羟基新戊醛直接电氧化合成羟基新戊酸的研究

在硫酸水溶液中,以质子交换膜为隔膜,以羟基新戊醛为原料,在PbO₂电极上直接电氧化制取羟基新戊酸.研究了羟基新戊醛浓度、pH、温度及氧化电位对目标产物选择性和电流效率的影响.结果发现,pH对产物选择性和电流效率的影响最大.选择性最高可达92.6%,电流效率最高可达61.4%.用高效液相色谱分析反应过程中原料和产物的浓度变化.通过熔点、红外光谱和元素分析对分离提纯后的产物进行了表征.     

New TEA-lasers based onD′→A′ transitions in halogen monofluoride compounds: ClF (284.4 nm), BrF (354.5 nm), IF (490.8 nm)

As an outcome of a systematic study of excitation kinetics and fluorescence spectra concerning theD′(3π_2u )→A′(3π_2g ) transitions in homonuclear diatomic halogens and corresponding transitions in interhalogen molecules [1], this paper describes, for the first time, TEA laser action in the three halogen monofluorides ClF, BrF, and IF. Output energies in the mJ range were demonstrated in a fast TEA discharge arrangement at the wavelengths of 284.4, 354.5, and 490.8 nm for ClF, BrF, and IF, respectively. The results suggest parameter scalability and wavelength tunability.     

三维介孔钴酸锌立方体的制备及其优异的储锂性能

采用简易、温和、实际耐用的水热方法制备了新型三维介孔立方体结构的钴酸锌纳米材料。每个钴酸锌立方体的边长大约在3-4μm之间,并由大量的纳米粒子和密集的孔隙所构成。通过氮吸附/脱附手段测试发现所制备的钴酸锌纳米材料具有较大的比表面积(41.4 m2?g~(-1))和介孔(6.32 nm)特性。使用钴酸锌纳米材料作为锂离子电池负极,金属锂作为正极组装锂电池并测试了材料的储锂性能。研究发现该电极材料在较高的电流密度下循环100周后,仍能呈现较高的可逆容量和超强的循环稳定性。这种优异的储锂性能主要归因于钴酸锌纳米材料的新型结构,这种介孔立方体结构能够加速锂离子的扩散,增加电极与电解液的接触面积并缓解锂离子嵌入/嵌出期间产生的体积膨胀。     

咔唑-N，S-杂冠醚类荧光探针的合成及其检测Ag+性质

以双(2?氯乙基)氨基甲酸叔丁酯、2,2?(乙烷?1,2?二丁基(氧基))二乙硫醇和N?乙基咔唑为起始原料,设计、合成了一种含有杂冠醚基团的新型荧光探针分子L,其结构经¹H NMR、¹³C NMR及高分辨质谱进行了表征。随后利用荧光光谱在水/乙醇溶剂(4∶1,V/V)中研究了探针L对Ag⁺的选择性识别。研究结果表明,探针L与Ag⁺以1∶1的比例配位。通过计算得到配位常数K_a为2.01×10⁵ L·mol^-1,检测限为4.13μmol·L^-1。通过实验证明,该探针分子可应用于河流等环境水样中Ag⁺的检测。     

弹性大变形问题中的应力状态描述、奇异性问题和余能原理

对弹性大变形理论中的3方面问题进行了综述.首先,对各种应变度量的共轭应力进行综述.大变形问题引起的应力状态描述的复杂性引起了许多学者的兴趣,对这个问题的研究也促进了大变形弹性理论的发展.在各种特定问题中,人们提出了不同的应力张量来描述应力状态,如Caucby应力张量、第一类和第一二类Piola-Kirchhoff应力张...     

多态系统部件维修成本评估分析

多态系统是可靠性理论中的一种重要系统,是指部件和系统具有多个状态。随着部件的劣化,系统的性能随之下降。为了提高系统的性能,部件需要进行一定的维修。本文考虑部件状态转移率与停留时间的关系,利用重要度理论来分析部件维修成本的变化规律,得出对系统维修成本影响最大的部件。首先,基于维修成本的函数关系,给出了重要度的表达式;其次,针对典型串联系统和并联系统,随着时间推移,给出维修成本的变化规律;最后算例仿真验证了提出方法的有效性和正确性。     

微波辐射条件下混合溶剂体系中AlPO4-5分子筛的晶貌控制

在微波辐射条件下于混合溶剂体系中实现了AlPO4-5分子筛晶体的形貌控制. 实验结果表明, AlPO4-5分子筛晶体的长径比(c/a)随体系中乙二醇与水体积比的增大而减小, 其长径比可以在1.7~6.3之间调变. 当在体系中加入晶种诱导时, 产物晶粒的大小随加入晶种量的增加和诱导时间的延长而明显减小. 在正丁醇与水的混合体系中, 当正丁醇与水的体积比达到5∶1时, 可以形成哑铃形的特殊晶貌.     

Highly Efficient Circularly Polarized Luminescence from Chiral Au13 Clusters Stabilized by Enantiopure Monodentate NHC Ligands

Chiral Au nanoclusters have promising application prospects in chiral sensing, asymmetric catalysis, and chiroptics. However, enantiopure superatomic homogold clusters with crystallographic structures emitting bright circularly polarized luminescence (CPL) remain challenging. In this study, we designed chiral N-heterocyclic carbenes (NHCs), and for the first time enantioselectively synthesized a pair of monovalent cationic superatomic Au₁₃ clusters. This new enantiomeric pair of clusters has a quasi-C₂ symmetric core and exhibited CPL with an unprecedent solution-state quantum yield (QY) of 61 % among those of the atomically precise Au nanoclusters. DFT calculations provided insights into the circular dichroism behavior, and revealed the origin of CPL from superatomic Au clusters. This work opens a new avenue for developing novel homochiral nanoclusters using chiral NHC ligands and provides fundamental understanding of the origin of the chiroptics of metal clusters.     

阿莫西林的荷移光谱测定方法研究

在丙酮介质中阿莫西林与 7,7,8,8-四氰基对二次甲基苯醌 (TCNQ)荷移反应 ,形成 1∶ 1络合物 ,在74 4nm和 84 5 nm处有较强光吸收 ,表观摩尔吸光系数分别为 1.2× 10 4L· mol-1· cm-1和 1.8× 10 4L·mol-1· cm-1,阿莫西林的浓度在 10— 15 0 mg· L-1范围内符合比耳定律。在乙醇介质中 ,阿莫西林与对苯醌 (p- BQ)反应 ,形成 1∶ 1络合物 ,最大吸收波长为 4 80 nm,表观摩尔吸光系数为 1.92× 10 3 L· mol-1·cm-1。阿莫西林的浓度在 2 0— 2 0 0 mg·L-1范围内符合比耳定律。两种方法相对标准偏差分别为 1.2 %和1.5 % (n=8) ,用于测定阿莫西林制剂的含量 ,结果与标准方法一致。     

Study on parameters influencing analytical performance of laser-induced breakdown spectroscopy

Lens-to-sample distances, delay time, atmospheric condition, laser pulse energy, etc. had obvious effects on the analytical performance of laser-induced breakdown spectroscopy. In this paper, these parameters are investigated in greater detail and we will explain how they have influences on the analytical performance. The results show that the focal plane under the sample surface can improve precision and detection limit, and the delay time should be decided according to sensitivity and accuracy. Spectral line intensity is stronger in argon than helium, nitrogen and air gas environment. Pulse energy should exceed energy threshold (about 50 mJ) which can generate plasma, and the energy should not exceed about 300 mJ to avoid plasma shielding. Under optimum parameters, concentration relative standard deviation of C, Si, Mn, P, S, Ni, and Cr for low-alloyed steel (sample number 11278) which were measured 11 times is 2.37%, 2.18%, 2.23%, 7.8%, 9.34%, 1.92%, and 2.13%, respectively. And the detection limit of C, Si, Mn, P, S, Ni, and Cr for pure steel is 0.0045%, 0.0072%, 0.0069%, 0.0027%, 0.0024%, 0.0047%, and 0.0024%, respectively.