Optimization of a radioanalytical procedure for the determination of uranium isotopes in environmental samples

A radiochemical procedure is described for the fast and sensitive measurement of uranium isotopes in gaseous and liquid effluents of nuclear facilities. Equally, this procedure is suitable to measure uranium isotopes in all kinds of environmental samples. Uranium is leached from ashed sample materials with HNO₃, HF, and Al(NO₃)₃ solution and separated from matrix elements by extraction with trioctylphosphinic oxide and backextraction with NH₄F. After radiochemical cleaning by coprecipitation with LaF₃ and anion exchange, uranium isotopes are electroplated on stainless steel discs from HCl/oxalate solution. The preparation is measured by alpha-spectrometry using surface barrier detectors. The detection limit for 1000 minutes of counting time is 2 mBq per sample and nuclide, the chemical yield is in the range of 50 to 80%.     

Determination of diphenhydramine in biological fluids by capillary gas chromatography using nitrogen-phosphorus detection. Application to placental transfer studies in pregnant sheep

A nitrogen-phosphorus detection-gas chromatographic method, which provides improved sensitivity and selectivity for diphenhydramine, is reported. A 25 m X 0.31 mm cross-linked, 5% phenylmethyl silicone-coated fused-silica capillary column (film thickness 0.52 micron) was used for all analyses. The splitless capillary injection mode was employed with a 2-microliter sample being introduced by an automatic liquid sampler. Standard curves, using orphenadrine as an internal standard, were linear in the range 2-320 ng of diphenhydramine per 0.5 ml of sheep plasma. This represents an amount of diphenhydramine from ca. 40 pg to 6.4 ng at the detector. Chromatographic separation of diphenhydramine and orphenadrine was excellent, with no interference from endogenous plasma constituents. Applicability of the method was demonstrated by a placental transfer study in a chronically instrumented pregnant sheep following a 100 mg intravenous injection of diphenhydramine to the ewe.     

Uncommon ferromagnetic interactions in a homometallic Co(II) chain bridged by a single end-to-end azide

A new one-dimensional heterochiral coordination polymer [Co(bmdt)(N3)2].MeCN (1.MeCN) with well-isolated chains was prepared via a self-assembly process. Magnetic data show that intrachain ferromagnetic couplings via the single end-to-end azide group are observed, which is an extraordinary case among the azide-bridged Co(II) systems.     

Self-assembled discotic nematic liquid crystals formed by simple hydrogen bonding between phenol and pyridine moieties

New discotic nematic liquid crystals have been prepared through intermolecular hydrogen bonding between the core of 1,3,5-trihydroxybenzene (phloroglucinol, PG) or 1,3,5-tris(4-hydroxyphenyl)benzene (THPB) and the peripheral molecules of stilbazole derivatives. The various nematic phases formed by new hydrogen bonding building blocks were investigated by differential scanning calorimetry, polarising optical microscopy and X-ray diffraction. The first discotic complexes of PG and trans-4-alkoxy-4′-stilbazoles exhibited nematic columnar (N_C) and hexagonal columnar phases depending on the length of alkyl chains, which were considered as the basic discotic structure. Several structural variations on the building blocks were attempted to examine their effects on the liquid crystalline properties of discotic complexes. The nematic lateral phase (N_L) with enhanced intercolumnar order was observed for the complexes of PG and trans-4-cyanoalkoxy-4′ stilbazoles due probably to the strong dipole interactions between cyano groups at the end of alkoxy chains. By introducing the nonlinear structure in three arms of supramolecular discotic mesogen, a discotic nematic phase (N_D) was observed for the complex of THPB and trans-4-octyloxy-4 -stilbazole. The single hydrogen bonding between phenol and pyridine moieties in this study provides a simple and effective method for preparing the rarely found discotic nematic liquid crystals.     

Selective Hydrogenation of CO2 to Ethanol over Cobalt Catalysts

Methods for the hydrogenation of CO₂ into valuable chemicals are in great demand but their development is still challenging. Herein, we report the selective hydrogenation of CO₂ into ethanol over non‐noble cobalt catalysts (CoAlO_x), presenting a significant advance for the conversion of CO₂ into ethanol as the major product. By adjusting the composition of the catalysts through the use of different prereduction temperatures, the efficiency of CO₂ to ethanol hydrogenation was optimized; the catalyst reduced at 600 ° gave an ethanol selectivity of 92.1 % at 140 °C with an ethanol time yield of 0.444 mmol g^?1 h^?1. Operando FT‐IR spectroscopy revealed that the high ethanol selectivity over the CoAlO_x catalyst might be due to the formation of acetate from formate by insertion of *CH_x, a key intermediate in the production of ethanol by CO₂ hydrogenation.     

Expression patterns of antioxidant proteins in brains of patients with sporadic Creutzfeldt-Jacob disease

Using two-dimensional gel electrophoresis (2-DE) and Western blot analysis, we were able to identify and quantify six antioxidant proteins, peroxiredoxin (Prx) I, Prx II, Prx III, 1-Cys Prx, putative peroxisomal antioxidant enzyme (PLP), and mitochondrial Mn superoxide dismutase (Mn-SOD) in two individual brain regions, cerebellum and frontal cortex of patients with sporadic Creutzfeldt-Jacob (sCJD). Among six antioxidant proteins, 1-Cys Prx showed significant increase (P > 0.05) in sCJD frontal cortex whereas Prx I was decreased (P > 0.01). In cerebellum, levels of all antioxidant proteins studied were comparable to those of controls. Our findings provide evidence for the link between aberrant expression of antioxidant proteins, 1-Cys Prx and Prx I and CJD neuropathogenesis and we discuss the neuropathological meaning of these dysregulated antioxidant proteins in sCJD brain.     

Spirometallodendrimers: terpyridine-based intramacromolecular cyclization upon complexation

The first examples of metallodendritic spiranes have been obtained via incorporation of single terpyridine units within each dendritic quadrant.     

The free surface on a liquid between cylinders rotating at different speeds. Part III

Summary This paper is a further contribution to our work on the Weissenberg effect. One goal of our work is to show how the free-surface deformations on a viscoelastic fluid which is sheared between two concentric rotating cylinders can be used to determine rheological data about the fluid. In this paper we report the results of an experimental program in which free surface shapes have been measured on three viscoelastic fluids undergoing shearing in an apparatus consisting of a stationary outer cylinder and four interchangeable rotating inner cylinders. Experimentally-measured profiles are compared with profiles predicted from second-order theory, and found to be in excellent agreement for STP and TLA-227 in the range of applicability of the second-order theory, but there is some disagreement in the results for a 2% solution of polyacrylamide in 49% water –49% glycerin.

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Zusammenfassung Diese Arbeit stellt einen weiteren Beitrag zu unseren Untersuchungen über den Weissenberg-Effekt dar. Ein Ziel dieser Untersuchungen ist es zu zeigen, wie die Deformation der freien Oberfläche einer zwischen zwei konzentrischen Zylindern gescherten viskoelastischen Flüssigkeit dazu verwendet werden kann, rheologische Kenngrößen der Flüssigkeit zu gewinnen. In dieser Arbeit wird über die Ergebnisse einer experimentellen Untersuchung berichtet, in der die Gestalt der freien Oberfläche bei drei viskoelastischen Flüssigkeiten gemessen wurde, die in einem Apparat geschert wurden, der aus einem stationären Außenzylinder und vier auswechselbaren rotierenden Innenzylindern bestand. Die experimentell bestimmten Profile werden mit solchen verglichen, die aufgrund einer Theorie zweiter Ordnung vorausgesagt worden sind. Man findet im Bereich der Anwendbarkeit dieser Theorie für STP und TLA-227 eine ausgezeichnete Übereinstimmung, wohingegen die Ergebnisse bei einer 2%igen Polyacrylamid-Lösung in einer 1:1-Wasser-Glycerin-Mischung gewisse Diskrepanzen aufweisen.

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With 12 figures and 1 table     

Nanomanipulator-assisted fabrication and characterization of carbon nanotubes inside scanning electron microscope

We have installed two nanomanipulators, which can travel about 20mm with a minimum increment of 1 nm, for manipulation of nanostructured materials inside field-emission scanning electron microscope (FE-SEM). Both manipulators render motions in x, y, and z directions, providing various manipulation freedoms such as moving, bending, cutting, and biasing. In addition, we have conducted in situ characterization of the electrical breakdown of multi-walled carbon nanotubes (MWCNTs). Our results demonstrate the possibility that MWCNTs can be used as a gas sensor.