Influence of catalyst on structural and morphological properties of TiO2 nanostructured films prepared by sol–gel on glass

Transparent TiO2 thin films have been prepared by the sol-gel method using titanium alkoxides as precursors.Thin films were deposited on glass supports by the dip-coating technique.The TiO2 layer acts as a self-cleaning coating generated from its photocatalysis and photoinduced superhydrophilicity.The crystalline structure of TiO2 films was dominantly identified as the anatase phase,consisted of uniform spherical particles of about 14-50 nm in size,which strongly depends upon catalyst-type and heat treatment temperature.Increasing heat treating temperature can lead to an increase in crystalline size.The results indicated that the sample S.S(sample derived from sol containing sulfuric acid as catalyst) exhibits superhydrophilic nature and better photocatalytic activity,which can be attributed to its higher anatase content and lower crystalline size.Morphological studies,carried out using Atomic Force Microscopy(AFM),confirm the presence of crystalline phase with such a grain size and low surface roughness.Thus,the applied films exhibiting high photocatalytic activity,superhydrophilic behavior,and low surface roughness can be used as an efficient self-cleaning coating on glass and other optical applications.     

K-shell single-electron capture in collision of fast protons with multi-electron atoms

Single-electron capture from the K shell of atomic targets by impact of protons at moderate and high energies has been studied using a first-order three-body Coulomb-Born continuum distorted wave approximation. The applied formalism satisfies the correct Coulomb boundary conditions. Single-zeta Roothaan-Hartree-Fock wave functions are used to describe the initial electronic bound state of the exchanged electron. Both differential and integral capture cross sections are calculated for impact of protons on carbon, nitrogen, oxygen, neon and argon atoms. The results are compared with the available measurements and other theories. The agreement between the calculations and experimental data is remarkable.     

Determination of ochratoxin A in grains by immuno-ultrafiltration and HPLC-fluorescence detection after postcolumn derivatisation in an electrochemical cell

The paper presents a new sample clean-up method based on immuno-ultrafiltration for the analysis of ochratoxin A in cereals. In contrast to immunoaffinity chromatography, in immuno-ultrafiltration, the antibodies are used in non-immobilised form. Ochratoxin A was extracted with ACN/water (60/40, v/v), and the extract was loaded onto the ultrafiltration device. After a washing step with phosphate-buffered saline, containing 0.05% Tween 20, ochratoxin A was eluted with MeOH/acetic acid (99/1, v/v). The detection of ochratoxin A was carried out with high-performance liquid chromatography and a fluorescence detector coupled to an electrochemical cell (Coring cell). The electrochemical cell was used to eliminate matrix interferences by oxidising matrix compounds. The method was validated by repeatedly analysing spiked barley and rye samples as well as a certified wheat reference material. Recoveries and standard deviations (1 SD) were found to be 71 ± 9%, 77 ± 12% and 77 ± 8% in wheat, barley and rye, respectively. The limit of detection (S/N = 3) and limit of quantitation (S/N = 10) were determined to be 0.4 μg kg^-1 and 1 μg kg^-1. The analysis of the certified reference material resulted in ochratoxin A concentrations which were in the range assigned by the producer. Additionally, the effect of the electrochemical cell on other widely used clean-up techniques, namely the immunoaffinity clean-up and multifunctional columns (Mycosep #229), was evaluated. In all clean-up methods, an improvement of the chromatogram quality was registered.     

Weak module amenability of triangular Banach algebras

Let A and B be unital Banach algebras and let M be a unital Banach A,B-module. Forrest and Marcoux [6] have studied the weak amenability of triangular Banach algebra \(\mathcal{T} = \left[ {_B^{AM} } \right]\) and showed that T is weakly amenable if and only if the corner algebras A and B are weakly amenable. When \(\mathfrak{A}\) is a Banach algebra and A and B are Banach \(\mathfrak{A}\)-module with compatible actions, and M is a commutative left Banach \(\mathfrak{A}\)-A-module and right Banach \(\mathfrak{A}\)-B-module, we show that A and B are weakly \(\mathfrak{A}\)-module amenable if and only if triangular Banach algebra T is weakly \(\mathfrak{T}\)-module amenable, where \(\mathfrak{T}: = \{ [^\alpha _\alpha ]:\alpha \in \mathfrak{A}\} \).     

Sol-gel immunoaffinity chromatography for the clean up of ochratoxin A contaminated grains

This paper describes the application of sol-gel immunoaffinity columns for clean up of ochratoxin A contaminated cereal crops. Monoclonal antibodies selective for OTA have been entrapped into the pores of a sol-gel matrix in order to prepare immunoaffinity columns. Different parameters such as amount of entrapped antibodies and loading conditions were optimized to obtain highest possible recoveries of OTA. The method has been found to be a suitable tool in sample preparation prior to HPLC-FLD determination and as selective as conventional commercially available immunoaffinity columns. In the clean up of different cereals mean recoveries of 82±5%, 90±6% and 91±3%, were obtained for wheat, barley and rye, respectively, with sol-gel columns containing 1mg of anti-OTA antibodies. The detection limit (signal-to-noise ratio, 3) was 0.5 μg/kg and the limit of quantification (signal-to-noise ratio, 10) determined to be 1 μg/kg. Sol-gel columns can be reused 7 times without significant loss of recovery. After 10 applications the recovery decreased to approx. 50%.     

Isocyanide-based multicomponent reactions: synthesis of 3,3-dicyano-N-alkyl-2-arylpropanamide derivatives

A new isocyanide-based multicomponent reaction between an aromatic aldehyde, malononitrile, an isocyanide, and acetic acid efficiently provides 3,3-dicyano-N-alkyl-2-arylpropanamide derivatives in excellent yields in ethanol at 70 °C. This reaction led to the construction of two carbon-carbon bonds and one amide group in a single synthetic step.     

Mesoporous silica SBA-15 modified with copper as an efficient NO2 adsorbent at ambient conditions

Copper oxide particles were synthesized by precipitation in sodium hydroxide and dispersed simultaneously in mesoporous SBA-15 silica. The materials were then submitted to thermal treatment under nitrogen at different temperatures. They were tested as novel NO(2) adsorbents in dynamic condition at room temperature. The surface of the initial and exhausted materials was characterized using N(2) adsorption, XRD, TEM, thermal analysis and FT-IR. The addition of Cu(2)O particles leads to a significant increase in the NO(2) adsorption capacity. However, no trend between the NO(2) capacity and the temperature of the thermal treatment of the materials has been observed. The amount of NO released during the NO(2) adsorption was found to be lower on the materials submitted to a low temperature treatment. On these materials, the formation of copper nitrites is favored, whereas on materials treated at higher temperature, copper nitrates are formed as a predominant species. The results suggest that silanol groups of the silica matrix play an important role in NO(2) adsorption and NO retention at room temperature.     

Electrochemical monitoring of photoelectrocatalytic degradation of rhodamine B using TiO2 thin film modified graphite electrode

A commercially available TiO₂ powder (Degussa P25) has been used to prepare thin films on graphite plates. The photoelectrochemical degradation of rhodamine B was investigated using this photoelectrode. The effects of applied potential, pH, and initial rhodamine B concentration on the photoelectrocatalytic (PEC) degradation of rhodamine B using ultraviolet illuminated TiO₂/graphite (TiO₂/C) thin film electrode were examined and discussed. Also, direct photolysis, electrochemical oxidation, photocatalytic, and PEC degradation of rhodamine B were compared. Results show that the best responses for PEC are obtained at applied potential of 1.2?V vs. reference electrode, pH?4.0, and initial rhodamine B concentration of 4.2?mg?L^?1.     

Permeability,Solubility, and Diffusivity of Methane and Butane in Diphenylsiloxane-Dimethylsiloxane Copolymer Membranes

Permeation and sorption of methane and n-butane gases in polydimethylsiloxane (PDMS) and diphenylsiloxane-dimethylsiloxane (DPh-DM) block copolymer membranes were studied at room temperature and different upstream pressures. The membranes were prepared via room temperature vulcanization of vinyl terminated siloxanes through platinum catalyzed hydrosilylation reactions by mixing stoichiometric amounts of polymer, crosslinker, and catalyst, and casting of the mixture solutions with hexane. Composite membranes of polysiloxanes on a polyacrylonitrile microporous support were synthesized for permeation experiments and single layer dense films were used in sorption experiments. The effect of upstream pressure on permeability, solubility, and diffusivity of these membranes was evaluated. It was found that selectivity of the DPh-DM copolymer membrane for n-C₄H₁₀ relative to CH₄ was up to 19% higher than that in PDMS membrane. Both solubility and diffusivity selectivities had positive contributions in permselectivity improvement. The improvement in selectivity was attained with less than a 6% decrease in permeability of n-C₄H_10. Up to 11% improvement in selectivity was also obtained in mixed gas experiment.