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Eingeladener Vortrag
- nein (1024)
Biofilms living on gold (Au) grains play a key role in the biogeochemical cycle of Au by promoting the dispersion of Au via the formation of Au nanoparticles as well as the formation of secondary biomorphic Au. Gold grains from Queensland, Australia, are covered by a polymorphic, organic-inorganic layer that is up to 40 μm thick. It consists of a bacterial biofilm containing Au nanoparticles associated with extracellular polymeric substances as well as bacterioform Au. Focused ion beam (FIB) sectioning through the biofilm revealed that aggregates of nanoparticulate Au line open spaces beneath the active biofilm layer. These aggregates (bacterioform Au type 1) resulted from the reprecipitation of dissolved Au, and their internal growth structures provide direct evidence for coarsening of the Au grains. At the contact between the polymorphic layer and the primary Au, bacterioform Au type 2 is present. It consists of solid rounded forms into which crystal boundaries of underlying primary Au extend, and is the result of dealloying and Ag dissolution from the primary Au. This study demonstrates that (1) microbially driven dissolution, precipitation, and aggregation lead to the formation of bacterioform Au and contribute to the growth of Au grains under supergene conditions, and (2) the microbially driven mobilization of coarse Au into nanoparticles plays a key role in mediating the mobility of Au in surface environments, because the release of nanoparticulate Au upon biofilm disintegration greatly enhances environmental mobility compared to Au complexes only.
EBSD is nowadays a common technique for the characterization of crystalline microstructures in scanning electron microscopy. The diffraction patterns are often interpreted by superimposing individual Kikuchi bands which are geometrically described by band edges derived from Braggs law. For the typically very simple crystal structures of technically applied materials, such a simplification of the Kikuchi pattern interpretation works sufficiently well, especially for orientation determinations as a main application of EBSD. The more complex crystal structures, however, are a challenge for EBSD indexing routines which in such cases often fail unpredictably. The use of only the intensities of single reflectors for a description of the Kikuchi band intensity and as a cut-off criterion for a pre-selection of the strongest bands are not satisfactory. Often the result will match too many phases, or there are certain deviations in the intensity prediction which must be adapted manually. This is already problematic if one is absolutely sure that the patterns are originating from the expected phase and it becomes a very questionable procedure for an unknown phase.
Modern EBSD systems perform diffraction pattern “quality” (PQ) calculations, essentially measurements of the contrast of the brighter bands in the pattern above background, for every pattern analyzed. Since the calculations are independent of EBSD indexing, data are generated from all points on the analyzed sample surface, regardless of indexability or the state of the material beneath. EBSD maps generated from PQ data are like microstructurally sensitive SEM images, collected at EBSD speeds and grid resolutions, with contrast arising from phase density, crystal structure, crystallographic orientation, grain boundary location, near-surface plastic strain, coating density/thickness, and to some extent topography. Grain boundaries and other aspects of sample microstructure are readily revealed, so the PQ map is a very useful characterization tool in its own right, and serves as a reference for EBSD maps generated from indexing-derived data, such as orientation, grain boundary character, phase distribution and strain maps.
The halophilic bacterium Halomonas elongata takes up the compatible solute ectoine via the osmoregulated TRAP transporter TeaABC. A fourth orf (teaD) is located adjacent to the teaABC locus that encodes a putative universal stress protein (USP). By RT-PCR experiments we proved a cotranscription of teaD along with teaABC. Deletion of teaD resulted in an enhanced uptake for ectoine by the Transporter TeaABC and hence a negative activity regulation of TeaABC by TeaD. Atranscriptional regulation viaDNA binding could be excluded. ATP binding to native TeaD was shown by HPLC, and the Crystal structure of TeaD was solved in complex with ATP to a resolution of 1.9 A ° by molecular replacement. TeaD forms a dimer-dimer complex with one ATP molecule bound to each monomer, which has a Rossmann-like R/β overall fold. Our results reveal an ATP-dependent oligomerization of TeaD, which might have a functional role in the regulatory mechanism of TeaD. USP-encoding orfs, which are located adjacent to genes Encoding for TeaABC homologues, could be identified in several other organisms, and their physiological role in balancing the internal cellular ectoine pool is discussed.
For the characterization of disperse and porous solids, usually single gas adsorption(GA) is employed. In the case of liquid adsorption (LA), the extraction of information on solids immediately becomes a more sophisticated matter since information on geometric as well energetic parameters of the solids is both superposed by liquid-mixture effects and displayed in excess terms. We have to ask if reliable solid parameters can be also obtained from LA isotherms. The enlarged data bank of gas and liquid adsorption measurements enables us to change systematically solid parameters (e.g., the pore width of MCM-41, the pore entrances of SBA-16, chemical heterogeneity) and to study in this way the influence of solid parameters on LA.
Certification report for the reference materials ERM-AE102a, -AE104a, -AE120, -AE121 and -AE122
(2010)
Isotope reference materials are essential to enable reliable and comparable isotope data. Besides the correction of mass fractionation or mass discrimination isotope reference materials are indispensible for validation and quality control of analytical procedures. This article describes the production and certification of a set of five isotope reference materials ERM-AE102a, 104a, AE120, 121 and 122, for boron isotope analysis. The isotopic composition of all materials has been adjusted by mixing boron mother solutions enriched in 10B or 11B with a boron mother solution having natural-like isotopic composition under full gravimetric control. All mother solutions have been analysed for their boron mass fraction as well as their boron isotopic composition by TIMS using IDMS as calibration technique. For all five reference materials the isotopic composition obtained on the basis of the gravimetric data agrees very well with the isotopic composition obtained from different TIMS techniques. Performed stability and homogeneity studies show no significant influence on the isotopic composition as well as on the related uncertainties.
The certified isotope abundances for 10B are 0.29995 (27) for ERM-AE102a and 0.31488 (28) for ERM-AE104a. The certified δ11B values are -20.2 (6) ‰ for ERM-AE120, 19.9(6) ‰ for ERM-AE121 and 39.7 (6) ‰ for ERM-AE122.
Together with the formerly certified ERM-AE101 and -AE103 a unique set of seven certified reference materials (CRM) for boron isotope analysis is now available from BAM.
Hochtemperaturtribologie
(2010)
Die Temperatur ist eine fundamentale Beanspruchungs- bzw. Einflussgröße für alle tribologischen Systeme. Für die in zahlreichen tribologischen Systemen benötigten Schmierstoffe liegen die thermischen Stabilitätsgrenzen bei etwa 400?°C. Es wird die tribologische Prüftechnik für Tribomaterialien beschrieben, die für den Einsatz in tribologischen Systemen bei hohen Betriebstemperaturen verwendbar sind. Ausgehend von metallurgischen Lösungsansätzen aus der Tribologieforschung werden Anwendungsmöglichkeiten hochtemperaturbeständiger Ingenieurwerkstoffe mit Beispielen aus der Automobiltechnik (Luftlagerung von Turboladern, Leistungssteigerung von Bremsmaterialien), der Fertigungstechnik (Standzeitverlängerung von Werkzeugen) und dem chemischen Anlagenbau (Effizienzsteigerung von Kühlkreisläufen) dargestellt.
Verification of activity release cpmpliance with regulatory limits within spent fuel transport casks
(2010)
Verification of activity release compliance with regulatory limits within spent fuel transport casks
(2010)
The Witness - Screen Test
(2010)
IAPRI World conference on packaging - Proceedings of the 17th IAPRI world conference on packaging
(2010)
Subjecting a thin NiTi specimen to uniaxial tension often leads to a localized martensitic transformation: macroscopic transformation bands form and propagate through the specimen, separating it into regions of fully transformed martensite and original austenite. In the present study, the alternating current potential drop (ACPD) technique is used to analyze the change in electrical resistance of ultra-fine grained NiTi wires subjected to a broad range of thermo-mechanical load cases: (i) uniaxial tensile straining at constant temperatures (pseudoelastic deformation); (ii) cooling and heating through the transformation range at constant load (actuator load case); (iii) a combination of mechanical and thermal loading. We monitor the ACPD signals in several zones along the gauge length of specimens, and we demonstrate that a localized type of transformation is a generic feature of pseudoelastic as well as of shape memory deformation. Moreover, the ACPD signals allow to differentiate between temperature-induced martensite (formed during cooling at no or relatively small loads), stress-induced martensite, and reoriented martensite (formed under load at low temperatures).
The paper presents technical details of the drop test performance as well as some experimental results of tests carried out with the Japanese 'Yoyushindo-disposal' waste container for intermediate depth disposal. The tests were accompanied by various metrology to collect data as basis for safety assessment.
This paper presents three examples of applied
numerical modeling and inverse profiling in electromagnetic
non-destructive testing. In the first example, we discuss
numerical modeling and optimization of eddy current sensors for
in-line inspection of hot wire steel. To detect longitudinal cracks
a series of new sensors are modelled and optimized by numerical
modeling and is successfully tested. The second example presents
the application of a time-domain technique to reconstruct the
unknown permittivity and electric conductivity profile of a onedimensional
slab of finite length. The inverse scattering problem
is solved by an Invariant Embedding Method which requires a
finite time trace of reflection data and therefore is suitable for
reconstructing the material parameters in real-time. The
implemented method is validated against synthetic and measured
Time Domain Reflectometry data. The third example
demonstrates the application of the Contrast Source Inversion
method to reconstruct the 2-D permittivity profile of a beech
tree. Thus, the discussed applications present an identified need
of numerical modeling and inverse profiling in electromagnetic
non-destructive evaluation.
Lamb waves travel in plates and hollow cylinders over large distances and propagate with multiple mode shapes. Therefore the waves can be used for integrity tests of large scale structures. Each propagating wave mode has a unique dispersive character and a frequency dependent vibration pattern. Therefore, by interacting with flaws each mode is assumed to generate an individual reflection pattern depending on the flaw type, flaw orientation and size. To extract this information a frequency as well as wave number dependent mode excitation is required ensuring a single mode excitation. The challenge, however, is to control the selective mode excitation electronically to allow a sequence of consecutive tests with different wave modes to collect the data. A method is proposed using phased array wedge transducers with fluid coupling for normal force excitation of Lamb wave modes. The excitation principle is investigated analytically on plates by modelling the wave generation in the wedge and the coupling between wedge and structure. The analytical results of the excitation principle are validated by corresponding experiments where the field patterns on the wedge surface and on the plate were scanned using a laser vibrometer. The directivity of the radiated field is investigated together with the direction dependent analysis of the mode content.
In this contribution a simulation tool is developed to compute the energy skewing angles and energy coefficients
for the reflected and refracted plane waves in following general cases: (1) reflection and refraction
of plane elastic waves at an interface between isotropic and transversely isotropic solid, (2) reflection
and refraction of plane elastic waves at an interface between transversely isotropic and isotropic solid, (3)
reflection and refraction of plane elastic waves at an interface between two general transversely isotropic
solid and (4) reflection of plane elastic waves from a stress free boundary of a transversely isotropic solid.
Computational results for analytically evaluated acoustic wave energy skewing angles and energy reflection
and transmission coefficients in acoustically anisotropic materials such as austenitic steel materials
exhibiting columnar grain orientation are presented. The obtained results show that the acoustic energy
skewing angles and coefficients in austenitic steel materials strongly depend upon the columnar grain
orientation and are less influenced by the grain orientations which are parallel and perpendicular to the
interface.
When dealing in ultrasonic testing with inhomogeneous and anisotropic material structure such as
diverse types of components made from austenitic or nickel based cast, which are currently used
for modern power plant concepts, data interpretation is quite difficult. For better understanding of
the complex interaction between the sound field and the component under test, the mathematical
modeling of sound propagation in solids is a substantial task to increase the probability of
detection of relevant defects.
First we present a mathematical approach for modeling the three dimensional transient
particle displacement as a function of time in each point in a half space excited by an impulsive
point load at the surface. The transient ultrasonic field of a rectangular array element is calculated
with this approach by a point source synthesis. Based on this solution we model the wave
propagation of a phased array transducer by time delayed superposition of the wave field of the
transducer elements.
Next we use an electrodynamic technique to visualize the grazing sound field at the surface
of a test block radiated by a phased array probe. By detecting the grazing beam at the samples
surface with a small electrodynamic probe, we measured the particle displacement as a function of
time. It allows for measuring the displacement in all three spatial directions. This comprises the
detection of the horizontal and vertical particle displacement with respect to the surface and thus
also the detection of longitudinal and shear waves is possible.
The calculated and measured wave fields will be compared for different delay laws in
isotropic and transversely isotropic media. The results support the theoretical activities to model
the wave propagation and to find optimal testing parameters for different components and
configurations.
The classification of solid oxidizers according to the GHS (Globally Harmonized System of Classifica-tion and Labelling of Chemicals) and according to regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and implemented in all carrier domains as transport by road, railway, sea, air) is performed on the basis of the results of the UN test O.1 (―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Danger-ous Goods, Manual of Tests and Criteria, Fifth revised edition, United Nations, New York and Geneva, 2009). This test was introduced into the UN Test Manual in 1995 as a replacement for a similar test from 1986. Even though the O.1 test is much better than the previous one there are still many prob-lems with this test. For this reason the IGUS-EOS working group (international group of experts on the explosion risks of unstable substances – working group: energetic and oxidizing substances) installed an ad-hoc working group in 2002 assigned with the task of proposing solutions for the existing prob-lems. The adequacy of such proposals has to be proven preferably by interlaboratory comparison (interlaboratory test) before they are presented to the UN Sub Committee for adoption into the UN Test Manual. The present report is the evaluation of an interlaboratory test which was designed by the Ad-hoc working group in order to find out whether the current method of comparing combustion times of test mixtures with those of reference mixtures is suitable in principle and whether some approaches for improvement of the method can be identified.
Die Ressourcenverknappung und steigende Preise rücken nachhaltiges Wirtschaften und die Wiederverwertung von Abfällen in den Blickpunkt der Forschung. Bauabfälle sind in Deutschland – mit 72,4 Mio.t im Jahr 2004 – der größte Abfallstrom. Es wird ein Überblick über den Stand der Technik zur Aufarbeitung und Verwertung von Bauabfällen gegeben und die Anforderungen an Bauabfälle, die als Sekundärrohstoff eingesetzt werden sollen, diskutiert. Die Forschung im Baustoffrecycling bezieht sich sowohl auf neue Aufbereitungstechniken als auch auf die Charakterisierung der Recyclingmaterialien sowie auf deren Einfluss auf die Betonqualität. Die Eignung und Verwertung von Bauabfällen als Sekundärrohstoffe für Baustoffe wird anhand ihrer chemischen Zusammensetzungen mit Hilfe von ternären Diagrammen diskutiert.----------------------------------------------------------------------
An overview about quantity of construction and demolition waste (CDW) and a state of the art of the reuse is given. The technology is described, which is applied for the processing of CDW in a stationary plant. The requirements on recycled aggregates, which shall be used in road construction or in manufacturing of concrete, can be divided in such related to the material and physical properties and such related to the environmental properties. The rules give guidance on the composition with the aim of excluding the constituents with unfavourable features. The environmental standards which yet in discussion are give threshold of the leachable components in recycled aggregates. The material potential of building waste is discussed. Information on the chemical composition of recycled materials is compared with the composition of pure materials. With the aid of ternary charts such building materials are identified, in which the recycled materials can be used as recycled feedstock.
Zwei Bildhauermodelle aus dem Georg-Kolbe-Museum Berlin standen
zur Restaurierung an. Das kleinere, 'Lucino' (1920), 41cm, wurde hochauflösend
mit CT gemessen, da mittels CT sowohl der Herstellungsprozeß einer Gipsstatue
als auch der innere Zustand, wie Ergänzungen, Klebungen und Armierungen,
festgestellt werden können. Aus den CT Bildern ergab sich eine für die vorher vermutete
Gipszusammensetzung ungewöhnliche innere Struktur. Mit einer Freihand
bedienten Röntgenpistole zur Messung der Röntgenfluoreszenz wurde daraufhin die
Zusammensetzung des Materials der Statuette als Terracotta bestimmt. Durch den
Einsatz von Helium als Spülmittel konnten auch leichte Materialien nachgewiesen
und so eine Unterscheidung zwischen Gips und gebranntem Ton durchgeführt werden.
Aus den CT Daten wurde eine virtuelle Darstellung der äußeren Geometrie gewonnen.
Ein damit versuchsweise erstelltes Replik (Rapid Prototyping, 3D-Drucker,
TU-Berlin) entsprach nicht den Anforderungen des Museums zur Erstellung einer
Gußform für eine Bronzekleinserie der Statuette.
Die zweite Statue, die 'Große Nacht' (1930) ist mit ihrer Größe von 2,12m und aufgrund
des durch korrodierende Metallarmierung verursachten Schadensbildes nicht
mehr transportfähig. Eine in-situ Untersuchung mit dem mobilen Tomographen, der
in den 1980ern zur Untersuchung von Bäumen gebaut und jetzt mit einem modernen
Flachdetektor und einer Röntgenröhre ausgestattet ist, wird vorgestellt. Die Möglichkeiten
der in-situ CT für große Skulpturen werden anhand der Ergebnisse diskutiert.
In internationalen Normen und Regelwerken werden zur Überprüfung der thermischen Belastbarkeit von Umschließungen für gefährliche Güter Versuche vorgeschrieben, die u. a. Vorgaben hinsichtlich der Wärmebelastung enthalten. Diese Vorgaben beziehen sich i. d. R. auf ein Kerosin- oder Heizölfeuer, denen die Gefahrgutumschließungen ausgesetzt werden müssen. Versuche mit diesen Medien belasten jedoch die Umwelt in einem heute nicht mehr tragbaren Umfang. Als alternatives Medium bietet sich verflüssigtes Propangemisch (LPG) an. Zur Ermittlung eines äquivalenten Wärmeeintrags mussten vergleichende Versuche durchgeführt werden. Hierzu hat die BAM Bundesanstalt für Materialforschung und -Prüfung neue Brandprüfstände entwickelt und die nachfolgend beschriebenen Untersuchungen durchgeführt.
The special properties of high molecular weight polyethylene (HMW-PE) and ultra high molecular
weight polyethylene (UHMW-PE) result basically from their extreme chain lengths and their high
degree of crystallinity. As high-performance polymers, they are used for a variety of applications.
UHMW-PE in particular is often utilized for endoprothesis (due to its excellent slip and wear
properties) and due to its high hydrogen content as a neutron moderator in casks for storage and
transport of radioactive materials.
To prepare the material for instance for its use as a total joint replacement, it is exposed to radiation
for several reasons, such as sterilization and crosslinking, leading to partial improvement of the
mechanical properties (e.g. fracture toughness, crack propagation resistance, wear resistance) and
better chemical stability.
To be applicable for long term radiation shielding purposes for instance over a period of 40 years,
PE has to withstand any type of degradation affecting safety relevant aspects.
The scope of our investigation comprises an estimation of the radiation impact on the molecular and
supra molecular structure of two types of PE and to what extent these changes are detectable by
thermo-analytical (TA) methods, such as Differential Scanning Calorimetry (DSC), Thermo
Mechanical Analysis (TMA), Dynamic Mechanical Analysis (DMA) and Thermo Gravimetric
Analysis (TGA). Additionally FT-IR spectroscopy as well as density and gas sorption
measurements were carried out.
Due to the poor solubility of HMW-PE and UHMW-PE, some classical analytical techniques are
not applicable. But TA-methods represent a feasible approach to detect structural and
morphological features of these materials as well as changes caused by external influences, such as
thermal treatment and/or irradiation. With the combination of the applied TA-techniques it is
possible to distinguish between crosslinking and degradation.
Packages for the transport of radioactive material are generally equipped with specific
structures (basket) to support the radioactive content in defined position. The safety function
of the basket depends on the kind of transported inventory. In case of transport cask for spent
fuel, the basket design has to ensure the subcriticality of the fissile material in all conditions
of transport in particular. Therefore the evaluation of structural integrity and neutron
absorption capability of the basket is an important part of complete safety analysis. Sufficient
heat transfer to maintain fuel assembly and cask temperature within allowable limits has to be
verified as well. Corrosion resistance is an additional requirement on basket materials owing
to contact with water during loading and unloading operations.
Computational and experimental methods or their combination along with additional material
and component tests can be used to analyse the mechanical and thermal basket behaviour
under transport conditions defined in IAEA regulations. By deciding between the analysis
methods, the design features (including material selection concept) as well as specific safety
function should be accounted.
In approval procedures of transport packages for radioactive materials, the competent
authority mechanical and thermal safety assessment is carried out in Germany by BAM. Some
questions of safety evaluation of basket designs are discussed in this paper based on the BAM
experience within approval procedures. The paper focuses primarily on the mechanical
behaviour of baskets with regard to the assumptions that have to be used in the criticality
safety demonstration. The state of the art methodologies for computational basket stress and
deformation analysis as well as for interpretation of drop tests results are presented.
In order to prevent incidents in the
industrial production of Teflon® from
Tetrafluoroethylene (TFE), the safety related
aspects of the self-heating process of TFE must
be taken into account. Simulations of this self
heating process were performed with COMSOL
Reaction Engineering Lab® and COMSOL®
COMSOL Multiphysics®. A complex reaction
net was employed, resulting in a model allows
for a good agreement with experimentally
achieved results.
Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon
(2010)
We analyze the contrast reversal of Kikuchi bands that can be seen in electron backscatter diffraction (EBSD) patterns under specific experimental conditions. The observed effect can be reproduced using dynamical electron diffraction calculations. Two crucial contributions are identified to be at work: First, the incident beam creates a depth distribution of incoherently backscattered electrons which depends on the incidence angle of the beam. Second, the localized inelastic scattering in the outgoing path leads to pronounced anomalous absorption effects for electrons at grazing emission angles, as these electrons have to go through the largest amount of material. We use simple model depth distributions to account for the incident beam effect, and we assume art exit angle dependent effective crystal thickness in the dynamical electron diffraction calculations. Very good agreement is obtained with experimental observations for silicon at 20 key primary beam energy.
Reinforced concrete bridge decks are exposed to several types of deterioration processes: corrosion, alkali silica reaction, carbonation, shrinkage, freeze thaw actions, and so forth. The most commonly found problem is corrosion-induced bridge deck delamination. Previous studies have shown that surveys of bridges relying on a single nondestructive evaluation (NDE) technology provide limited information about the condition of concrete bridge decks. To overcome limitations of individual technologies, a complementary approach using several NDE technologies should be used in bridge deck evaluation. The presented approach utilizes a suite of NDE technologies, namely, impact echo (IE), ultrasonic surface waves (USW), ground-penetrating radar (GPR), half-cell potential (HCP), and electrical resistivity (ER). The suite of NDE technologies was implemented in the evaluation of bridge decks on nine bridges in Iowa. The NDE was complemented by ground-truth measurements on the cores extracted from all nine bridge decks. Condition assessment with the five NDE technologies has clearly shown their advantages and limitations. For example, the GPR surveys provided assessment of concrete deterioration at relatively high speeds of data collection. In contrast, IE provided high accuracy in detection and characterization of delaminations in the deck but at a lower testing speed. HCP and ER tests provided assessment of the likelihood of corrosion, whereas the USW test provided accurate assessment of the effects of deterioration processes and defects on mechanical properties, primarily the degradation of the elastic modulus. Most important, the survey showed the advantages of use of multimodal NDE surveys in the comprehensiveness of condition assessment of concrete bridge decks.
Commercially available linear alkylbenzenesulfonates (LASs) are a mixture of various homologues and isomers, leading to 20 major species. In this work we investigated the commercial product by liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectrometry (LC-SPE-NMR/MS). The commercial product was separated into 17 fractions by liquid chromatography (LC). After chromatographic separation, 5% of the flow was split to a mass spectrometer (MS) while 95% was send to post-column solid phase extraction cartridges for enrichment of the analytes (LC-SPE). After elution from the SPE-cartridges a NMR-spectrometer equipped with a cryo-probe was used for the characterisation of the different LASs species. For the first time H-1-1D and H-H-COSY spectra for 14 LASs species out of 20 major isomers are presented, whereas the 6 remaining species are detected as mixtures in 3 H-1-1D and H-H-COSY spectra. These data were used to correlate the chromatographic retention of the LASs isomers to the substitution pattern of the alkyl chain.
The paper describes past and present efforts in modeling of laser-induced plasma and overviews plasma diagnostics carried out by pump-probe techniques. Besides general information on existing plasma models, the emphasis is given to models relevant to spectrochemical analysis, i.e. models of radiating plasma. Special attention is paid to collisional-radiative (CR) and collisional-dominated (CD) plasma models where radiative processes play an important role. Also, calibration-free (CF) models are considered which may endow with the possibility for standardless spectroscopic analysis. In the diagnostic part, only methods based on the use of additional diagnostic tools (auxiliary lasers, optics, and probes) are described omitting those based on plasma own radiation. A short review is provided on image-based diagnostics (shadowgraphy, schlieren, and interferometry), absorption and fluorescence, Langmuir probe, and less frequently used cavity ringdown and Thomson scattering methods.
Pulse thermography of concrete structures is used in civil engineering for detecting voids, honeycombing and delamination. Quantitatively realistic numerical 3D simulation is difficult due to the arising boundary layer at the heated surface and unreliable information about material parameters and environmental conditions. We address both issues by a semi-analytic reformulation of the heat transport problem and by parameter identification. Numerical results are compared with measurements of a test specimen.
Ground penetrating radar (GPR) was used to characterize the frequency-dependent dielectric relaxation phenomena in ordinary Portland cement (OPC) hydration in concrete changing from fresh to hardened state. The study was experimented by measuring the changes of GPR A-scan waveforms over a period of 90 days, and processed the waveforms with short-time Fourier transform (STFT) in joint time-frequency analysis (JTFA) domain rather than a conventional time or frequency domain alone. The signals of the direct wave traveled at the concrete surface and the reflected wave from an embedded steel bar were transformed with STFT, in which the changes of peak frequency over ages were tracked. The peak frequencies were found to increase with ages and the patterns were found to match closely with primarily the well-known OPC hydration process and secondarily, the evaporation effect. The close match is contributed to the simultaneous effects converting free to bound water over time, on both conventional OPC hydration and dielectric relaxation mechanisms.
The influence of humin preparations obtained from low-moor peat by the mechanochemical method on the changes in the microflora number and hydrocarbon composition in oil-polluted soils was studied. The intense growth of the microorganisms in number especially in the oil-polluted soil was observed upon the application of humin acids (at a concentration of 0.005 wt %) extracted from mechanically processed peat. In this case, the content of the extracted bitumoids decreased down to 40 wt %. The soil microflora stimulated by the humin preparations was shown to have highly destructive oil-oxidizing activity reflected in the indices of the hydrocarbon biodegradation. The mechanochemical activation of peat allows raising the efficiency of extracting the humic acids and can be a reason for increasing the availability of their individual components and parts of molecules, including micro- and macroelements that are used by microbial cells as sources of nutrition and energy.
In contrast to classical low temperature polymer electrolyte fuel cells (LT-PEFCs), the membrane conductivity in high temperature polymer electrolyte fuel cells (HT-PEFCs) (operating temperature ~ 160 °C) is based on proton transport within phosphorus-oxygen acids at different levels of hydration, orthophosphoric acid (H3PO4) being the simplest example. We present for the first time in-situ synchrotron X-ray radiography measurements applied to a HT-PEFC to gain insight into the local composition of the membrane electrode assembly (MEA) under dynamic operating conditions. Transmission changes during the radiographic measurements exhibit a clear influence of the formation of product water on the membrane composition.
The impact-echo method has been successfully applied to identify defects inside concrete. In addition, to detect ungrouted tendon ducts in a large concrete slab, a scanning impact-echo technique is developed. However, since resonant frequencies in the spectrum responsible for the travel paths via defects are only taken into account, the method could lead to erroneous results due to complicated spectra obtained in the tests. Consequently, Stack Imaging of spectral amplitudes Based on Impact-Echo (SIBIE) procedure has been developed to improve the data interpretation. Conventionally, SIBIE is applied to a single measurement data and a point information of defects is obtained at the area, where the impact test is performed. In this study, SIBIE is applied to scanning impact-echo data. Locations of ungrouted tendon ducts embedded in a large concrete specimen are investigated. In order to visualize the whole cross-section tested, the SIBIE analysis is modified, introducing an elliptical integration mode. It is demonstrated that ungrouted tendon ducts are successfully located by the modified SIBIE analysis, whereas results of the conventional B-scan analysis are not so good as the modified SIBIE analysis.
Improved large mesoporous ordered molecular sieves - Stabilization and acid/base functionalization
(2010)
The preparation of nanoporous materials with enhanced stability using an improved synthesis route using reactive inorganic silica and alumina species is reported. This way improved mesoporous molecular sieves were obtained. The synthesized aluminum substituted mesoporous molecular materials (Al-MMS) contain very large pores of 50200 Å size combined with an improved pore wall thickness. Increased wall thickness and Al substitution lead to an improved chemical stability against alkaline solution. The textural, structural and acid properties are investigated by physico-chemical methods. The catalytic performance acidic materials was tested in the benzoylation reaction; amino functionalized materials were studied in the base catalyzed Michael addition.
Thin metal-filled polyterafluoroethylene films with various metal concentration were produced by co-deposition in vacuum. Metal nanocluster size increased with metal concentration. Films were heated up to 300 degrees C, their optical spectra were recorded during heating. The changes in plasmon band shape and wavelength of the nanocluster ensemble during heating are not linearly related with metal concentration and heating temperature. This is caused by different thermal behavior of the complex processes, which are taking place in each of the two materials present in the film. The metal cluster size and optical properties of the whole ensemble can be purposefully formed by varying metal nature, its concentration and annealing temperature of the film. Nano- and micro-domains with properties different from original film were generated by focused excimer laser or electron beam. Gold-filled PTFE nano-structured films were used as substrate for surface enhanced Raman scattering measurements of ultrathin film of Rhodamine 6G dye.
Synchrotron radiation-based microcomputed tomography (SR-µCT) has become a valuable tool in the
structural characterization of different types of materials, achieving volumetric details with micrometre
resolution. Biomedical research dealing with porous polymeric biomaterials is one of the research fields
which can benefit greatly from the use of SR-µCT. This study demonstrates that current experimental setups
at synchrotron beamlines achieve a sufficiently high resolution in order to visualize the positions of
individual cartilage cells cultivated on porous gelatine scaffolds made by a freeze-structuring technique.
Depending on the processing parameters, the pore morphology of the scaffolds investigated was changed
from large-pore sized but non-ordered structures to highly directional and fine pored. The cell-seeded
scaffolds were stained with a combined Au/Ag stain to enhance the absorption contrast in SR-µCT. While
only some cells showed enhanced absorption contrast, most cells did not show any difference in contrast
to the surrounding scaffold and were consequently not detectable using conventional greyscale threshold
methods. Therefore, using an image-based three-dimensional segmentation tool on the tomographic data
revealed a multitude of non-stained cells. In addition, the SR-µCT data were compared with data obtained
from scanning electron microscopy, energy dispersive X-ray spectroscopy and histology, while further
linking the initial cell density measured via a MTT assay to the pore size as determined by SR-µCT.
This review introduces multifunctional optical nanosensors based on surface-enhanced Raman scattering (SERS) and demonstrates their application in live cells. The novel nanosensors have the potential to improve our understanding of cellular processes on the molecular level. The hybrid sensor consists of gold or silver nanoparticles with an attached reporter species. The sensor can be detected and imaged based on the SERS signature of the reporter. This results in several advantages, such as high spectral specificity, multiplex capabilities, improved contrast, and photostability. SERS sensors not only highlight cellular structures, based on enhanced Raman spectra of intrinsic cellular molecules measured in the local optical fields of the gold nanoparticles, they also provide molecular structural information on their cellular
environment. Moreover, the SERS signature of the reporter can deliver information on the local pH value inside a cell at subendosomal resolution. SERS sensors are suitable for one- and two-photon excitation.
In the approval procedure of transport packages for radioactive materials, the competent authority mechanical and thermal safety assessment is carried out in Germany by BAM Federal Institute for Materials Research and Testing.
The combination of experimental investigations and numerical calculations in conjunction with materials and components testing is the basis of the safety assessment concept of the BAM.
Among other mechanical test scenarios a 1 meter drop test onto a steel bar has to be considered for hypothetical accident conditions of Type B packages according to IAEA regulations.
Within the approval procedure for the new German package design of the HLW cask CASTOR® HAW 28M, designed by GNS Gesellschaft für Nuklear-Service Germany, a puncture drop test was performed with a half-scale model of the cask at -40°C.
For independent assessment and to control the safety analysis presented by applicant, BAM developed a complex finite element model for a dynamical ABAQUS/ExplicitTM analysis. This paper describes in detail the use of the finite element (FE) method for modeling the puncture drop test within an actual assessment strategy.
At first investigations of the behaviour of the steel bar are carried out. Different friction coefficients and the material law of the bar are analysed by using a 'rigid-body' approximation for the cask body.
In the next step a more detailed FE model with a more realistic material definition for the cask body is developed. Strain verification is possible by results of the strain gauges located at the relevant points of the cask model. The influence of the finite element meshing is described.
Finally, the verified FE half-scale model is expanded to full-scale dimension. Scaling effects are analysed. The model is used for safety assessment of the package to be approved.
Human factors approach to the reliability of NDT in nuclear waste management in Sweden and Finland
(2010)
Nuclear power industry has the responsibility to manage and dispose of all radioactive waste from its
plants. Finnish Posiva and Swedish SKB are leading in the world in the development of disposal of
spent nuclear fuel. Their method consists of encapsulating spent nuclear fuel in copper canisters and
depositing them in the bedrock at a depth of about 500 meters for the next 100 000 years, leaving the
radioactivity to decrease naturally through the decay of the radioisotopes in it. The copper canisters,
consisting of a copper tube, a lid and a bottom (which make the outer shell) and an insert made of a
cast iron, need to be inspected for their structural integrity to ensure no critical defects are present in
the materials and welds that could lead to a leakage of the waste into the environment. Data acquired
by 4 different non-destructive testing (NDT) methods (i.e. UT, ET, RT and VT with a remote camera)
are evaluated by skilled human operators and therefore could be subject to human error.
Human Factors approach lies in identifying potential errors made by the human, their causes
and ways of preventing them. A customized Failure Modes and Effects Analysis (FMEA) was
conducted to anticipate possible human failures during the data evaluation. The results led to
designing several experiments (e.g. diffusion of responsibility within the 4-eye principle, over trust in
automated systems) which are being experimentally tested in ongoing projects. The results are
expected to lead to the optimization of the procedures followed by the NDT operators and
consequently to the improvement of the overall NDT reliability.
The paper will give an overview of new methodology for evaluating the
reliability of NDE systems accurately, reliably and efficiently in accordance with the
specific requirements of industrial application. After a review of the substantive
issues from the previous workshops, the go forward guidance from these
interactions is considered.
At the beginning of the reliability analysis, the actual safety demands have to
be defined in order to fit the investigation to the level of risk when the component
would fail. Next, all the essential influencing parameters need to be documented and
transferred to an appropriate design of experiments (DOE) to determine the
reliability in terms of a qualitative assessment for lower risk or in terms of a
quantitative probability of detection (POD) or ROC (Receiver Operating
Characteristics) curves for higher safety demands. A new paradigm is offered to
consider the POD or reliability of the system as a function of the configuration of
input variables and use it for optimisation rather than for a final judgement. An
advantage for the end user is also to sample all single PODs to an integral 'Volume
POD' of a part.
Among the influencing parameters, the human factor is the most important one.
A systematic psychological approach shall help to find out where the bottlenecks are
but most importantly to provide best possible working conditions for the human
inspectors.
Creep damage of single-crystal nickel base superalloys: mechanisms and effect on low cycle fatigue
(2010)
The main mechanisms of creep damage of single-crystal nickel-base superalloys are the loss of the interface coherency, coarsening of the γ / γ'-microstructure, precipitation of topologically closed packed phases and growth of porosity. This degradation deteriorates the mechanical properties such as yield stress, creep lifetime and especially low-cycle fatigue life, which can be reduced nearly by a factor of 10. The degradation kinetics during creep was characterised quantitatively on the superalloy CMSX-4. A new non-destructive testing technique was applied to cover a wide test parameter range with few specimens in a relatively short time: repeated load annealing of wedge shaped specimens.
TGA-FTIR: From the investigation of pyrolysis to the elucidation of fire retardancy mechanisms
(2010)
Fire testing is an essential part of the hypothetical, cumulative mechanical and thermal accident test conditions that shall guarantee package safety in severe accidents. Not only for radioactive material transport packages but also for other containments of dangerous goods international standards require specific thermal load specifications. Following the guideline 'Safety in tech-nology and chemistry' BAM as a scientific and technical German federal government institute operates a 12 km² large open air test facility for experimental investigations of dangerous goods and their containments. On an area besides the well-known 200-ton drop test facility we put into operation new fire test facilities. This facility area provides two fire test stands that are utilized with liquid Propane as fuel from a central earth-covered 60 m³ LPG storage tank. From that stor-age the Propane is pumped via pipelines to the test stands where the gas is released from nozzles, and ignited by ignition burners. The fire exposed test facility areas are 12 m x 8 m. Fire test facil-ity B (with gas release nozzles below water-covered ground) is designed for fire testing of con-tainers that may burst during the test. Fire test facility A (with ring burner systems) is designed for heavy test objects up to 200 tons, e.g. for full-scale spent fuel casks.
The paper will present a detailed description of the facility, insight into first test performances, and results of calorimeter fire tests, using containers of various sizes, to verify the absorbed heat fluxes, demonstrating that regulatory fire test conditions are met, and that the Propane fire can be compared with a kerosene or heating oil pool fire.
Rubbers are widely used as main sealing materials for containers for low and intermediate level radioactive waste and as additional component to metal seals in spent fuel and high active waste containers. The save encapsulation of the radioactive container inventory has to be guaranteed according to legislation and appropriate guidelines for long term storage periods as well as down to temperatures of -40 °C during transport.
Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance.
It is known that the material properties of rubbers are strongly temperature dependent. At low temperatures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cooling the material changes from rubber-like entropy-elastic to stiff energy-elastic behaviour, that allows nearly no strain or retraction, due to the glass transition. Hence rubbers are normally used above their glass transition but the minimum working temperature limit is not defined precisely, what can cause problems during application. Therefore the lower operation temperature limit of rubber seals should be determined in dependence of the material properties.
The results of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are combined with the results of standardized measurements as the compression set according to ISO 815. To reduce the test time of the standard tests a faster technique was developed.
Additionally, the breakdown temperature of the sealing function of complete O-ring seals is measured in a component test setup to compare it with the results of the other tests. The experimental setup is capable of measuring the leakage rate at low temperatures by the pressure rise method.
A fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. Some materials (seals and test sheets) were purchased from a commercial seal producer and some materials were compounded and cured at BAM in form of rubber sheets.
The results from several laboratory studies of the relationships between electrical polarization and physical properties of porous media have prompted interest in the potential use of low-frequency electrical spectra to qualitatively or quantitatively map variation in hydrogeologic properties in the field. Compiling several published and unpublished data sets, supported by new measurements, we have examined the low-frequency electrical spectra of a range of natural and artificial porous media to assess the generality of proposed relationships between electrical and physical properties. Our work confirms a significant positive correlation between the magnitude of electrical polarization (quantified as imaginary conductivity at a specific frequency) and the surface-area/pore-volume ratio Spor. Analyzing the parameters of ageneralized Cole-Cole resistivity relaxation model fitted to many electrical spectra, we observe two apparent controls on the electrical relaxation. For samples with abundant relatively large pore throats, we observe a distinct increase in the time constant of the model with modal pore-throat size, in accordance with classical electrical relaxation models. However, for media with pore structures dominated by small pore throats, the diffusion-length scales do not appear to be controlled by modal pore-throat size. We conclude that for such media, the microstructure of the network of small pores leads to some connectivity of diffusion paths; thus, these samples exhibit relatively large time constants. There is potential value in addition to limitations when using electrical spectra to estimate physical properties of porous media, and we see the need for more appropriate generalized theories of electrical polarization in hydrogeologic media.
A number of recent investigations have highlighted the potential value of using relaxation times derived from electrical spectra to infer key physical properties of permeable rocks. To date, most studies have assumed a grain size or pore throat as a measure of the length scale of the ionic diffusive process, although this has been challenged in recent experimental investigations. We compare the electrical spectra of three sandstones, adopting a new approach in which the temperature of the rock samples is perturbed and the relaxation time measured as a function of temperature. Our results suggest that, for the sandstones tested here, the effective diffusion coefficient should be considered as a function of the electrical tortuosity. These findings may help explain the apparent long relaxation times observed in low-permeability rocks in recent experimental studies. We also highlight the need to account for temperature in related studies of electrical spectra.
A material testing program to characterize the concrete behavior under static and dynamic loads
(2010)
In this paper a comprehensive material testing program is described to characterize a German final repository concrete material (BERB1) subjected to static and dynamic loads. The BERB1 material was developed und specified by the German Bundesanstalt für Materialforschung und -prüfung (BAM) for targets used for drop tests according to the KONRAD requirements.
The testing consists of three concurrent laboratory experimental programs performed in the USA. An extensive preliminary testing program in Germany was performed to assure the required concrete specifications during fabrication and curing.
The first set of data is the static basic material test program consisting of structural tests to quantify macroscopic concrete properties under quasi-static loads. Cubic and cylindrical specimens are investigated under this effort. The second set of test data is from the static complete material test program, where cylindrical concrete specimens are subjected to a variety of quasi-static axial and radial stress and strain paths using a high-pressure hydraulic tri-axial chamber. The material is characterized for confining pressures up to 400 MPa. The third set of data is from the dynamic complete material test program, which uses a modified Split-Hopkinson Pressure Bar to induce dynamic compression and tension waves into cylindrical concrete specimens that generate strain-rates up to 400 s-1.
The ensemble of data generated in these experiments provides a complete set of data that effectively describes the behavior of this concrete and can be used to develop a constitutive calculation model. In addition, the results of the tests show a significant effect of moisture on the strength and rheology of this concrete for quasi-static pressures greater than 50 MPa. Numerical drop test simulations with the developed constitutive model in the Lagrangian finite element code, LS-DYNA, show good agreement with the experimental results from a BAM research project.
Within the last years BAM has carried out numerous drop tests with prototype casks made of ductile cast iron onto targets according to the requirements for final disposal of non-heat generating waste in the German KONRAD repository. The results have shown that the target specifications in the acceptance criteria have to be defined more accurately to get reproducible test results with high precision. Hence, a suitable test stand foundation was developed with much effort. The integrity of the upper concrete layer of this target must be preserved during a test.
Recently the geometrical properties of a tested cubic cast iron container led to a concentration of the impact forces beneath the container walls. The target was damaged strongly with the consequence of inadmissible reduction of cask stresses. For that reason the target construction was modified. However, the basic design was not changed. A prefabricated concrete slab was still joined by a mortar layer to the IAEA target of the BAM drop test facility. In the course of the optimization of the test stand foundation the concrete slab dimensions and the reinforcement were enlarged. During the drop test repetition the target kept intact. Additionally, the mechanical behavior of the cast iron container and the target was analyzed by finite element calculations.
This improved target construction is suggested as a reference target for drop tests with casks whose mass and base area are covered by the container types VI or VII respectively according to the KONRAD repository acceptance criteria.
The measurements during the drop tests with cast iron casks have provided the strains on the cask surface at selected positions. This allows the verification of finite element simulations of drop tests which show the stress distribution also inside the component. In September 2008 a drop test was carried out with a cylindrical cast iron cask containing an artificial material defect which was designed under consideration of critical stress states in the cask body. This drop test could demonstrate the safety against failure by fracture of a cask made of a special cast iron with reduced fracture toughness.
Transport casks for radioactive materials have to withstand the 9 m drop test, 1 m puncture drop test and dynamic crush test with regard to the mechanical requirements according to the IAEA regulations. The safety assessment of the package can be carried out on the basis of experimental investigations with prototypes or models of appropriate scale, calculations, by reference to previous satisfactory safety demonstrations of a sufficiently similar nature or a combination of these methods. Computational methods are increasingly used for the assessment of mechanical test scenarios. However, it must be guaranteed that the calculation methods provide reliable results. Important quality assurance measures at BAM are given concerning the preparation, run and evaluation of a numerical analysis with reference to the appropriate guidelines.
Hence, a successful application of the finite element method requires a suitable mesh. An analysis of the 1 m puncture drop test using successively refined finite element meshes was performed to find an acceptable mesh size and to study the mesh convergence using explicit dynamic finite element codes. The finite element model of the cask structure and the puncture bar is described. At the beginning a coarse mesh was created. Then this mesh was refined in two steps. In each step the size of the elements was bisected. The deformation of the mesh and the stresses were evaluated dependent on the mesh size. Finally, the results were extrapolated to an infinite fine mesh or the continuous body, respectively. The uncertainty of the numerical solution due to the discretization of the continuous problem is given. A safety factor is discussed to account for the uncertainty. The calculation results are compared with experimental data from a puncture drop test with a half-scale model of a cylindrical cask.
This paper supports the convergence studies of the Task Group on Computational Modeling for Explicit Dynamics reporting to the ASME BPV Code Working Group on Design Methodology.