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Paper des Monats
- ja (26)
High-Amplitude Surge of a Pitching Airfoil: Complementary Wind- and Water-Tunnel Measurements
(2018)
RECENT interest in gust response, rotorcraft forward flight and wind energy, among other applications, has focused on streamwise oscillations of nominally two-dimensional airfoils in attached and separated flows. The airfoil may be simultaneously held at constant incidence or execute some maneuver, such as pitch.
The relative freestream is spatially uniform but temporally unsteady, and this can be accomplished in a ground-test facility in two ways. The first method is to vary the output of the prime mover, such as the rotational speed of the impeller or the blower driving a wind tunnel, or (alternatively) to vary the pressure drop in the tunnel, thereby varying the flow speed in the test section, despite nominally constant primemover revolutions per minute. The second method is used to keep the tunnel’s operating speed constant, as well as to move the test article in the streamwise direction, fore and aft (for example, via an electric linear motor), such that the relative freestream speed felt by the test article varies according to some waveform. Typically, the latter approach is chosen in water tunnels, where there is too much tunnel-circuit inertia to vary the flow speed directly but where the usually low tunnel test section flow speeds enable large excursions in the relative freestream by oscillation of the test article. In fact, outright reverse flow is possible by moving the test article in the laboratory frame at a higher speed than the water-tunnel flow speed. In either case, a sinusoidal relative-speed waveform is the most intuitively realizable, and this can be combined with similar oscillations in the airfoil incidence angle or other kinematics. Although the two methods of realizing streamwise oscillations are mechanically distinct, experimental comparisons between an oscillating test article in a water tunnel and a stationary test article in a wind tunnel with a louvermechanismhave demonstrated agreement in themeasured lift and drag histories. Such experimentswere performed by Granlund et al. for a 10% freestream amplitude oscillation and fixed airfoil incidence, comparing a free-surface water tunnel and a closed-circuit wind tunnel. After buoyancy was subtracted from the wind-tunnel data (resulting from the louver pressure drop) and the model inertia subtracted from the water-tunnel data (resulting from acceleration of the test article), the remaining lift and drag histories matched well at the low freestream oscillation amplitude regime. The work of Granlund et al. was later extended to high-advance-ratio streamwise oscillations of 50% amplitude by Greenblatt et al., where the aerodynamic histories of the water-tunnel and wind-tunnel facilities were compared in combined pitch and freestreamoscillations (governed by relative pitch phase), pure pitch oscillations, and purely freestream oscillations. Agreement between the two facilities’ data for fixed-incidence streamwise oscillations was reasonably good, and in fact, better than agreement in just the static lift and drag, evidently owing to differences in blockage and model-support systems. Additionally, Greenblatt et al. determined there was no strong coupling between simultaneous freestream oscillations and pitch oscillations on resultant lift and moment coefficients.
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.
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.
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.
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.
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 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.
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.
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.
The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon
carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been revealed as a convenient technique for trace elemental imaging in tissue sections, providing elemental 2D distribution at a quantitative level. For quantification purposes, in the last years several approaches have been proposed in the literature such as the use of CRMs or matrix matched standards. The use of Isotope Dilution (ID) for quantification by LA-ICP-MS has been also described, being mainly useful for bulk analysis but not feasible for spatial measurements so far. In this work, a quantification method based on ID analysis was developed by printing isotope-enriched inks onto kidney slices from rats treated with antitumoral Pt-based drugs using a commercial ink-jet device, in order to perform an elemental quantification in different areas from bio-images. For the ID experiments ¹⁹⁴Pt enriched platinum was used. The methodology was validated by deposition of natural Pt standard droplets with a known amount of Pt onto the surface of a control tissue, where could be quantified even 50 pg of Pt, with recoveries higher than 90%. The amount of Pt present in the whole kidney slices was quantified for cisplatin, carboplatin and oxaliplatin-treated rats. The results obtained were in accordance with those previously reported. The amount of Pt distributed between the medullar and cortical areas was also quantified, observing different behavior for the three drugs.
Optical elemental analysis in the gas phase typically relies on electrically driven plasmas. As an alternative approach, laser-induced plasmas (LIPs) have been suggested but have so far been only scarcely used.
Here, a novel signal enhancement strategy for laser-based airborne plasma optical Emission spectroscopy for gas phase analytics is presented. In contrast to an electrically driven plasma, in the laser-induced analogue dynamic matter transport equilibrium builds up. The latter results in a rarefied density regime in the plasma core itself, surrounded by an area of compressed matter. The central rarefaction leads to a decrease in plasma intensity and analyte number density, both of which are detrimental for analytical purposes. Since the repetitive ignition of LIPs is a transient process, a restoration of the former gaseous medium by other dynamically equilibrated diffusion processes would be favourable. The presented combination of an airborne LIP and an ultrasonic acoustic resonator yields a fourfold signal enhancement while the Background contribution of ubiquitous air is at the same time effectively suppressed. Since the entire enhancement effect occurs without contact, no additional sources for abrasive sample contamination are introduced.