Filtern
Erscheinungsjahr
- 2014 (680) (entfernen)
Dokumenttyp
- Zeitschriftenartikel (389)
- Beitrag zu einem Tagungsband (218)
- Beitrag zu einem Sammelband (19)
- Vortrag (13)
- Dissertation (10)
- Buchkapitel (9)
- Forschungsbericht (9)
- Posterpräsentation (5)
- Zeitschriftenheft (Herausgeberschaft für das komplette Heft) (3)
- Forschungsdatensatz (2)
Sprache
- Englisch (680) (entfernen)
Schlagworte
- Corrosion (19)
- Concrete (13)
- LIBS (9)
- Nanoparticles (9)
- EDX (8)
- Welding (8)
- Ceramic (7)
- Mechanical properties (7)
- Monitoring (7)
- Non-destructive testing (7)
Eingeladener Vortrag
- nein (13)
Thermal and Dynamic Glass Transition in Ultrathin Films of Homopolymers and a Miscible Polymer Blend
(2014)
Nowadays nanoscale thin polymer films are widely used in many fields like coatings, membranes, sensors, electronic devices and so on. Meanwhile, a lot of research work has evidenced the fact that many physical properties (glass transition, crystallization, dewetting, physical aging, etc.) of ultrathin polymer films show strong deviations from their bulk behavior. Since the aforementioned properties of polymer are closely related to their application and functionality, the discrepancies motivated us to obtain a more complete understanding of how nanoscale confinement affects the physical properties of polymer. The research work presented in this thesis is focused on understanding how the free surface (air- polymer interface), the polymer-substrate interface and the film thickness influence the glass transition temperature (Tg) and the related segmental dynamics (α-relaxation process) in both homopolymers and miscible polymer blends of thin films. Complementary experimental techniques including Differential Scanning Calorimetry (DSC), Capacitive Scanning Dilatometry (CSD), Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS) have been used to investigate the glass transition of thin polymer films from both the thermodynamic and the kinetic point of view. In the thesis the film thickness dependence of Tg and segmental dynamics of different thin polymer films have been investigated. For ultrathin polycarbonate (PC) films capped between two aluminum (Al) layers an increase of both the glass transition temperature (Tg) and Vogel temperature (T0) with decreasing film thickness (d) was observed when the thickness became lower than 20 nm. The segmental relaxation time at a fixed temperature was found to increase for the ultrathin PC film of 19 nm measured by BDS, whereas no thickness dependency of the segmental dynamics was detected within the experimental error limit for the PC films supported on silicon dioxide (SiO2) (10-192 nm) in the SHS measurements. These properties are discussed in terms of the thin film geometry and the relevant interfacial interaction between the polymer and the substrate. In the case of thin polystyrene (PS) films with high molecular weight (Mw), Tg is decreasing with reducing film thickness while the segmental dynamics is independent of film thickness. Moreover, the effects of the Mw and the annealing protocol performed on thin PS films on their Tg and segmental dynamics is studied. In the part of thin poly(vinyl methyl ether) (PVME) films, no thickness dependence of the segmental dynamics was observed in the SHS measurements. The last part of the thesis was concentrated on the thin films of a miscible polymer blend, PS/PVME with the weight fraction of 50/50. It was observed that the segmental dynamics became faster with reducing the film thickness. This phenomenon is explained in terms of surface enrichment of PVME in the polymer blend system where PVME has a lower surface energy than PS. The segmental dynamics of the PVME-enriched free surface layer are faster than the bulk dynamics. Such free surface effect becomes so predominant with reducing the film thickness that it affects the segmental dynamics of the whole films detected by SHS using differential AC chip-based calorimetry. X-ray photoelectron spectroscopy (XPS) was used to probe the surface composition in order to confirm such surface enrichment phenomena.
Ultrasonic guided waves offer a wide range of applications in fields such as non-destructive testing, structural health monitoring or material characterization. They can be excited in thin-walled structures and propagate over comparably long distances. Due to their complex and dispersive propagation behavior, numerical methods are often required in order to analyze the guided wave modes that can be excited in a given structure and to simulate their interaction with defects. In the work presented in this thesis, highly efficient numerical methods have been developed that are specifically optimized for guided wave problems. The formulation is based on the Scaled Boundary Finite Element Method (SBFEM). The SBFEM is a semi-analytical method which evolved from the concept of Finite Elements but requires the discretization of the boundary of the computational domain only. To compute dispersion curves and mode shapes of guided waves, only the cross-section of the waveguide is discretized in the Finite Element sense, while the direction of propagation is described analytically. The wavenumbers of guided wave modes and the corresponding mode shapes are obtained as the eigenvalues and eigenvectors of a frequency-dependent Hamiltonian matrix. For the discretization, higher-order spectral elements are employed, leading to very low computational costs compared to traditional Finite Elements. Particular formulations are presented for plate structures as well as axisymmetric waveguides, where only the throughthickness direction has to be discretized. For the cases where the waveguide is embedded in or coupled to a quasi-infinite medium, a dashpot boundary condition is proposed in order to account for the effect of waves being transmitted into the surrounding medium. Though this approach is not exact, it leads to sufficiently accurate results for practical applications, while the computational costs are typically reduced by several orders of magnitude compared to other Finite Element based approaches. As a particular application, an experimental set-up for material characterization is discussed, where the elastic constants of the waveguide’s material are obtained from the analysis of waves propagating through the waveguide. A novel solution procedure is proposed in this work, where each mode of interest is traced over the required frequency range. The solutions are obtained by means of inverse iteration. To demonstrate the potential of the SBFEM for non-destructive testing applications, the interaction of guided wave modes with cracks in plates is simulated in the time domain for several examples. Particularly for the modeling of cracked structures, the SBFEM is very well suited, since the side-faces of the crack do not require discretization and the stress-singularity at the crack tip does not introduce additional difficulties. Hence, the computational costs can be reduced by typically a factor 100 compared to traditional Finite Elements and the meshing is straightforward.
Austenitic welds and dissimilar welds are extensively used in primary circuit pipes and pressure vessels in nuclear power plants, chemical industries and fossil fuelled power plants because of their high fracture toughness, resistance to corrosion and creep at elevated temperatures. However, cracks may initiate in these weld materials during fabrication process or stress operations in service. Thus, it is very important to evaluate the structural integrity of these materials using highly reliable non- destructive testing (NDT) methods. Ultrasonic non-destructive inspection of austenitic welds and dissimilar weld components is complicated because of anisotropic columnar grain structure leading to beam splitting and beam deflection. Simulation tools play an important role in developing advanced reliable ultrasonic testing (UT) techniques and optimizing experimental parameters for inspection of austenitic welds and dissimilar weld components. The main aim of the thesis is to develop a 3D ray tracing model for quantitative evaluation of ultrasonic wave propagation in an inhomogeneous anisotropic austeniticweld material. Inhomogenity in the anisotropic weld material is represented by discretizing into several homogeneous layers. According to ray tracing model, ultrasonic ray paths are traced during its energy propagation through various discretized layers of the material and at each interface the problem of reflection and transmission is solved. The influence of anisotropy on ultrasonic reflection and transmission behaviour in an anisotropic austenitic weld material are quantitatively analyzed in three dimensions. Theultrasonic beam directivity in columnar grained austenitic steel material is determined three dimensionally using Lamb’s reciprocity theorem. The developed ray tracing model evaluates the transducer excited ultrasonic fields accurately by taking into account the directivity of the transducer, divergence of the ray bundle, density of rays and phase relations as well as transmission coefficients. The ray tracing model is able to determine the ultrasonic wave fields generated by a point source as well as finite dimension array transducers.
Shape memory polymers (SMPs) can change their shape on application of a suitable stimulus. To enable such behavior, a ‘programming’ procedure fixes a deformation, yielding a stable temporary shape. In thermoresponsive SMPs, subsequent heating triggers entropy-elastic recovery of the initial shape. An additional shape change on cooling, i.e. thermoreversible two-way actuation, can be stimulated by a crystallization phenomenon. In this thesis, cyclic thermomechanical measurements systematically determined (1) the shape memory and (2) the actuation behavior under constant load as well as under stress-free conditions. Chemically cross-linked, star-shaped polyhedral oligomeric silsesquioxane polyurethane (SPOSS-PU) hybrid polymer networks and physically cross-linked poly(ester urethane) (PEU) block copolymers were investigated around the melting and crystallization temperatures of their polyester soft segments. (1) The SPOSS-PUs showed excellent shape fixities and recoverabilities of almost 100% at high cross-linking density, while PEUs exhibited pronounced shape memory properties at increased soft segment content. Furthermore, two-fold programmed SPOSS-PU specimens were able to recover their initial shape in two thermally separated events. Even a neck, which formed during deformation of SPOSS-PUs with high soft segment content, was reversed. (2) In PEUs, globally oriented crystallization on cooling drove expansion of the sample, in particular at high soft segment content and after application of a strong deformation. Melting reversed that orientation; the PEU sample contracted and thereby completed the thermoreversible actuation cycle. Under load, multiple polymorphic phase transitions enabled two successive expansion and contraction steps, while under stress-free conditions various geometric shape changes, including the increase and decrease of PEU sample length and thickness as well as twisting and untwisting could be experimentally witnessed. Such actuation technology allows for entirely new applications, enabling mimicry of reversible, bidirectional and repeated organic movements.
A novel optical detection method for partial discharge in HV/EHV cable terminations has been proposed. Optical sensor fibres integrated into the HV equipment provide high sensitivity as well as immunity to electromagnetic interference and enable therefore on-line monitoring in electromagnetically noisy environment. The availability of optically transparent silicone rubbers that meet strict dielectric and mechanical criteria is a crucial prerequisite for the implementation of this method. The optically transparent silicone rubbers can be applied for the fabrication of a modern rubber stress cone as well as for the development of a new optical sensing element sensitive to PD activities. In this thesis, AC dielectric strength behaviour and mechanical properties of three types of commercially available silicone rubbers were investigated. One of the characterized silicone rubbers was a translucent type whereas the two others were optically transparent types, however with different chemical curing reactions. The measurements of tensile strength and elongation at break were carried out according to the ISO 37 standard. For investigation of the dielectric strength Eb behaviour of the virgin and modified silicone rubbers, a new methodology was developed. It is, at the same time, highly reliable and efficient, saves time and reduces material consumption in comparison to previously reported methodologies. The key component of this methodology is a specifically developed test facility. Furthermore, the methodology comprises determinations for easy preparation and handling of high-quality test specimens. This test method provides various advantages over other methods that have previously been used for measurement of the fundamental quantity Eb value of silicone rubbers. Both technical and economic demands are satisfied. The new facility also enables cost-effective routine tests in material research laboratories. The high quality of the obtained test results was verified by statistical analysis based on the 2-parameter Weibull distribution function. The investigations revealed that the virgin translucent silicone rubber has a large elastic region with an acceptable plastic deformation and also provides an AC 50 Hz dielectric strength of approximately 24 kV/mm for 0.5 mm thickness. These values enable considering the tested translucent silicone as replacement material for an opaque elastomer that is currently used for a rubber stress cone of HV cable accessories Unfortunately, its optical transmittance is poor compared to optically clear transparent silicone rubbers. On the other hand, the mechanical properties of virgin transparent silicone rubbers do not comply with those demanded from push-on stress cones. In particular, their elongation at break is considered too low for that application. However they provide the AC dielectric strength values in either 28 kV/mm or 29 kV/mm for 0.5 mm thickness, which are higher than those of the translucent type. Moreover, it was found that the post-curing process does not provide a positive impact on the ultimate elongation of silicone rubbers. Hence, the elongation at break of virgin transparent silicone rubbers must be improved before they can be used as insulating material for a rubber stress cone. In addition, the influence of mechanical tensile stress on the dielectric strength of the virgin translucent silicone rubber was investigated. The results show that mechanical tensile stress does not negatively influence on dielectric strength of such silicone rubber, so it can be well-operated under combined electrical and mechanical stresses. Beside the improvement of optical PD detection performance in the translucent silicone insulation materials, the influence of fluorescent dye’s modification was investigated. The results indicate that the commercially available fluorescent dyes of 0.02 wt. % mixed into the translucent silicone polymer do not negatively influence on the Eb value of such silicone material. So an optically compatible silicone rubber is perfectly suitable for the fabrication of novel fluorescent silicone optical fibres, which can be integrated into the modified transparent rubber stress cones of HV cable terminations. The final outcomes of this investigation are experimentally substantiated recommendations for future revision of IEC 60243-1, especially the chapter dealing with the determination of AC dielectric strength of silicone rubbers. Recommendations and suggestions for further investigations are addressed in the final chapter of this thesis.
Black fungi are recently described microorganisms and amongst the most stress-tolerant eukaryotes currently known. They are a taxonomically diverse, but morphologically similar group of filamentous fungi that share two distinct signature characteristics, i.e. melanisation of the cell wall and compact colony morphology, which confer them passive, constituent extremotolerance. Albeit morphologically undifferentiated, black fungi show extensive phylogenetic and ecological diversity. Due to their persistence in unfavourable niches, they are ubiquitous on deserts and in glaciers and are permanent settlers of rock and other atmosphere-exposed material surfaces as well as man-made environments like salterns, humidifiers and dishwashers, and thus widespread in temperate regions worldwide. Some members are devastating opportunistic pathogens of invertebrates or vertebrates, including humans; others show symbiotic potentials with co-occurring microorganisms in extreme ecosystems. Beside their interest for fundamental biology, black fungi are important for several applied applications, e.g. in biotechnology, astrobiology, bioremediation and material preservation. Despite recent advances in the study of these fungi, many biological questions remain to be clarified regarding the molecular mechanisms underlying persistence, their physiology and nutritional modes, and their specific interactions with putative symbiotic partners. Models for pathogenic and halotolerant black fungi are established; however, no model was yet available for rock- and material-inhabiting ones. This thesis introduces the strain Knufia petricola A95 as a suitable model to study rockinhabiting lifestyle. For this purpose, the strain was characterised at the physiological and molecular levels by phenotype microarrays, growth experiments and genome analyses as well as further methods. Cell- wall mutants of K. petricola A95 isolated during the course of this study were described and included in the comparative analysis to investigate effect of melanisation on physiology and stress tolerance. Direct comparisons were also performed between the model strain and the phylogenetically distant but ecologically, biogeographically and morphologically highly similar rock inhabitant Coniosporium apollinis. Preliminary observations of a model biofilm of K. petricola A95 and the photosynthetic cyanobacterium Nostoc punctiforme ATCC 29133 are introduced to study symbiotic interactions of rock-inhabiting microorganisms. Data presented here are a contribution to the understanding of ecophysiology and extremotolerance of rock-inhabiting black fungi.
Cultural Heritage objects are in many cases invaluable and irrecoverable, therefore their protection is a prior goal. One threat arises by intentionally defacing such objects with graffiti. One possibility to face the imminent threat is the application of a surface protection in form of anti-graffiti systems (AGS). However, the knowledge about the performance and durability of AGS on substrates used for historical buildings is still fragmented. The goal of the presented study was to investigate the performance of a newly developed agent in comparison to a selection of commercial anti-graffiti agents on different substrates, which were used for historical buildings. Four commercial anti-graffiti agents with different chemical formulations were selected and tested with the new agent on different stone and brick substrates. The results showed clearly that AGS based on dense, water vapour impermeable coatings are not suitable to porous substrates such as sandstone, brick or porous limestone due to their impair of the hygric properties and the visual appearance of a substrate. The new agent could not completely reach the cleaning efficacy of the dense coatings but exhibited a much lower impact on the properties of the substrate and was therefore better compatible to historical surfaces.
The Synthetic Aperture Focusing Technique (SAFT) is an algorithm applied in non-destructive ultrasonic testing which provides an image of flaws within a specimen. The image is reconstructed from A-scans measured at different positions. Reliable evaluation of the images obtained by the SAFT-algorithm, however, depends on the representation of the reconstructed data, which is initially given in terms of positive and negative local values only. A suitable way of processing this data for evaluation is to calculate the envelope, which can be achieved by means of the analytic signal. The extension of this concept to the multidimensional case is neither trivial nor unique and although extensive work on this subject has been carried out in the past, a correct envelope calculation in multidimensional data remains difficult since it depends on an additional condition, namely the separability of the signal. In this paper, the concept of analytic signals with single-quadrant spectra is applied to process 2-dimensional data obtained by the SAFT-algorithm. Furthermore, we present a procedure to overcome the limitations of that approach by selecting local magnitude values from a number of rotated frames after evaluating the signals separability in each frame, which is briefly validated against synthetic and experimental data.
The process chain for Carbon Capture and Sequestration (CCS) includes tubing for injection of CO2 into saline aquifers. The compressed CO2 is likely to contain specific impurities; small concentrations of SO2 and NO2 in combination with oxygen and humidity are most harmful. In addition, CO2 saturated brine is supposed to rise in the well when the injection process is interrupted. The material selection has to ensure that neither CO2 nor brine or a combination of both will leak out of the inner tubing. In this comprehensive paper the investigated materials range from low-alloy steels and 13% Cr steels up to high-alloy materials. Electrochemical tests as well as long term exposure tests were performed in CO2, in brine and combination of both; pressure was up to 100 bar, temperature up to 60 °C. Whereas the CO2 stream itself can be handled using low alloy steels, combinations of CO2 and brine require more resistant materials to control the strong tendency to pitting corrosion. The corrosion behavior of heat-treated steels depends on factors such as microstructure and carbon content. For different sections of the injection tube, appropriate materials should be used to guarantee safety and consider cost effectiveness.
Solvent-cast films from shape memory poly(ester urethane) (PEU) containing different weight contents of microencapsulated thermochromic pigments (T-PIGs) were prepared by drying in air. Spectrophotometric investigations unveiled that gradual loading with T-PIG black resulted in continuous darkening of the films up to filler contents of 20 wt%, accompanied by a steady enhancement of thermochromic properties. Taking this composition as standard, PEU films equipped with T-PIG black, blue and red were deposited atop PEU plaques to obtain laminate structures. Herein, the cover layer thickness (100 ± 5 µm) and the good dispersion of T-PIGs inside the polymer matrix were verified by scanning electron microscopy. Machine-readable information carriers were prepared by laser engraving quick response (QR) codes into the cover layer of the laminates and subsequently cutting cuboidal samples therefrom. Finally, thermo-mechanical programming of the QR code carriers was applied to randomly distort the code patterns, thus rendering them unreadable. Upon heating, surface decolorization and shape recovering occurred; during the ensuing cooling, the surface color and contrast reappeared whereupon the QR codes could be read out. Spectrophotometric, calorimetric and thermo-mechanical investigations gave evidence that the color switching temperature of the T-PIGs roughly coincided with the melting temperature of the ester-based switching segment and thus with the activation temperature of the shape memory effect. Apart from that unique functionality, manifold design concepts may render information carriers difficult-to-copy. Therefore, we anticipate tremendous potential as anti-counterfeiting technology.
The aim of the present work was to investigate the possibilities of hybrid laser arc welding regarding reliable production of longitudinal welds of high strength pipe steels X80 and X120 and to evaluate achievable mechanical properties of laser hybrid welds. The study focused on weld toughness examination in low temperature range up to –60°C. Suitable filler materials were identified in the context of this task. It could be shown that metal cored electrodes guaranteed sufficient Charpy impact toughness at low temperature for both investigated materials. Modern arc welding technologies such as modified pulsed spray arc were used to promote deeper penetration of the filler material into the narrow laser welding gap. Edge preparation with a 14 mm deep root face was considered as optimum, because no penetration of the filler material could be detected beyond this depth limit, and therefore, any metallurgical influences on the weld metal properties through the welding wire could be excluded.
Carbon fiber reinforced polymer (CFRP) specimens with artificial delaminations and with impact damage have been characterized using active thermography with flash excitation. Systematic investigations have been performed in four different experimental configurations of flash lamps and infrared (IR) camera in transmission as well as in reflection alignment. It is shown here that the diffusivities determined for the sound and for the damaged areas give a good measure for damage characterization. Although reflection measurements also give information about defect depth, reflection measurements from only one side are not sufficient for assessing the whole cross section of the specimens. Thus, depending on sample thickness the lateral size of damage could only be determined from reflections measurements from both sides or from transmission measurements. In this paper, measurement accuracy and limits of flash thermography for the investigation of CFRP specimens are presented in detail together with quantitative data concerning the defects.
Quantitative evaluation of ultrasonic C-scan images in homogeneous and layered anisotropic austenitic materials is of general importance for understanding the influence of anisotropy on wave fields during ultrasonic non-destructive testing and evaluation of these materials. In this contribution, a three dimensional ray tracing method is presented for evaluating ultrasonic C-scan images quantitatively in general homogeneous and layered anisotropic austenitic materials. The directivity of the ultrasonic ray source in general homogeneous columnar grained anisotropic austenitic steel material (including layback orientation) is obtained in three dimensions based on Lamb's reciprocity theorem. As a prerequisite for ray tracing model, the problem of ultrasonic ray energy reflection and transmission coefficients at an interface between (a) isotropic base material and anisotropic austenitic weld material (including layback orientation), (b) two adjacent anisotropic weld metals and (c) anisotropic weld metal and isotropic base material is solved in three dimensions. The influence of columnar grain orientation and layback orientation on ultrasonic C-scan image is quantitatively analyzed in the context of ultrasonic testing of homogeneous and layered austenitic steel materials. The presented quantitative results provide valuable information during ultrasonic characterization of homogeneous and layered anisotropic austenitic steel materials.
TRIP-steels offer a good combination between strength and ductility. Therefore TRIP-steels are widely used in the automobile industries. The aim of this work is to study the stability of involved phases during heating and to identify the kinetics of the occuring phase transformations. For that purpose, in-situ diffraction measurements, using high energy synchrotron radiation were conducted. The analysis revealed the decomposition of the metastable austenitic phase into carbide and ferrite along the heating process and the regeneration of the austenite by further heating of the sample.
In this paper we propose an algorithm to compute specific parts of the dispersion curves for elastic waveguides. The formulation is based on an axisymmetric representation of the Scaled Boundary Finite Element Method, where the wavenumbers of propagating modes are obtained as solutions of a Hamiltonian eigenvalue problem. The novel solution procedure involves tracing selected modes over a given frequency range and computing the corresponding solutions by means of inverse iteration. The resulting algorithm is applied in the context of material characterization, where the efficiency of the computation is crucial.
Welding residual stress is of major concern for structural integrity assessment in industrial components. Shear and volume strains resulting from the austenite-martensite-transformation affect the development of residual stress during welding. Controlling the phase transformation allows adjustment of the welding residual stress. Low transformation temperature (LTT) weld filler materials exhibiting reduced MS-temperatures allow postponing the phase transformation. The associated strain arising from the delayed transformation compensates for the thermal contraction strains and as such may reduce tensile or even introduce compressive residual stress. In this article we discuss the tri-axial residual stress distribution in 15 mm S690Q steel plates joined with LTT filler materials with 10 wt% Cr and a Ni-content that varies from 8 to 12 wt%. Using complementary synchrotron X-ray and neutron diffraction stress analysis the macroscopic residual stress was derived from the phase specific lattice strain and phase fraction of martensite and retained austenite, respectively. The local phase specific unstrained lattice parameters were determined using stress relieved combs. The investigation revealed increasing phase fraction of retained austenite with increasing Ni-content. Further, independent of the Ni-content in each weld in the fusion zone, significant compressive residual stresses were found in the longitudinal direction, which are balanced by tensile residual stresses in the heat affected zone (HAZ). In the weld transverse and normal direction the stress distribution is qualitatively similar but less in magnitude. The increased amount of retained austenite reduces the compressive stress arising from shear and volume strains during the delayed phase transformation and therefore no significant increase in compression was observed for decreasing MS-temperatures.
The developments in the field of residual stress determination during the last decades have contributed to a better understanding of the origins and sources of residual stresses in different engineering disciplines. The many investigations concerning the behavior of residual stresses under mechanical loading have also provided a solid foundation to clarify the important aspects of residual stresses and fatigue. The question that arises now is if this available body of knowledge is being used effectively in the field of welding technology to design and construct structures with better fatigue performances. In this paper the necessity of the development of the concept residual stress engineering for welds in which wanted residual stress states are tailored for specific cases by appropriate means will be discussed. The possibilities of the quantitative consideration of the benefits in the fatigue design codes will be presented in a practical example.
Innovative low transformation temperature (LTT) welding filler materials are featuring a characteristic chemical composition which favors the formation of martensite at comparatively low temperatures. This permits deliberate adjustment of welding residual stresses. Even though numerous investigations can be found in the literature on this issue, they provide only little insight into the interaction between phase transformation and resulting welding residual stresses. For this purpose, a component weld test was performed in a special large-scale testing facility. The results illustrate that the desired residual stress control by using LTT alloys is actually feasible. With increasing shrinkage restraint, however, higher tensile residual stresses are formed in transverse direction of the weld. By contrast, the residual stress level in longitudinal weld direction is nearly independent of the restraint conditions. On-line stress analysis revealed that the amount of stress reduction during cooling of the individual weld runs is dependent on the weld volume undergoing phase transformation. Overall, evidence was furnished that the approach of residual stress engineering by LTT alloys is suitable even in the case of large-scale multilayer welding.
A three-dimensional turbulent steady state numerical model was used to investigate the influence of an alternating current (AC) magnetic field during high power laser beam keyhole welding of 20 mm thick stainless steel AISI 304 being modeled as an ideal non-ferromagnetic material. Three-dimensional heat transfer and fluid dynamics as well as the electromagnetic field equations were solved with the finite element package COMSOL Multiphysics 4.2 taking into account the most important physical effects of the process. Namely, the thermo-capillary (Marangoni) convection at the weld pool boundaries, natural convection due to gravity and density differences in the melt volume as well as latent heat of solidliquid phase transitions at the phase boundaries were included in the model.
It is shown that the gravity drop-out associated with the welding of thick plates due to the hydrostatic pressure can be prevented by the application of AC magnetic field between 80 mT and 135 mT for corresponding oscillation frequencies between 1 kHz and 10 kHz below the weld specimen. Experimentally, a value of the magnetic flux density of around 230 mT was found to be necessary to allow for single-pass laser beam welding without sagging or drop-out of melt for a 20 mm thick combination of austenitic stainless steel AISI 304 and ferritic construction steel S235JRC at an oscillation frequency of around 2.6 kHz.
Morphological and compositional features regarding blue and yellow pigments used in glazed ceramics from Portugal are investigated by means of a SEM/EDX system. Fragments of samples produced in the main pottery-making centres between the XVIXVIII centuries (Lisbon and Coimbra) were the objects of study. The main question to be answered is whether there are differences in the manufacturing procedures employed. For this purpose, two types of samples were analysed: faiences and wall-tiles (the famous 'Azulejos', in Portuguese). Differences between the manufacturing techniques of the two production centres were veritably found. The expected linkage between Fe–Co–Ni–As–Bi was challenging to investigate. Thus, Co was found in Fe- or Ni-rich structures, but with no structural connection to As or Bi. However, the As-needle-like structures were always identified in blue regions. One interesting finding related particularly to the blue pigment was the presence of SnO2 agglomerates throughout the whole glaze, which suggests its intentional addition for 'lightening' the well known dark Co blue. Concerning the yellow pigment differences established in the crystal shape and size are indicative of different firing temperatures used.
Hydrogen interaction with residual stresses in steel studied by synchrotron X-ray diffraction
(2014)
The residual stress state in a material has an important role in the mechanism of cracking, induced or assisted by hydrogen. In this contribution, the beamline EDDI in BESSY II instrument in Berlin was used in order to investigate the influence of hydrogen upon the residual stresses state existing in a Supermartensitic stainless steel sample. The method used for investigating the residual stresses is the sinus square ψ method. This method involves the usage of high energy X-ray diffraction in order to measure the residual stress state and magnitude. It was found that hydrogen presence has a significant influence upon the magnitude of the residual stresses, as its value decreases with high hydrogen content. This effect is reversible, as hydrogen desorbs from the sample the residual stress magnitude gains its initial value before hydrogen charging.
Fully aromatic polyimides are synthesized via solid-state polymerization of the corresponding monomer salts. The crystal structure of salts shows strong hydrogen bonding of the reactive groups and thereby paves the way for solid-state transformations. The polycondensation yields copies of the initial salt crystallite habits, accompanied by the development of a porosity especially suited for CO2.
Amuay refinery disaster (2012) is another recent example of Vapor Cloud Explosion (VCE) and fire accidents preceded by Buncefield (2005), Puerto-Rico (2009) and Jaipur (2009), respectively [9]. The incident has left many safety issues behind which must be repeatedly addressed. Unfortunately, the lessons taught by previous similar events are just not understood carefully. It reveals that the proper safety measures for such facilities were either underestimated or were not accounted seriously. Consequently, the resulting overpressures from explosion and the subsequent thermal radiation from tank fires have once again proved to be disastrous to both mankind and infrastructure. This article highlights the aftermaths of Amuay incident and addresses the challenges put forward by it. Furthermore, a comparative study is performed between such incidents to analyze the similarities and how they could have been avoided.
Elimination of Artifacts in NMR SpectroscopY (EASY) is a simple but very effective tool to remove simultaneously any real NMR probe background signal, any spectral distortions due to deadtime ringdown effects and -specifically- severe acoustic ringing artifacts in NMR spectra of low-gamma nuclei. EASY enables and maintains quantitative NMR (qNMR) as only a single pulse (preferably 90°) is used for data acquisition. After the acquisition of the first scan (it contains the wanted NMR signal and the background/deadtime/ringing artifacts) the same experiment is repeated immediately afterwards before the T1 waiting delay. This second scan contains only the background/deadtime/ringing parts. Hence, the simple difference of both yields clean NMR line shapes free of artefacts.
In this Part I various examples for complete 1H, 11B, 13C, 19F probe background removal due to construction parts of the NMR probes are presented. Furthermore, 25Mg EASY of Mg(OH)2 is presented and this example shows how extremely strong acoustic ringing can be suppressed (more than a factor of 200) such that phase and baseline correction for spectra acquired with a single pulse is no longer a problem. EASY is also a step towards deadtime-free data acquisition as these effects are also canceled completely. EASY can be combined with any other NMR experiment, including 2D NMR, if baseline distortions are a big problem.
Reaction products and strength development of wastepaper sludge ash and the influence of alkalis
(2014)
Wastepaper sludge ash (WSA) from a newsprint paper mill was investigated for its mineralogical composition and its reaction products and strength development after activation with water and sodium and potassium hydroxide solutions. The results showed the WSA to consist of calcite, free lime, gehlenite, tricalcium aluminate, belite, talc, quartz and probably a glassy phase. The principle reaction product was monocarboaluminate (CO3–AFm) for the water- as well as for the alkali-activated WSA. Formation of monocarboaluminate and strength gain was more rapid for the alkali-activated WSA until 1 day of curing. However, afterwards reactions proceeded much slower when alkali solutions were used, leading to an about twice as high compressive strength for water-activated WSA mortars after 28 days of curing. The observed behavior is tentatively ascribed to a less uniform microstructure of the alkali-activated WSA. Significant differences between NaOH- and the KOH-activated WSA were not observed.
In the last ten years, monitoring the integrity of the civil infrastructure has been an active research topic, including in connected areas as automatic control. It is common practice to perform damage detection by detecting changes in the modal parameters between a reference state and the current (possibly damaged) state from measured vibration data. Subspace methods enjoy some popularity in structural engineering, where large model orders have to be considered. In the context of detecting changes in the structural properties and the modal parameters linked to them, a subspace-based fault detection residual has been recently proposed and applied successfully, where the estimation of the modal parameters in the possibly damaged state is avoided. However, most works assume that the unmeasured ambient excitation properties during measurements of the structure in the reference and possibly damaged condition stay constant, which is hardly satisfied by any application. This paper addresses the problem of robustness of such fault detection methods. It is explained why current algorithms from literature fail when the excitation covariance changes and how they can be modified. Then, an efficient and fast subspace-based damage detection test is derived that is robust to changes in the excitation covariance but also to numerical instabilities that can arise easily in the computations. Three numerical applications show the efficiency of the new approach to better detect and separate different levels of damage even using a relatively low sample length.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.
Despite their enormous diversity, the bauplan of adult winged insects (pterygotes) is remarkably conservative since the Lower Devonian: a five-segmented head, a three-segmented thorax with three pairs of walking legs and an eleven-segmented abdomen without any non-sexual appendages 1 and 2. The only known exceptions are the abdominal appendages of adult male sepsid flies on the fourth segment; however, these are also used as copulatory organs and are supposedly maintained through sexual selection [3]. Here, we report a rod-like paired appendage from the third and fourth abdominal segments in adults of the Southeast-Asian Hemiptera taxon Bennini (Figure 1A,B; Supplemental information). These are fully musculated, innervated, and movable and bear highly organized sensory and secretory units. The appendages, termed LASSO (lateral abdominal sensory and secretory organs), are consistent in topology and structure in all species studied and not sexually dimorphic. The existence of these non-sexual abdominal appendages reveals the potential of the 300 million year old conserved bauplan of insects.
A detailed characterization of metal-tagged antibodies is the prerequisite for the implementation of quantitative concepts in inductively coupled plasma–mass spectrometry (ICP-MS)-based bioanalysis or future medical diagnosis. In this paper, the common modification with bifunctional ligands containing maleimide residues as a reactive group was investigated in detail via size exclusion chromatography (SEC)-ICP-MS and liquid chromatography–time-of-flight (LC-TOF)-MS to determine the preservation of the antibody structure after tagging. Mouse monoclonal IgG modified with metal-coded tags (MeCATs) was used as a model system. Several antibody fragments were identified carrying different numbers of metal tags. In a second step, a functionality test was performed with isolated fragments where the antigen specificity was tested in a dot blot immunoassay.
After some months of operation, a number of PV modules develop a discolouration defect called 'snail trails', or 'snail traces', which appear as irregular dark stripes across the cells. Whereas these traces were soon identified as discoloured silver contacts along the cell edges or at micro cracks, the chemical and mechanistic reasons for this phenomenon have not yet been resolved in detail. In this work we show that silver nanoparticles accumulating within the encapsulation foil cause the brownish discolouration, and that certain additives of encapsulation and back sheet foils trigger the formation of these nanoparticles.
This review gives representative examples of the various types of synthetic cationic polymers or polyampholytes (chemical structure, architecture, etc) that can be used to complex DNA (forming polyplexes) for their application in gene delivery. In designing polycations for gene delivery, one has to take into account a balance between protection of DNA versus loss of efficiency for DNA condensation and efficient condensation versus hindering of DNA release. Indeed, if the polyplexes are not stable enough, premature dissociation will occur before delivery of the genetic material at the desired place, resulting in low transfection efficiency; on the other hand, a complex that is too stable will not release the DNA, also resulting in low gene expression. The techniques generally used to determine these properties are gel electrophoresis to test the DNA/polymer complexation, ethidium bromide or polyanion displacement to test the affinity of a polymer for DNA, and light scattering to determine the extent of DNA condensation. Moreover, with the development of more precise instruments for physico-chemical characterization and appropriate biochemical and biophysical techniques, a direct link between the physico-chemical characteristics of the polyplexes and their in vitro and in vivo properties can be drawn, thus allowing tremendous progress in the quest towards application of polyplexes for gene therapy, beyond the research laboratory.
Sewage sludge ash (SSA) based P-fertilisers were produced by thermochemical treatment of SSA with Cl-donors at approximately 1000 °C. During this thermochemical process heavy metals are separated as heavy metal chlorides via the gas phase. Chromium cannot be separated under normal conditions. The risk of the development of toxic Cr(VI) during the thermochemical process was investigated. X-ray Absorption Spectroscopy measurements showed that SSA and thermochemically treated SSA with CaCl2, MgCl2 and NaCl contain Cr(III) compounds only. In contrast, treating SSA with elevated quantities of Na2CO3, to enhance the plant-availability of the phosphate phases of the fertiliser, developed approximately 10–15% Cr(VI). Furthermore, Raman microspectroscopy showed that using Mg-carbonate reduces the risk of a Cr(VI) development during thermochemical treatment. Additionally, leaching tests showed that only a Crwater solubility >10% is an indicator for Cr(VI) in SSA based P-fertilisers.
A combination of simultaneous milling and extraction known as micropulverized extraction was developed for the quantification of the alcohol marker ethyl glucuronide (EtG) in hair samples using a homogeneous reference material and a mixer mill. Best extraction results from 50 mg of hair were obtained with 2-mL plastic tubes containing two steel balls (Ø = 5 mm), 0.5 mL of water and with an oscillating frequency of 30 s-1 over a period of 30 min. EtG was quantified employing a validated GC-MS procedure involving derivatization with pentafluoropropionic acid anhydride. This micropulverization procedure was compared with dry milling followed by separate aqueous extraction and with aqueous extraction after manual cutting to millimeter-size snippets. Micropulverization yielded 28.0±1.70 pg/mg and was seen to be superior to manually cutting (23.0±0.83 pg/mg) and equivalent to dry grinding (27.7±1.71 pg/mg) with regard to completeness of EtG extraction. The option to process up to 20 samples simultaneously makes micropulverization especially valuable for the high throughput of urgent samples.
Microcrack formation during gas metal arc welding of high-strength fine-grained structural steel
(2014)
The recent development of high-performance-modified spray arc processes in gas metal arc welding due to modern digital control technology and inverter power sources enables a focused spray arc, which results in higher penetration depths and welding speed. However, microcracks occurred in the weld metal while approaching the process limits of the modified spray arc, represented by a 20-mm double layer DV-groove butt-weld. These cracks were detected in structural steel exhibiting a yield strength level of up to 960 MPa and are neither dependent on the used weld power source nor a consequence of the modified spray arc process itself. The metallographic and fractographic investigations of the rather exceptional fracture surface lead to the classification of the microcracks as hot cracks. The effects of certain welding parameters on the crack probability are clarified using a statistical design of experiment. However, these microcracks do not impact the design specification for toughness in the Charpy V-notch test (absorbed energy at -40 °C for the present material is 30 J).
Pure U-[13C18]-labelled cis-zearalenone (cis-ZEA) has been prepared and characterised as internal standard (ISTD) for a reliable quantification of cis-ZEA in contaminated food and feed products. The cis-isomer of the naturally trans-configurated Fusarium mycotoxin zearalenone is often neglected. However, isomerisation easily occurs by exposure of ZEA to (UV-)light. Thus, the applicability of the new cis-ZEA ISTD was demonstrated in a long-term isomerisation study comparing naturally trans-ZEA-contaminated edible oil with spiked edible oil. To estimate the benefits of the newly prepared cis-ZEA ISTD, various approaches to quantify cis-ZEA by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) were compared. As a result, a significant bias was revealed if no appropriate cis-ZEA standards are used. Furthermore, the new ISTD was applied to the analysis of 15 edible oils by stable isotope dilution analysis in combination with HPLC-electrospray ionisation-MS/MS. One of the maize germ oils showed the presence of cis-ZEA above LOD (>0.3 µg/kg), whereas two out of 15 maize germ oils were found to be contaminated with trans-ZEA (range 17.0-31.0 µg/kg).
Industrial production of the cell protectant ectoine: protection mechanisms, processes, and products
(2014)
Bacteria, Ärchaea and Eukatya can adapt to saline environments by accumulating compatible solutes in order to maintain an osmotic equilibrium. Compatible solutes are of diverse Chemical structure (sugars, polyols, amino acid derivatives) and are beneficial for bacterial cells not only as osmoregulatory solutes, but also as protectants of proteins by mitigating detrimental effects of ffeezing, drying and high temperatures. The aspartate derivative ectoine is a wide spread compatible solute in Bacteria and possesses additional protective properties compared with other compatible solutes, and stabilizes even vvhole cells against stresses such as UV radiation or cytotoxins. The protective properties of ectoine for proteins can be explained by its strong (kosmotropic) interaction with water and subsequent exclusion ffom Protein surface, the decrease of the solubility of the peptide backbone and the strengthening of intramolecular hydrogen bonds (secondary structures). The stabilizing and UV-protective properties of ectoine attracted industry, which saw the potential to market ectoine as a novel active component in health care products and cosmetics. In joint efforts of industry and research large-scale fermentation procedures have been developed with the halophilic bacterium Halomonas elongata used as a producer strain. The two key technologies that allow for the annual production of ectoine on a scale of tons are the bacterial milking procedure and the development and application of ectoine-excreting mutants (“leaky” mutant). The details of these two procedures including the strain development and fermentation processes will be introduced and current and future applications of ectoine will be discussed.
A computationally efficient solution scheme is presented for the mechanical problems whose formulations include the Kuhn–Tucker or Signorini–Fichera conditions. It is proposed to reformulate these problems replacing inequalities in these conditions by equations with respect to new unknowns. The solutions of the modified problems have simple physical meanings and determine uniquely the unknowns of the original problems. The approach avoids application of multi-valued operators (inclusions or inequalities) in formulation of the problems. Hence, the modified formulations are suitable for numerical analysis using established powerful mathematical methods and corresponding solvers developed for solving systems of non-linear equations.
To demonstrate the advantages of the proposed approach, it is applied for solving problems in two different areas: constitutive modeling of single-crystal plasticity and mixed boundary value problems of elastic contact mechanics with free boundaries. The original formulations of these problems contain respectively the Kuhn–Tucker and Signorini–Fichera conditions. A problem of the former area is integrated using an implicit integration scheme based on the return-mapping algorithm. The derived integration scheme is free of any update procedure for identification of active slip systems. A problem of the latter area is reduced to solution of non-linear integral boundary equations (NBIEs). Numerical examples demonstrate stability and efficiency of the solution procedures and reflect the mathematical similarities between the both non-linear problems.
Bioanalytical, clinical, and security applications increasingly require simple, efficient, and versatile strategies to measure an ever increasing number of analytes or events in parallel in a broad variety of detection formats as well as in conjunction with chromatographic separation techniques or flow cytometry. An attractive alternative to common optical multiplexing and encoding methods utilizing spectral multiplexing/color encoding and intensity encoding is lifetime multiplexing, which relies on the discrimination between different fluorescent reporters based on their fluorescence decay kinetics. Here, we propose a platform of surface-functionalizable polymeric nanoparticles stained with fluorophores differing in their fluorescence lifetimes as a new multiplexing and encoding approach. Proof-of-concept measurements with different sets of lifetime-encoded polystyrene nanoparticles are presented, obtained via staining of preformed particles with visible (vis)- and near-infrared (NIR)-emissive organic dyes, which display very similar absorption and emission spectra to enable excitation and detection at the same wavelengths, yet sufficiently different fluorescence decay kinetics in suspension, thereby minimizing instrumentation costs. Data analysis was performed with a linear combination approach in the lifetime domain. Our results and first cell experiments with these reporter sets underline the suitability of our multiplexing strategy for the discrimination between and the quantification of different labels. This simple and versatile concept can be extended to all types of fluorophores, thereby expanding the accessible time scale, and can be used, e.g., for the design of labels and targeted probes for fluorescence assays and molecular imaging, cellular imaging studies, and barcoding applications, also in conjunction with spectral and intensity encoding.
Gas separation is a key issue in various industrial fields. Hydrogen has the potential for application in clean fuel technologies. Therefore, the separation and purification of hydrogen is an important research subject. CO2 capture and storage have important roles in 'green chemistry'. As an effective clean technology, gas separation using inorganic membranes has attracted much attention in the last several decades. Membrane processes have many applications in the field of gas separation. Cement is one type of inorganic material, with the advantages of a lower cost and a longer lifespan. An experimental setup has been created and improved to measure twenty different cement membranes. The purpose of this work was to investigate the influence of gas molecule properties on the material transport and to explore the influence of operating conditions and membrane composition on separation efficiency. The influences of the above parameters are determined, the best conditions and membrane type are found, it is shown that cementitious material has the ability to separate gas mixtures, and the gas transport mechanism is studied.
The time-dependent sorption of biodiesel in a typical polyethylene for container applications is investigated in comparison to conventional diesel fuel at three different temperatures. In this context, the desorption behavior is also addressed. Subsequently, the effects of both penetrants on mechanical properties are characterized in terms of impact strength and dynamic-mechanical analysis. The discussion of property changes is firstly based on the sorption kinetics of biodiesel and diesel, which is determined by immersion experiments allowing for the calculation of respective diffusion coefficients. Changes in impact strength as determined by the Charpy method are further characterised in more detail by analyzing the fracture surfaces, and correlated with results of dynamic-mechanical analysis.
High temperature SSRT - ductility data from cathodic hydrogen charging of 10CrMo910 and 7CrMoVTiB1010 are implemented into a mathematical model of SCC at various operational conditions including temperatures, pH and dissolved hydrogen/oxygen contents as well as global stresses and material properties. The results show that, as a consequence of experimentally verified local acidification at initial anodic path corrosion, subsequent local hydrogen assisted cracking can be a controlling factor for SCC in high temperature water. As a particular effect at global stresses close to the yield point, operational temperatures around 270°C exhibit peak crack growth rates depending on dissolved hydrogen, oxygen, pH and global stress, which has been found to be consistent for both, experimental studies and mathematical modeling.
Aiming at the rational design and the identification of brilliant fluorescent reporters for targeted optical probes and fluorescence assays in biological matrices, we systematically assessed the correlation between dye–protein binding, dye aggregation, and dye hydrophilicity for bioanalytically relevant fluorescent labels. Here, we report on the influence of sulfonic acid groups on dye aggregation and dye–serum protein interactions exemplarily for a family of NIR-emissive cyanine dyes, the DY-67x fluorophores. For highly hydrophobic dyes like DY-675 and DY-676, which show a strong tendency for aggregation in phosphate buffer saline solution, the dye–protein binding constants determined spectroscopically using a 2-state binding model, which considers only protein-bound and unbound dye molecules, can be influenced by the dimerization of the unbound dyes. To consider and quantify this influence, we expanded this common photometric method to a 3-state model that accounts for the presence of dye aggregates in the binding studies. Our results can be exploited for the screening of fluorescent reporters, efficiently providing information on the size of dye–protein interactions and on maximally achievable fluorescence quantum yields in biological systems.
The current European legislation requires that combined effects of the active substances and any substance of concern contained in biocidal products are taken into account in environmental risk assessment. The hypothesis whether the consideration of active substances together with all formulation additives that are labeled as presenting an environmental hazard is sufficient for a reliable environmental risk assessment was tested in the present study by investigating 3 wood preservative products. Relevant single substances in the products, some of their generic mixtures, the biocidal products themselves, and aqueous eluates prepared from the products (representing potential environmental mixtures) were tested for effects on algal growth and Daphnia acute immobilization as well as reproduction. Predictions for the products and the eluates were based on the concept of concentration addition and were mostly found to provide reliable or at least protective estimates for the observed acute and chronic toxicity of the mixtures. The mixture toxicity considerations also indicated that the toxicity of each product was dominated by just 1 of the components, and that assessments based only on the dominating substance would be similarly protective as a full-mixture risk assessment. Yet, there remained uncertainty in some cases that could be related to the toxicity of transformation products, the impact of unidentified formulation additives, or synergistic interaction between active substances and formulation additives.
In 1976, a pressure vessel of a tank wagon burst during gravity shunting. The pressure vessel was filled with cold fluid carbon dioxide and failed by cleavage fracture explosively. Big parts of the vessel were flung up to 300 m, a building was destroyed, and rails as well as the superstructure of the gravity shunting yard were damaged.
The initiation sites of the fracture and the orientations of crack propagation were determined by means of the patterns on the fracture surfaces of the broken parts. The initiation sites were located in the heat-affected zone (HAZ) of welds, close to transitions of cross-sections and the starting and end points, respectively, of the welds. The primary initiation of crack propagation was almost certainly on the left side, close to the weld of the fixed bearing connecting the vessel with the carriage.
The results of metallographic investigations indicated the development of cold weld cracks during welding. Mechanical behavior assessments on specimens extracted from the failed vessel indicated sufficient strength and ductility in tensile loading. The values of the notched-bar impact energy or toughness were within the limits according to industry rules and standards, except for one metal sheet of the vessel that was welded to the left fixed bearing.
During shunting, two tank wagons were inappropriately braked, and began to roll too quickly. One rail brake used for deceleration of the wagons caused impulsive noises and vibrations, resulting in high impulsive loading of the first wagon. The cold weld cracks in the heat-affected zones near the fixed bearing of the pressure vessel were initiation points for unstable crack growth. As the result of very low notched-bar impact toughness, crack propagation was not arrested and unstable cleavage fracture occurred.
Due to a second similar accident, happened one year before, a program was started to assess characteristic values of pressure vessel materials and the influence of weld parameters by the manufacturer, the inspecting authority, and BAM. The scientific findings led to modifications of industry rules and standards with regard to using ISO-V specimens and to higher required values for notched-bar impact energy for fine grain structural steels.
Increased use of nanomaterials in everyday products leads to their environmental release and therefore, the information need on their fate and behaviour. Nanomaterials have to be suspended with high repeatability and comparability for studies on environmental effects. They also have to be well characterised with a focus on the state of agglomeration and particle size distribution. Dynamic light-scattering (DLS) is a common technique used for these measurements. If suspensions are prepared in different laboratories, then concern has risen about the comparability of the measured results, especially when different DLS instruments are used. Therefore, for quality assurance, a round-robin test was conducted to assess the comparability of different DLS instruments and a dispersion protocol in ten independent laboratories. Polystyrene and TiO2 were chosen as test (nano)materials. For the comparability of the DLS instruments, the average sizes of the PSL and a stabilised TiO2 suspension were measured. The measured average hydrodynamic diameter shows an overall good inter-laboratory comparability. For the PSL suspension, an average hydrodynamic diameter of 201 ± 13 nm and for the TiO2 suspension an average diameter of 224 ± 24 nm were detected. For the TiO2 suspension that was prepared at each laboratory following an established suspension preparation protocol, an average hydrodynamic diameter of 211 ± 11 nm was detected. The measured average particle size (mode) increased up to 284 nm with a high standard deviation of 119 nm if the preparation protocol could not established and different procedures or different equipment were employed. This study shows that no significant differences between the employed DLS instrument types were determined. It was also shown that comparable measurements and suspension preparation could be achieved if well-defined suspension preparation protocols and comparable equipment can be used.
A calibrated instrumental setup was specially developed for the purposes of accurate measurements of absolute X-ray spectra emitted by modern micro-focus, low-power X-ray tubes. By knowing all the instrumental parameters the spectra measured with the 16 m long setup are recalculated into emitted X-ray tube spectra in photons per eV per msr per nA per s.