Surfactant mediated synthesis of spherical binary oxides photocatalytic with enhanced activity in visible light

Spherical silica and zirconia mixed titania and pure titania samples were prepared in presence of cetyltrimethylammonium bromide (CTAB) through controlled hydrolysis of corresponding metal alcoxides. Effect of surfactant amount and calcinations temperature on morphology, surface area and photocatalytic activity is studied using PXRD, SEM, FTIR, Solid state UV-vis spectroscopy and BET surface area. It is well observed that in presence of 2 mol% CTAB, uniform sized spherical oxide particles can be synthesized. However, increasing or decreasing the surfactant amount does not favor the spherical particle formation. Material synthesis in presence of CTAB not only helps in the spherical particle formation but also increases the surface area and visible light absorption. Studies on photocatalytic lead removal with respect to calcination temperature indicate that the calcination at 500 degrees C is most suitable for the best photocatalytic activity. Mixing of zirconia and silica helps in anatase phase stabilization even at 900 degrees C calcination. Accordingly low decrease in surface area even at 900 degrees C calcination is observed. Due to the phase stabilization and higher surface area binary oxide materials showed comparatively better photocatalytic activity even after calcination at 900 degrees C. So it can be concluded that present synthesis approach can produce uniform sized spherical binary oxide materials with better photocatalytic activity in visible light.     

水中高压脉动气泡水射流形成机理及载荷特性研究

具有脉动特性的气泡(如水下爆炸气泡、螺旋桨空泡和气枪气泡)动力学行为很大程度上取决于其边界条件. 实验已证实,近自由液面气泡在坍塌过程中常常产生背离自由液面的水射流现象,而近刚性边界气泡在坍塌阶段产生朝向壁面的高速水射流,严重威胁水中结构的局部强度. 前人基于 Rayleigh-Plesset 气泡理论和 “Bjerknes” 力来预测气泡射流方向,然而理论方法难以透彻的揭示气泡射流的初生、发展和砰击过程中丰富的力学机理. 本文首先采用水下高压放电技术产生气泡,并通过高速摄影对不同边界条件下气泡的运动特性进行实验研究. 然后,采用边界积分法模拟气泡非球状坍塌过程. 研究表明,边界条件改变了气泡周围的流场压力梯度方向,进而影响气泡射流初生位置;射流在发展阶段,气泡附近流场的局部高压区和射流之间存在“正反馈效应”,从而揭示了气泡射流速度在短时间内即可增加到百米每秒的力学机理. 射流砰击会在流场中造成局部高压区,随着气泡回弹,射流速度和砰击压力逐渐减小. 本文还探讨了无量纲距离参数对气泡运动及射流砰击载荷的影响,旨为近场水下爆炸等相关领域提供参考.      

Single-nucleotide polymorphism analysis by allele-specific extension of fluorescently labeled nucleotides in a microfluidic flow-through device

We describe a microfluidic approach for allele-specific extension of fluorescently labeled nucleotides for scoring of single-nucleotide polymorphism (SNP). The method takes advantage of the fact that the reaction kinetics differs between matched and mismatched configurations of allele-specific primers hybridized to DNA template. A microfluidic flow-through device for biochemical reactions on beads was used to take advantage of the reaction kinetics to increase the sequence specificity of the DNA polymerase, discriminating mismatched configurations from matched. The volume of the reaction chamber was 12.5 nL. All three possible variants of an SNP site at codon 72 of the p53 gene were scored using our approach. This work demonstrates the possibility of scoring SNP by allele-specific extension of fluorescently labeled nucleotides in a microfluidic flow-through device. The sensitive detection system and easy microfabrication of the microfluidic device enable further miniaturization and production of an array format of microfluidic devices for high-throughput SNP analysis.     

Facile stereoselective synthesis of cis- and trans-3-alkoxyazetidin-2-ones

A highly stereoselective synthesis of cis- and trans-3-alkoxy-3-phenyl/benzylthioazetidin-2-ones is described. The reaction of α-chlorosulfide-β-lactams with various alcohols catalyzed by a Lewis acid such as ZnCl₂ in the presence of molecular sieves (3-4 Å) leads to cis-3-alkoxy-3-phenyl/benzylthio-β-lactams whereas treatment of potassium 2-alkoxy-2-phenylthioethanoate with appropriate Schiff's base using POCl₃ in the presence of triethylamine leads to the formation of trans-3-alkoxy-3-phenylthioazetidin-2-ones as major products.     

Liquid chromatographic determination of residual nitrite/nitrate in foods: NMKL collaborative study

Nitrite and nitrate are used as additives in the food industry to provide color and taste and to control undesirable gas and flavor production by anaerobic bacteria by virtue of their antimicrobial properties. The analytical method that has been widely used to determine nitrite and nitrate involves the use of toxic cadmium. In response to a request from the Nordic Committee on Food Analysis, a study was performed to obtain an alternative chromatographic method to determine residual nitrite and nitrate in meat products. The study was done in 3 stages: (1) comparative evaluation of the performance of 3 liquid chromatographic methods, (2) internal validation of the selected ion chromatographic method, and (3) a collaborative study in which 17 laboratories from European countries participated. Furthermore, the applicability of the method to matrixes other than meat and meat products was demonstrated. The results of the collaborative study show that the European Prestandard prENV 12014-4 is well suited for the determination of nitrite and nitrate in different foods (e.g., meat products, vegetables, baby food, and cheese). The limits of detection for nitrite and nitrate ions are 1 and 10 mg/kg, respectively. Recoveries of residual nitrite/nitrate ranged from 96 to 108%. Repeatability and reproducibility were satisfactory.     

Synthesis and characterization of novel trans-3-benzyl/(diphenyl)methyl/naphthyl seleno substituted monocyclic β-lactams: X-ray structure of trans-1-(4′-methoxyphenyl)-3-(diphenyl)methylseleno-4-(4′-methoxyphenyl)azetidin-2-one

Several novel trans-3-benzyl/(diphenyl)methyl/naphthylseleno substituted monocyclic β-lactams (5-7) have been synthesized in high yields. The reaction scheme inolves [2 + 2] cycloaddition (Staudinger) reaction between suitably substituted imines 4(a-h) and ketenes (B) accessed from 2-benzyl/(diphenyl)methyl/naphthylselenoethanoic acids (1-3) using POCl₃ and triethylamine in refluxing toluene. Characterization of these newly synthesized seleno substituted β-lactams has been performed by various spectroscopic techniques viz. NMR (¹H, ¹³C and ⁷⁷Se), FTIR, mass spectrometry and elemental analysis. The molecular structure of trans-1-(4′-methoxyphenyl)-3-(diphenyl)methylseleno-4-(4′-methoxyphenyl)azetidin-2-one (6b) has also been established with the help of single crystal X-ray analysis.     

Multifractal analysis of drop‐casted copper (II) tetrasulfophthalocyanine film surfaces on the indium tin oxide substrates

This paper applies multifractal spectrum theory to characterize the structural complexity of 3D surface roughness of copper (II) tetrasulfophthalocyanine (CuTsPc) films on the indium tin oxide (ITO) substrate, obtained with atomic force microscopy (AFM) analysis. CuTsPc films were prepared by drop cast method on ITO substrate. CuTsPc films surface roughness was studied by AFM in tapping‐mode?, in air, on square areas of 2500 µm². A novel approach, on the basis of computational algorithms for analysis of 3D roughness surface applied for AFM data, was presented. Results revealed that the 3D surface roughness of CuTsPc films prepared by drop cast method on ITO substrate can be described using the multifractal geometry. The generalized dimensions D_q and the multifractal spectrum f(α) provided quantitative values that characterize the local scale properties of CuTsPc films surface geometry at nanometer scale. Data provide valuable information to describe the spatial arrangement of 3D surface roughness of CuTsPc films on ITO substrate, which was not taken into account by classical surface statistical parameters. Copyright © 2014 John Wiley & Sons, Ltd.