Solubility of Triethylamine in Tetraethylammonium Chloride Aqueous Solutions from 20 to 35°C

Solubilities of triethylamine in aqueous tetraethylammonium chloride solutions were measured at 20, 25, and 35°C. The molalities in Et₄NCl of the aqueous solvents ranged from 0.03 to 1 mol-kg^–1. The data were evaluated from density measurements using a vibrating-tube densimeter. At each temperature, least-squares method was used to fit experimental density data points to double polynomial equations of various degrees. Triethylamine molalities of the saturated aqueous phases were estimated by extrapolation from those equations. Experimental data were interpreted in terms of hydrophobic and electrostatic perturbed domains in the hydration shells of the noneleceory and of the cation of the salt, as a function of temperature and salt concentration. The conclusions obtained are consistent with previous volumetric studies.     

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.     

A New Approach to α—Bromochalcones

α-Bromo benzolymethylene triphenylphosphorane 3 has been synthesized by the reaction of benzoylmethylene triphenylphosphorane 1 with N-bromosuccinimide in the yield of 87% and can react with aromatic aldehydes 4 to give α-bromochalcones 5 in good yields.     

Terbium-sensitized luminescence determination of levofloxacin in tablets and human urine and serum

A selective and sensitive luminescence method for the determination of levofloxacin is described. The method is based in the luminescence signal from a terbium(III)-levofloxacin complex, in a micellar solution of sodium dodecyl sulfate (SDS), using a chemical deoxygenation agent (Na2SO3). The method allows the determination of 8-600 ng mL-1 of levofloxacin in 10 mM SDS solution containing 0.04 M acetic acid-sodium acetate buffer (pH 6) and 7.5 mM Na2SO3 with lambda exc = 292 nm and lambda em = 546 nm. The luminescence method was applied to the determination of the levofloxacin in a Spanish commercialized pharmaceutical formulation Tavanic (Hoechst Marion Roussel). Good concordance was found between the nominal and experimental values (500 and 488 mg, respectively), with a relative standard deviation (RSD) of 0.6%. The proposed method was shown to be 100-fold more sensitive than the spectrophotometric method, and nearly 2-fold more sensitive than the fluorescence method. The method was also applied to levofloxacin determination in human serum (by external calibration method) and urine (by standard additions method), spiked at levels found after drug administration at normal clinical doses. Average recoveries found were 90.1 (RSD 1%) and 102 (RSD 1.9%), respectively.     

Compatibility mechanisms between EVA and complex impact heterophasic PP-EPx copolymers as a function of EP content

Compatibility mechanisms between EVA and complex heterophasic iPP-EPx copolymers have been studied as a function of EP content. Systematic studies were made in order to characterize the thermal, morphological and mechanical behavior, before and after blending a series of PP-EPx/EVA concentrations. Multiple melting, proportional to the EP content, was observed for the neat copolymers and an explanation was given for its evolution in terms of rejection-like secondary crystallization. After blending with EVA, the generation of a single T_g was taken as an indication of compatibility between both polymers. A morphological transition toward compatibility was first determined at 20 wt.% EVA which was in correlation with a morphological change from isolated spherical domains to interconnected voids. A second morphological transition from interconnected voids to fibrous crystals was observed above 40 wt.% EVA. This last transition marked the beginning of compatibility. Overall, the evolution of blends was explained in terms of the nature of the complex heterophasic copolymers. Tensile mechanical studies were also consistent with morphological changes. Increases in the x content in EPx and in EVA concentration worked in favor of impact resistance.     

Synthesis and reactivity of N-[α-acetoxy)-4-pyridylmethyl]-3,5-dimethylbenzamide

The synthesis of N-[(α-acetoxy)-4-pyridylmethyl]-3,5-dimethylbenzamide (4) and its reactivity are described. Since the acetoxy is a good leaving group, 4 gives S_N processes easily.     

Characterization of cyclodextrin-modified infrared chemical sensors: Part I. Modeling the mechanisms of interaction

To explore the properties of cyclodextrins (CDs) as an optical sensing phase, the behavior of immobilized CD in interaction with analytes was studied in this work. CDs having different cavity sizes were immobilized onto the surface of infrared (IR) internal reflection-sensing element (IRE) to kinetically monitor the behavior of CD in interaction with analytes. Several aromatic compounds having various molecular sizes and functional groups were used to characterize the interaction mechanism. A two-layer modification method was proposed in this work, which utilized a thin hydrophobic film (polyvinyl benzyl chloride) to stick on the IRE and to covalently bond to the CDs through an ethylene diamine linker. The synthesized CD phases exhibited high stability in aqueous solution. To analyze the behavior during the formation of complexes between the guest molecules and the CD phases, we modeled the interaction behavior and treated the kinetic data with the theoretical equations developed in this work. The results indicate that the behavior of the interaction between guest molecules and CDs was explained by considering the formation of two types of complexes: adsorbed complexes and inclusion complexes. The formation of the inclusion complexes was relatively fast, the time required to reach equilibrium could be shorter than a few minutes. The adsorbed complexes were also observed, but their rate of formation was relatively slow; equilibrium could be reached at times greater than 60 min. Based on the signals observed under equilibrium conditions, the concentration of inclusion complexes was approximately three times than that of the adsorbed complexes.     

Zeolite NaY-mediated oxidation of dyes with H2O2: unique heterogeneous non-transition metal center cleavage of H2O2 under visible light irradiation

This study investigated the visible-light catalysis mediated by zeolite NaY on the oxidation of dyes with H₂O₂. The results demonstrated that zeolite NaY acts as a sink for the electron from the photo-excited dye in the heterogeneous catalysis. Furthermore, the electron can effectively activate H₂O₂ to produce ^·OH radical that is a powerful oxidant for the oxidation of dye at room temperature. The effects of the framework topology, Si/Al ratio, and exchangeable cation of the zeolite on the oxidation of various dyes were also shown.