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Eingeladener Vortrag
- nein (1008)
Sulfur is one of the major impurity elements in copper. Previously applied methods for the quantification of sulfur in copper and other pure metals revealed a lack of traceability and showed inconsistent result. Therefore, in this study a procedure was developed for the quantification of total sulfur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). A major challenge for the quantification of sulfur in copper (alloyed/unalloyed) by ICPMS is the copper matrix itself, causing matrix effects and making an extensive cleaning (cones, extraction lens) necessary after measurements. Matschat et al investigated the analysis of high-purity metals (including copper) by high resolution ICP-MS and found that the copper matrix shows strong matrix effects on the sensitivity resulting from Cu deposition on the cones. Therefore, the major part of the copper matrix has to be separated, which was accomplished by adding ammonia which forms a complex with the copper while releasing the sulfur. This was followed by a chromatographic separation using a weak cation resin. After that the sulfur fraction was further purified by chromatographic means using an anion exchange method followed by a chelating resin.
The anion exchange resin (AG1X8), however, is selective to sulfate and sulfite but less-selective to sulfide. Therefore, when quantifying total sulfur in copper, the different species of sulfur need to be oxidized to sulfate prior to the sulfur-matrix separation on the AG1X8 resin in order to avoid any measurement bias. When applying the HPA oxidation with concentrated HNO3 and H2O2 a complete conversion from sulfide and sulfite to sulfate could be achieved. The recovery of all investigated sulfur species is quantitative within measurement uncertainties. The copper samples investigated in this study contain copper in the range of 0.85-0.99 kg·kg-1 and zinc from <10 to 300 g·kg-1. Approximately 0.10-0.25 g of these samples were used to perform the sulfur-copper separation. After applying the complete three stage separation procedure the mass fractions of both elements were significantly reduced to below 400 ng·g-1 for copper and below 50 ng·g-1 for zinc, respectively. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (> 99.999%) while keeping the recovery of sulfur above 80%.
The procedure blank was determined by IDMS as well and yielded values for the individual IDMS measurement sequences ranging from 3 ng to 53 ng. The average of these individual procedure blanks (n=22) was calculated and yielded a total procedure blank of 14 ng sulphur with standard deviation of 12 ng. The limit of detection (LOD, blank+3SD) calculated on this basis was 0.20 µg·g-1 while the limit of quantification (LOQ, blank+10SD) was 0.54 µg·g-1, when considering a sample weight of 0.25 g.
The quantification of low sulfur contents (< 15 µg/g) by conventional IDMS is hindered by the very high Cu/S ratio, which clearly affects the separation in a negative way: The recovery of sulfur dropped to about 30 % for four replicates, while two further replicates even showed recoveries below 10%. To enable measurement without completely changing the separation procedure, an exact amount of sulfur was added prior to spiking, such that the sulfur mass fraction was shifted to the optimum working range of the separation procedure. Thus exact amounts of sulfur were added to enhance the mass fraction of sulfur from 15 µg·g-1 to 40 µg·g-1, then the IDMS analysis was performed as usual and finally the added sulfur amount was subtracted. The so obtained measurement result agreed well with the certified value within the uncertainties. The relative expanded measurement uncertainties for conventional IDMS are below 1%. When applying the modified IDMS procedure, where back-spike is added to the sample before spiking, the relative expanded measurement uncertainties are larger and up to 5%. With the presented sulfur-matrix procedure a working range from approximately 15 µg·g-1 to 1500 µg·g-1 can be achieved.
The developed procedure for the quantification of low sulfur amounts in copper has been validated here via three different routes: first an inter-laboratory comparison at highest metrological level, second a step-by-step validation by checking each single step of the procedure and third the setup of a complete uncertainty budget.
The procedure is sufficient to facilitate value assignment of total sulfur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated below 1 % and the measurement results are traceable to the SI, which is clearly demonstrated in this work. The procedure reported in this study is a new reference procedure for sulfur measurement in copper, well meeting the requirements of the two major purposes: the certification of reference materials and the assignment of reference values for inter-laboratory comparison.
Derzeit gibt es intensive Diskussionen über die Entlassung von Deponien aus der Nachsorgephase. Die Deponie müsste dafür nach der Deponieverordnung (DepV) u. a. „insgesamt dauerhaft standsicher" sein. Geokunststoffe erfüllten ihre Funktion über einen Zeitrahmen von lediglich mindestens hundert Jahren. Dies stehe somit im Widerspruch wird argumentiert. Das neue LANUV-Arbeitsblatt 33 schließt daher im Moment eine Entlassung aus der Nachsorge von Deponien faktisch aus, wenn in den Böschungen Geokunststoffprodukte eingesetzt wurden. Auch der Fachbeirat der BAM zur Zulassung von Geokunststoffen, Polymeren und Dichtungskontrollsystemen hat sich daher mit der Thematik beschäftigt. Die aktuelle Situation soll daher auf dieser Grundlage diskutiert werden.
Design challenges for offshore wind-farms. From foundation mechanics to wind-farm aerodynamics
(2018)
This talk provides a brief introduction on general engineering aspects of offshore wind energy production. Then some geomechanical issues for the foundation of OWTs into the seabed are introduced, while the results from experimental investigations and coupled computational analysis are discussed.
In the second part of the seminar, the hydromechanical Wave–Tower interaction is firstly discussed. Then, some general aspects of the windfarm aerodynamics are introduced. On the one hand, some modelling possibilities for the wake analysis of single turbines and turbine groups are discussed. And on the other hand the relevance of such analyses for a proper windfarm layout optimization is pointed out.
Concerning the geomechanical issues the talk shows that: i) The pile’s bearing capacity can degrade under cyclic loading (waves, wind, …). ii) The time effects can be relevant: Capacity improvement can be substantial, but also fragile. iii) There are cyclic PWP effects: Cyclic interaction with pore water may lead to soil softening and an uncoupled analysis (current design practice) is potentially unsafe.
And concerning the hydromechanical and aerodynamical design considerations, this seminar shows that: i) Numerical analysis of turbine’s interaction with wind/waves is useful and affordable. ii) Simplified models can provide insight into windfarm aerodynamics. iii) Turbulent wake analysis is very relevant for the windfarm layout.
Abstract: Hybrid silicon-based organic/inorganic (multi)block
copolymers are promising polymeric precursors to create
robust nano-objects and nanomaterials due to their sol–gel active moieties via self-assembly in solution or in bulk. Such nano-objects and nanomaterials have great potential in bio-medicine as nanocarriers or scaffolds for bone regeneration as well as in materials science as Pickering emulsifiers, pho-
tonic crystals or coatings/films with antibiofouling, antibac-
terial or water- and oil-repellent properties. Thus, this Review outlines recent synthetic efforts in the preparation of these hybrid inorganic/organic block copolymers, gives an
overview of their self-assembled structures and finally presents recent examples of their use in the biomedical field and
material science.
The possible impact of ultrafine particles from laser printers on human health is controversially discussed although there are persons reporting substantial symptoms in relation to these emissions. A randomized, single-blinded, cross-over experimental design with two exposure conditions (high-level and low-level exposure) was conducted with 23 healthy subjects, 14 subjects with mild asthma, and 15 persons reporting symptoms associated with laser printer emissions. To separate physiological and psychological effects, a secondary physiologically based categorization of susceptibility to particle effects was used. In line with results from physiological and biochemical assessments, we found no coherent, differential, or clinically relevant effects of different exposure conditions on subjective complaints and cognitive performance in terms of attention, short-term memory, and psychomotor performance. However, results regarding the psychological characteristics of participants and their situational perception confirm differences between the participants groups: Subjects reporting symptoms associated with laser printer emissions showed a higher psychological susceptibility for adverse reactions in line with previous results on persons with multiple chemical sensitivity or idiopathic environmental intolerance. In conclusion, acute psychological and cognitive effects of laser printer emissions were small and could be attributed only to different participant groups but not to differences in exposure conditions in terms of particle number concentrations.
Elektromagnetische Schmelzbadkontrolle wurde erfolgreich für Laser-MSG-Hybridprozess an einem (ferromagnetischen) 20 mm Baustahl und einem Pipelinestahl eingesetzt.
Einlagiges Laserstrahlschweißen von dickwandigen(>20 mm) in PA-Position bei geringeren Schweißgeschwindigkeiten prinzipiell möglich.
Reduzierung der Schweißgeschwindigkeit beim Laserstrahlschweißen hat eine Verringerung der notwendigen Laserleistung und eine Verbesserung der mechanisch-technologischen Eigenschaften von Schweißverbindungen zur Folge.
Structural changes of highly active Pd/MeOx (Me = Fe, Co, Ni) during catalytic methane combustion
(2018)
Fe2O3, Co3O4 and NiO nanoparticles were prepared via a citrate method and further functionalized with Pd by impregnation. The pure oxides as well as Pd/Fe2O3, Pd/Co3O4, and Pd/NiO (1, 5 and 10 wt % Pd) were employed for catalytic methane combustion under methane lean (1 vol %)/oxygen rich (18 vol %, balanced with nitrogen) conditions. Already, the pure metal oxides showed a high catalytic activity leading to complete conversion temperature of T100 ≤ 500 °C. H2-TPR (Temperature-programmed reduction) experiments revealed that Pd-functionalized metal oxides exhibited enhanced redox activity compared to the pure oxides leading to improved catalytic combustion activity at lower temperatures. At a loading of 1 wt % Pd, 1Pd/Co3O4 (T100 = 360 °C) outperforms 1Pd/Fe2O3 (T100 = 410 °C) as well as 1Pd/NiO (T100 = 380 °C). At a loading of 10 wt % Pd, T100 could only be slightly reduced in all cases. 1Pd/Co3O4 and 1Pd/NiO show reasonable stability over 70 h on stream at T100. XPS (X-ray photoelectron spectroscopy) and STEM (Scanning transmission electron microscopy) investigations revealed strong interactions between Pd and NiO as well as Co3O4, respectively, leading to dynamic transformations and reoxidation of Pd due to solid state reactions, which leads to the high long-term stability.
Lanthanide-based upconversion nanoparticles (UCNPs) offer new strategies for luminescence-based sensing and imaging. One of the best studied materials are hexagonal ß-NaYF4 UCNPs doped with 20% Yb3+ and 2% Er3+, which efficiently convert 976 nm light to photons emitted at 540 nm, 655 nm, and 845 nm, respectively, reveal Long luminescence lifetimes (> 100 µs), and are very photostable and chemically inters.[1,2] The properties of their upconversion (UC) luminescence (UCL) are, however, strongly influenced by particle size, concentration and spatial arrangement of dopant Ions, surface chemistry, and microenvironment.[3,4] In addition, the multiphotonic absorption processes responsible for UCL render UCL dependent on excitation power density (P).
The rational design of brighter UCNPs particle architectures encouraged us to assess systematically the influence of these parameters on UCL for differently doped UCNPs relying on the commonly used ß-NaYf4 matrix using steady state and time resolved fluorometry as well as integrating sphere spectroscopy for P varied over almost three orders of magnitude. This includes comprehensive studies of the influence of size and shell, Yb3+ and Er3+ dopand concentrations, and energy Transfer processes from UCNPs to surface-bound organic dyes or vice versa [5]. Our results underline the need for really quantitative luminescence studies for mechanistic insights, the potential of high p to compensate for UCL surface quenching, and the matrix- and P-dependence of the optimum dopand concentration.
Die Versalzung und Verunreinigung von Metalloberflächen durch chloridhaltige Aerosole hat eine große Bedeutung für das Korrosionsverhalten von beschichteten Metalloberflächen im maritimen Bereich und bei Offshore-Anwendungen. So ist z. B. zu klären, ob und in welchem Maße eine Versalzung der Oberfläche Einfluss auf die Haftung und Dauerhaftigkeit von Beschichtungen hat. Dafür sind Detailfragen zu klären, etwa mit welcher Versalzung nach welchem Zeitraum zu rechnen ist oder wie für systematische Untersuchungen eine definierte und reproduzierbare Versalzung im Labor nachgestellt werden kann. Der Beitrag widmet sich diesen Fragestellungen. Es werden Ergebnisse eines Feldversuches auf Helgoland gezeigt und ein einfaches Verfahren zur definierten Beladung von Metalloberflächen mit Chloriden im Labormaßstab vorgestellt.
Die Versalzung und Verunreinigung von Metalloberflächen durch chloridhaltige Aerosole hat eine große Bedeutung für das Korrosionsverhalten von beschichteten Metalloberflächen im maritimen Bereich und bei Offshore-Anwendungen. So ist z. B. zu klären, ob und in welchem Maße eine Versalzung der Oberfläche Einfluss auf die Haftung und Dauerhaftigkeit von Beschichtungen hat. Dafür sind Detailfragen zu klären, etwa mit welcher Versalzung nach welchem Zeitraum zu rechnen ist oder wie für systematische Untersuchungen eine definierte und reproduzierbare Versalzung im Labor nachgestellt werden kann. Der Beitrag widmet sich diesen Fragestellungen. Es werden Ergebnisse eines Feldversuches auf Helgoland gezeigt und ein einfaches Verfahren zur definierten Beladung von Metalloberflächen mit Chloriden im Labormaßstab vorgestellt.
Improving the energy efficiency of products was identified as the most important short-term opportunity to decrease energy consumption and therefore CO2-emission worldwide. More efficient products are created due to technical innovation. Restricting market access to efficient products only and making the most efficient products stand out by energy labelling are legislative approaches to encourage this development. Market surveillance authorities’ checks are fundamental to protect the consumer from wrongly declared goods on the market and ensure fair competition between manufacturers. However, the activities of market surveillance authorities are limited by their financial resources. Testing all product efficiency parameters in an accredited laboratory is very time consuming and cost intensive. In this article, a theoretical concept is presented which can be used to develop screening tests enabling market surveillance authorities to perform product tests with less financial resources. The concept identifies components which lead to non-compliance or make a product less energy efficient with minimum effort. The principle is based on a combination of random product tests, disassembling specific products and comparing components. This represents a new approach in product testing procedures beyond the current market surveillance activities. The concept is being tested within a research project funded by the German government.
TAHYA Kick-Off Meeting
(2018)
Beim Bau einer Salzgrotte für eine Wellnesslandschaft im Keller eines Wohnhauses kam es zu einer folgenschweren Explosion: Die bei der Verwendung des Bauschaums freigesetzten Gase und Dämpfe sammelten sich im Keller und entzündeten sich schließlich. Durch die Explosion starben zwei Arbeiter, ein weiterer Arbeiter sowie die Käuferin der Salzgrotte erlitten massive Verbrennungen.
Dieser Aufsatz stellt das Gerichtsurteil gegen die Geschäftsführer der ausführenden GmbH vor, bereitet die wesentlichen Aussagen zu Gefährdungsbeurteilung, Schutzmaßnahmen, Betriebsanweisung, Unterweisung und Aufsichtsführung auf, erläutert sie und ergänzt Bezüge zur heute einschlägigen Gefahrstoffverordnung (GefStoffV).
The tribological characteristics of pure and graphite filled polymers were investigated in gaseous hydrogen at ambient temperatures and in LH2 at -253°C. It could be shown that the tribological properties of PI and PEEK materials is related to the formation of a transfer film. The influence of both hydrogen and cryogenic temperatures will be discussed in the presentation.
The tribological characteristics of pure and graphite filled polymers were investigated in gaseous hydrogen at ambient temperatures and in LH2 at -253°C. It could be shown that the tribological properties of PI and PEEK materials is related to the formation of a transfer film. The influence of both hydrogen and cryogenic temperatures will be discussed in the presentation.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
The wear rates of self-mated alumina couples show that friction as well as wear is largely determined by the above-mentioned hydro-thermal conditions. The presence of water and its amount available in the surrounding system either in liquid or in gaseous form plays a key role for friction and wear behavior and can be beneficial for the tribological profile of steam degradation resistant materials. Hot steam enhances the tribo-chemical formations of oxides and hydroxides on MgO-ZrO2 alumina and antimony impregnated carbon.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
The wear rates of self-amted alumina couples show that friction as well as wear is largely determined by the above mentioned hydro-thermal conditions. The presence of water and ist amount available in the surrounding system either in liquid or in gaseous from plays a key role for friction and wear behavior and cabe benefical for the tribological profile of steam degradation resistant materials. Hot steam enhances the tribo-chemical formations of oxides and hydroxides on MgO-ZrO2, alumina and antimony impregnated carbon.
Recent DNA-based studies have shown that the built environment is surprisingly rich in fungi. These indoor fungi – whether transient visitors or more persistent residents – may hold clues to the rising levels of human allergies and other medical and building-related health problems observed globally. The taxo¬nomic identity of these fungi is crucial in such pursuits. Molecular identification of the built mycobiome is no trivial undertaking, however, given the large number of unidentified, misidentified, and technically compromised fungal sequences in public sequence databases. In addition, the sequence metadata required to make informed taxonomic decisions – such as country and host/substrate of collection – are often lacking even from reference and ex-type sequences. Here we report on a taxonomic annotation workshop (April 10–11, 2017) organized at the James Hutton Institute/University of Aberdeen (UK) to facilitate reproducible studies of the built mycobiome. The 32 participants went through public fungal ITS bar¬code sequences related to the built mycobiome for taxonomic and nomenclatural correctness, technical quality, and metadata availability. A total of 19,508 changes – including 4,783 name changes, 14,121 metadata annotations, and the removal of 99 technically compromised sequences – were implemented in the UNITE database for molecular identification of fungi (https://unite.ut.ee/) and shared with a range of other databases and downstream resources. Among the genera that saw the largest number of changes were Penicillium, Talaromyces, Cladosporium, Acremonium, and Alternaria, all of them of significant importance in both culture-based and culture-independent surveys of the built environment.
Soiling of photovoltaic (PV) systems compromises their performance causing a significant power loss and demanding periodical cleaning actions. This phenomenon raises great concerns in the solar energy field, thus leading to notable research efforts over the last decades. Soiling is caused by a dual action of dust deposition and biofouling. However, surprisingly, the microbiological contribution to PV soiling is often overlooked or underestimated. In this study, a variety of qPCR-based methods have been developed to quantify the microbial load of fungi, bacteria and phototrophs on PV panels. These protocols were evaluated by comparison with culturedependent methods, and were implemented with real solar plants for two years. The results show that the developed molecular methods are highly sensitive and reliable to monitor the microbial component of the soiling. Fungal biomass was clearly dominant in all analysed PV modules, while bacteria and phototrophs showed much lower abundance. Light microscopy and qPCR results revealed that melanised microcolonial fungi and phototrophs are the main biofilm-forming microorganisms on the studied solar panels. In particular, the fungal qPCR protocol is proposed as a useful tool for monitoring of PV soiling, and investigating the microbial contribution to specific soiling cases.
Fuel contamination of soils display complex and variable hydrocarbon mixtures with different volatility and toxicity characteristics. A recently suggested headspace procedure for the structure-based quantification of volatile hydrocarbons is evaluated regarding repeatability, reproducibility, and practical robustness. Three aliphatic and three aromatic fractions covering the boiling range between 69 and 216°C were defined as summation parameters by their respective equivalent carbon number ranges. A standard mixture of 35 aliphatic and aromatic hydrocarbons was used for calibration on basis of selected mass fragments specific for the aliphatics and aromatics, respectively. Two standard soils were fortified with the standard mixture or different fuels, respectively, and submitted to the analytical procedure. Limit of detection (LOD) and limit of quantification (LOQ) were for all fractions lower than 0.1 and 0.3 mg/kg, respectively. Analyte recovery was linear up to between 20 and 110 mg hydrocarbons/kg soil depending on the fraction. Hydrocarbon recovery ranged between 80% and 110% depending on the fraction and the repeatability was typically better than 10%. Finally, the impact of extraction solvent variation, column solid-phase polarity, and alternative summation of fractions were investigated. The procedure was applied to liner samples taken from a site contaminated with aviation fuel and its practicability is discussed.
Alkali-activated slag materials are known for their high Chloride penetration resistance. This makes them potentially applicable as repair systems for damaged steel-reinforced concrete structures, which are exposed to chloride attack. For this purpose, the influence of the activator composition, i.e. the SiO2 and Na2O concentration of the alkaline solution on a) the compressive strength, b) shrinkage and mass change and c) the resistance against chloride penetration of four alkali-activated slag mortars (AASM) were studied. An ordinary Portland cement-based mortar was used as the reference sample. Increasing SiO2 and Na2O concentrations increased the strength, shrinkage and mass loss of the AASMs. The resistance of the mortars against chloride penetration was evaluated using the non-steady-state migration coefficient Dnssm obtained from NT BUILD 492. The results indicate that the Dnssm is related to differences in the pore solution of the AASMs rather than to differences in their microstructure. An upcoming study of the authors is going to evaluate this hypothesis by the accelerated chloride penetration (diffusion) test.
A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a sharp interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, investigated at the HERMES beamline is presented for demonstration. This STXM based methodology yields particle dimensions in good agreement with the scanning electron microscopy (SEM) results (deviation equal or less than 10%). Extension of this methodology to core-shell nanoparticles with inorganic core and organic shell will also be presented and the challenges encountered will be highlighted.
Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter.
Powder X-ray diffraction is a time-consuming and challenging task, especially for preparation of sensitive phases like ettringite and calcium-silicate-hydrate (C-S-H) phases. Fine-grained ultrahigh-performance concrete (UHPC) with an average grain size <100 μm could be investigated directly without time-consuming milling. As a proof of concept, small UHPC cylinders with plain surfaces were investigated with a newly designed sample holder. The comparison with conventionally prepared powder shows the feasibility of fast qualitative phase analysis using this approach. As a great benefit, a depth-dependent analysis, as well as a comparison of surface layers and core material, was carried out.
In order to satisfy the growing requirements towards lightweight design and resource efficiency in modern steel constructions, e.g., mobile cranes and bridges, high-strength steels with typical yield strength ≥ 690 MPa are coming into use to an increasing extent. However, these steels require special treatment in welding. The susceptibility for degradation of the mechanical properties
in the presence of hydrogen increases significantly with increasing yield strength. In case of missing knowledge about how and the amount of hydrogen that is uptaken during welding, hydrogen-assisted cracking (HAC) can be a negative consequence.
Moreover, modern weld technology like the modified spray arc process enables welding of narrower weld seams. In this context,
a reduced number of weld beads, volume, and total heat input are technical and economical benefits. This work presents the influence of welding parameters on the diffusible hydrogen content in both (1) single-pass and (2) multi-layer welds. Different
hydrogen concentrations were detected by varied contact tube distance, wire feed speed, arc length, and varied arc type (transitional
arc and modified spray arc). The results show that all welding parameters have significant influence on the diffusible hydrogen concentration in the single-pass welds. By increasing the number of weld beads in case of multi-layer welding, the
hydrogen concentration has been reduced. Whereby, differences in hydrogen concentrations between both arc types are present.
Anregungen aus dem N.i.Ke.-Workshop 2017 und künftige Anforderungen. BEMMA steht für Bewertung von Emissionen aus Materialien für Museumsausstattungen. Es ist die Kurzbezeichnung für ein Schema/Verfahren zur Untersuchung und Bewertung flüchtiger organischer Verbindungen aus Werkstoffen, die im mittelbaren Kontakt mit historischen Materialien des Kunst- und Kulturgutes stehen. Hier wird der Status-Quo des Erreichten dargestellt. Wie wird das Schema in der Museumsöffentlichkeit wahrgenommen und seine Akzeptanz.
Normgerechte Ausführung resultiert in Qualität, aber sie ist nicht allein ein Garant auch für hohe Qualität. Hierfür sind begleitend immer auch nachgeordnete Richtlinien wie z. B. spezifische Gütekriterien zu erfüllen. Der Vortrag erklärt die Normungsarbeit auf nationaler und internationaler Ebene und schildert die Stärken aber auch die Schwächen bei der Erstellung von Normen. Dabei ist die Konsensbildung zwischen unterschiedlichen interessierten Kreisen mit deren Partikularinteressen oftmals ein Hindernis, das aber über Zusatzvereinbarungen und der Norm nachgeordneten Regeln überwunden werden kann.
Several models of range hoods were tested by independent and accredited testing institutes. The results have been compared to the information declared by the manufacturer on the energy efficiency label and the product fiche. The measured electric power input of the lighting System and the measured grease absorption factor often differed significantly from the declared values.
The reasons for these observations and the necessary steps to ensure accurate measurements and a meaningful EU energy efficiency label are elucidated. It is suggested that the ranges of the lighting efficiency classes are readjusted to fit the nowadays prevalent LED technology.
Furthermore the tolerance in the regulation for the nominal electric power input of the lighting could be extended by a minimum absolute tolerance. The grease absorption test method may need a rework to achieve a satisfying accuracy.
In situ laser-induced breakdown spectroscopy measurements in stainless steels during TIG welding
(2018)
Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects. A prototype of a LIBS controlled welding process is presented.
BEMMA steht für Bewertung von Emissionen aus Materialien für Museumsausstattungen. Es ist die Kurzbezeichnung für ein Schema/Verfahren zur Untersuchung und Bewertung flüchtiger organischer Verbindungen aus Werkstoffen, die im mittelbaren Kontakt mit historischen Materialien des Kunst- und Kulturgutes stehen. Ergebnisse der Untersuchungen seit ca. 2010 bis 2017 werden präsentiert und diskutiert.
Metallische Druckgefäße werden aus Gründen der Gewichtseinsparung zunehmend durch Composite-Druckgefäße ersetzt. Während der Alterungsprozess bei metallischen Druckgefäßen durch Wöhlerkurven hinreichend beschrieben wird, ist der Alterungsmechanismus bei Composite-Druckgefäßen noch nicht vollständig geklärt. Im Rahmen des BAM-interne Themenfeldprojekts COD-AGE werden mit diversen Verfahren alterungsbegleitende, zerstörungsfreie Prüfungen an Composite-Druckgefäßen durchgeführt. Nach einem kurzen Überblick über die BAM und den FB 8.4 werden zunächst die allgemeine Funktionsweise der Wirbelstromprüfung und die bildgebende Wirbelstromprüfung erklärt. Anschließend werden Ergebnisse der konventionellen und hochfrequenten Wirbelstromprüfung vorgestellt.
Der letzte Teil des Vortrages beschäftigt sich mit der Prüfbarkeit von Kunststoffen aus Kunstharz und 3D-Druck mit dem Wirbelstromverfahren durch Zugabe ferromagnetischer Nanopartikel bzw. Verwendung von ferromagnetischem Filament.
Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering.
In vielen Industriebranchen werden zunehmend hochfeste Feinkornbaustähle mit Streckgrenzen ≥ 690 MPa eingesetzt. Allerdings werden mit zunehmender Festigkeit deutlich höhere Anforderungen an deren schweißtechnische Verarbeitung gestellt, da gerade die Sensibilität gegenüber einer Degradation der mechanischen Eigenschaften, durch den beim Schweißen aufgenommenen Wasserstoff, mit steigender Festigkeit stark zunimmt. In der vorliegenden Präsentation sind Ergebnisse aus vergleichenden Untersuchungen mit konventionellem Übergangslichtbogen und modifiziertem Sprühlichtbogen mit reduziertem Nahtöffnungswinkel hinsichtlich der Wasserstoffaufnahme beim Schweißen unter Variation von Streckenenergie, Arbeitstemperatur und Nachwärmprozedur dargestellt. Grundsätzlich ist den erarbeiteten Ergebnissen zu entnehmen, dass im Schweißgut von Stumpfstoßverbindungen mit reduziertem Nahtöffnungswinkel erhöhte mittlere Wasserstoffkonzentrationen vorliegen. Geeignete Wärmeführungen führten zu einer signifikanten Reduzierung der Wasserstoffkonzentration beim Einsatz der Nahtkonfiguration mit abgesenktem Nahtöffnungswinkel. Dabei erwies sich eine Nachwärmprozedur aus der Schweißwärme heraus als zielführend. Des weiteren sind Gradienten der Wasserstoffkonzentration in Blechdickenrichtung aufgezeigt.
Distortions in Additive Manufacturing (AM) Laser Metal Deposition (LMD) occur in the newly-built component due to rapid heating and solidification and can lead to shape deviations and cracking. This paper presents a novel approach to quantify the distortions experimentally and to use the results in numerical simulation validation. Digital Image Correlation (DIC) is applied together with optical filters to measure in-situ distortions directly on a wall geometry produced with LMD. The wall shows cyclic Expansion and shrinking with the edges bending inward and the top of the sample exhibiting a slight u-shape as residual distortions. Subsequently, a structural Finite Element Analysis (FEA) of the experiment is established, calibrated against experimental temperature profiles and used to predict the in-situ distortions of the sample. A comparison of the experimental and numerical results reveals a good agreement in length direction of the sample and quantitative deviations in height direction, which are attributed to the material model used. The suitability of the novel experimental approach for measurements on an AM sample is shown and the potential for the validated numerical model as a predictive tool to reduce trial-and-error and improve part quality is evaluated.
Calciumcobaltit und Calciummanganat gehören zu den vielversprechendsten thermoelektrischen Oxiden im Temperaturbereich zwischen 600 °C und 800 °C an Luft. Mittels thermoelektrischer Generatoren kann ein Temperaturgradient direkt in elektrische Leistung umgewandelt werden. Für die kostengünstige Pulverherstellung von Funktionsmaterialien wird im industriellen Maßstab meist die Festphasenreaktion (bzw. Kalzinierung) verwendet. Da es sich dabei um einen Hochtemperaturprozess handelt, ist diese Kalzinierung sehr energieintensiv. In der Literatur werden sehr unterschiedliche Prozessbedingungen zur Pulversynthese thermoelektrischer Oxide genutzt. Soweit dem Autor bekannt, ist keine systematische Untersuchung des Einflusses der Pulversynthesebedingungen auf die thermoelektrischen Eigenschaften publiziert.
Deshalb wurde eine systematische Untersuchung des Einflusses der Pulversynthesebedingungen (Temperatur, Haltezeit, Partikelgröße, Wiederholungen) auf die thermoelektrischen Eigenschaften von Calciumcobaltit und Calciummanganat durchgeführt.
Es konnte gezeigt werden, dass sich ein höherer Energieeintrag während der Kalzinierung negativ auf die thermoelektrischen Eigenschaften auswirkt.
Chemical functionalization for quantitative spectroscopic labeling on macroscopically flat surfaces
(2018)
This chapter highlights the application of chemical derivatization (CD) to facilitate the quantification of surface functional groups being an important issue for a wide field of applications. The selective attachment of a chemical label to a surface functional group being afterwards exclusively detectable by a highly sensitive technique overcomes the problem of characterizing low amounts of functional groups on macroscopically flat surfaces. The most frequently employed methods include CD X-ray photoelectron spectroscopy, ultraviolet/visible absorption, and fluorescence spectroscopy, as well as time-of-flight secondary ion mass spectrometry. Herein, the basic conditions for the different techniques regarding the specific surface functional group which need to be quantified are discussed. Additionally, the substrate highly influences the compatibility of the corresponding method. Because not just the quantification but also the preparation of the desired application is important, a summary of different preparation methods for glass, polymer and gold substrates is presented.
Time-resolved phase-contrast microscopy is employed to visualize spatio-temporal thermal transients induced by tight focusing of a single Ti:sapphire fs-laser pulse into a solid dielectric sample. This method relies on the coupling of the refractive index change and the sample temperature through the thermo-optic coefficient dn/dT. The thermal transients are studied on a timescale ranging from 10 ns up to 0.1 ms after laser excitation. Beyond providing direct insights into the laser–matter interaction, analyzing the results obtained also enables quantifying the local thermal diffusivity of the sample on a micrometer scale. Studies conducted in different solid dielectrics, namely amorphous fused silica (a-SiO2), a commercial borosilicate glass (BO33, Schott), and a custom alkaline earth silicate glass (NaSi66), illustrate the applicability of this approach to the investigation of various glassy materials.
Photoelectron spectroscopy
(2018)
Grundkenntnisse zum besseren Verständnis der Funktionsweise der Elektronenstrahl-Mikroanalyse (ESMA) werden präsentiert und anhand Beispielen diskutiert.
Das physikalische Messprinzip von ESMA am REM, das Wechselwirkungs- und Informationsvolum und die Anregung der charakteristischen Röntgenlinien werden erklärt. Verschiedene potentielle Artefakte, wie z.B. Heterogenität der Probenzusammensetzung, Oberflächenbeschaffenheit der Probe und Linienüberlagerung werden eingeführt.
Die physikalischen Grenzen der analytischen Methode werden spezifiziert.
Reaction procedures have been improved to achieve higher yields and shorter reaction times: one possibility is the usage of microwave reactors. In the literature, this is under discussion, for example, nonthermal effects resulting from the microwave radiation are claimed. Especially for the synthesis of nanomaterials, it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare the syntheses of ultra-small silver nanoparticles via conventional and microwave heating. We employed a versatile one-pot polyol synthesis of poly(acrylic acid)-stabilized silver nanoparticles, which display superior catalytic properties. No microwave-specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering and dynamic light scattering, are revealed. Because of the characteristics of a closed system, microwave reactors give access to elevated temperatures and pressures. Therefore, the speed of particle formation can be increased by a factor of 30 when the reaction temperature is increased from 200 to 250 °C. The particle growth process follows a cluster coalescence mechanism. A postsynthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particle size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A compromise between short reaction times and high yields can be found at a temperature of 250 °C and a corresponding reaction time of 30 s.
Metallische Druckgefäße werden aus Gründen der Gewichtseinsparung zunehmend durch Composite-Druckgefäße ersetzt. Während der Alterungsprozess bei metallischen Druckgefäßen durch Wöhlerkurven hinreichend beschrieben wird, ist der Alterungsmechanismus bei Composite-Druckgefäßen noch nicht vollständig geklärt. Im Rahmen des BAM-interne Themenfeldprojekts COD-AGE werden mit diversen Verfahren alterungsbegleitende, zerstörungsfreie Prüfungen an Composite-Druckgefäßen durchgeführt. Im ersten Teil dieses Vortrages werden Ergebnisse der konventionellen und hochfrequenten Wirbelstromprüfung vorgestellt.
Der zweite Teil des Vortrages beschäftigt sich mit der Prüfbarkeit von Kunststoffen aus Kunstharz und 3D-Druck mit dem Wirbelstromverfahren durch Zugabe ferromagnetischer Nanopartikel bzw. Verwendung von ferromagnetischem Filament.
In this paper, a comparative study on the initial shear strength of
masonry with earth mortars is presented. Triplet tests were carried out to characterise the shear bond strength of five different types of earth mortar, three purely mineral and two with vegetable additives (wood and straw chaff), using calcium silicate blocks. In spite of their lower bulk densities, mortars with chaffs reached a value of compressive strength comparable to the values shown by the purely mineral mortars. The characteristic initial shear strengths of all the tested earth mortars were between two and five times higher than the minimum values for initial shear strengths required by standards.
To assess the influence of blocks pre-wetting, a comparison between calcium silicate blocks and earth blocks was performed to evaluate the results obtained from the standard test procedure compared to the more common practice of using earth mortars in combination with earthen blocks.