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Klärschlammaschen weisen hohe Gehalte an Phosphor auf, dieser ist allerdings schlecht für Pflanzen verfügbar. Des Weiteren enthalten sie Schwermetalle die vor dem Einsatz als Düngemittel entfernt werden müssen. Vor diesem Hintergrund wurden in den letzten Jahren nasschemische und thermochemische Verfahren entwickelt und zum Teil bereits in Demonstrationsanlagen getestet. Ein thermochemischer Verfahrensansatz wird in diesem Beitrag näher vorgestellt. Klärschlammaschen werden mit Klärschlamm als Reduktionsmittel und Natriumsulfat als Aufschlussmittel im Drehrohrofen thermisch behandelt. Bei diesem Prozess wird pflanzenverfügbares NaCaPÜ4 gebildet, unerwünschte Elemente wie As, Cd, Hg und Pb werden zum Teil über die Gasphase separiert. Die Ergebnisse eines Demonstrationsversuchs werden vorgestellt.
Oxidation of a Fe –13Cr alloy under water vapor at 600°C produced a zone of nano-sized precipitation underneath the outside scale formed by iron oxides and Fe–Cr spinel. The majority of the spinel layer shows a fixed orientation relationship to the ferritic matrix: {1 0 0}α || {1 0 0}sp & <0 1 1>α || <0 0 1>sp . However, also the discovered precipitated particles are characterized by the same crystallographic orientation relationship to the respective ferritic parent grain. The habit of the precipitates is best described by a lath morphology with their main axis parallel to <1 0 0> of ferrite. Energy dispersive X-ray spectroscopy (EDX) and electron backscatter diffraction (EBSD) in scanning electron microscope (SEM) have been applied to characterize the oxide layer in micrometer scale. The clearly smaller precipitates were subsequently investigated by transmission electron microscopy (TEM). Specimens have been prepared by focused ion-beam (FIB) milling at an area previously characterized by EBSD. They cover the ferritic base material, but mainly the precipitation zone and the Fe–Cr spinel layer. Energy filtered selected area diffraction (SAD) in the conventional (C)TEM and high-angle annular dark field (HAADF) imaging in the scanning (S)TEM mode were employed in the characterization of the specimens.
Samples of 474 forest stands in Germany were analysed for concentrations of polycyclic aromatic hydrocarbons (PAHs) in three sampling depths. Enhanced concentrations were mainly found at spots relatively close to densely industrialized and urbanized regions and at some topographically elevated areas. Average enrichment factors between mineral soil and humic layer depend on humus type i.e. decrease from mull via moder to mor. Based on their compound-patterns, the observed samples could be assigned to three main clusters. For some parts of our study area a uniform assignment of samples to clusters over larger regions could be identified. For instance, samples taken at vicinity to brown-coal strip-mining districts are characterized by high relative abundances of low-molecular-weight PAHs. These results suggest that PAHs are more likely originated from local and regional emitters rather than from long-range transport and that specific source-regions can be identified based on PAH fingerprints.
In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L-1 in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP–MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250–1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the experimental conditions are drawn. This work shows that SPE is a convenient technique for TBT pre-concentration at pico-trace levels and a robust approach: in fact (i) number of different experimental conditions led to satisfactory results and (ii) the participation of two institutes to the experimental work did not impact the developed model.
Two different hair reference materials, one produced from authentic hair displaying an ethyl glucuronide (EtG) content of about 25 pg/mg and one obtained by fortification of blank hair to an EtG level of 85 pg/mg were submitted to accelerated aging between 4 degrees C and 60 degrees C for periods between one and 24 months. Subsequently, the EtG content was determined in the aged samples and untreated reference samples stored at -22 degrees C under repeatability conditions following the so-called isochronous approach. The EtG content remained stable even at 40 degrees C for 24 months and at 60 degrees C over six months. This is in contrast to many organic analytes contained in trace concentrations in diverse matrices. A slight but significant increase of the recovered EtG in case of authentic hair samples having been exposed for 24 months between 4 degrees C and 60 degrees C may be due to a temperature-driven process that allows increased recoveries of the physiologically embedded EtG.
Recently three of the authors of this paper presented analytical solutions for reference loads of plate geometries with semi-elliptical surface cracks subjected to tension, bending, combined tension-bending and biaxial tension. These solutions were shown to provide more accurate crack driving force estimates than the conventional limit load solutions available in the literature, and the method behind them allowed for a wider application range. Within the present paper a methodology for the fracture analysis of thick-wall pressurized pipes using the R6 assessment method and considering both, biaxial and combined tension-bending loading is developed and validated. The analyses are carried out analytically, and the comparison between the predicted critical loads and experimental burst test failure loads shows satisfying agreement, this way demonstrating the potential of the proposed method.
We have studied the mechanisms of water-based quenching of the upconversion photoluminescence of upconverting nanophosphors (UCNPs) via luminescence decay measurements for a better understanding of the non-radiative deactivation pathways responsible for the relatively low upconversion luminescence efficiency in aqueous solutions. This included both upconversion luminescence measurements and the direct excitation of emissive energy states of Er3+ and Yb3+ dopants in NaYF4:Yb3+,Er3+ UCNPs by measuring the decays at 550 and 655 nm upon 380 nm excitation and at 980 nm upon 930 nm excitation, respectively. The luminescence intensities and decays were measured from both bare and silanized NaYF4:Yb3+,Er3+ and NaYF4:Yb3+,Tm3+ UCNPs in H2O and D2O. The measurements revealed up to 99.9% quenching of the upconversion photoluminescence intensity of both Er3+ and Tm3+ doped bare nanophosphors by water. Instead of the multiphonon relaxation of excited energy levels of the activators, the main mechanism of quenching was found to be the multiphonon deactivation of the Yb3+ sensitizer ion caused by OH-vibrations on the surface of the nanophosphor. Due to the nonlinear nature of upconversion, the quenching of Yb3+ has a higher order effect on the upconversion emission intensity with the efficient Yb–Yb energy migration in the ~35 nm nanocrystals making the whole nanophosphor volume susceptible to surface quenching effects. The study underlines the need of efficient surface passivation for the use of UCNPs as labels in bioanalytical applications performed in aqueous solutions.
Quantitative laser-induced breakdown spectroscopy (LIBS) analysis operates on the assumption that the sample is completely dissociated and diffused within the highly energetic plasma on time-scales of analyte analysis, resulting in analyte emission ideally at the bulk plasma temperature and a signal that is linear with analyte mass concentration. However, recent studies focusing on aerosol analysis have found the heat and mass diffusion rates within laser-induced plasmas to be finite, resulting in particle-rich, locally perturbed areas within the hot bulk plasma. The goal of this study is to observe any related plasma differences, by calculating the bulk and local (i.e. analyte rich regions) plasma temperatures and electron density, to better understand the time frame of equilibrium between the local and bulk plasma properties. This study also seeks to determine whether the presence of large quantities of a matrix element can significantly alter the local plasma conditions, thereby generating matrix effects. We report the temporal profiles of particle-derived species, adding additional insight into the effect of local perturbation of plasma properties, with the conclusion that significant plasma residence (tens of microseconds) is necessary to minimize such effects.
Train-induced ground vibration can be excited by wheel and track irregularities and by two kinds of irregularities of the soil, by geometric irregularities or by the spatially varying soil stiffness. For both types of irregularities, the effective track irregularity on top of the track is calculated in wavenumber domain and with wavenumber integrals. For a general multi-beam track model, the wavenumber integrals are solved numerically. The irregularities of the soil are filtered by the track when transferred from the bottom to the top of the track. The high-wavenumber irregularities are strongly reduced due to the bending stiffness of the track and the compliance of the support. In addition, soft track elements reduce directly the stiffness variation of the support. Therefore, the mitigation effect of elastic track elements for these excitation components seems to be important. For under-sleeper pads and slab tracks, calculation and measurements are presented including additional excitation components and the dynamic vehicle–track interaction, and the relevance of the excitation mechanisms is discussed based on the dynamic forces which are acting on the ground. Due to the restricted amplitudes, the parametric excitation by the stiffness variation seems to be less important than the geometric irregularities. The calculations yield the correct trends of the measurements and many details of the measured ballast, slab, and under-sleeper-pad tracks.
The reduction of train-induced ground vibration by elastic elements such as rail pads and sleeper pads has been analyzed by a combined finite-element boundary-element method. The dynamic compliance of the track, the transfer function of the total force on the ground and the ground vibration ratios have been calculated for a variety of isolated and un-isolated track systems. It has been found that the soil force transfer, which describes the excitation force of the soil, is an appropriate quantity to predict the reduction of the ground vibration and the effectiveness of isolated tracks. All force transfer functions of isolated tracks display a vehicletrack resonance where the wheelset on the compliant track is excited by wheel and track irregularities. At higher frequencies, considerable reductions of the amplitudes are observed as the benefit of the resilient element. The influence of the stiffness of the rail or sleeper pads, the ballast and the soil, and the mass of the sleeper and the wheelset on the resonance frequency and the reduction has been investigated. Sleeper pads are advantageous due to the higher mass that is elastically supported compared to the rail-pad track system. The combination of elastic rail and sleeper pads has been found to be disadvantageous, as the second resonance occurs in the frequency range of intended reduction.
Ground vibrations due to different technical sources are analysed in theory and experiment for the dispersion of Rayleigh waves and the admittance spectra. Both tasks are theoretically based on the same concept: The admittance function in frequencywavenumber domain yields the dispersion as its maxima, and the admittance function in space domain is obtained by integrating it over the wavenumbers. On the experimental side, many signal processing methods have been applied to many sites and have been developed by the authors in the last 35 years, i.e., time-domain methods, including the cross-correlation method, and frequency-domain methods such as the spectral analysis of surface waves with two or multiple sensors, the wavenumber-transform method, and the spatial autocorrelation method. All methods are presented by their basic formula and by at least one example site. Different sensor arrays and deterministic and stochastic sources have been tested for the spatial autocorrelation method and the wavenumber-transform method at several sites. In addition, all frequency-domain methods are presented for a specific layered site comparing their quality. The evaluated dispersion curves are very similar, but a somewhat higher frequency range has been found for the fastest method, i.e., the multi-sensor spectral-analysis-of-surface-waves method. The theoretical solutions have been used for the inversion of the measured dispersion to the soil profile of the specific layered soil. The theoretical soil model has subsequently been used to predict the ground vibration spectra of hammer and railway excitation that exhibit a good agreement with the corresponding measurements. Thus, the contribution shows the benefit of active and passive seismic methods for the prediction of railway vibration, including a new version of the spatial autocorrelation method for technical vibrations. On the other hand, technical and namely railway vibrations are considered a seismic source for the exploration of near surface soils.
We investigate a single-pixel camera (SPC) that relies on non-mechanical scanning with a terahertz (THz) spatial light modulator (SLM) and Compressed Sensing (CS) for image generation. The camera is based on a 350 GHz multiplier source and a Golay cell detector. The SLM consists of a Germanium disc, which is illuminated by a halogen lamp. The light of the lamp is transmitted through a thin-film transistor (TFT) liquid crystal display (LCD). This enables the generation of light patterns on the Germanium disc, which in turn produce reflecting patterns for THz radiation. Using up to 1000 different patterns the pseudo-inverse reconstruction algorithm and the CS algorithm CoSaMP are evaluated with respect to image quality. It is shown that CS allows a reduction of the necessary measurements by a factor of three without compromising the image quality.
Spatial light modulators (SLM) can be used for many applications, including imaging and beam steering. With the emergence of THz SLMs being able to control thousands of pixels, the aforementioned applications become feasible for the THz region. The degree of control that can be exerted with a SLM and in turn its usefulness directly depends on the light pattern it creates. The resulting light patterns can be quite different from the intended light patterns, due to systematic and random non-uniformities, especially for large THz wavelengths. Here we present results on the performance of a Germanium based THz SLM. These results enable the efficient application of Compressed Sensing techniques in THz SLM imaging settings.
This paper shows how Angle-Resolved Scattering can reveal wear on engineered surfaces. The samples studied, three discs made of steel 100Cr6H used in gear wheels in the automotive industry, were assessed after they had undergone ball-on-disc tests. Scattering maps recorded for spatial frequencies from 0.1 µm-1 to 2.7 µm-1 show a contrast inversion around 0.36 µm-1 revealing the wear trace. Besides measurements of rms roughness, where mean values are 20 nm and 24 nm depending on the locations considered, stationarity and isotropy, we demonstrate the ability of the technique to reveal localized wear on this type of surface in a rapid, robust and convenient way. We show that the tool trace is influenced by the load magnitude rather than by the number of oscillation cycles and highlight the key role played by surface roughness in how the sample responds to wear tests.
Pitting corrosion is one of the most common mechanisms of local passivity breakdown on stainless steels. Electrochemical methods have preferentially been applied for the evaluation of pitting corrosion resistance of stainless steels in laboratory. Nevertheless, some of them are not reliable enough and in general the application of electrochemical methods in the field becomes difficult because of a required deep understanding of corrosion phenomena and measurement technology. A new approach for the evaluation of the pitting corrosion susceptibility of stainless Steel surfaces in the laboratory as well as in the field is frequently demanded by representatives of the metalworking industry. Therefore, the KorroPad-test was invented and patented as part of a research project at the BAM Federal Institute for Materials Research and Testing in Germany.
Contents of deformation-induced martensite in the lattice structure of austenitic stainless steels lead to an either beneficial or detrimental change of mechanical and magnetic properties depending on the prospective application. Whereas these changes are well-known and investigated widely the influence of deformation-induced martensite on the corrosion behaviour is frequently an issue of scientific discussions. There are opposing opinions that depend on the type of corrosion mechanism being investigated for example regarding pitting corrosion resistance in Chloride containing media. In it is stated that pitting resistance is not influenced by deformationinduced martensite while in it is discussed that more pitting occurs on martensitic structure. The same conflictive opinions appear regarding active dissolution in acidic media or intergranular corrosion. In addition, when having deeper insight into literature it can be concluded that even the type of test method, i. e. dynamic or static testing, has a big influence on the obtained results concerning the influence of martensite in austenitic stainless steels.
Polypropylen (PP) ist als Niedrigenergie-Polymer ohne nass- und plasmachemische Vorbehandlung weder haftfest zu beschichten noch verbundfest zu kleben. Typische Haft- bzw. Klebfestigkeiten liegen für die unbehandelte Polymeroberfläche bei maximal 0,5 MPa. Hinzu kommt, dass bei der Bestimmung von Haft- und Klebfestigkeiten der unmodifizierten Oberfläche mit großen Streuungen zu rechnen ist, die bezogen auf die Spannweite durchaus einem Faktor 5 entsprechen können. Generell besteht bei Prüfung der Haftfestigkeit mittels Stirnabzugsversuch und bei der Prüfung der Klebfestigkeit die Notwendigkeit eines statistisch validierten Herangehens. Hierzu sind zeitaufwändige Ein-Proben-Klebungen und -Prüfungen nur eingeschränkt geeignet. Zudem ist, insbesondere für geringe Haft- bzw. Klebfestigkeiten, ein querkraftfreies Prüfen Grundvoraussetzung. Im vorliegenden Beitrag werden verschiedenartige plasmagestützte Oberflächenfunktionalisierungen von PP sowie das Mehr-Proben-Konzept zur Klebung/Prüfung von bis zu acht Proben vorgestellt. Dazu werden ein BAM-Funktionsmuster einer Mehr-Proben-Kleb-Vorrichtung und eine kommerzielle analytische Zentrifuge zum Prüfen verwendet.
The memory effect in polyolefinic products: A tool for confirming the steam sterilization process
(2015)
DSC-Messungen von dampfsterilisierten medizinischen Produkten aus Polyolefinen zeigen beim ersten Heizvorgang als auffällige Besonderheit eine zusätzliche Stufe, bekannt als Temperpeak. Das Ziel dieser Untersuchungen ist, dieses Phänomen nachzuvollziehen und zu verstehen, um es als Nachweis für die Dampfsterilisation nutzen zu können. Dafür wurden PP- und PE-Proben unter verschiedenen Bedingungen dampfsterilisiert und im Ofen thermisch behandelt. Anschließend wurden die Proben mittels DSC untersucht und die Einflüsse der thermischen Behandlung und der mechanischen Beanspruchung analysiert. Um den Einfluss unterschiedlicher Materialspezifikationen zu prüfen, wurden zusätzlich verschiedene Referenzmaterialien (PE und PP) untersucht und GPC-Messungen durchgeführt. Des Weiteren wurde die Beständigkeit des Signals gegenüber der Zeit und der Temperatureinflüssen betrachtet. Die Untersuchungen zeigen, dass sich ein stabiler Memory-Effekt erzeugen lässt.
The safety of components or constructions is of great importance in the manufacturing and processing of metallic materials. Solidification cracking as well as the weldability of materials remain still for many years a highly contentious issues, particularly with regard to the causes of the hot crack formation. Many of studies have been conducted to determine the critical condition of occurrence of the solidification cracking. In this study different digital image correlation measuring techniques in conjunction with laser diodes as the illuminating source have been employed to measure the arising strain field during the laser welding process at the surface of the workpiece directed to the laser beam in the close vicinity of the weld pool. The Controlled Tensile Weldability test (CTW) was used to apply an external tensile load during the laser beam welding in order to generate the solidification cracks. The results showed that by means of those techniques it is possible to measure the strain field without any disturbances from the intense welding light or the smoke. Additionally, the strain and the strain rate as a critical factor determining solidification crack formation can be measured and analyzed.
The combination of two analytical methods including time-resolved in situ X-ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for a detailed analysis of the key mechanisms of milling reactions. To prove the general applicability of our setup, we investigated the mechanochemical synthesis of four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. The reaction mechanism for each model compound could be elucidated. The results clearly show the unique advantage of the combination of XRD and Raman spectroscopy because of the different information content and dynamic range of both individual methods. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structures and thus obtaining reliable data for mechanistic studies.