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Eingeladener Vortrag
- nein (1030)
Die beiden in dieser Arbeit dargestellten Beispiele zeigen, dass sich die Low-strain-Pfahlintegritätsprüfung noch über den bisherigen, schon sehr erfolgreichen Stand hinaus entwickeln kann. Der Einsatz von Vibratortechnik und passender mathematischer Methoden bietet das Potential, Prüfungen auch unter bisher nicht lösbaren Randbedingungen durchzuführen. Dazu gehören sehr schlanke Pfähle und Messungen bei hohem Störpegel. Der erhöhte Mess- und Auswerteaufwand ist jedoch im Einzelfall gegenüber dem erzielbaren Erfolg abzugleichen. Apparativ müssen noch Entwicklungsarbeiten geleistet werden, um einen einfachen und zuverlässigen Einsatz in der Praxis zu ermöglichen. Die Messung mit mehreren Sensoren entlang des Pfahls kann schon heute in der Praxis eingesetzt werden. In vielen Fällen lassen sich damit auch Messungen an Pfählen im Bestand durchführen, bei denen die konventionelle Pfahlprüfung aufgrund von überlagernden Signalen aus der aufgehenden Struktur versagt.
Partial discharge in polymeric insulation of high voltage equipment causes cumulative damage that progressively deteriorates the insulation, leading to eventual failure. The electrical detection of related discharge current pulses may be challenged by electromagnetic interference from the environment. In such situations the detection of acoustic emission from partial discharge can greatly enhance its detectability, especially when electromagnetically immune fiber-optic acoustic sensors are used. During experiments involving such fiber-optic sensors that were specifically designed for the detection of partial discharge in elastomeric insulation, an unexpected type of acoustic emission was observed in silicone elastomer specimens with tip–plate electrode configurations and under DC electrical stress. We present and discuss experimental results that indicate space charge injection and subsequent spontaneous dynamical processes as the source of the detected acoustic emission. We use sensitive conventional partial discharge measurement instrumentation to show that the apparent acoustic efficiency of the processes leading to the observed acoustic emission is very high. Acoustic emission triggered by discharge events with individual apparent charge values of only a few femtocoulombs could be detected.
Revealing the inner secrets of intumescent chars by advanced small scale tests combined with µ-CT
(2015)
The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate General of the European Commission, operates the International Measurement Evaluation Program (IMEP). IMEP organises inter-laboratory comparisons in support of European Union policies. This paper presents the results of two proficiency tests (PTs): IMEP-116 and IMEP-39, organised for the determination of total Cd, Pb, As, Hg and inorganic As (iAs) in mushrooms. Participation in IMEP-116 was restricted to National Reference Laboratories (NRLs) officially appointed by national authorities in European Union member states. IMEP-39 was open to all other laboratories wishing to participate. Thirty-seven participants from 25 countries reported results in IMEP-116, and 62 laboratories from 36 countries reported for the IMEP-39 study. Both PTs were organised in support to Regulation (EC) No. 1881/2006, which sets the maximum levels for certain contaminants in food. The test item used in both PTs was a blend of mushrooms of the variety shiitake (Lentinula edodes). Five laboratories, with demonstrated measurement capability in the field, provided results to establish the assigned values (Xref). The standard uncertainties associated to the assigned values (uref) were calculated by combining the uncertainty of the characterisation (uchar) with a contribution for homogeneity (ubb) and for stability (ust), whilst uchar was calculated following ISO 13528. Laboratory results were rated with z- and zeta (ζ)-scores in accordance with ISO 13528. The standard deviation for proficiency assessment, σp, ranged from 10% to 20% depending on the analyte. The percentage of satisfactory z-scores ranged from 81% (iAs) to 97% (total Cd) in IMEP-116 and from 64% (iAs) to 84% (total Hg) in IMEP-39.
Ober die europäischen Produktnormen für Geokunststoffe (hEN) wird gestritten: Dienen sie nur einem einheitlichen Verfahren der CE-Kennzeichnung oder werden darin alle relevanten geotechnischen Eigenschaften so verbindlich festgelegt, dass darüber hinausgehende nationale Vorschriften ungültig werden? Der Streit wurde durch ein Urteil des Europäischen Gerichtshofs weiter angefacht. Davon noch nicht betroffen ist der Deponiebau. Die Deponie ist ein besonderes Bauwerk, bei dem vor allem abfallrechtliche Regelungen beachtet werden müssen. In der deutschen Deponieverordnung wurde daher eine mit der Europäischen Kommission abgestimmte Gleichwertigkeitsklausel für CE-gekennzeichnete Bauprodukte verankert, die diese Besonderheit berücksichtigt. Wir zeigen, dass das in den hEN festgelegte Eigenschaftsspektrum der Bauprodukte im Wesentlichen nicht gleichwertig zu dem Spektrum ist, das sich aus den Anforderungen der Deponieverordnung ergibt. Die Qualitätssicherung der hEN, die nur eine zertifizierte werkseigene Produktionskontrolle jedoch keine Fremdüberwachung vorsieht, entspricht ebenfalls nicht den Anforderungen der Deponieverordnung. Eine CE-Kennzeichnung kann daher eine BAM-Zulassung nicht gleichwertig ersetzen. Auch für andere geotechnische Anwendungsgebiete gilt, dass die geltenden hEN die Geokunststoffe nicht ausreichend charakterisieren. Die Antwort auf die Frage, wie verbindlich diese mangelhaften hEN werden könnten, ist daher von weitreichender Bedeutung für die gesamte Geotechnik.
Tribological performance of femtosecond laser-induced periodic surface structures on titanium
(2015)
The analysis of physical and chemical properties of artefacts provides important data for answering questions that cannot be solved by historical and philological methods alone. In its individual materiality, each manuscript is the result of various influences (e.g. production, storage, restoration, preservation). Given the recent technological developments (e.g. miniaturization of structural units, enlargement of memory capacity), technical diagnostics of art and cultural objects are becoming increasingly sought after in trans-disciplinary research. In this review we present a multi-instrumental approach to the investigation of manuscripts. Several case studies will illuminate our methodology.
Using plastic jerrycans or plastic containers, dangerous goods are transported as air freight in commercial aircrafts. Liquids or gases can escape by leakage or permeation effects from these plastic containers. The German Federal Institute for Materials Research and Testing (BAM) conducted prior research which showed that the lower explosion limit can be reached when transporting dangerous goods in sea-freight containers under normal transportation situations. The presented study is motivated based on these findings. The research objective of this study is to analyze the transportation situation of dangerous goods in cargo compartments of commercial airplanes. The scope of this paper is to present the experimental method used for validating a numerical model for CFD (Computational Fluid Dynamics) simulations and to present some simulation results of the mass transport of dangerous goods in the cargo compartment.
The velocity profiles and the mass transport is calculated using numerical simulations and measured by Laser-Doppler-Anemometry (LDA) experiments. The mock-up is a generic model of a wide-body aircraft lower deck cargo compartment in a 1: 10 scale. Geometry, air exchange rates and inlet as well as outlet flow conditions in the cargo compartment are modeled using realistic boundary conditions. The commercial CFD (Computational Fluid Dynamics) code ANSYS CFX 14 is used for numerical flow simulations applying RANS (Reynolds-Averaged-Navier-Stokes) equations and turbulence models. The turbulence models studied are the renormalization group k-e-model (RNG), the BSL-Reynolds-Stress model (BSL) and the SST-k-co-model by Menter (SST).
The flow measurement with LDA in the mock-up of a cargo compartment proves to be a feasible method for producing data to validate CFD simulations. Qualitative evaluation of the results shows a good overall agreement between numerical and experimental results. The experimental validation indicates that the implemented CFD model is capable of reproducing the flow situation in the model mock-up
In this work the determination of Cd, Cu, Cr, Fe and Sb as organic and inorganic additives in in-house plastic materials (ABS, LDPE) using electrothermal vaporization combined with inductively coupled plasma optical emission spectroscopy is described. The influence of CCl2F2 as gaseous halogenation modifier was investigated. Especially for the carbide forming elements the sensitivity was improved and the memory effects were significantly reduced. Calibration was performed by external calibration and standard addition with aqueous standard solutions added directly into the sample boats. Absolute limits of detection (3s-criterion) range between 0.1 ng (Cd) and 9 ng (Fe) which corresponds to relative values of 0.1 mg kg-1 and 1.6 mg kg-1, respectively, taking 5 mg as typical sample mass. The detection limits are sufficient to monitor the element contents of plastic materials according to European directives such as European directive on the safety of toys. The developed ETV-ICP-OES method allows a fast analysis with a high sample throughput (3 minutes per analysis), low sample consumption and good trueness and precision for the analyzed elements. Sample preparation is reduced to ashing the samples in a muffle furnace. Furthermore, measurements are possible regardless of the chemical form in the additives. For verification the results obtained with the developed method were compared with measurement results of independent methods ICP-MS/OES after digestion. In addition Cd, Cr and Pb were determined in a solid plastic reference material BAM-H010 to confirm the applicability and accuracy of the method.
Commercial platforms consisting of ready-to-use microarrays printed with target-specific DNA probes, a microarray scanner, and software for data analysis are available for different applications in medical diagnostics and food analysis, detecting, e.g., viral and bacteriological DNA sequences. The transfer of these tools from basic research to routine analysis, their broad acceptance in regulated areas, and their use in medical practice requires suitable calibration tools for regular control of instrument performance in addition to internal assay controls. Here, we present the development of a novel assay-adapted calibration slide for a commercialized DNA-based assay platform, consisting of precisely arranged fluorescent areas of various intensities obtained by incorporating different concentrations of a 'green' dye and a 'red' dye in a polymer matrix. These dyes present 'Cy3' and 'Cy5' analogues with improved photostability, chosen based upon their spectroscopic properties closely matching those of common labels for the green and red channel of microarray scanners. This simple tool allows to efficiently and regularly assess and control the performance of the microarray scanner provided with the biochip platform and to compare different scanners. It will be eventually used as fluorescence intensity scale for referencing of assays results and to enhance the overall comparability of diagnostic tests.
Die grundsätzliche Eignung des Verfahrens zur Beurteilung der Passivschichtstabilität konnte mit den vorliegenden Untersuchungen nachgewiesen werden und Grenzen der Anwendbarkeit aufgezeigt werden. Es sind verschiedene Einflüsse in Parameterstudien gezielt untersucht und mit bekannten Methoden zur Beschreibung der Korrosionsbeständigkeit verifiziert worden. Das KorroPad-Prüfverfahren wirkt vorrangig oberflächenspezifisch und eignet sich zur vergleichenden Prüfung von nichtrostenden Stahloberflächen hinsichtlich ihrer Korrosionsbeständigkeit. Der Feuchtlagerung frisch bearbeiteter Oberflächen vor einer KorroPad-Prüfung kommt dabei eine große Bedeutung zu, um eine sichere Differenzierung von korrosionsanfälligen und -beständigen Oberflächen zu gewährleisten.
The automotive industry places significant importance on downsizing components to achieve greater efficiency. The goal of reducing CO2 emissions has led to the development of lightweight materials that are also able to enhance performance. In light of these aspirations, the aim of this study is to characterize two novel, high-performance steels, as well as a 'classical' gear steel for comparison with each other and currently applied materials. The gear steel underwent carburization and subsequent deep freezing treatments in an attempt to yield discrete sample groups with respect to residual austenite. The high-performance steels were heat treated as recommended by their respective manufacturers, and were not carburized. Elemental analyses were conducted by multiple methods to ensure accurate results. Residual austenite contents of the steels and the depth profiles of residual stresses were determined by X-ray diffraction (XRD). Hardness profiles were taken from the testing surfaces into the material core. The carburization of 20MnCr5 led to higher hardness and the greater concentration of carbon in the carburization zone more representative of a hardened SAE E52100, or 100Cr6/102Cr6, than of a non-carburized 20MnCr5. Residual austenite contents ranging from approximately 6–14 vol% were generated, though effectively providing only two, rather than the desired four discrete sample groups. Residual stresses from machining and carburization were measured directly at the sample surface, and from carburization alone below the surface. The high-performance steels fulfilled manufacturer expectations in terms of elemental content, hardness between 50 and 55 HRC and strongly martensitic microstructure character. Finally, slip-rolling endurance testing (T=+120 °C, 10,000,000 cycles, approximately 19 days in a factory fill engine oil) was carried out on all materials, whereby coefficient of friction distributions during testing and wear coefficients after testing were calculated. Testing was performed up to and including P0Mean=1.94 GPa (P0Max=2.91 GPa, FN=2000 N). Ultimately, the non-carburized high-performance steels showed competitive wear performance and better friction behaviour than the carburized 20MnCr5, which has been attributed to their work hardening capability.
This study aims at improving the detection of near-surface defects in magnetizable and conductive specimens by combining the measurements of eddy current, magnetic flux leakage and thermography testing. Different signal processing methods for data normalization are proposed to enable data fusion at the pixel level. These methods are applied to a test specimen which contains 10 variably-sized defects. We quantitatively evaluate the performances of a total of 29 detection methods with respect to false alarm reduction at a fixed level of true positive rate. We report that false positive rate could be reduced from 1.65% down to 0.28% by the best multi-sensor method compared to the best single-sensor performance on the smallest defect, when 50% found flaw pixels are required for successful detection.
In the last years, new approaches for the evaluation of the corrosion resistance of martensitic stainless steels were developed, which allow nearly non-destructive as well as short-term corrosion testing. This work analyzes the sensitive influence of microstructure and surface treatment on the corrosion resistance. The effect of alloy composition and microstructure, which is always present in addition to the influence of various surface treatments will be evaluated and discussed. The corrosion behavior was investigated with conventional evaluation of the pitting potential, electrochemical potentiodynamic reactivation (EPR), electrochemical noise (EN), and the 'KorroPad' (KP) technique. EPR provided information about the passivation ability and the extent of chromium content reduction due to chromium carbide precipitation in the microstructure. The use of EN and KP aims to detect the influence of different surface treatment parameters on the corrosion resistance in a nearly non-destructive way. Furthermore the results shall demonstrate the functionality and convenience of the short-term corrosion test methods EN and KP in order to gain more acceptance within the scientific community. The results will allow the extraction of surface treatment effects on the corrosion behavior of the martensitic stainless steels 1.4116, 1.4034, and 1.4021.
ln den letzten Jahren hat sich gezeigt, dass die Ermittlung des Schwellenwertes DeltaKth nach den bestehenden Standardvorschriften für verschiedene Materialien zu nichtkonservativen Werten führt. Das ergibt sich im Vergleich mit Schwellenwerten, die man mit Anrissen erhält, die hinsichtlich der Ober- und der Unterlast komplett im Druckbereich erzeugt wurden. Dort, wo die Diskrepanz auftritt, verstärkt sie sich mit abnehmendem Spannungsverhältnis. ln der vorliegenden Studie wurden an einem mittel- und einem hochfesten Stahl bei unterschiedlichen Spannungsverhältnissen Schwellenwerte bestimmt. Anwendung fanden die konventionelle Lastabsenkungsmethode nach ASTM-Standard und ein Verfahren, bei dem der Langrissscbwellenwert als Endpunkt der sogenannten Zyklischen R-Kurve erhalten wird. Dieses folgt im Wesentlichen der von Pippan et al. entwickelten Methode, ergänzt diese jedoch durch eine eigene Verfahrensvariante.
In Deutschland fallen aktuell über 5 Mio. Tonnen Hausmüllverbrennungsaschen (HMVA) pro Jahr an. Aus diesen werden nur ca. 8 % Metalle (davon ca. 1 % NE-Metalle) zurückgewonnen. Zur Beurteilung des Wertstoffpotentials werden die HMVA nach standardisierten Vorschriften beprobt, für die Analytik vorbehandelt/vorbereitet/aufgearbeitet und auf ihre Inhaltsstoffe analysiert. Im nachfolgenden Beitrag wird der Schwerpunkt auf die Probenvorbehandlung und -vorbereitung gelegt, wobei der Merkmalstransfer von der Ausgangs-(Feld-)Probe über die Laborprobe und die Prüfprobe bis zur Mess-(Analysen-) Probe am Beispiel von NE-Metallen einer nassaufbereiteten HMVA untersucht wurde. Die Ergebnisse wurden mit Hilfe statistischer Methoden bewertet. Die Ergebnisse zeigen, dass die Verteilung der NE-Metalle in den einzelnen Schritten der Probenbehandlung elementspezifisch ist. Bei Blei ist ein Erhalt der Merkmalsverteilung über alle Behandlungsschritte erkennbar. Bei Kupfer nehmen die Konzentrationen in den aufeinander folgenden Behandlungsschritten deutlich ab. Die Ursache könnte das in der Feinfraktion enthaltene metallische Kupfer mit seinen spezifischen Eigenschaften sein. -------------------------------------------------------------------------------------------------------------------------------------------
More than 5 billion tons of municipal solid waste incineration bottom ashes (MSWI BA) are generated by incineration per year in Germany. Currently only 8 % of metals (of these 1 % are non-ferrous metals) are recovered from MSWI BA. For characterization of recovery potential, MSWI BA samples have to be taken, pre-treated and analyzed according to standardized methods. This manuscript focuses on sample pre-treatment and preparation of a MSWI BA sample aiming to investigate the characteristics transfer over the process of sub-sampling from the original (field) sample to the laboratory sample, test sample until the analytical sample. All results have been evaluated with statistical methods. The results show that influence of each single pre-treatment and preparation step on metal content differs for the individual metals. For lead a conservation of characteristics distribution can be observed, while for copper a continuous decline of solid concentration is observed over all preparation steps. One possible reason may be the fact that copper is mainly contained in the fine fraction as metallic copper with specific properties.
We report on the formation of polymer-stabilized superparamagnetic single-core and multi-core maghemite nanoparticles. The particle formation was carried out by coprecipitation of Fe(II) and Fe(III) sulfate in a continuous aqueous process using a micromixer system. Aggregates containing 50 primary particles with sizes of 2 nm were formed at a reaction temperature of 30 °C. These particles aggregated further with time and were not stable. In contrast, stable single-core particles with a diameter of 7 nm were formed at 80 °C as revealed by small-angle X-ray scattering (SAXS) coupled in-line with the micromixer for particle characterization. X-ray diffraction and TEM confirmed the SAXS results. X-ray absorption near-edge structure spectroscopy (XANES) identified the iron oxide phase as maghemite.
Particle size modality in bi-modal iron oxide suspensions was resolved by exploiting complex ac-susceptibility (ACS), small angle X-ray scattering (SAXS) and photon cross-correlation spectroscopy. To explain dynamic magnetic response of bi-modal suspensions, the Debye model was expanded to a linear superposition form allowing for the contribution of both particle fractions. This modified and adopted model is able to resolve the bi-modal particle size distributions. The SAXS curves of mono- and bi-modal suspensions were fitted well using a Monte Carlo simulation scheme, allowing the detection of bi-modal particle size distributions with high precision.
Resovist® originally developed as a clinical liver contrast agent for Magnetic Resonance Imaging exhibits also an outstanding performance as a tracer in Magnetic Particle Imaging (MPI). In order to study the physical mechanism of the high MPI performance of Resovist®, we applied asymmetric flow fieldflow fractionation (A4F) and static magnetic fractionation (SMF) to separate Resovist® into a set of fractions with defined size classes. As A4F based on an elution method separates MNP according to their hydrodynamic size, SMF fractionates a particle distribution by its magnetic moment. The obtained fractions of both separation techniques were then magnetically characterized by magnetorelaxometry measurements to extract the corresponding effective magnetic anisotropy and hydrodynamic size distribution parameters. Additionally, the MPI performance of each fraction was assessed using magnetic particle spectroscopy. With both separation techniques fractions (normalized to their iron amount) an MPI signal gain of a factor of two could be obtained, even though the distribution of effective anisotropy and hydrodynamic size were significantly different. Relating these findings to the results from magnetic characterization allows for a better understanding of the underlying mechanisms of MPI performance of Resovist®. This knowledge may help to improve the design of novel MPI tracers and development of separation methods.
Shedding light onto the spectra of lime: Raman and luminescence bands of CaO, Ca(OH)2 and CaCO3
(2015)
In microscopy studies of 19th-century cement stone, we found free lime in the form of darkened spherical structures, as they were described in the literature already. When trying to determine their phase composition by Raman spectroscopy, we encountered contradictive assignments in literature spectra of the lime phases CaO, Ca(OH)2 and CaCO3 and observed strong spectral features that have been ignored or erroneously assigned so far. In this study we present Raman spectra of pure lime phases and of a naturally grown calcite crystal, burnt limestone (quick lime, mainly CaO), aged slaked lime putty (mainly Ca(OH)2), and carbonated lime putty (mainly CaCO3). Based on the results, we shed light mainly onto these two questions: (1) Does CaO have a Raman spectrum? (2) Which features in the spectra are luminescence bands that could be (and already have been) misinterpreted as Raman bands? We proof our assignment of luminescence bands in lime phases by using three different laser wavelengths for excitation, and give hypotheses on the origin of the luminescence as well as practical advices on how to identify these misleading features in Raman spectra. This article is mainly addressed to users of Raman spectroscopy in different fields of material analysis who might not be aware of the presence of interfering bands in their spectra.
Thermal ionisation, also known as surface ionisation, was one of the first ionisation techniques developed for mass spectrometry, having been invented as early as 1918. The ionization process, described by the empirically derived “fractionation laws”, is widely understood. Isotope ratio measurements can be achieved with high precision and accuracy. Due to this, thermal ionisation has paved the way for great scientific achievements including: the discovery of new isotopes, the determination of radioactive half-lives and atomic weights of the elements, the accurate determination of the age of the earth and investigations on human society in the past such as mobility and trade. TIMS is still regarded as ‘golden standard’ in isotope ratio measurements. Thus the method is a reference technique that remains at the forefront of isotopic analysis particularly in the fields of metrology. A concise overview is given here of the technical background of thermal ionisation as well as the numerous applications of this technique in earth sciences, industry, metrology, and nuclear forensics.
This paper indicates that the tribological behavior under dry sliding of a Fe3Al-niobium carbide (NbC) composite prepared by pyrometallurgical synthesis was compared to NbC-based hard metals bonded by cobalt or Fe3Al. The dry sliding wear resistance (0,1-7/10 m/s) of the present Fe3Al-NbC with ∼60% NbC was close to those known of NbC-based hard metals. No grain pull-outs or fragmentations of the NbC grains were seen in the wear tracks, as a metallurgical interphase was formed between matrix and NbC grains.
Measurement strategies
(2015)
Designing an appropriate measurement strategy for a particular analytical question is not always obvious, since a number of factors have to be considered, whereby some of them might be difficult to define. A set of key questions generally precede the experimental design in analytical measurements and help to choose the measurement strategy, which is fit for the intended use – in the particular case of the content of this book – either for quantification, elemental ratio or isotope ratio analyses, accordingly.
Maintenance, Repair and Overhaul (MRO) is acquiring increasing commercial and socio-economic significance. For products and goods with high investment costs and a long lifespan, especially in the sectors of energy and transportation, a considerable portion of commercial profits are generated by after-sales services. In the field of research and development, not enough attention has been paid so far to tasks and approaches involving MRO. The field thus has a limited scientific background, despite a high potential in the business sector for technological and scientific optimization. The challenges and chances of MRO for sustainable enterprises will be explained with reference to the Fraunhofer Innovation Cluster Maintenance, Repair and Overhaul in Energy and Transport. The developments and project results of the four fields of innovation »Cleaning«, »Repair and Overhaul«, »Condition Monitoring and Diagnosis«, as well as »MRO Planning and Digital Assistance« will be explained.