锡苯和铅苯二聚反应的理论研究

采用密度泛函理论B3LYP方法,研究了锡苯和铅苯的[2+2],[4+2]及[4+4]二聚反应的微观机理和势能剖面,考察了Sn(Pb)原子上的2,4,6-三甲基苯基(Mes)取代基对反应势能剖面的影响.研究结果表明,所有反应均为协同过程,且大多数情况下,2个C—Sn(Pb)键同步形成.[2+2]和[4+2]反应在热力学和动力学上均比相应的[4+4]反应容易进行,而[4+2]反应在动力学上比相应的[2+2]反应有利.Sn(Pb)原子上的Mes取代基在热力学和动力学上均不利于反应的进行.铅苯的动力学稳定性与锡苯相当,但其热力学稳定性高于锡苯.     

扩宽OMA-Ⅵ同时谱宽的新方法

OMA－Ⅵ存在同时谱宽窄的缺点，本文用一种新方法大幅度地扩宽了它的同时谱宽，且不降低其系统分辨率，应用效果甚佳。     

Fe(Ⅲ)-磺基水杨酸-甲基紫-聚乙烯醇体系光度法测定痕量铁

提出了在聚乙烯醇存在下,Fe(Ⅲ)-磺基水杨酸-甲基紫三元配合物光度法测定Fe(Ⅲ)的方法.该法灵敏度高(ε=3.44×105L@mol-1@cm-1),选择性及精密度均好,用于水中痕量铁的测定,结果满意.     

Crystal Structures of Two Potential Tumor Imaging Agents and Therapeutic Agents Copper（Ⅱ） Ternary Complexes with Salicylidene-tyrosinato Schiff Base and Nitrogen-donor Chelating Lewis Base

The crystal structures of two potential tumor imaging agents and therapeutic agents -copper(Ⅱ) complexes with salicylidene-tyrosinato Schiff base and nitrogen-donor chelating Lewis base, [Cu(sal-tyr)(bipy)] 1 and [Cu(sal-tyr)(phen)]2CH3OH 2 are presented. Our work is helpful to get deep understanding of novel 64Cu tumor imaging agents and therapeutic agents.     

示波极谱法测定保健药品中的褪黑激素

褪黑激素与HNO3在室温下发生硝基化反应生成褪黑激素的硝基化合物,加NH3·H2O终止反应并用甲酸 甲酸钠缓冲液控制反应液pH3,在原点电位-0.20V(vs.SCE),测量-0.50V处的二阶导数峰高。方法检出限为1μg/L,线性范围为1μg/L～200μg/L,相对标准偏差为2.6%～8.0%,加标回收率为92 0%～110 0%,测定结果与高效液相色谱法进行比较,无显著性差异。     

Effects of Substrate Temperature on Helium Content and Microstructure of Nanocrystalline Titanium Films

Helium-charged nanocrystalline titanium films have been deposited by HeAr magnetron co-sputtering. The effects of substrate temperature on the helium content and microstructure of the nanocrystalline titanium films have been studied. The results indicate that helium atoms with a high concentration are evenly incorporated in the deposited titanium films. When the substrate temperature increases from 60℃ to 350℃ while the other deposition＇parameters are fixed, the helium content decreases gradually from 38.6 at.% to 9.2at.%, which proves that nanocrystalline Ti films have a great helium storage capacity. The 20 angle of the Bragg peak of （002） crystal planes of the He-charged Ti film shifts to a lower angle and that of （100） crystal plane is unchanged as compared with that of the pure Ti film, which indicates that the lattice parameter c increases and a keeps at the primitive value. The grain refining and helium damage result in the diffraction peak broadening.     

催化动力学光度法测定痕量铝

痕量铝在硝酸介质中能催化加速过氧化氢和高碘酸钾与二甲苯胺兰FF之间的褪色反应。研究了反应的最佳实验条件,建立了测定痕量铝的新方法。方法检出限为6.1×10-10gAl3+/mL,检测范围为0-1.0μgAl3+/25mL。本方法具有高灵敏度,选择性较好,操作简便,快速的特点。用以测定水样中的痕量铝,获得满意结果。     

光度法测定冶金用五氧化二钒中磷

利用光度法测定磷的研究已有报道[1] ,但主要是针对岩石、矿石及污水中的磷 ,对冶金用五氧化二钒中磷的测定很少 ,由于冶金用五氧化二钒产品呈片状 ,采用酸溶方法溶解不完全 ,只能用碱熔方法。冶金用五氧化二钒中磷的测定存在基体效应现象 ,本文采用标准中加入基体的方法予以克服 ,通过对测定波长、酸度、显色剂用量、显色时间等条件的优化选择 ,方法的精密度达到 2 7% ,平均回收率达到10 0 .5 %。能满足冶金用五氧化二钒中磷的测定。1　试验部分1.1　仪器与主要试剂UV75 5B型紫外可见分光光度计过硫酸铵溶液 :30 0g·L- 1钼酸铵溶液 :5 …