Elastic and viscoelastic properties of sugarcane bagasse-filled poly(vinyl chloride) composites

Elastic and viscoelastic properties of sugarcane bagasse-filled poly(vinyl chloride) were determined by means of three-point bending flexural tests and dynamic mechanical and thermal analysis. The elastic modulus, storage modulus, loss modulus, and damping parameter of the composites at fibre contents of 10, 20, 30, and 40% in mass were determined, as well as those of the unfilled matrix. There was a correlation between the elastic modulus and storage modulus of the composites. Moreover, the elastic and viscoelastic properties of the composites were highly influenced by fibre content.     

Centerband-Only Detection of Exchange NMR with Natural-Abundance Correction Reveals an Expanded Unit Cell in Phenylalanine Crystals

The NMR pulse sequence CODEX (centerband-only detection of exchange) is a widely used method to report on the number of magnetically inequivalent spins that exchange magnetization via spin diffusion. For crystals, this rules out certain symmetries, and the rate of equilibration is sensitive to distances. Here we show that for ¹³C CODEX, consideration of natural abundance spins is necessary for crystals of high complexity, demonstrated here with the amino acid phenylalanine. The NMR data rule out the C₂ space group that was originally reported for phenylalanine, and are only consistent with a larger unit cell containing eight magnetically inequivalent molecules. Such an expanded cell was recently described based on single crystal data. The large unit cell dictates the use of long spin diffusion times of more than 200 seconds, in order to equilibrate over the entire unit cell volume of 1622 ų.     

Effective electrodeposition of Co-Ni-Cu alloys nanoparticles in the presence of alkyl polyglucoside surfactant

The effect of alkyl polyglucoside (APG) surfactant on the electrodeposition Co-Ni-Cu alloys nanoparticles has been investigated. In a typical electrodeposition experiment, it was found that as prepared Co-Ni-Cu alloys nanoparticles characteristics, such as size homogeneity, density, dispersion on the electrode substrate and the chemicals composition, depended strongly on the concentration of APG used in the reaction as well as the applied deposition potential. For the case of chemicals composition, low APG concentration (below CMC) was found to be effective for the preparation of excellent composition of the nanoalloys. Meanwhile, for the case of size homogeneity, density, and dispersion on the surface, high APG concentration (above CMC) and high deposition potential were preferred. It was also found that, at concentration above the CMC, the APG surfactant showed a metals ions deposition inhibition characteristic that caused increasing in the electrodeposition overpotential of the entire metals ions, namely cobalt, nickel and copper. As the result the copper was found to place a high percentage in the nanoalloys deposits. Owing to its simple procedure in controlling the composition and the nanoalloys growth characteristic, present approach should find a potential application in preparing Co-Ni-Cu magnetic nanoparticles for used in currently existing applications.     

Simultaneous quantification of curcuminoids and xanthorrhizol in Curcuma xanthorrhiza by high-performance liquid chromatography

A new method for simultaneous quantification of curcuminoids and xanthorrhizol (XNT) in Curcuma xanthorrhiza was developed and validated using high-performance liquid chromatography with diode-array UV–Vis detector. The chromatographic separation was achieved on a Phenomenex C18 at room temperature with the mobile-phase acetonitrile ?0.001% formic acid in gradient elution system and delivered at a flow rate of 1?mL/min. Detection wavelength 425?nm was used for curcuminoids and 224?nm for XNT. System suitability, linearity, precision, accuracy, limit of detection, limit of quantitation, and stability were evaluated and were found in good agreement with Association of Official Analytical Chemists guidelines for single-laboratory validation. The proposed method was found to be precise, accurate, and reliable and also could be applied for the simultaneous quantitative analysis of curcuminoids and XNT in C. xanthorriza raw material and its herbal medicinal product.     

Insight into the extractability of metals from soils using an implementation of the linear adsorption isotherm model

This paper deals with an often overlooked artifact in sequential and single extraction of metals from soils, viz. the volume to mass (V/m) ratio as a potential source for inadequate extraction yields. We offer a theoretical framework to get a grip on this intricate parameter and came up with a model based on a linear adsorption isotherm to derive the correct maximal metal extractability for a certain extractant. We verified the model experimentally using 0.1 mol l⁻¹ nitric acid for extraction of seven metals (Cr, Co, Cu, Cd, Pb, Ni and Zn) from an urban soil sample, and concluded that commonly used V/m ratios in the range of 10-40 ml g⁻¹ may give as much as 50% too low extraction yields. Thus, a strong caveat is in place as to be very critical what V/m ratios to use and preferably apply the model derived to obtain the correct maximal extractability using a variable V/m ratio method.     

Synthesis, characterization, and electrochemical and electrochromic properties of sandwich dilutetium tetraphthalocyanine

A new sandwich-tpype dilutetium tetraphthalocyanine 4 has been synthesized by the reaction of dimeric lutetium(III) phthalocyanine 3 with two equiv. of dilithium octakishexylthiophthalocyanine in amyl alcohol. Compound 3 was prepared from 4',5',4",5"-tetraiminoisoindoline(1,4,7,10-tetrathia-12-crown-4) 1, 4,5-bis(hexylthio)-1,2-diiminoisoindoline and lutetium acetate in amyl alcohol. Compounds 3 and 4 were characterized by elemental analysis, UV/visible, IR, (1)H NMR and ESR spectroscopy. The electrochemical and electrochromic properties of 3 and 4 have been examined by cyclic voltammetry. Both 3 and 4 displayed well-defined electrochromic behavior.     

Reaktionen cyclischer Oxalylverbindungen, 34. Mitt.: Synthese von Dibenzoylacet-N-carboxyalkylamiden und semiempirische Rechnungen zur Keto-Enol Tautomerie

Summary 4-Benzoyl-5-phenylfuran-2,3-dione (1) and the urethanes2 combine under loss of carbon monoxide yielding the open chain dibenzoylacetic acid derivatives3 and4. 3a, b only can be cyclized to the oxazinone5. The keto-enole tautomerism3 4 is further investigated with aid of semiempirical quantum chemical calculations, based upon the molecular geometry of3a, deduced from an X-ray study.

Frau Univ. Prof. Dr. Helga Wittmann mit den besten Wünschen zum 70. Geburtstag gewidmet.     

Processes associated with ionic current rectification at a 2D-titanate nanosheet deposit on a microhole poly(ethylene terephthalate) substrate

Films of titanate nanosheets (approx. 1.8-nm layer thickness and 200-nm size) having a lamellar structure can form electrolyte-filled semi-permeable channels containing tetrabutylammonium cations. By evaporation of a colloidal solution, persistent deposits are readily formed with approx. 10-μm thickness on a 6-μm-thick poly(ethylene-terephthalate) (PET) substrate with a 20-μm diameter microhole. When immersed in aqueous solution, the titanate nanosheets exhibit a p.z.c. of − 37 mV, consistent with the formation of a cation conducting (semi-permeable) deposit. With a sufficiently low ionic strength in the aqueous electrolyte, ionic current rectification is observed (cationic diode behaviour). Currents can be dissected into (i) electrolyte cation transport, (ii) electrolyte anion transport and (iii) water heterolysis causing additional proton transport. For all types of electrolyte cations, a water heterolysis mechanism is observed. For Ca²⁺ and Mg²⁺ions, water heterolysis causes ion current blocking, presumably due to localised hydroxide-induced precipitation processes. Aqueous NBu₄⁺ is shown to ‘invert’ the diode effect (from cationic to anionic diode). Potential for applications in desalination and/or ion sensing are discussed.

     

T-x-y diagram of the Ni-Bi-Se system

Some polythermal sections of the Ni-Bi-Se system have been investigated by DTA, X-ray powder diffraction, microstructural analysis, and microhardness measurements. The liquidus surface has been constructed for this system. The compounds NiBi₂Se₄ and Ni₃Bi₂Se₂ are formed by dystectic reactions and melt at 1088 and 980 K, respectively. The regions of primary and joint phase crystallization have been determined. A commutation of Bi₂Se₃-based thermoelements with a metal nickel bus-bar has been proposed.