Silica Chloride–Catalyzed Synthesis of Thiiranes from Oxiranes Under Solvent-Free Conditions

A mild, simple, and efficient method for the synthesis of thiiranes from epoxides using a catalytic amount of silica chloride under solvent-free conditions has been developed. Experimental simplicity, simple work-up procedure, and solvent-free reaction conditions are important features of the present protocol.     

Bioglycerol-Based Sulfonic Acid-Functionalized Carbon Catalyst as an Efficient and Reusable Catalyst for One-Pot Synthesis of 3- Substituted-2H-1,4-Benzothiazines

Abstract

A simple and efficient synthetic protocol has been developed for the synthesis of 3-substituted-2H-1,4-benzothiazines by using bioglycerol-based sulfonic acid-functionalized carbon catalyst, devoid of corrosive acidic and basic reagents. The developed method has the advantages of good to excellent yields, short reaction times, operational simplicity, and a recyclable catalyst.     

A glassy carbon electrode modified with poly(eriochrome black T) for sensitive determination of adenine and guanine

A thin film of poly(eriochrome black T) was deposited on the surface of glassy carbon electrode by cyclic voltammetry, and this system is shown to enable the sensitive determination of adenine (A) and guanine (G). Scanning electron microscopy, Fourier transform infrared spectroscopy and electrochemical impedance spectroscopy were carried out to characterize the film which exhibits excellent electrocatalytic activity toward the oxidation of A and G in 0.1 M phosphate buffer solution (pH 4.0). Square wave voltammetry reveals an oxidation peak at 1084 mV whose current is linearly related to the concentration of A in the range from 0.05 to 1.00 μM. The oxidation peak for G occurs at 788 mV, and its current is linearly related to the concentration of G in the range from 0.025 to 1.00 μM. The detection limits are 0.017 μM for A and 0.008 μM for G (at S/N?=?3), respectively. The modified electrode displays good reproducibility and selectivity for the determination of A and G. The sensor was applied to quantify A and G in fish sperm DNA with satisfactory results.

Preparation and characterization of nanosized TiO2 powder as an inorganic adsorbent for aqueous radionuclide Co(II) ions

In this research TiO₂ sample was synthesized by a simple sol–gel method and was characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) techniques. The XRD result indicated that the obtained product was anatase titanium dioxide with high purity, the TEM image clearly showed that the particle sizes of TiO₂ nanoparticles were in the range of 30–70 nm, and the measured BET surface area of the heated TiO₂ nanoparticles was 147.14 m²/g. In this work, the prepared TiO₂ sample was used as a new adsorbent for the adsorption of radionuclide Co(II) ions from aqueous solutions, and the influence of pH, contact time, ionic strength and temperature in the presence or absence of humic acid/fulvic acid (HA/FA) were also investigated. The experimental results indicated that the adsorption of Co(II) ions onto TiO₂ was strongly pH-dependent. Based on the surface complexation, the presence of HSs enhanced the adsorption of Co(II) ions and the influence of Co(II) adsorption onto FA–TiO₂ hybrids was much stronger than that of HA–TiO₂ at pH values of 2.0–9.0. Adsorption of Co(II) ions onto TiO₂ powder was strongly dependent on ionic strength. The adsorption process mainly occured in the first contact time of 2 h and could be fitted by a pseudo-second-order rate model. The calculated thermodynamic data indicated that the adsorption of Co(II) ions onto TiO₂ was a spontaneous process and favorable at high temperatures.     

Studies on the Effects of Additional Components on Micellization of CTAB via Surface Tension Measurements

The effects of Tris-HCl buffer solution on the cmc of cetyltrimethylammonium bromide (CTAB) were studied by surface tension measurement. The result shows that the effect of the buffer solution depends on the interaction between CTAB and NaCl and the structure accelerants of water, Tris. A series of parameters, including the critical micelle concentration (cmc), the surface tension at cmc (γ_cmc), the adsorption efficiency (pC₂₀), and the effectiveness of surface tension reduction (∏_cmc) were obtained from the surface tension measurements in the presence of glycine with different concentration in the Tris-HCl buffer solution at 27°C. In addition, maximum surface excess concentration (Γ _max) and minimum surface area per molecule (A_min) at the air-water interface were estimated according to the Gibbs adsorption isotherm. The thermodynamic parameters (Δ C _p,m , Δ H _m,tr , Δ C _p,m,tr ) of micellization for CTAB in the absence and presence of glycine at different temperature were also been obtained.     

Determination of 12 potential nephrotoxicity biomarkers in rat serum and urine by liquid chromatography with mass spectrometry and its application to renal failure induced by Semen Strychni

In previous nephrotoxicity metabonomic studies, several potential biomarkers were found and evaluated. To investigate the relationship between the nephrotoxicity biomarkers and the therapeutic role of Radix Glycyrrhizae extract on Semen Strychni‐induced renal failure, 12 typical biomarkers are selected and a simple LC–MS method has been developed and validated. Citric acid, guanidinosuccinic acid, taurine, guanidinoacetic acid, uric acid, creatinine, hippuric acid, xanthurenic acid, kynurenic acid, 3‐indoxyl sulfate, indole‐3‐acetic acid, and phenaceturic acid were separated by a Phenomenex Luna C₁₈ column and a methanol/water (5 mM ammonium acetate) gradient program with a runtime of 20 min. The prepared calibration curves showed good linearity with regression coefficients all above 0.9913. The absolute recoveries of analytes from serum and urine were all more than 70.4%. With the developed method, analytes were successfully determined in serum and urine samples within 52 days. Results showed that guanidinosuccinic acid, guanidinoacetic acid, 3‐indoxyl sulfate, and indole‐3‐acetic acid (only in urine) were more sensitive than the conventional renal function markers in evaluating the therapeutic role of Radix Glycyrrhizae extract on Semen Strychni‐induced renal failure. The method could be further used in predicting and monitoring renal failure cause by other reasons in the following researches.     

Effect of Axial Ligands on the Molecular Configurations,Stability, Reactivity,and Photodynamic Activities of Silicon Phthalocyanines

To demonstrate the effect of axial ligands on the structure–activity relationship, a series of axially substituted silicon phthalocyanines (SiPcs) have been synthesized with changes to the axial ligands. The reactivity of the axial ligand upon shielding by the phthalocyanine ring current, along with their stability, photophysical, and photodynamic therapy (PDT) activities were compared and evaluated for the first time. As revealed by single‐crystal XRD analysis, rotation of the axial ? OMe ligands was observed in SiPc 3 , which resulted in two molecular configurations coexisting synchronously in both the solid and solution states and causing a split of the phthalocyanine α protons in the ¹H NMR spectra that is significantly different from all SiPcs reported so far. The remarkable photostability, good singlet oxygen quantum yield, and efficient in vitro photodynamic activity synergistically show that compound 3 is one of the most promising photosensitizers for PDT.     

电泳法制备的致密氧化锡薄膜及其在高稳定性钙钛矿太阳能电池中的应用

在平面型钙钛矿太阳能电池中常采用SnO₂作为电子传输层材料,相应的SnO₂薄膜常采用溶液旋涂法制备。但是由于前驱液中的纳米颗粒可能会发生部分团聚、基底和溶液难以完全避免灰尘等杂质颗粒混入,且最佳的SnO₂电子传输层的厚度通常仅有约20 nm,所以这种方法制备的电子传输层难以保证严格致密和无纳米针孔。在本工作中,我们报道了一种电泳沉积制备致密SnO₂薄膜的方法,并用其有效地提高了钙钛矿太阳能电池的光电转换效率和工况稳定性。通过电泳法,表面带负电荷的SnO₂纳米颗粒在电场的作用下沉积到氧化铟锡(ITO)阳极表面,这种方法得到的薄膜比旋涂法制备的更为致密。将其应用于n-i-p结构的钙钛矿太阳能电池中,能够使得暗电流降低并抑制载流子的非辐射复合,从而提高电池的短路电流和开路电压,进而实现更高的光电转换效率(从18.17%提高到19.52%),且能消除迟滞效应。更重要的是,长期工况稳定性测试表明基于电泳-旋涂法制备的器件在1个太阳的光照下、最大功率点处连续工作960 h后,仍然能够保持71%的初始效率;然而基于旋涂法制备的器件在工作100 h后即降低到初始效率的70%。本工作提供了一种全新的SnO₂电子传输层的制备方法,显著地提高了器件性能和工况稳定性,后续有望应用于制备大面积器件和电池模组。     

马尿酸分子印迹电化学传感器的制备及应用

采用超声法制备g-C3N4/NiO复合催化材料,将其滴涂在玻碳电极(GCE)表面构建g-C3N4/NiO/GCE催化电极。采用电聚合方法,以马尿酸为模板分子,邻苯二胺为功能单体构建M IP/g-C3N4/NiO/GCE传感器。采用时间-电流法对传感器制备条件优化。结果表明,复合催化材料对H2O2具有良好的催化效果。分子印迹传感器对马尿酸具有良好的选择性。在优化条件下,马尿酸质量浓度在0.05~2 mg/L范围内,电极电流响应与浓度呈良好的线性关系,检出限为7.1μg/L。将电极用于尿液中马尿酸的检测,回收率在87.3%~95.3%之间。     

Experimental characterization of transition to chaos in the presence of noise

Transition to chaos in the presence of noise is an important problem in nonlinear and statistical physics. Recently, a scaling law has been theoretically predicted which relates the Lyapunov exponent to the noise variation near the transition. Here we present experimental observation of noise-induced chaos in an electronic circuit and obtain the fundamental scaling law characterizing the transition. The experimentally obtained scaling exponent agrees very well with that predicted by theory.