5-(2′-苯骈噻唑偶氮)-8-氨基喹啉的合成及应用——分光光度法测定钯的新试剂

本文报道了新试剂5-(2′-苯骈噻唑偶氮)-8-氨基喹啉(BTAQ)的合成。研究了在溴化十六烷基三甲铵(CTMAB)增溶下,在弱酸性介质中它与钯的显色反应。建立了分光光度法测定微量钯的高选择性新方法,用于钯催化剂中微量钯的测定,结果满意。     

STUDY ON LONG CHAIN BRANCHING IN POLYBUTADIENES BY GPC COUPLED WITH CAPILLARY VISCOMETER

The long chain branching of polybutadienes (PB) was measured with gel permeation chroma-tography coupled to an automatically recording capillary viscometer. In this method the experimentalrelation [η] (V) was translated into the calibration curve [η] (V_R) for the monodisperse species. The curve is combined with the universal calibration so that the molecular weight distributionand an additional parameter, e.g. the average branching factor of this samples may be obtained. Longchain branching molecular weight changes with polyemerization conditions.     

马来酸二丁基锡的合成及其共聚合

马来酸二丁基锡的合成及其共聚合刘云桥金根河李福绵（北京大学化学与分子工程学院北京１００８７１）关键词马来酸二丁基锡，醋酸乙烯酯，交替共聚物，光聚合关于马来酸酐［１］，马来酰亚胺 Ｎ 取代物［２，３］与富电子烯类单体如苯乙烯，醋酸乙烯酯，乙烯基烷基醚...     

大鼠肾组织的超低温快速冷冻固定和冷冻置换研究

超低温快速冷冻固定以极高的冷冻速率（１００００Ｋ／ｓ）对生物组织进行物理固定，可使生物组织结构、组织内可溶性离子及游离性物质得到保存，使被固定后的生物组织保持最接近于原自然状态，这种样品制备方法大大优于化学制备法，因而在Ｘ－射线微分析及免疫细胞化学中得到广泛应用。生物样品超低温快速冷冻后，利用冷冻置换法，在低温下将生物组织内的结晶水缓慢置换出来，而后常规包埋切片，可获得理想的组织结构及组织内待分析成分。本文应用超低温快速冷冻固定技术及冷冻置换法对大鼠肾皮质部的快速冷冻固定及损伤进行探讨。     

Synthesis,crystal structure and ferro-magnetic interaction of a binuclear copper(II) complex with the 1,4-dinitro-2,3,5,6-tetracarboxylatobenzenic anion as bridging ligand

A binuclear complex [Cu₂(DTB)(DMF)₄(H₂O)]·2DMF (DTB = 1,4-dinitro-2,3,5,6-tetracarboxylatobenzenic anion; DMF = N,N-dimethylformamide) has been synthesized and its crystal structure determined by X-ray crystallography. In the complex Cu ion is located in a distorted square pyramidal environment with two oxygen atoms O(1) and O(3) from two carboxylate groups, another two oxygen atoms O(7) and O(8) from terminal ligands of two DMF molecules, and a fifth coordinated oxygen atom O(9) from the terminal ligand of one H₂O molecule, in which the O(8) atom is situated in the apex of the pyramid. DTB as bridging ligand coordinates two Cu ions through its four carboxylate groups. The variable-temperature magnetic susceptibility of the complex was measured in the 5–300 K range. The magnetic coupling parameter is consistent with a ferromagnetic exchange between the two copper(II) centers and the data fit a binuclear magnetic exchange model based on the Hamiltonian operator ( = -2J₁₂, ₁ = ₂= 1/2), giving the ferromagnetic coupling parameter of 2J = 1.80 cm^{- 1}. This is the first example of a tetracarboxylatobenzenic bridging complex exhibiting ferromagnetic interaction.     

Preparation of Nanoelectrode Ensembles by Assembly of Nano—Silver Colloid on Gold Surface

A novel method for preparing silver nanoelectrode ensembles(SNEEs) and gold nanoelectrode ensembles (GNEEs) has been developed. Silver colloid particles were first absorbed to the gold electrode surface to form a monolayer silver colloid. N-hexadecyl nercaptan was then assembled on the electrode to form a thoil monolayer on which hydrophilic ions cannot be transfered. The SNEEs was prepared by removing thiol from silver colloid surface through applying and AC voltage with increasing frequency at 0.20V(vs.SCE). Finally,GNEEs was obtained by immersing a SNEEs into 6 mol/L HNO3 to remove the silver colloid particles. By comparison with other methods such as template method ect., this method enjoys some advantages of lower resistance, same diameter,easy preparation,controllable size and density.     

高压下C60晶体玻璃化行为的理论研究

通过构造C_(60)分子间的相互作用，研究了在不同压力下C_(60)晶体中的取向有序结构．利用计算出来的两个取向之间的能量差和相隔势驿，研究了热平衡时取向占有几率和玻璃化转变温度的压力相关性．结果与实验符合．     

LiCoO2中锂离子固相扩散系数随循环次数的变化

The solid diffusion coefficient of lithium-ion in LiCoO₂ cathode material has been investigated by the capacity intermittent titration technique (CITT) at different voltages and at different charge/discharge cycles. By SEM, XRD and FTIR techniques, the structure of LiCoO₂ was studied before and after charge-discharge cycles, and the relationship between solid diffusion coefficient and crystal structure was further discussed. CITT results show that the value of Li⁺ solid diffusion coefficient of LiCoO₂ is about 10^-12 cm²·s^-1. During the whole charge-discharge cycles, the Li⁺ solid diffusion coefficient decreased within the voltage of 4.0～4.3 V, which is attributed to the change of the structure of LiCoO₂.     

N-(取代)对三氟甲基苯基-1,3,5-三取代吡唑-4-酰胺衍生物的合成与生物活性

设计合成10个未见文献报道的N-对三氟甲基苯基-1,3,5-三取代吡唑-4-酰胺类化合物, 其结构经元素分析, ¹H NMR, IR 确证. 初步生物活性测试结果表明, 部分化合物对水稻纹枯病、小麦赤霉病、辣椒枯萎病和马铃薯晚疫病有一定的杀菌活性.