化学实验操作技能测试评分者效应研究*

基于Rasch模型对化学实验操作技能测试的评分者效应开展研究。通过对Infit、Outfit、t、怀特图和宽严度波动图等的分析,研究测试中评委的宽严度、内部一致性、外部一致性以及评委与考生间的偏差规律。得到系列减弱化学实验操作技能测试中评分者效应的建议。     

螺栓松动边界下纤维增强复合薄板的振动测试方法

提出了基于预埋压力传感器的量化测试方法,研究了螺栓松动边界对纤维增强复合薄板振动特性的影响。首先,自主设计并开发了带有预埋压力传感器的螺栓松动边界下复合薄板的振动测试系统,并详细介绍了系统各个部件的组成和功能;然后,归纳出一套合理、规范的松动边界下复合薄板的振动测试流程,并对HF10碳纤维/树脂复合薄板进行了实际测试。结果表明:随着螺栓松动程度的不断增加,复合薄板的固有频率逐渐降低,模态振型的节线位置也发生了不同程度的变化,但其阻尼结果呈现先增大后减小的趋势;而共振和非共振响应呈现先减小后增大的趋势。     

石英砂粒径对水合物沉积物力学性质的影响

利用自主研发的水合物沉积物原位合成与力学性质测试的高压低温三轴仪,通过多级加荷的试验方法,以不同粒径的砂粒作为沉积物骨架进行三轴压缩试验,得到了剪切过程的应力-应变关系曲线,以及不同粒径尺寸沉积物的强度,还有剪切过程中的体积变化关系。结果表明:含水合物沉积物强度随着沉积物粒径尺寸的增大而增强;在降压剪切过程中,所有粒径的水合物沉积物式样均有明显的剪缩现象。     

Synthesis of Heat-resistant Polymers by Thiol–Ene Reaction of N-Allylmaleimide Copolymers Using Glycoluril Crosslinkers with Rigid Molecular Structures

We carried out the thermal curing of the copolymers of N-allylmaleimide (AMI) and 2-ethylhexyl acrylate (2EHA) using 1,3,4,6-tetra(2-mercaproethyl)glycoluril ( G1 ), 1,3,4,6-tetra(3-mercaptopropyl)glycoluril ( G2 ), 1,3,4,6-tetraallylglycoluril ( G3 ), triallylisocyanurate (TAIC), and pentaerythritol tetrakis(3-mercaptobutyrate) (PEMB) as the crosslinkers. Based on the results for the analysis of thiol–ene reactions monitored by IR spectroscopy, it was confirmed that the curing rate significantly depended on the combination of the used crosslinkers. The insoluble fraction after curing was more than 90% for the systems using the glycoluril crosslinkers, while the conversion of the allyl groups was suppressed due to the rigid structure of these crosslinkers. The heat resistance and the mechanical properties of the crosslinked polymers were investigated by thermogravimetric analysis, differential scanning calorimetry, dynamic mechanical analysis, and mechanical tensile tests. For the products cured using the glycoluril crosslinkers, the glass transition temperature (T_g) and the maximum temperature of thermal decomposition (T_max) were 54–59 °C and 395–409 °C, respectively, being higher than those for the cured product prepared with PEMB and TAIC as the conventional crosslinkers. The elasticity (75–139 MPa), the maximum strength (3.0–4.1 MPa), and the adhesion strength (6.7–10.7 MPa) for the polymers cured with the glycoluril crosslinkers, determined by the mechanical tensile and single lap-shear adhesion tests, were higher than those for cured materials produced with PEMB. Thus, the thermal and mechanical properties of the maleimide copolymers were efficiently enhanced by crosslinking using the rigid glycoluril compounds. © 2020 Wiley Periodicals, Inc. J. Polym. Sci. 2020 , 58, 923–931     

Micro/Nanoengineered α-Fe2O3 Nanoaggregate Conformably Enclosed by Ultrathin N-Doped Carbon Shell for Ultrastable Lithium Storage and Insight into Phase Evolution Mechanism

The Fe-based transition metal oxides are promising anode candidates for lithium storage considering their high specific capacity, low cost, and environmental compatibility. However, the poor electron/ion conductivity and significant volume stress limit their cycle and rate performances. Furthermore, the phenomena of capacity rise and sudden decay for α-Fe₂O₃ have appeared in most reports. Here, a uniform micro/nano α-Fe₂O₃ nanoaggregate conformably enclosed in an ultrathin N-doped carbon network (denoted as M/N-α-Fe₂O₃@NC) is designed. The M/N porous balls combine the merits of secondary nanoparticles to shorten the Li⁺ transportation pathways as well as alleviating volume expansion, and primary microballs to stabilize the electrode/electrolyte interface. Furthermore, the ultrathin carbon shell favors fast electron transfer and protects the electrode from electrolyte corrosion. Therefore, the M/N-α-Fe₂O₃@NC electrode delivers an excellent reversible capacity of 901 mA h g⁻¹ with capacity retention up to 94.0 % after 200 cycles at 0.2 A g⁻¹. Notably, the capacity rise does not happen during cycling. Moreover, the lithium storage mechanism is elucidated by ex situ XRD and HRTEM experiments. It is verified that the reversible phase transformation of α↔γ occurs during the first cycle, whereas only the α-Fe₂O₃ phase is reversibly transformed during subsequent cycles. This study offers a simple and scalable strategy for the practical application of high-performance Fe₂O₃ electrodes.     

大豆脲酶诱导碳酸钙沉淀的多因素影响分析

本文探究了多个影响因素对大豆脲酶诱导碳酸钙沉淀(SICP)的影响,以优选出主要影响因素并提供其最佳范围。首先分析了脲酶浓度和温度对脲酶活性的影响;之后通过正交实验设计,进行25种工况的SICP水溶液实验,研究不同因素组合下Ca²⁺利用率的变化规律;最后借助扫描电子显微镜观测不同工况下生成碳酸钙的形态。结果表明:低温有利于脲酶的保存及活性发挥,5 ℃时脲酶活性能保持21 d以上;同一温度下,脲酶浓度越大,脲酶初始活性越高,脲酶完全失活所需时间越短。pH值、脲酶与胶结液体积比是影响Ca²⁺利用率的主要因素。为达到较高的Ca²⁺利用率,脲酶和胶结液最佳体积比为1,氯化钙与尿素最佳浓度比为1.5,Ca²⁺最佳浓度为1 mol/L。当脲酶浓度较低时生成的六面体状碳酸钙较多;随着脲酶浓度的增大,所沉淀的碳酸钙向球形转变。大豆中富含的天冬氨酸是控制碳酸钙形态的重要因素。     

A theory of finite tensile deformation of double-network hydrogels

A continuum damage model was developed to describe the finite tensile deformation of tough double-network (DN) hydrogels synthesized by polymerization of a water-soluble monomer inside a highly crosslinked rigid polyelectrolyte network. Damage evolution in DN hydrogels was characterized by performing loading-unloading tensile tests and oscillatory shear rheometry on DN hydrogels synthesized from 3-sulfopropyl acrylate potassium salt (SAPS) and acrylamide (AAm). The model can explain all the mechanical features of finite tensile deformation of DN hydrogels, including idealized Mullins effect and permanent set observed after unloading, qualitatively and quantitatively. The constitutive equation can describe the finite elasto-plastic tensile behavior of DN hydrogels without resorting to a yield function. It was showed that tensile mechanics of DN hydrogels in the model is controlled by two material parameters which are related to the elastic moduli of first and second networks. In effect, the ratio of these two parameters is a dimensionless number that controls the behavior of material. The model can capture the stable branch of material response during neck propagation where engineering stress becomes constant. Consistent with experimental data, by increasing the elastic modulus of the second network the finite tensile behavior of the DN hydrogel changes from necking to strain hardening.     

Ensuring robustness in the quality of antibiotic susceptibility test discs for four novel antibiotics

Antibiotic susceptibility test (AST) discs are used as an in-vitro diagnostic tool to select the appropriate antibiotic to treat an infection. Generally, the concentration of the drug loaded on to the AST discs is measured by studying its activity against quality control organisms. This methodology has several limitations—it is time consuming, requires trained manpower, has a wider acceptance criteria of zone of inhibitions—causing ambiguity in judging smaller variations in drug concentration. To overcome these issues, we have developed and validated high-performance liquid chromatographic (HPLC) methods for the determination of strength of AST discs for in-house researched antibiotics, namely Levonadifloxacin/WCK 771, Nafithromycin/WCK 4873, Cefepime-Tazobactam/WCK 4282, and Cefepime-Zidebactam/WCK 5222. The drugs were extracted from the AST discs using an appropriate solvent. The developed methods are simple, accurate, precise, reproducible, rugged, and robust. They are efficient in terms of time, and can be easily conducted in a quality control laboratory during release as well as stability evaluation of AST disc. Application of HPLC methods for the determination of strength of AST discs ensures flawless quality and, consequently, a better selection of drugs to treat bacterial infections in clinics.     

A novel lipid droplets-targeting fluorescent probe based on dicyanisophorone and carbazole for Cu2+ and its application

A novel fluorescent probe, LCH , based on dicyanisophorone and carbazole, was prepared for the visual detection of Cu²⁺. The probe LCH could recognize Cu²⁺ by fluorescence quenching in EtOH/H₂O (1/4, v/v) solution, which could be easily identified under the 365 nm UV lamp, and the detection limit was as low as 0.785 μM. The recognition mechanism of probe LCH with Cu²⁺ was determined by combining ¹H NMR titration, MS, and theoretical calculations. Practical application experiments showed that probe LCH could be used to detect Cu²⁺ in the test strip experiments. Cell imaging experiments showed that the probe LCH owned good cell permeability and could be applied to the imaging of Cu²⁺ in HepG2 cells. In addition, fluorescence colocalization experiments showed that LCH could target lipid droplets. These results indicate that the probe LCH will have a good application prospect in environmental detection and clinical medicine.     

石英的顺磁中心在电子自旋共振测年中的特性及应用

沉积物的电子自旋共振测年是利用石英矿物中的顺磁中心浓度确定总辐射能量,进而推定石英矿物的埋藏年代。石英中可用于测年的顺磁中心包括E’心、Al心、Ti心和Ge心。E’心需要经过热活化后才能测年。Al心是一种电子空穴心,在低温下可观测到较强的信号值。光照可以使Al心漂白,但有残留值存在。Ti心、Ge心都是电子中心,Ti心在低温测试中可见,信号微弱。Ge心光晒退最敏感,在常温观测中可见。不同顺磁中心的形成机理不同导致它们具有不同的特性,适用于不同沉积环境中的样品测年,在冰碛物中Ge心测年更具有可行性。电子自旋共振测试时降低温度可使信号增强,Ti心在10 K和15 K时信号强度最大;Al心在20 K时信号最强。Ge心在200 K时信号明显增强。在电子自旋共振测年中可根据不同顺磁中心信号强度的变化调整测试温度获得信号的最优值。在以后的ESR测试中可以选取信号最强时的测试温度进行测试,以增强微弱信号的信噪比,有利于对复杂的信号形态的分辨确定,提高对信号强度定量的准确性。