磷含量对NiMo/γ-Al_2O_3催化剂活性相结构的影响

采用程序升温还原(TPR)、高分辨透射电镜(HRTEM)和X射线光电子能谱(XPS)表征手段对共浸渍法制备的不同磷含量NiMo/γ-Al2O3催化剂进行了表征,研究了磷含量对NiMo/γ-Al2O3催化剂活性相结构的影响。TPR研究表明,磷能够减少四面体配位Mo物种的数量,增加八面体配位Mo物种的数量,促进高活性Ⅱ型"Ni-Mo-S"活性相的形成。HRTEM研究表明,随磷含量的增加,MoS2颗粒堆积层数增加,催化剂的加氢选择性提高;适量磷能够增加边角位有效Mo原子的分散度(fMo),增加催化剂表面加氢脱硫(HDS)和加氢脱氮(HDN)活性位的数量。上述结论得到了XPS表征的证实:适量磷增加了催化剂表面Mo原子浓度、提高有效助剂比率(PR)和提升比率(Ni/Mo),相应催化剂表现出最高的HDS和HDN活性;但过高磷含量能够引起MoS2颗粒过度堆积,片层长度过长,导致活性位数量减少,催化活性降低。     

生物合成咖啡酸苯乙酯体系的液相色谱-串联质谱快速分析

建立液相色谱-串联质谱(LC-MS/MS)检测生物合成咖啡酸苯乙酯体系中咖啡酸(Caffeic acid,CA)和咖啡酸苯乙酯(Caffeic acid phenethylester,CAPE)的方法。采用LC-MS/MS电喷雾电离(ESI),负离子选择反应监测(SRM)模式检测。以V(乙腈)∶V(水)∶V(冰醋酸)=55∶45∶0.5为流动相,流速1.0mL/min,Hypersil C18色谱柱分离并检测生物合成咖啡酸苯乙酯体系中的咖啡酸以及咖啡酸苯乙酯的含量,并对生物合成咖啡酸苯乙酯的收率进行了动力学分析。本方法在进样量为0.2～20μg时具有良好的线性关系,咖啡酸和咖啡酸苯乙酯样品的加标回收率分别为93.4%～98.2%和90.3%～97.8%,相对标准偏差分别为1.79%～2.56%和1.82%～3.67%,咖啡酸苯乙酯收率在3d内可以达到15.54%,表明本方法简便、快速、可靠。     

钼硫碘纳米线结构特性和化学改性的理论研究

 采用第一性原理密度泛函理论研究了纳米线结构的钼硫碘材料. 结构的理论模拟结果显示, 钼硫碘纳米线机械性能很高, 且其形变过程中显示出一种特殊的磁滞现象. 形成能、投影态密度以及电荷密度的计算结果显示, 使用电负性接近硫的碳元素可对钼硫碘纳米线化学改性同时不失去其良好的结构性能和电子性能. 该结果为化学改性钼硫碘纳米线材料应用于催化提供了依据. 这些钼硫碘纳米线材料将在纳米电子学、纳米机械学、催化、纳米限域等研究中有潜在应用.     

Synthesis and Single-crystal Structure of a Silver(Ⅰ) Carboxyarylphosphonate: [Ag(H_2BCP)(4,4'-bipy)]·2H_2O

The title compound, a novel Ag(Ⅰ) carboxyarylphosphonate [Ag(H2BCP)(4,4'- bipy)]·2H2O (H3BCP = p-H2O3PCH2C6H4COOH, 4,4'-bipy = 4,4'-bipyridine), was synthesized by a hydrothermal reaction and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. It belongs to monoclinic system, space group P21/c with a = 5.7038(11), b = 22.397(4), c = 5.602(4) ?, β = 106.26(3)°, V = 1913.4(7) 3, Z = 4, C18H20N2O7PAg, Mr = 515.20, Dc = 1.788 g/cm3, μ = 1.182 mm-1, F(000) = 1040, the final R = 0.0404 and wR = 0.1216 for 4178 observed reflections with I 2σ(Ⅰ). In the structure, the Ag(Ⅰ) cations are bridged by 4,4'-bipy to give rise to 1D chains running along the b axis. These chains are linked further by the interactions of O (from BCP ligands) and Ag atoms to yield 2D layers. Hydrogen bonding interactions and weak π-π stacking interactions between 4,4'-bipy rings assemble such adjacent layers to generate a 3D supramolecular architecture.     

仪器分析理论课程教学实践与探索

仪器分析是一门实践性较强的专业基础课,其原理抽象、理论性强、内容广泛。在分析了仪器分析课程特点及实践教学中出现的问题的基础上,对该课程的教学模式及观念提出了改革措施,以激发学生学习兴趣,提高课堂教学效率,培养学生创新及实践能力。     

Solvothermal synthesis, cubic structure and multicolor upconversion emission of ultrasmall monodisperse lanthanide-doped BaYF5 nanocrystals

Lanthanide (Ln³⁺) doped BaYF₅ (Ln=Yb³⁺, Er³⁺, Tm³⁺) nanocrystals (NCs) with a mean size of approximately 10 nm are synthesized by a solvothermal method using oleic acid as a stabilizing agent at 210 °C. The size of BaYF₅ NCs can be controlled by simply tuning the reaction parameters such as reaction temperature, reaction time and the molar ratio of F⁻/Y³⁺. The detailed structure investigation reveals that the as-synthesized BaYF₅ NCs are in the cubic structure with space group Fm3¯m instead of the reported tetragonal structure. Ln³⁺ cations occupy crystal lattice positions with lower point symmetry, which may lead to high upconversion efficiency under the excitation of a 980 nm diode laser. By adjusting the dopant concentrations of Yb³⁺, Er³⁺ and Tm³⁺, intense near-infrared, blue, yellow and white upconversion emissions are readily realized, respectively. The desirable property of the ultrasmall monodisperse NCs makes it the promising material for the applications in miniaturized solid-state light sources, multicolor three-dimensional display devices and fluorescent labels for biomedicine imaging.     

A study of the active thermal control for the high energy detector on the HXMT

A thermal control system (TCS) based on the resistance heating method is designed for the High Energy Detector (HED) on the Hard X-ray Modulation Telescope (HXMT). The ground-based experiments of the active thermal control for the HED with the TCS are performed in the ambient temperature range from -15 to 20 ℃ by utilizing the pulse width to monitor the interior temperature of a NaI(Tl) crystal. Experimental results show that the NaI(Tl) crystal's interior temperature is from 17.4 to 21.7 ℃ when the temperature of the PMT shell is controlled within (20±3) ℃ with the TCS in the interesting temperature range, and the energy resolution of the HED is maintained at 16.2% @ 122 keV, only a little worse than that of 16.0% obtained at 20 ℃. The average power consumption of the TCS for the HED with a low-emissivity shell is about 4.3 W, which is consistent with the simulation.     

用于ICF驱动器的取样光栅的矢量分析与计算

 在ICF的终端光学聚焦系统中，采用取样光栅(BSG)将透射的三倍频光按一定比例送入能量计中进行能量诊断。本文采用精确耦合波矢量分析方法分析了衍射效率与光栅周期、刻槽深度、占空比等的关系，为光栅的实际制作提供了一些有意义的结果。     

电感耦合等离子体发射光谱法测定铝合金中La、Ce、Pr、Nd、Sm

利用ICP—AES仪测定稀土铝合金中微量的La、Ce、Pr、Nd、Sm。试样用酸分解,直接上机测定,对光谱干扰情况和仪器参数的选择进行了研究。实验结果和推荐值核对相符。