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A novel core–shell species for the adsorption-based separation of carbon dioxide (CO2) from methane (CH4) is introduced by hydrothermal synthesis of Ni-MOF-74 on mesoporous spherical Al2O3 carrier substrate. The material was characterized and the shell thickness determined by means of optical and scanning electron microscopy as well as volumetric adsorption and fluid displacement experiments. Kinetic experiments with Ni-MOF-74@Al2O3 core–shell composites carried out at 303.15 K and at pressures up to 10 bar expose remarkably dominating uptake rates for CO2 over CH4. In the contrary Ni-MOF-74@Al2O3 appears to be unselective according to equilibrium data at the same conditions. Dynamic breakthrough experiments of binary CH4/CO2-mixtures (at 303.15 K and 5 bar) prove the prevailing effect of adsorption kinetics and the storage function of the mesoporous core. This statement is supported by a considerable boost in CO2-selectivity and capacity compared to adsorption equilibria measured on pure Ni-MOF-74 by the factor of 55.02 and up to 2.42, respectively.
Erstmalig wurde Synchrotron-basierte nukleare inelastische Streuung (NIS) unter Nutzung des Mößbauer-Isotops 161Dy für die Untersuchung der vibronischen Eigenschaften eines DyIII-basierten Einzelmolekülmagneten, [Dy(Cy3PO)2(H2O)5]Br3⋅2 (Cy3PO)⋅2 H2O⋅2 EtOH, eingesetzt. Die experimentelle partielle Phononen-Zustandsdichte, die alle Schwingungen mit einer Auslenkung des DyIII-Ions enthält, wurde mit Hilfe von auf Dichtefunktionaltheorie (DFT) basierenden Simulationen reproduziert, was die Zuordnung aller intramolekularen Schwingungsmoden des Moleküls ermöglicht. Diese Studie zeigt, dass 161Dy-NIS als eine experimentelle Methode ein hohes Potential besitzt, um zur Klärung der Rolle von Phononen in Einzelmolekülmagneten beizutragen.
VIPP proteins aid thylakoid biogenesis and membrane maintenance in cyanobacteria, algae, and plants. Some members of the Chlorophyceae contain two VIPP paralogs termed VIPP1 and VIPP2, which originate from an early gene duplication event during the evolution of green algae. VIPP2 is barely expressed under nonstress conditions but accumulates in cells exposed to high light intensities or H2O2, during recovery from heat stress, and in mutants with defective integration (alb3.1) or translocation (secA) of thylakoid membrane proteins. Recombinant VIPP2 forms rod-like structures in vitro and shows a strong affinity for phosphatidylinositol phosphate. Under stress conditions, >70% of VIPP2 is present in membrane fractions and localizes to chloroplast membranes. A vipp2 knock-out mutant displays no growth phenotypes and no defects in the biogenesis or repair of photosystem II. However, after exposure to high light intensities, the vipp2 mutant accumulates less HSP22E/F and more LHCSR3 protein and transcript. This suggests that VIPP2 modulates a retrograde signal for the expression of nuclear genes HSP22E/F and LHCSR3. Immunoprecipitation of VIPP2 from solubilized cells and membrane-enriched fractions revealed major interactions with VIPP1 and minor interactions with HSP22E/F. Our data support a distinct role of VIPP2 in sensing and coping with chloroplast membrane stress.
The Griffith-Ley oxidation of alcohols to aldehydes and ketones is performed with either RuCl3 ⋅ (H2O)x or a highly stable, well-defined ruthenium catalyst and with cheap trimethylamine N-oxide (TMAO) as the oxygen source. The use of n-heptane as the solvent, which forms a second phase with TMAO and a part of the alcohol, allows the reactions to be performed with a minimum amount of catalyst. This results in high local concentrations and thus to very rapid conversions. Detailed quantum chemical calculations suggest, that the Griffith-Ley oxidation not necessarily requires high oxidation states of ruthenium but can also proceed with RuII/RuIV species.
Sulfinate salts have attracted considerable attentions due to their versatile reactivity. They have emerged as highly useful building blocks for the construction of all kinds of sulfonyl-group containing molecules, such as sulfones or sulfonamides, and for the construction of various carbon–carbon- and carbon–heteroatom-bonds via sulfur dioxide (SO2) extrusion. Herein, we want to summarize the latest developments in the synthesis of sulfinate salts. Both improvement of classical methods and the development of various novel protocols will be discussed. Also selected one-pot methods directly utilizing in situ generated sulfinate salts as intermediates will be covered in this review article.
Herein, experimental demonstration of the parallel parametric generation of spin waves in a microscaled yttrium iron garnet waveguide with nanoscale thickness is presented. Using Brillouin light scattering microscopy, the parametric excitation of the first and second waveguide modes by a stripline microwave pumping source is observed. Micromagnetic simulations reveal the wave vector of the parametrically generated spin waves. Based on analytical calculations, which are in excellent agreement with experiments and simulations, it is proved that the spin-wave radiation losses are the determinative term of the parametric instability threshold in this miniaturized system. The used method enables the direct excitation and amplification of nanometer spin waves dominated by exchange interactions. The presented results pave the way for integrated magnonics based on insulating nanomagnets.
A palladium-catalyzed three-component synthesis of α-arylglycines from benzoic acids, sulfonamides and glyoxylic acid is reported. This novel reaction offers straightforward access to the important arylglycine motif in good yields and high structural diversity. By replacing boronic with carboxylic acids as nucleophilic component, this method can be considered as a more sustainable version of the classical Petasis reaction for synthesis of arylglycines.
Enantiomerically pure, C2-symmetric 2,6-bis(pyrazol-3-yl) pyridine ligands were obtained by treatment of diethyl-2,6-pyridinedicarbonate with (1R,4R)-(+)-camphor in the presence of NaH followed by ring closure with hydrazine. After twofold N-alkylation at the pyrazole rings, the addition of iron(II) chloride led to the according pentacoordinate dichloridoiron(II) complexes. All intermediates of the ligand synthesis, the ligands bearing NCH3 and NCH2C6H5 groups and the derived iron(II) complexes were structurally characterized by means of X-ray structure analysis. In-situ reaction with iron(II) carboxylates resulted in the formation of iron(II) carboxylate complexes, which turned out to be highly active in the hydrosilylation of acetophenone. However, even at room temperature, the enantiomeric excess of the product 1-phenylethanol is poor. 57Fe Mössbauer spectroscopy gave an insight into the species formed during catalysis.
This DFG-funded research project aimed to gain a better understanding of the mechanisms of the W-Cl repair principle within the framework of fundamental investigations, to contribute to the creation of the necessary basis for a broader application of the repair principle in practice. The focus was on the development of a model to describe the chloride redistribution after the application of a system sealing surface protective coating. On the basis of Fick's second law of diffusion, a mathematical model with a self-contained analytical solution was developed, with the help of which the chloride redistribution after application of a system sealing surface protective coating can be calculated under the idealized assumption of complete water saturation of the concrete. Furthermore, the influence of the dehydration of the concrete, expected as a result of the application of the repair principle W-Cl, on the chloride redistribution was investigated. On the basis of laboratory tests and numerical simulations, material-specific reduction functions were developed to quantify the relationship between the chloride diffusion coefficient and the ambient humidity.
The fundamental differences in hydrodynamics of the froth and spray regime account for the ongoing interest in search for the point of phase inversion. This short communication presents a new approach for identification of phase inversion on sieve trays in terms of an image-based measurement technique. Image analysis of entrained droplets reveals a distinct increase in Sauter mean diameter and droplet frequency during phase inversion. Further measurement methods like pressure drop, gravimetric analysis of entrained liquid, froth height assessment and photographic observation of the flow regime serve as a reference value and complement the discussion. A flow map based on the experimental data comprises each regime and shows a good agreement with phase inversion correlations from literature.
Algorithmic decision-making (ADM) systems have come to support, pre-empt or substitute for human decisions in manifold areas, with potentially significant impacts on individuals' lives. Achieving transparency and accountability has been formulated as a general goal regarding the use of these systems. However, concrete applications differ widely in the degree of risk and the accountability problems they entail for data subjects. The present paper addresses this variation and presents a framework that differentiates regulatory requirements for a range of ADM system uses. It draws on agency theory to conceptualize accountability challenges from the point of view of data subjects with the purpose to systematize instruments for safeguarding algorithmic accountability. The paper furthermore shows how such instruments can be matched to applications of ADM based on a risk matrix. The resulting comprehensive framework can guide the evaluation of ADM systems and the choice of suitable regulatory provisions.
We describe a novel technique for the simultaneous visualization of multiple scalar fields, e.g. representing the members of an ensemble, based on their contour trees. Using tree alignments, a graph-theoretic concept similar to edit distance mappings, we identify commonalities across multiple contour trees and leverage these to obtain a layout that can represent all trees simultaneously in an easy-to-interpret, minimally-cluttered manner. We describe a heuristic algorithm to compute tree alignments for a given similarity metric, and give an algorithm to compute a joint layout of the resulting aligned contour trees. We apply our approach to the visualization of scalar field ensembles, discuss basic visualization and interaction possibilities, and demonstrate results on several analytic and real-world examples.
Synchrotron-based nuclear resonance vibrational spectroscopy (NRVS) using the Mössbauer isotope 161Dy has been employed for the first time to study the vibrational properties of a single-molecule magnet (SMM) incorporating DyIII, namely [Dy(Cy3PO)2(H2O)5]Br3⋅2 (Cy3PO)⋅2 H2O ⋅2 EtOH. The experimental partial phonon density of states (pDOS), which includes all vibrational modes involving a displacement of the DyIII ion, was reproduced by means of simulations using density functional theory (DFT), enabling the assignment of all intramolecular vibrational modes. This study proves that 161Dy NRVS is a powerful experimental tool with significant potential to help to clarify the role of phonons in SMMs.
This article proposes a new clock-dependent gain-scheduled dynamic output feedback controller for delayed linear parameter varying systems with piecewise constant parameters. The proposed controller guarantees ℒ2-performance. By employing a clock-dependent Lyapunov–Krasovskii functional, a sufficient condition for the existence of the controller is provided in terms of clock- and parameter-dependent linear matrix inequalities. A case study on output feedback control of delayed switched systems is also provided. To illustrate the efficacy of the result, it is applied to a practical VTOL helicopter model.
The digitization of extraction columns requires a profound knowledge of the present hydrodynamics/mass transport interaction as well as appropriate measurement techniques for the detection of relevant input and target values. In this article, the different techniques for droplet size distribution as well as concentration determination are presented and new methods for online evaluation are discussed. In combination with the simulation of droplet size, holdup and solute concentration distribution, an online-capable process tool for controlling and optimizing extraction columns will be obtained.
Microcrystalline cellulose pellets for oral drug delivery are often produced by a combined wet extrusion-spheronization process. During the entire process, the cylindrical as well as the spherical pellets are exposed to various stresses resulting in a change of their shape and size due to plastic deformation and breakage. In this work, the effect of moisture content of pellets on their mechanical behavior is studied. In static compression tests, the strong influence of water content on deformation behavior of pellets is confirmed. Moreover, impact tests are performed using a setup consisting of three high-speed cameras to record pellet-wall collisions. Material properties, such as stiffness, restitution coefficient, breakage force, and displacement, were analyzed depending on the water content.
A highly water-dispersible heterogeneous Brønsted acid surfactant was prepared by synthesis of a bi-functional anisotropic Janus-type material. The catalyst comprises ionic functionalities on one side and propyl-SO3H groups on the other. The novel material was investigated as a green substitute of a homogeneous acidic phase transfer catalyst (PTC). The activity of the catalyst was investigated for the aqueous-phase oxidation of cyclohexene to adipic acid with 30 % hydrogen peroxide even in a decagram-scale. It can also be used for the synthesis of some other carboxylic acid derivatives as well as diethyl phthalate.
Machining is very common in industry, e.g. automotive industry and aerospace industry, which is a nonlinear dynamic problem including large deformations, large strain, large strain rates and high temperatures, that implies some difficulties for numerical methods such as Finite element method. One way to simulate such kind of problems is the Particle Finite Element Method (PFEM) which combines the advantages of continuum mechanics and discrete modeling techniques. In this work we introduce an improved PFEM called the Adaptive Particle Finite Element Method (A-PFEM). The A-PFEM introduces particles and removes wrong elements along the numerical simulation to improve accuracy, precision, decrease computing time and resolve the phenomena that take place in machining in multiple scales. At the end of this paper, some examples are present to show the performance of the A-PFEM.
One technique to describe the failure of mechanical structures is a phase field model for fracture. Phase field models for fracture consider an independent scalar field variable in addition to the mechanical displacement [1]. The phase field ansatz approximates crack surfaces as a continuous transition zone in which the phase field variable varies from a value that indicates intact material to another value that represents cracks. For a good approximation of cracks, these transition zones are required to be narrow, which leads to steep gradients in the fracture field. As a consequence, the required mesh density in a finite element simulation and thus the computational effort increases. In order to circumvent this efficiency problem, exponential shape functions were introduced in the discretization of the phase field variable, see [2]. Compared to the bilinear shape functions these special shape functions allow for a better approximation of the steep transition with less elements. Unfortunately, the exponential shape functions are not symmetric, which requires a certain orientation of elements relative to the crack surfaces. This adaptation is not uniquely determined and needs to be set up in the correct way in order to improve the approximation of smooth cracks. The issue is solved in this work by reorientating the exponential shape functions according to the nodal value of phase field gradient in a particular element. To be precise, this work discusses an adaptive algorithm that implements such a reorientation for 2d and 3d situations.
In grinding, the crystal grain size of the workpiece material is relatively same range compared to the removal depth. This raises a question if an anisotropic material model, which considers the effect of the crystal grain size and orientations, would better predict the process forces when compared to an isotropic material model. Initially, a simple micro-indentation process is chosen to compare the two models. In this work, a crystal plasticity model and an isotropic Johnson-Cooke plasticity model are employed to simulate micro-identation of a twinning induced plasticity (TWIP) steel. The results of the two models are compared using the force-displacement curves from the micro-indentation experiments. In the future, the study will be extended to describe the material removal process during a single grit scratch test.