Study on EPR Spectra of Three Gadolinium Complexes With Noncyclic Polyether Schiff Bases

The EPR spectra of three new gadolinium complexes with noncyclic polyether Schiff bases in powder and those of these complexes in organic solvents were investigated at different temperatures. It was observed that EPR spectra of nine and four peaks of Gd(Ⅲ) complexes in polycrystalline powder and freezing samples appeared at low temperature respectively for the first time. The interpretations of these results obtained on the basis of spin Hamiltonian of s = 7/2 system are satisfactory. The correlations of EPR feature between crystal-field strength in complexes and local symmetry around Gd3+ ions were revealed. The crystal-field parameters b20 and the asymmetry parameters λ' of complexes were estimated. A series of interesting regularity and new results were obtained.     

在活化剂邻菲罗啉存在下溴酸钾氧化胭脂红褪色催化光度法测定微量铁

基于在弱硫酸介质中及活化剂邻菲罗啉存在下 ,微量铁对溴酸钾氧化胭脂红的褪色反应有强烈的催化作用 ,由此建立了催化光度法测定微量铁的方法。该方法的检出限为 1.2× 10 - 10 g·ml- 1,测定范围为 0～ 0 .2 μg/2 5ml ,催化反应的表观活化能为 15 2 .7kJ·mol- 1。方法应用于大米、水样中微量铁的测定 ,结果满意。     

钴铬水滑石的合成及表征

采用共沉淀法合成了一系列不同Co/Cr物质的量比的碳酸根型水滑石。用X－衍射、红外光谱、差热、热重、分光光度等方法对其组成和结构进行了研究。结果表明Co/Cr投料比为2到3时能形成结晶度好、纯度高的水滑石。初步推测了部分产物的组成及所含水滑石的化学式。     

聚苯胺纳米点阵列的制备和库仑台阶现象

本文制备了PANI纳米点阵列, 利用导电原子力显微镜(C-AFM)表征了其形貌和导电性能, 在室温下观察到PANI纳米点的库仑台阶(Coulomb staircase)现象, 并利用库仑阻塞效应的理论进行了初步的分析.     

反应原料组成对单分散苯乙烯微球粒径及其分布的影响

采用分散聚合工艺制备微米级单分散聚苯乙烯微球，并对分散聚合反应的内部影响因素(分散稳定剂、助稳定剂、单体、引发剂)进行了研究．结果表明，随着分散稳定剂和助稳定剂用量的增加，聚苯乙烯微球的粒径减小；随着单体和引发剂用量的增加，聚苯乙烯微球的粒径增大．分散稳定剂和单体用量是影响聚苯乙烯微球粒径分布的两个主要内部因素．     

Synthesis and Crystal Structure of rac-N,N-Dimethyl-1- ferrocenylethylamine Hydrochloride

Ferrocene with planar chirality are of increasing importance in the synthesis of chiral ligands used in asymmetric catalysis and asymmetric synthesis.[1～3] To prepare Ugi type of chiral base, the most common method is the resolution of rac-N,N-dimethyl- 1-ferrocenylethylamine (1).     

3-氟-6-碘吡嗪-2-羧酸甲酯的合成及晶体结构

以3-氨基吡嗪-2-羧酸为原料，经酯化反应、亲电反应和重氮化反应合成了3-氟-6-碘吡嗪-2-羧酸甲酯（1），总收率62.34%，其结构经¹H NMR、¹³C NMR和MS确证，用X-单晶衍射法测定了化合物的晶体结构。结果表明：1（CCDC: 1986368）属单斜晶系，空间群C2/c，晶胞参数a=17.6566(5) Å, b=4.74850(10) Å，c=19.6368(6) Å，β=95.6540(10)°，V=1638.39(8) ų，Z=8，R_gt(F)=0.0173，wR_ref(F²)=0.0465，F(000)=1056，μ=3.885 mm^-1。      

从静态应力松弛实验求材料准松弛时间谱的一种数值计算方法

避开繁琐困难的函数求解过程，采用数值计算方法，从常规的静态应力松弛实验，直接求被测材料的松弛单元的表现松弛强度．主松弛时间τ０由单－ＭＡＸＷＥＬＬ模型求得，其他松弛时间分别约取为１０（－２）·τ０，１０（－１）·τ０，１０１·τ０，１０３·τ０。应力松弛万程取５参数模型，记为谱的强度ａｉ（或Ａｉ）通过多元线性回归，由最小二乘法确定．对一种天然橡胶试样在不同温度下的松弛曲线进行处理，回归值与原始实验值吻合良好，不同温度下的松弛单元对总松弛的贡献，反映出温度对松弛过程的活化作用．     

One Novel Vanadium-Phosphate Cluster [PV_(2.5)O_(8.5)]-3.83{H_2O} with Three-Dimensional Architecture

A novel vanadium-phosphate compound [PV_2.5O_8.5]·3.83{H_2O}(1)was obtained from the hydrothermal reac-tion and structurally characterized by elemental analysis and single-crystal X-ray diffraction,which exhibited thatthe title complex crystallized in cubic space group I-43m with crystal data:a=1.6115(1)nm,V=4.1848(1)nm~3,Z=12,D_c=1.783 g/cm~3,F(000)=2278,R_1=0.0528,and wR_2=0.1329[I>2σ(I)](all data).The basic unit of{PV_2.5O_8.5}symmetrically extended to closed sphere-like structure of{P_4V_(10)O_(34)},which was further linked to in-terleaving three-dimensional network via sharing four phosphate through μ_3-oxygen atoms around the closedsphere-like structures.     

Dienone—phenol Rearrangement of C—9 Oxygenated Decalinic Dienone and Analogs through B—Ring Cleavage

Dehydrogenation of 9-hydroxy decalinic enones and analogs with DDQ resulted in a formal dienone-phenol type rearrangement via B-ring cleavage, while the corresponding dienone acetates underwent base-catalyzed formal dienone-phenol type rearrangement analogously.