三(邻甲苯基)氢化锡与1-乙炔基环戊醇和1-乙炔基环己醇的加成物的合成及晶体结构

通过三(邻甲苯基)氢化锡与1-乙炔基环己醇和1-乙炔基环戊醇发生加成反应,得到两个加成物:(Z)-1-[2-(三-邻甲苯基锡基)乙烯基]环戊醇(1)和(Z)-1-[2-(三-邻甲苯基锡基)乙烯基]环己醇(2).通过元素分析、红外光谱和核磁共振氢谱等手段对其结构进行了表征.用X射线单晶衍射测定了加成物1和2的晶体结构.二者均为具有分子内O→Sn弱配位的扭曲四面体结构.1属于单斜晶系,P21/n空间群,晶胞参数:a=1.0496(2)nm,b=1.7658(4)nm,c=1.3193(3)nm,β=90.60(3)°,V=2.4451(8)nm3,Z=4,R=0.0317,wR=0.0820.2属于三斜晶系,空间群P1,晶胞参数:a=O.85592(17)nm,b=0.93016(19)nm,c=1.6368(3)nm;α=83.76(3)°,β=82.69(3)°,γ=78.05(3)°;V=12600(4)nm3,Z=2,R=0.0377,wR=O.1030.     

铟(Ⅲ)与桑色素共存时电化学行为的研究和分析应用 Ⅱ.桑色素及其与铟(Ⅲ)共存时电极反应过程

桑色素(H_5L),铟(Ⅲ)在盐酸-氯化钾(pH2.2～2.6)溶液中,分别以 H_4L~-及In(H_2O)_4Cl(_2~+)形态存在,但未形成缔合物,在电极表面,H_4L~-吸附诱导 In(H_2O)_4Cl(_2~+)与之形成缔合物,使 In(Ⅲ)还原电流增敏,文中提出了桑色素及其与铟(Ⅲ)共存时(pH2.4)各自的电极反应机理,对阴离子表面活性剂的增敏作用也进行了探讨。     

色谱－质谱联用法测定荧光灯中气体杂质及充气压强

］实验出一种色质联用法测定荧光灯中气体杂质及充气压强的新方法。使用两根并联色谱柱（柱1：Φ3mmi.d.×0.6m13XM.S.（分子筛60-80目；柱23mmi.d.×1.5mPorapakQ（80-100目），室温下可同时测定灯中H2，O2，N2，CH4，CO，CO2等多种气体杂质分压强。其测定下限分别为4×10-3，3×10-3，6×10-3，6×10-4，10-24×10-3Pa。并研究出了一种简易快速的破灯装置及标准气配制装置。导出了计算灯中各气体压强及杂质气浓度公式。     

Surface plasmon enhanced photoluminescence in amorphous silicon carbide films by adjusting Ag island film sizes

Ag island films with different sizes are deposited on hydrogenated amorphous silicon carbide (α-SiC:H) films, and the influences of Ag island films on the optical properties of the α-SiC:H films are investigated. Atomic force microscope images show that Ag nanoislands are formed after Ag coating, and the size of the Ag islands increases with increasing Ag deposition time. The extinction spectra indicate that two resonance absorption peaks which correspond to out-of-plane and in-plane surface plasmon modes of the Ag island films are obtained, and the resonance peak shifts toward longer wavelength with increasing Ag island size. The photoluminescence (PL) enhancement or quenching depends on the size of Ag islands, and PL enhancement by 1.6 times on the main PL band is obtained when the sputtering time is 10 min. Analyses show that the influence of surface plasmons on the PL of α-SiC:H is determined by the competition between the scattering and absorption of Ag islands, and PL enhancement is obtained when scattering is the main interaction between the Ag islands and incident light.     

Influence of substrate bias voltage on the microstructure of nc-SiOx:H film

Amorphous silicon oxide containing nanocrystalline silicon grain(nc-SiO_x:H) films are prepared by a plasmaenhanced chemical vapor deposition technique at different negative substrate bias voltages.The influence of the bias voltage applied to the substrate on the microstructure is investigated.The analysis of x-ray diffraction spectra evidences the in situ growth of nanocrystalline Si.The grain size can be well controlled by varying the substrate bias voltage,and the largest size is obtained at 60 V.Fourier transform infrared spectra studies on the microstructure evolutions of the nc-SiO_x:H films suggest that the absorption peak intensities,which are related to the defect densities,can be well controlled.It can be attributed to the fact that the negative bias voltage provides a useful way to change the energies of the particles in the deposition process,which can provide sufficient driving force for the diffusion and movement for the species on the growing surface and effectively passivate the dangling bonds.Also the larger grain size and lower band gap,which will result in better photosensitivity,can also be obtained with a moderate substrate bias voltage of 60 V.     

函数型Probit模型的sieve极大似然估计

研究函数型Probit模型的sieve极大似然估计的渐近性质.在一定的条件下,证明了估计的强相合性和渐近正态性以及该估计的非参数部分达到最优收敛速度.最后给出了一个模拟研究,表明sieve极大似然估计有较好的有限样本性质.     

含氟聚合物表面能的测算

通过测定参照液体在聚合物表面的接触角,应用Zisman,Fowkes和筏·義人提出的三种方法,测算了数种国产含氟聚合物的表面能。     

不同因素对柠檬酸浸提-硅钼蓝比色法测试土壤有效硅的影响及优化措施

准确测定土壤中有效硅含量可以了解土壤硅素肥力状况,有助于指导施肥、改善土壤质量。同时土壤中有效硅含量作为第三次全国土壤普查必测的一项参数,有利于全面摸清土壤硅的含量水平。通过改变浸提方式、浸提剂浓度以及显色方式等参数对柠檬酸浸提-硅钼蓝比色法测试土壤有效硅进行考察,对测试过程中的影响因素进行分析,并进行针对性的优化,最后对改进后的测试条件进行方法学研究。结果表明,浸提时间不足、浸提剂浓度偏低以及显色时温度不稳定均会导致所测的有效硅含量偏低。采用连续振荡2 h的方式浸提、增加浸提剂浓度为0.050 mol/L、显色过程全程于35℃水浴中操作等措施可以较好地减少误差,获得更准确的结果。改进后的方法线性良好,相关系数r为0.999 6,检出限为1.0 mg/kg,精密度RSD(n=6)最大为2%,准确度相对误差最大为-4.7%。测定结果可靠,可以为第三次全国土壤普查内业检测提供参考和借鉴。     

液相色谱法分离金属螯合物的进展

综述了用薄层液相色谱法和柱液相色谱法分离金属螯合物的进展及其在金属离子分析方面的应用。     

谈土木建筑中的热力学

本文从土木建筑的结构、构造、性能、朝向等方面进行研究分析，总结了热力学在土木建筑中的应用，说明了热力学与土木建筑密切相关．