亲水作用色谱-串联质谱法测定动物源运动食品中3种氨基糖苷类抗生素的残留量

该研究建立了一种亲水交互作用色谱-串联质谱（HILIC-MS/MS）法测定动物源运动食品中潮霉素B、新霉素、安普霉素3种氨基糖苷类抗生素残留量的方法。结果表明，样品经Sielc Obelisc R柱分离，采用0.1%甲酸水溶液-乙腈梯度洗脱，可以实现3种目标物组分的分离。在此条件下，3种氨基糖苷类抗生素在5～500 ng/mL的质量浓度范围内线性关系良好，相关系数R2为0.999 5～0.999 9，检出限均为15 μg/kg，定量限均为50 μg/kg，保留时间的日间和日内相对标准偏差（RSD）分别为3.5%～7.9%和3.5%～4.1%，峰面积的日间和日内RSD分别为3.6%～7.4%和3.2%～3.9%，加标回收率为85.7%～93.6%，回收率试验结果的RSD为3.1%～5.2%。该方法可以满足动物源运动食品中3种氨基糖苷类抗生素的检测需求。     

Comb-shaped diblock copolystyrene for anion exchange membranes

To improve the properties of diblock copolystyrene-based anion exchange membranes (AEMs), a series of AEMs with comb-shaped quaternary ammonium (QA) architecture (QA-PS_m-b-PDVPPA_n-xC where x denotes the number of carbon atoms in different alkyl tail chains and has values of 1, 4, 8, and 10 and C denotes carbon) were designed and synthesized via subsequent quaternization reactions with three different alkyl halogens (methyl iodide and N-alkane bromines (CH₃[CH₂] _x-1Br where x = 4, 8, and 10). Compared with triblock analogues quaternized with methyl iodide in our previous research, QA-PS_m-b-PDVPPA_n-xC (x = 4, 8, and 10) AEMs are more flexible with the introduction of a long alkyl tail chain; this probably impedes crystallization of the rigid polystyrene-based main chain and induces sterically adjustable ionic association. An increase in the pendant alkyl tail chain length generally led to enhanced microphase separation of the obtained AEMs, and this was confirmed using small-angle X-ray scattering and atomic force microscopy. The highest conductivity (25.5 mS cm⁻¹) was observed for QA-PS₁₂₀-b-PDVPPA₈₀-10C (IEC = 1.94 meq g^–1) at 20 °C. Furthermore, the water uptake (<30%) and swelling ratio (<13.1%) of QA-PS_m-b-PDVPPA_n-xC AEMs are less than half of these corresponding values for their triblock counterparts. The QA-PS₁₂₀-b-PDVPPA₈₀-10C membrane retained a maximum stability that was as high as 86.8% of its initial conductivity after a 40-day test (10 M NaOH, 80 °C), and this was probably because of the steric shielding of the cationic domains that were surrounded by the longest alkyl tail chains. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47370.     

Efficient hydrogen evolution by liquid phase plasma irradiation over Sn doped ZnO/CNTs photocatalyst

In this study, the liquid phase plasma (LPP) was irradiated over pure zinc oxide (ZnO), strontium (Sn) doped ZnO, and Sn doped ZnO/CNTs photocatalysts for hydrogen evolution from pure water and from aqueous solution of water-methanol. The possible relationship between hydrogen evolution and optical emissions from LPP for activation of ZnO based photocatalysts was revealed. The role of carbon nanotubes (CNTs) as a support material for improved photocatalytic hydrogen evolution was also investigated in this study. The photocatalytic hydrogen evolution from water mixed methanol under LPP irradiation was compared with pure water splitting. The photolysis produced negligible amount of hydrogen due to minimal photodecomposition of water molecules under LPP irradiation. The plasma born reactive species also played crucial role in photolysis. However, the hydrogen evolution rate increased significantly in the presence of ZnO photocatalyst. Further improvement in hydrogen evolution rate was noticed on Sn doping of ZnO and compositing with CNTs. The highest hydrogen evolution rate of 11.46 mmh⁻¹g⁻¹ from water mixed methanol was achieved with Sn doped ZnO/CNTs photocatalyst. This hydrogen evolution rate from water-methanol solution was 9 times higher than from the splitting of pure water. This hydrogen evolution rate is attributed to excessive production of hydroxyl radicals, red shift in optical band gap of Sn doped ZnO/CNTs photocatalyst, slow electron-hole recombination and fast decomposition of methanol as sacrificial reagent.     

Hydrogenation process in multiphase alloys of Ti-Zr-Mn-V system on the example of Ti42.75Zr27Mn20.25V10 alloy

The influence of phase composition and microstructure of Ti_42.75Zr₂₇Mn_20.25V₁₀ alloy on its hydrogenation kinetic and phase composition of hydrogenated product was studied. It is established that the process of dissociation of hydrogen molecules begins on the surface of Laves phase crystallites. The dissolution of atomic hydrogen in the material volume leads to the formation of cracks in the intermetallic crystallites, which further appear as additional centers of dissociation of hydrogen molecules and noticeably accelerate the diffusion of hydrogen into the bulk material. It was shown that the Laves phase acts as a donor of atomic hydrogen for the BCC solid solution during hydrogenation of two-phase structure, initiating intensive hydrogenation of the BCC phase at room temperature.     

Liquid-phase epoxidation of propylene with molecular oxygen by chloride manganese meso-tetraphenylporphyrins

Propylene molecule owns two active sites, the direct epoxidation of propylene by dioxygen is still a challenge due to the limitation of selectivity. In this work, the direct liquid-phase propylene aerobic epoxidation protocol by chloride manganese meso-tetraphenylporphyrin (MnTPPCl) was developed. The conversion of propylene was 12.7%, and the selectivity towards PO (propylene oxide) reached up to 80.5%. The formation of PO was attributed to the mechanism via high-valent Mn species, which was confirmed by means of in situ UV–vis spectrum.     

Evolution of core–rim structures and phase transformations in infra-red transmitting Y-α-SiAlON ceramics

Core–rim structures were observed as common features in Y-α-SiAlON ceramics hot-pressed between 1550?1950 °C. We found most dopants were taken into α’-rims, and a transition layer grown first on α-cores from liquid-phase over-saturated with metal solutes. Elongated β’-grain were formed as minor phase with α’- or AlN-cores thus only after the α’ matrix had consumed up all Y solutes, revealing that the α’ → β’ transformation is controlled by the transient liquid-phase and similar defects and dangling bonds could be detected in both SiAlON phases by cathodoluminescence. Quantitative assessment of Y_m/3Si_12?(m+n)Al_m+nO_nN_16?n demonstrates the multiphase evolution, initiated by over-saturation of Y solutes at low temperatures thus retaining α-phase as cores to lower the infra-red transmittance, dictated by homogenization of Al solutes at higher temperature. The elimination of those phase boundaries leads to better dopant and sintering design for achieving transparent and high-performance SiAlON ceramics.     

Microstructure,mechanical and tribological properties of Mo–V–Cu–N coatings prepared by HIPIMS technique

A combination of high wear-resistance and low-friction is crucial for improving the wear performance of self-lubricating coatings, which is generally determined by an excellent lubricating effect and mechanical strength. In this study, the Mo–V–Cu–N coatings were prepared by HIPIMS technique with a spliced target of Mo–V–Cu at various charge voltages. The results revealed that Mo–V–Cu–N coatings presented a solid solution phase of B1–MoVN with (200) preferred orientation, and the preferred orientation was enhanced at high charge voltages. Whereas the Cu atoms formed an amorphous phase in Mo–V–Cu–N coatings due to a low Cu content of 2.3–3.6 at.%. As the charge voltage increased to 750 V, more charged metallic ions were accelerated and bombarded substrate surface efficiently, forming smooth and dense Mo–V–Cu–N coatings with a high hardness of 31.0 GPa. All the coatings presented a low friction coefficient of 0.34–0.39 due to the formation of MoO₂, VO₂ and CuO mixed oxides, and the wear mechanism was dominated by abrasive and tribo-oxidation wear at room temperature.     

利用菊池衍射花样鉴定晶体结构的方法研究

电子背散射衍射(Electron Backscatter Diffraction, EBSD)是研究材料显微结构的重要手段之一, 通过EBSD获取的菊池衍射花样是材料内部微观晶体结构的直观反映。本研究通过识别菊池花样中的对称轴, 结合晶体对称定律, 提出了一种利用菊池花样进行晶体对称性分析和晶体结构鉴定的方法。通过该方法成功对三个未知样品的对称性和晶体结构进行了判断。其中一个样品确定到所属晶系, 另两个样品锁定到部分点群, 通过确定晶系和点群排除了部分不符合对称性的相鉴定结果。研究结果表明, 利用菊池花样进行对称性分析是判断晶体结构的有效方法。同现有方法相比, 菊池衍射花样法大大缩小了相鉴定的检索范围, 显著提高了相鉴定的准确性和可靠性, 是一种有望用于新一代EBSD设备的标定技术。     

LWD仪器临界电压数据读取分析与解决

锂电池是LWD仪器正常工作的动力来源,是仪器的心脏。仪器出井后,需要在井口读取数据,当锂电池的电量接近耗尽时,会导致数据读取失败的问题。该问题处理不当,会造成长期占用井口,影响钻井时效,严重时还可能会因短路造成昂贵的LWD仪器损坏。锂电池的临界电压问题暴露了该仪器的设计缺陷,在此通过技术方法充分利用INSITE系统本身提供的功能,绕过其设计缺陷将问题解决。     

射频电缆的幅相稳定性测试研究

对射频电缆幅相稳定性进行了介绍,阐述了射频测试电缆相位和幅度变化的因素,并详细分析了射频电缆相位性能以及幅度性能的不同测试方法,最后通过实测数据的展示,总结说明了在日常测试中该如何正确使用测试电缆。