无机固态材料中气体元素分析的现状与进展

本文介绍了气体元素分析样品表面处理的最新研究成果,综述了热导法、红外吸收法、库仑滴定法、飞行时间质谱法和火花源原子发射光谱法等分析方法在无机固态材料气体分析中的应用现状,分析了各自的特点及存在的问题,并展望了气体分析的发展方向(引用文献85篇)。     

A single-cell encapsulation method based on a microfluidic multi-step droplet splitting system

Single cell analysis is of great significance to understand the physiological activity of organisms.Microfluidic droplet is an ideal analytical platform for single-cell analysis. We developed a microfluidic droplet splitting system integrated with a flow-focusing structure and multi-step splitting structures to form 8-line droplets and encapsulate single cells in the droplets. Droplet generation frequency reached1021 Hz with the aqueous phase flow rate of 1 m L/min and the oil phase flow rate of 15 mL /min. Relative standard deviation of the droplet size was less than 5% in a single channel, while less than 6% in all the8 channels. The system was used for encapsulating human whole blood cells. A single-cell encapsulation efficiency of 31% was obtained with the blood cell concentration of 2.5× 10~4cells/mL, and the multicellular droplet percentage was only 1.3%. The multi-step droplet splitting system for single cell encapsulation featured simple structure and high throughput.     

Quantum-chemical study on the catalytic activity of TinRumO2(1 1 0) surfaces on chlorine evolution

Based on the generalized gradient approximation (GGA), Perdew-Wang-91 (PW91) combined with a periodic slab model has been applied to study the catalytic activity of chlorine evolution on TinRumO2(1 1 0) surface. Metal oxide model TinRumO2 has been established with pure TiO2 and RuO2 on the basis set of Double Numerical plus polarization (DNP), in which the proportion of n:m was 3:1, 1:1, or 1:3. Analysis on the reaction activity in the electrochemical reaction and the electrochemical desorption reaction was based on Frontiermolecular orbital theory. The results show that the TinRumO2 with a ratio of Ti:Ru at 3:1 is best facilitates the electrochemical reaction and electrochemical desorption reaction to produce M-Clads intermediate and precipitate Cl2. In addition, the adsorption energy of Cl on the surface of Ti3Ru1O2 possesses the minimum value of 2.514 eV, and thus electrochemical desorption reaction could occur most easily.     

Graphene Nanoribbons from Tetraphenylethene‐Based Polymeric Precursor: Chemical Synthesis and Application in Thin‐Film Field‐Effect Transistor

Graphene nanoribbons (GNRs) with a non‐zero bandgap are regarded as a promising candidate for the fabrication of electronic devices. In this study, large‐scale solution synthesis of narrow GNRs was firstly achieved by the intramolecular cyclodehydrogenation of kinked tetraphenylethene (TPE) polymer precursors prepared by A₂B₂‐type Suzuki‐Miyaura polymerization. After the cyclization reaction, the nanoribbons have a better conjugation than the twisted polymer precursor, resulting in obvious red shift in UV/vis absorption and photoluminescence (PL) spectra. The efficient formation of conjugated nanoribbons was also investigated by Raman, FTIR spectroscopy, and microscopic studies. Furthermore, such structurally well‐defined GNRs have been successfully developed for top‐gated field‐effect transistor (FET) by directly solution processing. The AFM images show that the prepared‐GNRs thin films form crystalline fibrillar intercalating networks, which can effectively facilitate the charge transport. These FET devices with ion‐gel gate dielectrics exhibit low‐voltage operation (<5 V) with excellent mobility up to 0.41 cm²·V^?1·s^?1 and an on‐off ratio of 3×10⁴, thus opening up new opportunities for flexible GNRs‐based electronic devices.     

Deoxygenation of methyl laurate to hydrocarbons on silica-supported Ni-Mo phosphides: Effect of calcination temperatures of precursor

SiO2-supported Ni-Mo bimetallic phosphides were prepared by temperature-programmed reduction(TPR) method from the phosphate precursors calcined at different temperatures. Their properties were characterized by means of ultraviolet-visible diffuse reflectance spectroscopy(UV-Vis DRS), H2temperature-programmed reduction(H2-TPR), X-ray diffraction(XRD), transmission electron microscopy(TEM), CO chemisorption, H2 and NH3temperature-programmed desorptions(H2-TPD and NH3-TPD). Their catalytic performances for the deoxygenation of methyl laurate were tested in a fixed-bed reactor. When the precursors were calcined at 400 and 500?C, respectively, Ni Mo P2 phase could be formed apart from Ni2 P and Mo P phases in the prepared C400 and C500 catalysts. However, when the precursors were calcined at600, 700 and 800°C, respectively, only Ni2 P and Mo P phases could be detected in the prepared C600, C700 and C800 catalysts. Also, in C400, C500 and C600 catalysts, Mo atoms were found to be entered in the lattice of Ni2 P phase, but the entering extent became less with the increase of calcination temperature. As the calcination temperature of the precursor increased, the interaction between Ni and Mo in the prepared catalysts decreased, and the phosphide crystallite size tended to increase, subsequently leading to the decrease in the surface metal site density and the acid amount. C600 catalyst showed the highest activity among the tested ones for the deoxygenation of methyl laurate. As the calcination temperature of the precursor increased, the selectivity to C12 hydrocarbons decreased while the selectivity to C11 hydrocarbons tended to increase. This can be mainly attributed to the decreased Ni-Mo interaction and the increased phosphide particle size. In sum, the structure and performance of Ni-Mo bimetallic phosphide catalyst can be tuned by the calcination temperature of precursor.     

Determination of five sesquiterpenoids in Xingnaojing injection by quantitative analysis of multiple components with a single marker

A quantitative analysis of multiple components with a single‐marker method was established for the simultaneous determination of five sesqutiterpenoids in Xingnaojing injection. This method was established with Xingnaojing injection determined by high‐performance liquid chromatography coupled with diode array detection. The durability and system suitability of the established method were evaluated, and the reliable relative correction factors were obtained with curdione selected as an internal reference. The contents of the five components in all Xingnaojing injections were determined by external standard method and the contents of curcumenone, curcumenol, curzerenone, and germacrone were also calculated with the obtained relative correction factors. Then, relative error was investigated to estimate the difference of the two methods. As a result, the established new method possesses good adaptability, and there is no significant difference between the two methods, except for the content of curzerenone in eight samples. To put the established method into practice, the limits of quantitation of the established method of the five components were proposed and defined. Thus, the developed methodology can also be utilized to the quality evaluation of Xingnaojing injection, in spite of the difference found in the content of curzerenone between the external standard method and the newly established method.     

Self‐Assembled Colloidal Particle Clusters from In Situ Pickering‐Like Emulsion Polymerization via Single Electron Transfer Mechanism

A simple route is reported to synthesize colloidal particle clusters (CPCs) from self‐assembly of in situ poly(vinylidene fluoride)/poly(styrene‐co‐tert‐butyl acrylate) [PVDF/P(St‐co‐tBA)] Janus particles through one‐pot seeded emulsion single electron transfer radical polymerization. In the in situ Pickering‐like emulsion polymerization, the tBA/St/PVDF feed ratio and polymerization temperature are important for the formation of well‐defined CPCs. When the tBA/St/PVDF feed ratio is 0.75 g/2.5 g/0.5 g and the reaction temperature is 35 °C, relatively uniform raspberry‐like CPCs are obtained. The hydrophobicity of the P(St‐co‐tBA) domains and the affinity of PVDF to the aqueous environment are considered to be the driving force for the self‐assembly of the in situ formed PVDF/P(St‐co‐tBA) Janus particles. The resultant raspberry‐like CPCs with PVDF particles protruding outward may be promising for superhydrophobic smart coatings.

     

波长校准用低压石英汞灯驱动电源的研制

研制波长校准用低压石英汞灯电源,用于驱动汞灯起辉并维持稳态发光。电路由EMI滤波电路、桥式整流电路、LCC半桥谐振逆变电路、控制电路和保护电路5部分组成。采用系统建模与仿真验证电路的可行性并计算电路参数理论值,利用示波器和功率表验证电源输出参数,功率输出稳定性不大于0.03 W。根据紫外可见近红外分光光度计国防最高计量标准对研制的电源驱动汞灯的工作效果进行评价。结果表明,汞灯能够输出系列特征谱线,谱线相对强度稳定性不大于5.16%;汞灯工作3 h后,灯管外壳表面温度为43℃。该驱动电源的性能参数满足JJG112–2015《低压石英汞灯波长标准器检定规程》的要求。     

微波消解–石墨炉原子吸收光谱法测定空气中碲

建立微波消解–石墨炉原子吸收光谱法测定空气中的碲。采用微孔滤膜收集样品,以硝酸–双氧水混合体系微波消解滤膜,氯化钯为基体改进剂,在优化的仪器工作条件下测定。碲的质量浓度在0~15μg/L范围内与吸光度线性关系良好,相关系数为0.999 5,方法检出限为0.14μg/L。样品加标回收率在95.6%~104.0%之间,测定结果的相对标准偏差为1.15~1.37%(n=7)。该方法操作简单、灵敏度高,适用于空气中微量碲的测定。     

Thickness difference induced pore structure variations in cellulosic separators for lithium-ion batteries

The pore structure of the separator is crucial to the performance of a lithium-battery as it affects the cell resistance. Herein, a straightforward approach to vary the pore structure of Cladophora cellulose (CC) separators is presented. It is demonstrated that the pore size and porosity of the CC separator can be increased merely by decreasing the thickness of the CC separator by using less CC in the manufacturing of the separator. As the pore size and porosity of the CC separator are increased, the mass transport through the separator is increased which decreases the electrolyte resistance in the pores of the separator. This enhances the battery performance, particularly at higher cycling rates, as is demonstrated for LiFePO₄/Li half-cells. A specific capacity of around 100 mAh g^?1 was hence obtained at a cycling rate of 2 C with a 10 µm thick CC separator while specific capacities of 40 and close to 0 mAh g^?1 were obtained for separators with thicknesses of 20 and 40 µm, respectively. As the results also showed that a higher ionic conductivity was obtained for the 10 µm thick CC separator than for the 20 and 40 µm thick CC separators, it is clear that the different pore structure of the separators was an important factor affecting the battery performance in addition to the separator thickness. The present straightforward, yet efficient, strategy for altering the pore structure hence holds significant promise for the manufacturing of separators with improved performance, as well as for fundamental studies of the influence of the properties of the separator on the performance of lithium-ion cells.