基于漂浮有机液滴凝固液相微萃取的黄酮类化合物分配系数及含量测定

以漂浮有机液滴凝固液相微萃取（SFODLPME）对中药中黄酮类化合物进行富集,建立SFODLPME-HPLC快速测定中药材样品中低丰度黄酮类化学成分含量的方法. 并讨论了黄酮类化合物富集倍数与浓度之间的关系、富集倍数与供相体积之间的关系,定义和阐述了EF1μg?mL-1及其物理意义,计算了漂浮有机液滴凝固相体积及黄酮类化合物的表观分配系数. 在SFODLPME的优化条件下结合高效液相色谱测得8种黄酮类成分的线性范围均为0.01~10.00μg/ml;检测限在1.0~0.01ng/mL;精密度RSD<7.0%;药材中分析物的回收率在96.0% ~104.2%. 当加入萃取溶剂体积为40μl 时,形成漂浮有机液滴凝固相体积为52±14μl;8种黄酮类成分的表观分配系数在44.8~243.9之间.     

The preparation and characterization of La doped TiO2 nanoparticles and their photocatalytic activity

In this paper, pure and La doped TiO₂ nanoparticles with different La content were prepared by a sol-gel process using Ti (OC₄H₉)₄ as raw material, and also were characterized by XRD, TG-DTA, TEM, XPS, DRS and Photoluminescence (PL) spectra. We mainly investigated the effects of calcining temperature and La content on the properties and the photocatalytic activity for degrading phenol of as-prepared TiO₂ samples, and also discussed the relationships between PL spectra and photocatalytic activity as well as the mechanisms of La doping on TiO₂ phase transformation. The results showed that La³⁺ did not enter into the crystal lattices of TiO₂ and was uniformly dispersed onto TiO₂ as the form of La₂O₃ particles with small size, which possibly made La dopant have a great inhibition on TiO₂ phase transformation; La dopant did not give rise to a new PL signal, but it could improve the intensity of PL spectra with a appropriate La content, which was possibly attributed to the increase in the content of surface oxygen vacancies and defects after doping La; La doped TiO₂ nanoparticles calcined at 600°C exhibited higher photocatalytic activity, indicating that 600°C was an appropriate calcination temperature. The order of photocatalytic activity of La doped TiO₂ samples with different La content was as following: 1>1.5>3>0.5>5>0 mol%, which was the same as the order of their PL intensity, namely, the stronger the PL intensity, the higher the photocatalytic activity, demonstrating that there were certain relationships between PL spectra and photocatalytic activity. This could be explained by the points that PL spectra mainly resulted from surface oxygen vacancies and defects during the process of PL, while surface oxygen vacancies and defects could be favorable in capturing the photoinduced electrons during the process of photocatalytic reactions.     

N-Bridged Acyclic Trimeric Poly-Cyclodiphosphazanes: Highly Tuneable Cyclodiphosphazane Building Blocks

We have synthesized a completely new family of acyclic trimeric cyclodiphosphazane compounds comprising NH, NⁱPr, N^tBu and NPh bridging groups. In addition, the first NH-bridged acyclic dimeric cyclophosphazane has been produced. The trimeric species display highly tuneable characteristics so that the distance between the terminal N(H)R moieties can be readily modulated by the steric bulk present in the bridging groups (ranging from ≈6 to ≈10 Å). Moreover, these species exhibit pronounced topological changes when a weak non-bonding NH⋅⋅⋅π aryl interaction is introduced. Finally, the NH-bridged chloride binding affinities have been calculated and benchmarked along with the existing experimental data available for monomeric cyclodiphosphazanes. Our results underscore these species as promising hydrogen bond donors for supramolecular host–guest applications.     

Terbium and holmium trans-2,3-dimethylacrylic acid complexes with 1,10-phenanthroline

Novel dinuclear complexes, [REL₃(phen)]₂ (where RE = Tb, Ho; HL = trans-2,3-dimethylacrylic acid; phen = 1,10-phenantheoline), were synthesized and determined by elemental analysis, infrared absorption spectra (IR), thermogravimetric analysis (TGA), and X-ray diffraction. The Tb complex crystallizes in space group P2_1/n with the cell dimensions a = 12.939(2) Å, b = 13.018(2) Å, c = 15.400(3) Å and = 94.72(1)°. The Ho complex crystallizes in P ⁽⁹⁾ with a = 12.406(3) Å, b = 13.280(3) Å, c = 9.823(2) Å, = 110.80(2)°, = 103.42(2)°, = 63.67(1)°. The Tb atom is nine coordinate and the separation of Tb...Tb* is 3.97 Å. The Ho atom is eight coordinate and the separation of Ho...Ho* is 4.01 Å.     

垃圾渗出液中微量蒽的高效液相色谱法测定

用反相高效液相色谱法定量测定垃圾渗出液中微量的蒽，线性范围为1－100mg/L，最小检测质量浓度为0．05mg/L，实际样品分析相对标准偏差为3．1％（n＝3），回收率90％－105％，结果令人满意。     

Preparation,characterization and catalytic behavior of hierachically porous CuO/α-Fe_2O_3/SiO_2 composite material for CO and o-DCB oxidation

Hierachically porous (HP) CuO/α-Fe2O3/SiO2 composite material was fabricated by sol-gel method and multi-hydrothermal processes using HP-SiO2 as support.The resulting material was characterized by N2 adsorption-desorption,X-ray diffraction and scanning electron microscopy.The as-prepared CuO/Fe2O3/HP-SiO2 sample,with α-Fe2O3 and CuO nanocrystals,possessed a co-continuous skeleton,through-macroporous and mesoporous structure.Its catalytic behavior for CO and o-DCB oxidation was investigated.The result showed that CuO/Fe2O3/HP-SiO2 catalyst exhibited high catalytic activity for both CO and o-DCB oxidation,indicating its potential application in combined abatement of CO and chlorinated volatile organic compounds.     

聚酰亚胺/铜纳米颗粒复合物的分子动力学模拟研究

通过分子动力学模拟对聚酰亚胺/铜纳米颗粒复合物的形态结构、 热力学性质、力学特性进行计算, 分析其随模拟温度和纳米颗粒尺寸的变化规律. 模拟结果表明, 聚酰亚胺/铜纳米颗粒复合物为各向同性的无定形态结构, 铜纳米颗粒与聚酰亚胺基体之间通过较强的范德华作用结合在一起使结构更加稳定, 铜纳米颗粒表面多个原子层呈现无定形状态, 在铜颗粒和聚酰亚胺基体之间形成界面层, 界面区域随颗粒尺寸和温度的增加分别减小和增加. 聚酰亚胺/铜纳米颗粒复合物的等容热容随着颗粒尺寸增大而明显增高, 随温度变化比聚酰亚胺体系更为缓慢, 在较低温度下较小颗粒尺寸复合物的热容比聚酰亚胺体系更低. 聚酰亚胺/铜纳米颗粒复合物的热压力系数随颗粒尺寸增加而显著增大, 比聚酰亚胺体系的热压力系数更小, 且随温度升高而减小的程度要小得多. 聚酰亚胺/铜纳米颗粒复合物的热力学性质表现出明显的尺度效应, 温度稳定性明显高于聚酰亚胺体系. 聚酰亚胺/铜纳米颗粒复合物的力学特性表现出各向同性材料的弹性常数张量, 具有比聚酰亚胺体系更低的杨氏模量和泊松比, 随温度升高分别减小和增大, 与聚酰亚胺体系随温度的变化趋势相反, 且杨氏模量的温度稳定性显著提高, 同时泊松比随纳米颗粒尺寸增大而减小, 具有明显的尺度效应. 加入铜纳米颗粒形成复合物可获得与聚酰亚胺体系显著不同的力学新特性. 关键词： 分子动力学模拟 聚合物纳米复合物 聚酰亚胺 纳米颗粒     

CSNS加速器真空控制系统的设计与实现

中国散裂中子源（CSNS）加速器真空控制系统负责真空数据采集、设备监控和闸板阀控制与联锁,是设备运行和故障诊断以及超高真空保持的重要保障。本文介绍了加速器真空需求,基于实验物理及工业控制系统EPICS软件框架的真空控制系统设计与实现,使用横河可编程逻辑控制器PLC控制与联锁设备,摩莎MOXA工控机监测真空状态,EPICS PV数据直接进入声音报警系统和历史数据库系统,为工作人员及时发现和处理问题、进行后续数据分析和机器研究等提供了便捷途径和可靠保障。目前,该系统已完成现场安装和调试,并已正式投入运行。运行结果表明,该系统具有稳定性好、可靠性高、人机交互友好的特点,很好地满足了加速器真空控制系统运行的需要。