Synthesis and characterization of molybdenum incorporated mesoporous aluminophosphate

A synthesis of molybdenum incorporated mesoporous aluminophosphate with long-chain n-alkylamine as template material had been prepared under non-aqueous condition. These materials were extensively characterized by using X-ray diffraction (XRD), nitrogen sorption isotherms, nuclear magnetic resonance of ²⁷Al and ³¹P (NMR), inductive coupled plasma (ICP), electron spin resonance (ESR), Fourier transform infrared (FTIR) and thermogravimetric-differential thermal analysis (TG-DTA). Morphology of the materials had been observed by using transmission electron microscope (TEM) that revealed the mesoporous materials possessed wormhole-like structures. Alkaline solvent extraction using n-butylamine/ethanol had been efficiently removed the n-alkylamine from the mesoporous samples which yielded BET surface areas around 550-730 m²/g. BJH analysis showed a narrow pore size distribution which increased with increasing of the carbon chain length of alkylamine (template). Valence state and coordination of the molybdenum in the obtained samples were investigated by using ESR and FTIR where it was found that Mo⁴⁺ and Mo⁶⁺ molybdenum species existed in the molybdenum incorporated mesoporous aluminophosphate in tetrahedral coordination.     

Design of an experimental procedure for energy evaluation from biomass

The rational and sustainable exploitation of nature resources is one of the priority objectives of our society. In this article a method is proposed to evaluate and exploit the energetic resources contained in different forest formations. This method is based on the use of a combustion bomb calorimeter to determine the calorific values of the different samples studied. These results were complemented with chemical analysis of the samples and with environmental and geomorphological studies of the zones were samples were taken. The results obtained during the last 3 years for the residual biomass originated from the forest formations existing in Galicia ensure the reliability and usefulness of the method that can be extended to any forest formation all over the world.     

FT-IR study on solvent effects in building blocks of bioactive compounds. V

3-Hydroxy-4-hydroxymethyl pyrrolidin-2-ones, easily prepared from the Baylis–Hillman adduct 1-ethyl-4-methyl-2-hydroxy-3-methylenebutanedioate, are useful intermediates in the synthesis of bioactive compounds. In order to understand the mechanism involved in this reaction, vibrational and Montecarlo molecular mechanics conformational analysis on 1-ethyl-4-methyl-2-hydroxy-3-methylenebutanedioate were carried out, confirming the existence of a low energy intramolecular H-bonded five-member ring.     

Residual currents and corridor of flow in the Rio de la Plata

The Rio de la Plata is a large and shallow water body that discharges onto the Atlantic Ocean. The main driving forces for the river flow are the bathymetry, tides, the outflow from the Paraná and Uruguay rivers and the winds. A numerical model covering the entire river was set up with the objective of increasing our understanding of the hydrographical features and morphological dynamics in the Estuary. The simulations revealed a counter-clockwise residual circulation in the Samborombón Bay and an eastward net flow near the Uruguayan coast. The residual flow is forced by both the tides and the bathymetry. The residence time for the entire river ranges from 40 to 80 days. However, residence times above 120 days was found in the Samborombón Bay. Three corridors of flow have been identified.     

Optimization of the synthesis of non-symmetrical alkyl dimethyl sulfonium halides

This work is aimed at the optimization of the yield and purity of non-symmetrical trialkyl sulfonium halide salts. The effects of parameters such as solvent, temperature and concentration were studied. The products were carefully analyzed and the crystal structure of [{n-CH₃(CH₂)₁₅}(CH₃)₂S]Br determined. The overall aim of the present study is future syntheses of low-dimensional magnetic materials.     

Memory effects in gas chromatographic detection with a microwave-induced plasma

Capillary gas chromatography coupled to microwave-inducedplasma detection furnishes sensitivity adequate for trace analysis when the signal is monitored at a carbon emission line. Work performed with one of these systems at high electronic gain for the carbon signal has revealed solvent band widths in excess of four minutes; these impeded quantification of peaks eluting after the solvent. This report discusses two phenomena which could be related to the unexpected intensity of this solvent response: photomultiplier tube saturation and carbon deposits in the quartz plasma discharge tube.     

Deposition conditions in tailoring the morphology of highly porous reticular films prepared by electrostatic spray deposition (ESD) technique

Spongy-like reticular structure is a unique morphology fabricated by electrostatic spray deposition (ESD) technique. The effects of solvent, substrate temperature, precursor feeding rate, static electric field strength, and deposition time on tailoring the reticular structure were investigated. Scanning electron microscopy was used to observe the film morphology. MnO_x or LiMn₂O₄ were selected as the model materials. It is found that in addition to the conventional solvent butyl carbitol, other kinds of solvents such as ethylene glycol and propylene glycol can also be used to obtain reticular films at a suitable substrate temperature. Porous films with a low cross-linking degree pore structure can be prepared by increasing precursor feeding rate or decreasing substrate temperature. Increasing the deposition time or the electric field strength helps to obtain reticular films with more homogeneous pore size distribution. In addition, the addition of a high boiling-point solvent in mixed alcohol solvent results in the increase of proper substrate temperature. It is concluded that the fluidity of the spray droplets on the surface of a hot substrate is an important factor to form a reticular film.     

A polymer onium acting as phase-transfer catalyst in halogen-exchange fluorination promoted by microwave

A polymerized quaternary ammonium salt polydiallyldimethylammonium chloride, exhibiting high stability to heat and base, was prepared and applied as phase-transfer catalyst (PTC) in halogen-exchange (Halex) fluorination of chloronitrobenzenes to give excellent yields of corresponding fluoronitrobenzenes. Dimethyl sulfoxide was found to be the best solvent when microwave was applied as heating resource.     

双（十二烷基亚磺酰）乙烷溶剂萃取钯及其机理的研究

本文研究用双（十二烷基亚磺酰）乙烷萃取钯的性能，在ＫＩ存在下从７ｍｏｌ／Ｌ盐酸介质中用含有ＢＤＳＥ的氯仿能定量萃取钯，有机的钯可被硫脲或氨溶液反萃继之用ＴＭＫ－ＴｒｉｔｏｎＸ－１００光度法测定，研究了萃取的最佳条件及干扰情况，斜率法测得萃合物组成为Ｐｄ：Ｉ：ＢＤＳＥ＝１：２：１，红外光谱证实萃合物中ＢＤＳＥ的二个亚砜以硫原子与钯配位，萃合物为异位体络合物，提出了选择性萃取分离钯的新方法。     

SIMS analysis of residual gas elements with a Cameca IMS-6f ion microprobe

In this paper, we present experimental data for SIMS analysis of residual gas elements (RGEs) with a Cameca IMS-6f ion microprobe. We considered a simple experimental technique, which provides an effective separation of the secondary ions, sputtered from the bulk of a target, and from the molecules, adsorbed on the analyzed surface from the residual atmosphere. The technique needs the sputtering yield of one monolayer (ML) per second to be applied. The method improves (in more than one order of magnitude) the detection limit for RGEs in SIMS analysis, and simultaneously, provides information about the residual atmosphere at the sample surface and in the main chamber of the experimental instrument. The method provides a calibration method for an ion gauge, and can be used for SIMS analysis with a gas (O₂) flooding.