On the kinetics of AlH3 decomposition and the subsequent Al oxidation

Metal hydrides are used for hydrogen storage. AlH₃ shows a capacity to store about 10 wt% hydrogen. Its hydrogen is split-off in the temperature interval of 400–500 K. On dehydrogenation a nano-structured Al material emerges with specific surfaces up to 15–20 m²/g. The surface areas depend on the heating rate because of a temperature dependent crystallite growth. The resulting Al oxidizes up to 20–25% weight on air access forming an alumina passivation layer of 3–4 nm thickness on all exposed surfaces. The heat released from this Al oxidation induces a high risk to this type of hydrogen storage if the containment might be destroyed, accidentally. The kinetics of the dehydrogenation and the subsequent oxidation is investigated by methods of thermal analysis. A reaction scheme is confirmed which consists of a starting Avrami-Erofeev mechanism followed by formal 1st order oxidation on unlimited air access. The kinetic parameters, activation energies and pre-exponentials are evaluated and can be used to calculate the reaction progress. Together with the heat of the Al oxidation the overall heat release and the related rate can be estimated.     

Reactor Concept for Contactless Kinetic Measurement in Oscillating Droplets via Raman Spectroscopy

A millistructured reactor and spectroscopic setup for contactless kinetic measurements in oscillating droplets is presented in this work. The polymerization of acrylic acid serves as a model reaction. Design and construction of the reactor focus on the optical access for Raman measurement, the nearly isothermal behavior, and the preservation of droplets during long‐term reactions with a high increase of viscosity. Another key aspect is the possibility of full automation at a later stage.     

In-house and interlaboratory validation of a method for the extraction of DNA from maize starch

Here, we describe the procedure of a DNA extraction method from maize starch including the method??s validation by in-house and interlaboratory tests. The amplifiable amount of maize DNA tested by real-time PCR was used as parameter for evaluating our method. The practical (i.e. relative) limit of detection (LOD) was used as key criterion for assessing the suitability of the extraction method with respect to genetically modified organism analysis. In a round-robin test with ten participating laboratories, satisfactory results were achieved with practical LODs in the range of 0.1?% with three native maize starch materials. In-house tests showed that this protocol??with an additional purification step??can also be applied for extracting DNA from chemically or enzymatically modified starch.     

Arduino-based slider setup for gas–liquid mass transfer investigations: Experiments and CFD simulations

The implementation of traditional sensors is a drawback when investigating mass transfer phenomena within microstructured devices, since they disturb the flow and reactor characteristics. An Arduino based slider setup is developed, which is equipped with a computer-vision system to track gas–liquid slug flow. This setup is combined with an optical analytical method allowing to compare experimental results against CFD simulations and investigate the entire lifetime of a single liquid slug with high spatial and temporal resolution. Volumetric mass transfer coefficients are measured and compared with data from literature and the mass transfer contribution of the liquid film is discussed.     

Residual tumor after laser ablation of human non-small-cell lung cancer demonstrated by ex vivo staining: correlation with invasive temperature measurements

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Histology is the gold standard for confirming thermally induced necrosis. Generally, however, no specimen is obtained from thermal ablation therapy for pathological examination. The aim of this study was to provide evidence for the relationship between temperatures reached and resulting tissue coagulation during laser ablation in a near-physiological ex vivo lung tumor model by combining viability staining and direct temperature measurement.     

Methacrylated calix[4]arene phosphonic acids as functionalized crosslinker for radical polymerization

We describe the synthesis of 5,11,17,23‐tetra‐tert‐butyl‐25,27‐dioxypropylphosphonic acid‐26,28‐dimethacryloyloxy‐calix [4]arene and 5,11,17,23‐tetra‐tert‐butyl‐25‐oxypropylphosphonic acid‐27‐hydroxy‐26,28‐dimethacryloyloxy‐calix[4]arene starting from para‐tert‐butyl‐calix[4]arene. The complete reaction was proved by matrix‐assisted laser desorption ionization time of flight mass spectrometry and nuclear magnetic resonance spectroscopy. The influence of these compounds on the kinetics of the radical polymerization of methyl methacrylate was shown by dilatometry. Furthermore, the adhesive properties of dental adhesives containing these calix[4]arene derivatives were investigated. Copyright © 2012 Society of Chemical Industry     

Dynamic mechanical behavior and nanostructure morphology of hyperbranched‐modified polypropylene blends

Polypropylene (PP) was modified utilizing two types of polyesteramide‐based hyperbranched polymers (amphiphilic PS and hydrophilic PH). A maleicanhydride‐modified PP (PM) was used as a reactive dispersing agent to enhance the modification by grafting the hyperbranched polymers onto the PP chains. Pure PP, two different non‐reactively modified samples, i.e. excluding PM, and two different reactively modified samples, i.e. including PM, were studied. Investigating the morphology of the samples was performed by scanning electron microscopy. To follow the effect of the modification on the dynamic mechanical properties, dynamic mechanical analysis experiments both in the melt (rheometric mechanical spectrometry) and in solid state (dynamic mechanical thermal analysis) were carried out. In the next step, the nanocrystalline structure of the samples was studied by small angle X‐ray scattering (SAXS) in two different modes, i.e. static and recrystallization. Hundreds of SAXS patterns were analyzed automatically using procedures written in PV‐WAVE image‐processing software. The chord distribution function (CDF) was calculated and the long period (l_p) of the crystal lamellae was extracted from the CDFs. The rheometric mechanical spectrometry results show that both hyperbranched polymers decrease complex viscosity η^* and enhance liquid‐like behavior. This happens more significantly when PM is included. The dynamic mechanical thermal analysis results reveal that T_g decreases when PS and PH are added. In the reactively modified samples this reduction is compensated most probably because of the crosslinked structure formed through the grafting reaction between the hyperbranched polymers and PM. Such structure is confirmed by SAXS data and calculated CDFs in the recrystallization mode. Static SAXS data also show enhancement in the crosshatched morphology of the crystalline lamellae of PP for reactively modified samples compared with non‐reactively modified samples. © 2013 Society of Chemical Industry     

Modification of poly(propylene) by grafted polyester‐amide‐based dendritic nanostructures with the aim of improving its dyeability

Fiber‐graded poly(propylene) was modified by polyester‐amide‐based dendritic nanostructures with the aim of improving its dyeability. Two different dendritic polymers were used and the dendritic nanostructures were formed in situ via reactive blending with maleic anhydride‐modified poly(propylene). Samples were chosen exploiting a 4‐component mixture design. Thermal, morphological, and rheological characterizations showed domains with different size and distribution were formed and primary properties of the dendritics determined the characteristics of the resulted domains. Morphological parameters were quantified by digital analysis of scanning electron microscope images. Thermal and rheological behavior also demonstrated good agreements with the inferred morphology of the formed dendritic domains. The modified samples were then dyed with dispersed dyestuffs. A variety of substantivities were obtained, and some of the modified samples showed a significant enhancement in dyeing properties. A predictive model was developed for K/S ratio, where K and S are absorption and scattering coefficients of the Kubelka‐Munk one constant theory, respectively. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Micro- and nanostructured Al2O3 surfaces for controlled vascular endothelial and smooth muscle cell adhesion and proliferation

The effect of the micro- and nanotopography on vascular cell-surface interaction is investigated using nano- and microstructured Al₂O₃ as model substrate. Two different nanostructured Al₂O₃ surfaces composed of low density (LD) and high density (HD) nanowires (NWs) were synthesized by chemical vapour deposition (CVD) and commercially available microstructured Al₂O₃ plates were used for comparison. A clear diverging response of human umbilical vein endothelial cells (HUVEC) and human umbilical vein smooth muscle cells (HUVSMC) was observed on these nano- and microstructured surfaces. LD Al₂O₃ NWs seem to enhance the proliferation of HUVECs selectively. This selective control of the cell-surface interaction by topography may represent a key issue for the future stent material design.