrotron (BESSY II) analysiert. Beide Verfahren spiegeln in guter Übereinstimmung die Charakteristiken dieser Werkstoffklasse in Bezug auf die Fertigungsqualität und die Schädigungsme-chanismen wider.
Detection of the electronic structure of iron-(III)-oxo oligomers forming in aqueous solutions
(2017)
The nature of the small iron-oxo oligomers in iron-(III) aqueous solutions has a determining effect on the chemical processes that govern the formation of nanoparticles in aqueous phase. Here we report on a liquid-Jet photoelectron-spectroscopy experiment for the investigation of the electronic structure of the occurring iron-oxo oligomers in FeCl3 aqueous solutions. The only iron species in the as-prepared 0.75 M solution are Fe3+ monomers. Addition of NaOH initiates Fe3+ hydrolysis which is followed by the formation of iron-oxo oligomers. At small enough NaOH concentrations, corresponding to approximately [OH]/[Fe] = 0.2–0.25 ratio, the iron oligomers can be stabilized for several hours without engaging in further aggregation. Here, we apply a combination of non-resonant as well as iron 2p and Oxygen 1s resonant photoelectron spectroscopy from a liquid microjet to detect the electronic structure of the occurring species. Specifically, the oxygen 1s partial electron yield X-ray absorption (PEY-XA) spectra are found to exhibit a peak well below the onset of liquid water and OH (aq) absorption. The iron 2p absorption gives rise to signal centered between the main absorption bands typical for aqueous Fe3+. Absorption bands in both PEY-XA spectra are found to correlate with an enhanced photoelectron Peak near 20 eV binding energy, which demonstrates the sensitivity of resonant photoelectron (RPE) spectroscopy to mixing between iron and ligand orbitals. These various signals from the iron-oxo oligomers exhibit Maximum intensity at [OH]/[Fe] = 0.25 ratio. For the same ratio, we observe changes in the pH as well as in complementary Raman spectra, which can be assigned to the Transition from monomeric to oligomeric species. At approximately [OH]/[Fe] = 0.3 we begin to observe particles larger than 1 nm in radius, detected by small-angle X-ray scattering.
Health monitoring von größeren Strukturen erfordert die Betrachtung der gesamten Struktur, indem sowohl jener Bereich, der experimentell behandelt wird, als auch derjenige, der einer analytischen mechanischen Untersuchung unterzogen wird, in einem Gesamtzusammenhang erfasst wird. Die umfassende Behandlung des Problems gelingt dann in einer Gesamtmatrix, die im Beitrag vorgestellt wird. Auf eine Erweiterung der Methode zur Detektierung anwachsender Schädigungen wird hingewiesen.