Chimie des complexes de metaux de transition avec des hydrocarbures cyanes : III. Quelques observations sur la conformation et la reactivite de complexes dicyclopentadienyles du molybdene et du tungstene

A new class of cyclic telluronium salts has been prepared. All the salts are stable in solution in CHCl₃ or dimethylsulphoxide (DMSO). Conductivity measurements in DMSO and dimethylformamide (DMF) have shown that considerable ion pairing occurs in solution. Infrared, ¹H, ¹³C, ¹²⁵Te NMR, and mass spectra are reported and discussed.     

Activation analysis of alkaline rocks. A comparison between destructive and non-destructive methods

The United States Geological Survey reference sample AGV-1 andesite, and three alkaline rocks from the apatite mine of Jacupiranga, Brasil, were analyzed by thermal neutron activation analysis using destructive and non-destructive methods, and high resolution Ge(Li) gamma-ray detectors. One of the rocks, a carbonatite, was also analyzed by instrumental activation analysis with epithermal neutrons. A greater number of elements can be determined using the radiochemical separation, but the precision and accuracy attained by INAA and RNAA were of the same order for most of the elements analyzed. Epithermal activation was more advantageous for tantalum, terbium and holmium. Comparison of the analytical results for USGS reference sample (AGV-1) with the data published by others gave good agreement. Statistical tests used for comparison of the results of destructive and non-destructive methods, as well as other results are presented.     

Titanosilicates as Supports for an Enzymatic Alcoholysis Reaction

Novel [Cr^III(amp)(bipy)(Cl)] (1) (H₂amp = N-(hydroxyphenyl)salicyldimine; bipy = 2,2-bipyridyl) and [Cr^III(app)(bipy)(Cl)]⁺ (2) (H₂app = N-(hydroxyphenyl)pyridine-2-carboxaldimine; bipy = 2,2-bipyridyl) complexes have been synthesized and characterized by physico-chemical methods. Complexes 1 and 2 have been employed as catalysts in the oxidation of both saturated and unsaturated hydrocarbons using tert-butylhydroperoxide (t-BuOOH). The significance of the results with respect to oxo-functionalization of C-H bonds both in unsaturated and saturated hydrocarbons is noted.     

Elemental concentration in the cortex and hippocampus of Wistar rats by X-ray total reflection fluorescence with synchrotron radiation

Summary The study of trace element levels is of great importance due to their relevance in agingand several neurodegenerative diseases. This work compares the elemental concentrations in different postnatal ages and between the temporal cortex, entorhinal cortex and hippocampus from Wistar rats, using X-ray total reflection fluorescence with synchrotron radiation. Ten elements were determined in brain samples: Ti, Cr, Mn, Fe, Cu, Zn, (at trace level) and P, S, Cl and K (at major levels). The elements that increased with aging in cortical areas were: S, K, Fe, Cu and Zn. Ca and Zn levels decreased with advancing age in the hippocampus. In addition to this, Ti, Mn and Fe levels were more conspicuous in the entorhinal cortex.     

Synthesis and characterization of MCM-48 tubular membranes

MCM-48 membranes have been prepared on alumina supports of different pore sizes. A battery of characterization techniques has been used to study the physical properties and the quality of the membranes prepared. The highest quality membranes were prepared on supports with pore size of up to 60 nm. The MCM-48 membranes were tested in the separation of gas phase mixtures and a cyclohexane/O₂ selectivity higher than 270 was obtained. The selective separation of organic compounds from inert components is a result of the cooperative effects of capillary condensation in MCM-48 pores and of the specific interactions of the permeating compounds and the membrane material.     

Determination of manganese in ores by activation analysis using a californium-252 neutron source

A²⁵²Cf neutron source has been used to analyse manganese in ores such as pyrolusite, rodonite (manganese silicate) and blends used in dry-batteries. Samples with about 150 mg and standards of manganese dioxide were irradiated for about 20 min and counted using a well-type NaI(Tl) scintillation counter and scaler, with or without pulse-height discriminator between the detector and the scaler. The interferences of nuclear reactions⁵⁶Fe(n,p)⁵⁶Mn and⁵⁹Co(n,α)⁵⁶Mn were studied, as well as problems in connection with neutron shadowing during irradiation, gamma-rays attenuation during counting and influence of granulometry of samples. Some of the samples were also analysed by wet-chemical method (sodium bismuthate) in order to compare results.     

Effect of Bauhinia monandra Kurz Leaf Preparations on Embryonic Stages and Adult Snails of Biomphalaria glabrata (Say, 1818), Schistosoma mansoni Cercariae and Toxicity in Artemia salina

Biomphalaria glabrata snails constitute the main vector of schistosomiasis in Brazil, and Bauhinia monandra Kurz, the leaves of which contain BmoLL lectin with biocidal action, is a plant widely found on continents in which the disease is endemic. This work describes the composition of B. monandra preparations and the effect on embryos and adult snails, their reproduction parameters and hemocytes. We also describe the results of a comet assay after B. glabrata exposure to sublethal concentrations of the preparations. Additionally, the effects of the preparations on S. mansoni cercariae and environmental monitoring with Artemia salina are described. In the chemical evaluation, cinnamic, flavonoid and saponin derivatives were detected in the two preparations assessed, namely the saline extract and the fraction. Both preparations were toxic to embryos in the blastula, gastrula, trochophore, veliger and hippo stages (LC₅₀ of 0.042 and 0.0478; 0.0417 and 0.0419; 0.0897 and 0.1582; 0.3734 and 0.0974; 0.397 and 0.0970 mg/mL, respectively) and to adult snails (LC₅₀ of 6.6 and 0.87 mg/mL, respectively), which were reproductively affected with decreased egg deposition. In blood cell analysis, characteristic cells for apoptosis, micronucleus and binucleation were detected, while for comet analysis, different degrees of nuclear damage were detected. The fraction was able to cause total mortality of the cercariae and did not present environmental toxicity. Therefore, B. monandra preparations are promising in combating schistosomiasis since they can control both the intermediate host and eliminate the infectious agent, besides being safe to the environment.     

Green Extraction Techniques as Advanced Sample Preparation Approaches in Biological,Food, and Environmental Matrices: A Review

Green extraction techniques (GreETs) emerged in the last decade as greener and sustainable alternatives to classical sample preparation procedures aiming to improve the selectivity and sensitivity of analytical methods, simultaneously reducing the deleterious side effects of classical extraction techniques (CETs) for both the operator and the environment. The implementation of improved processes that overcome the main constraints of classical methods in terms of efficiency and ability to minimize or eliminate the use and generation of harmful substances will promote more efficient use of energy and resources in close association with the principles supporting the concept of green chemistry. The current review aims to update the state of the art of some cutting-edge GreETs developed and implemented in recent years focusing on the improvement of the main analytical features, practical aspects, and relevant applications in the biological, food, and environmental fields. Approaches to improve and accelerate the extraction efficiency and to lower solvent consumption, including sorbent-based techniques, such as solid-phase microextraction (SPME) and fabric-phase sorbent extraction (FPSE), and solvent-based techniques (μQuEChERS; micro quick, easy, cheap, effective, rugged, and safe), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), in addition to supercritical fluid extraction (SFE) and pressurized solvent extraction (PSE), are highlighted.     

Production of metakaolin from industrial cellulose waste

Research focused on the transformation and utilization of industrial wastes into products of commercial interest plays an increasingly important role. Residual pulp can become useful in the manufacture of different materials, providing high value to this waste and reducing its environmental impact when disposed of improperly in the environment. The main constituents of this waste are kaolin and calcium carbonate (CaCO₃). Starting from kaolin, metakaolin can be produced by calcination of the residue at 630?°C for 2?h in a rotary reactor with air flow, followed by solubilization with hydrochloric acid to remove the CaCO₃. The development of technological alternatives aimed at the reuse of certain wastes can result in applications of real economic interest to the chemical industry and ceramics and glass, which is the case in this study. The raw material and metakaolin obtained were analyzed by thermogravimetric analysis and derivative thermogravimetric analysis, X-ray diffraction, and X-ray fluorescence spectroscopy with promising results. This is because metakaolin was obtained free of contamination by other materials.