Synthesis and acid digestion of biomorphic ceramics: determination of alkaline and alkaline earth ions

Ceramic and glass are some of the more recent engineering materials and those that are most resistant to environmental conditions. They belong to advanced materials in that they are being developed for the aerospace and electronics industries. In the last decade, a new class of ceramic materials has been the focus of particular attention. The materials were produced with natural, renewable resources (wood or wood-based products). In this work, we have synthesised a new biomorphic ceramic material from oak wood and Si infiltration. After the material characterization, we have optimized the dissolution of the sample by acid attack in an oven under microwave irradiation. Experimental designs were used as a multivariate strategy for the evaluation of the effects of varying several variables at the same time. The optimization was performed in two steps using factorial design for preliminary evaluation and a Draper-Lin design for determination of the critical experimental conditions. Five variables (time, power, volume of HNO3, volume H2SO4 and volume of HF) were considered as factors and as a response the concentration of different metal ions in the optimization process. Interactions between analytical factors and their optimal levels were investigated using a Draper-Lin design.     

Energy landscapes for water clusters in a uniform electric field

The behavior of small water clusters, (H2O)n, n=2-5 and n=8, in a uniform electric field is investigated for three related rigid-body models. Changes in the properties of the low-lying potential energy minima and the rearrangement pathways between them are examined. Results for certain structural transitions are compared with recent ab initio calculations. The models are found to give qualitatively similar trends, and there is some evidence that as the applied field strength is increased the quantitative differences between the models are also reduced.     

Analysis of ochratoxin A in milk after direct immunoaffinity column clean-up by high-performance liquid chromatography with fluorescence detection

The present work describes a new analytical method for direct immunoaffinity column clean-up of ochratoxin A (OTA) in milk samples followed by determination of the toxin using high-performance liquid chromatography with fluorescence detection (HPLC-FD). Two different immunoaffinity cartridges (IAC) were investigated, and Ochraprep columns were chosen because they showed the best results. An average recovery of 89.8% and a mean RSD of 5.8% for artificially contaminated cow's milk in the range of 5-100 ng/L were attained. The calculated limit of detection (LOD) and limit of quantitation (LOQ) were as low as 0.5 and 5 ng/L, respectively. This new easy and fast method avoids a previous liquid-liquid extraction step and therefore the use of toxic chlorinated solvents. Chromatograms of the final extracts were clean and OTA could be easily detected at a retention time of 8.4 min without interferences. To assess the presence of the toxin in cow's milk eight samples of skimmed and four samples of whole milk were analysed and OTA was not detected over the established detection limit.     

Chromium(III) complexes with terdentate 2,6-bis(azolylmethyl)pyridine ligands: Synthesis, structures and ethylene polymerization behavior

Reactions of 2,6-bis(bromomethyl)pyridine with 3,5-dimethylpyrazole and 1H-indazole yield the terdentate ligands 2,6-bis(3,5-dimethylpyrazol-1-ylmethyl)pyridine (5) and 2,6-bis(indazol-2-ylmethyl)pyridine (6). The molecular structure of the new compound 6 was determined by single-crystal X-ray diffraction. These ligands react with the CrCl₃(THF)₃ complex in THF to form neutral complexes of general formula [CrCl₃{2,6-bis(azolylmethyl)pyridine-N,N,N}] (7, 8) which are isolated in high yields as stable green solids and characterized by means of elemental analysis, magnetic moments, IR, and mass spectroscopy. Theoretical calculations predict that the thermodynamically preferred structure of the complexes is the fac configuration. After reaction with methylaluminoxane (MAO) the chromium(III) complexes are active in the polymerization of ethylene.     

Products of Jacobians as Prym-Tyurin varieties

Let X ₁, ..., X _m denote smooth projective curves of genus g _i ≥ 2 over an algebraically closed field of characteristic 0 and let n denote any integer at least equal to . We show that the product JX ₁ × ... × JX _m of the corresponding Jacobian varieties admits the structure of a Prym-Tyurin variety of exponent n ^m-1. This exponent is considerably smaller than the exponent of the structure of a Prym-Tyurin variety known to exist for an arbitrary principally polarized abelian variety. Moreover it is given by explicit correspondences.      

Controlled release from a nanocarrier entrapped within a microcarrier

This study illustrates the entrapment of the dye molecule fluorescein sodium salt (FSS) by hydrogel nanoparticles, which are in turn confined inside a water-in-oil-in-water double-emulsion globule, and its subsequent release by the action of the competing agent hydrochloric acid (HCl). Thus, a "double carrier" concept is being introduced in which a nanoscale delivery vehicle is being transported by a microscale delivery vehicle in order to simultaneously take advantage of both systems. This may facilitate storage and handling while protecting the active substance and improving its action upon application.     

Meso-scale modelling of the size effect on the fracture process zone of concrete

The size effect on the fracture process zone in notched and unnotched three point bending tests of concrete beams is analysed by a meso-scale approach. Concrete is modelled at the meso-scale as stiff aggregates embedded in a soft matrix separated by weak interfaces. The mechanical response of the three phases is modelled by a discrete lattice approach. The model parameters were chosen so that the global model response in the form of load-crack mouth opening displacement curves were in agreement with experimental results reported in the literature. The fracture process zone of concrete is determined numerically by evaluating the average of spatial distribution of dissipated energy densities of random meso-scale analyses. The influence of size and boundary conditions on the fracture process zone in concrete is investigated by comparing the results for beams of different sizes and boundary conditions.