Highly selective coextraction of rhodamine B and dibenzyl phthalate based on high‐density dual‐template imprinted shells on silica microparticles

A simple one‐pot approach based on molecularly imprinted polymer shells dispersed on the surface of silica for simultaneous determination of rhodamine B and dibenzyl phthalate (DBzP) has been developed. Highly dense molecularly imprinted polymer shells were formed in the mixture of acetonitrile and toluene by the copolymerization of methacrylic acid and ethylene glycol dimethacrylate, as well as two templates, rhodamine B and dibenzyl phthalate, directed by the vinyl end groups functional monolayer at surface silica microspheres after 3‐methacryloxypropyl trimethoxysilane modification. The obtained imprinted polymer shells showed large average pore diameter (102.5 nm) and about 100 nm shell thickness. The imprinted particles also showed high imprinting factor (α_RhB = 3.52 and α_DBzP = 3.94), rapid binding kinetics, and excellent selective affinity capacity for rhodamine B and dibenzyl phthalate containing another three competitors in mixed solution. Moreover, the imprinted particles coupled with ultra high performance liquid chromatography was successfully applied to simultaneous analysis of rhodamine B and dibenzyl phthalate in two spiked beverage samples with average recoveries in the range of 88.0−93.0% for rhodamine B and 84.0–92.0% for dibenzyl phthalate with the relative standard deviation lower than 5.1%.     

Zinc sulfide nanosheets as a novel solid‐phase extraction material for flavonoids

As a novel solid‐phase extraction material, zinc sulfide nanosheets were prepared by a simple method and were used to extract flavonoids. We used scanning electron microscopy to show its nanosheet morphology and energy dispersive X‐ray spectroscopy and powder X‐ray diffraction to confirm its chemical and phase compositions. Coupled to a high‐performance liquid chromatography, the zinc sulfide nanosheets were packed into a microcolumn and were used to extract four model flavonoids to examine their extraction ability. The parameters of sample loading and elution were investigated. Under optimized conditions, the analytical method for flavonoids was established. For the method, wide linearities from 1 to 250 μg/L and low limits of detection from 0.25 to 0.5 μg/L were obtained. The relative standard deviations for single column repeatability and column to column reproducibility were less than 7.7 and 10.4%, respectively. The established method was also used to analyze two real samples and the recoveries from 88.7 to 98.2% further proved the reliability of the method. Moreover, the zinc sulfide nanosheets have good stability and that in one column can be reused for more than 50 times. This work proves that the prepared zinc sulfide nanosheets are a good candidate as the flavonoids sorbent.     

Deposition of ZnS thin film by ultrasonic spray pyrolysis: effect of thickness on the crystallographic and electrical properties

Zinc sulfide (ZnS) thin films have been deposited on Si (1 0 0) substrate using ultrasonic spray pyrolysis. X-ray diffraction (XRD) analysis revealed that the films are (0 0 2) preferentially oriented with c-axis-oriented wurtzite structure. The crystallinity has been found to improve with film thickness in the 180–6000 nm range. Film structure has been analyzed by XRD, scanning electron microscope, FTIR, and Raman spectroscopies, while the stoichiometry has been verified by energy-dispersive spectroscopy and particle-induced X-ray emission techniques. Electrical properties of the grown films were characterized by current–voltage and capacitance–voltage measurements where, the films show better conducting behavior at higher thickness.     

Novel WS2/Fe0.95S1.05 Hierarchical Nanosphere as a Highly Efficient Electrocatalyst for Hydrogen Evolution Reaction

Fe_0.95S_1.05 with high reactivity and stability was incorporated into WS₂ nanosheets via a one-step solvothermal method for the first time. The resulted hybrid catalyst has much higher catalytic activity than WS₂ and Fe_0.95S_1.05 alone, and the optimal WS₂/Fe_0.95S_1.05 hybrid catalyst was found by adjusting the feed ratio. The addition of Fe_0.95S_1.05 was proven to be able to enhance the hydrogen evolution reaction (HER) activity of WS₂, and vice versa. At the same time, it was found that the catalytic effect of the hybrid catalyst was the best when the feed ratio was W : Fe=2 : 1. In other words, we confirmed that there is a synergistic effect between W- and Fe-based sulfide hybrid catalysts, and validated that the reason for the improved HER performance is the strong interaction between the two in the middle sulfur. WS₂/Fe_0.95S_1.05-2 hybrid catalyst leads to enhanced HER activity, which shows a low overpotential of ∼0.172 V at 10 mA cm⁻², low Tafel slope of ∼53.47 mV/decade. This study supplies innovative synthesis of a highly active WS₂/Fe_0.95S_1.05 hybrid catalyst for HER.     

Determination of Dimethyl Sulfide in Gas Samples by Single Photon Ionization Time of Flight Mass Spectrometry

It is difficult to determine sulfur-containing volatile organic compounds in the atmosphere because of their reactivity. Primary off-line techniques may suffer losses of analytes during the transportation from field to laboratory and sample preparation. In this study, a novel method was developed to directly measure dimethyl sulfide at parts-per-billion concentration levels in the atmosphere using vacuum ultraviolet single photon ionization time-of-flight mass spectrometry. This technique offers continuous sampling at a response rate of one measurement per second, or cumulative measurements over longer time periods. Laboratory prepared samples of different concentrations of dimethyl sulfide in pure nitrogen gas were analyzed at several sampling frequencies. Good precision was achieved using sampling periods of at least 60 seconds with a relative standard deviation of less than 25%. The detection limit for dimethyl sulfide was below the 3 ppb olfactory threshold. These results demonstrate that single photon ionization time-of-flight mass spectrometry is a valuable tool for rapid, real-time measurements of sulfur-containing organic compounds in the air.     

Protein‐Directed Synthesis of Mn‐Doped ZnS Quantum Dots: A Dual‐Channel Biosensor for Two Proteins

Proteins typically have nanoscale dimensions and multiple binding sites with inorganic ions, which facilitates the templated synthesis of nanoparticles to yield nanoparticle–protein hybrids with tailored functionality, water solubility, and tunable frameworks with well‐defined structure. In this work, we report a protein‐templated synthesis of Mn‐doped ZnS quantum dots (QDs) by exploring bovine serum albumin (BSA) as the template. The obtained Mn‐doped ZnS QDs give phosphorescence emission centered at 590 nm, with a decay time of about 1.9 ms. A dual‐channel sensing system for two different proteins was developed through integration of the optical responses (phosphorescence emission and resonant light scattering (RLS)) of Mn‐doped ZnS QDs and recognition of them by surface BSA phosphorescent sensing of trypsin and RLS sensing of lysozyme. Trypsin can digest BSA and remove BSA from the surface of Mn‐doped ZnS QDs, thus quenching the phosphorescence of QDs, whereas lysozyme can assemble with BSA to lead to aggregation of QDs and enhanced RLS intensity. The detection limits for trypsin and lysozyme were 40 and 3 nM , respectively. The selectivity of the respective channel for trypsin and lysozyme was evaluated with a series of other proteins. Unlike other protein sensors based on nanobioconjugates, the proposed dual‐channel sensor employs only one type of QDs but can detect two different proteins. Further, we found the RLS of QDs can also be useful for studying the BSA–lysozyme binding stoichiometry, which has not been reported in the literature. These successful biosensor applications clearly demonstrate that BSA not only serves as a template for growth of Mn‐doped ZnS QDs, but also impacts the QDs for selective recognition of analyte proteins.     

Preparation of Primary Thioamides From Nitriles Using Sodium Hydrogen Sulfide and Diethylamine Hydrochloride

Primary thioamides are prepared in moderate to excellent yields by treating nitriles with sodium hydrogen sulfide and diethylamine hydrochloride in an appropriate solvent with mild heating.     

Convenient and Efficient Synthesis of 1,1‐Bis‐(4‐alkylthiophenyl)‐1‐alkenes via Tandem Friedel–Crafts Acylation and Alkylation of Sulfides and Acyl Chlorides

1,1‐Bis(4‐alkylthiophenyl)‐1‐alkenes were conveniently and efficiently prepared from alkyl phenyl sulfides and acyl chlorides via a tandem Friedel–Crafts acylation and alkylation in the presence of anhydrous aluminum chloride. The scope, limitation, and mechanism of the tandem reaction were also discussed.     

富氮掺杂碳空心纳米笼协同钴镍硫化物提升超级电容器性能

采用简单的热解-硫化两步法成功制备了一种新型的富氮掺杂碳空心纳米笼(NC)负载双元金属硫化物纳米颗粒(CoNi_xS_y)的复合材料 CoNi_xS_y/NC。该策略以丁二酮肟镍为镍源,增加了活性位点,同时前驱体 ZIF-8@Ni-ZIF-67的核壳结构为空心碳纳米笼的构建提供了可能性。这种独特的负载多金属硫化物纳米颗粒的中空结构使CoNi_xS_y/NC作为电极材料时具有更多的活性位点、更高的导电性和结构稳定性,从而使其具有较高的比容量(1 A·g^-1时比容量为629.2 F·g^-1),优异的循环稳定性(1 A·g^-1下1 000次循环测试后容量保持率为93.4%)。当将其进一步组装成对称超级电容器后,在1 A·g^-1下可提供207.2 F·g^-1的比电容,1 000圈循环稳定后的容量保持率为85.36%。     

化学浴沉积方法制备硫化铟敏化太阳电池及其性能研究

硫化铟是一种稳定、低毒性的半导体材料. 本文采用低成本的化学浴沉积方法制备了硫化铟敏化太阳电池, X射线衍射(XRD)、光电子能谱(XPS)和扫描电镜(SEM)结果表明形成了硫化铟敏化的二氧化钛薄膜. 化学浴沉积温度对所得硫化铟敏化薄膜的形貌有显著的影响, 进而影响电池性能. 温度太低时, 化学浴沉积反应速率太低, 只发生少量沉积; 温度太高时, 化学浴沉积反应速率较快, 硫化铟来不及沉积到二氧化钛多孔薄膜内部. 当温度在40℃时, 硫化铟沉积均匀性最好, 薄膜的光吸收性能最佳, 电池的短路电流最大, 另外, 填充因子达到最佳, 为65%, 电池总体光电转换效率为0.32%.