草酸锰分解过程的机理函数判别和动力学研究

用等温热重和线性升温热重分析法研究了草酸锰热分解过程,提出了判断其机理函数的3步判别法。经实验和理论分析证明,该反应受随机成核和晶核随后生长的过程(A_3a机理)支配,其活化能E=103.95 kJ/mol,频率因子A=4.448×10~8min~(-1).动力学补偿效应为IgA=0.09661E-1.2856     

C9‐Iridoids from Scrophularia buergeriana

Four new iridoids, buergerinins B–E ( 1 – 4 ), along with three known iridoids, were isolated from the roots of Scrophularia buergeriana. Their structures were identified on the basis of spectroscopic analysis.     

Alkylation of benzene with 1-hexene in acidic ionic liquid systems: Et3NHCl-FeCl3and Et3NHCl-AlCl3ionic liquids

Summary The alkylation of benzene with 1-hexene has been investigated in different triethylamine hydrochloride-ferric chloride (Et₃NHCl-FeCl₃) and triethylamine hydrochloride-aluminium chloride (Et₃NHCl-AlCl₃) ionic liquids. Both high catalyst activity and monoalkylation selectivity were observed for these two type of ionic liquids. Systems prepared by modification with HCl in Et₃NHCl-FeCl₃ionic liquids prove to be very suitable solvents and catalysts for the reaction. When employing Et₃NHCl-AlCl₃ionic liquids as catalysts, the reaction takes place in biphasic mode with facile catalyst separation and catalyst recycling.     

利用选择性激发核磁共振对混合物中的两种化合物进行结构解析

利用现代NMR的1D、2D技术对一个混合物进行了分析。结果表明：混合物由两种化合物组成。为了同时准确确定两种化合物的结构，本工作应用了1D-TOCSY技术，利用该技术选择性强的特点来补充常规的1D、2DHMR实验所提供的分子结构的信息。在没有进行预分离的条件下，顺利地完成了样品中两种化合物的核磁信号归属，并最终确定了它们的结构。     

α-亚甲基-γ-丁内酰胺衍生物的合成进展

α-亚甲基-γ-丁内酰胺衍生物具有细胞毒性、抗肿瘤等生理活性, 有关这些化合物的合成方法一直是人们感兴趣的课题之一。本文拟就(1)含必要官能团的开链前体的成环反应, (2)现成的γ-丁内酰胺的α-亚甲基化反应等两个方面对α-亚甲基-γ-丁内酰胺的合成方法进行综述。     

Catalytic Adsorptive Stripping Voltammetry of Germanium(IV) in the Presence of Gallic Acid and Vanadium(IV)‐EDTA

A highly sensitive and selective catalytic adsorptive cathodic striping procedure for the determination of trace germanium is presented. The method is based on adsorptive accumulation of the Ge(IV)‐gallic acid (GA) complex onto a hanging mercury drop electrode, followed by reduction of the adsorbed species. The reduction current is enhanced catalytically by addition of vanadium(IV)‐EDTA. The optimal experimental conditions include the use of 0.03 mol/L HClO₄ (pH1.6), 6.0×10^?3 mol/L GA, 3.0×10^?3 mol/L V(IV), 4.0×10^?3 mol/L EDTA, an accumulation potential of ?0.10 V(vs. Ag/AgCl), an accumulation time of 120 s and a differential pulse potential scan mode. The peak current is proportional to the concentration of Ge(IV) over the range of 3.0×10^?11 to 1.0×10^?8 mol/L and the detection limit is 2×10^?11 mol/L for a 120 s adsorption time. The relative standard deviation at 5.0×10^?10 mol/L level is 3.1%. No serious interferences were found. The method was applied to the determination of germanium in ore, mineral water and vegetable samples with satisfactory results.     

3,5-diBr-DMPAP直接光度法测定葡萄糖酸锌含量

为建立一种快速、简便、灵敏测定葡萄糖酸锌含量的方法,在非离子型表面活性剂聚氧乙烯异辛基苯基醚(TritonX-100)存在下,用2-(3,5-二溴-2-吡啶偶氮)-5-二甲氨基酚(3,5-diBr-DM-PAP)作显色剂,直接光度法测定了葡萄糖酸锌。结果表明,该法显色络合物最大吸收波长为560 nm,线性范围为0~1.5μg.mL-1,表观摩尔吸光系数为1.10×105L.mol-1.cm-1,回收率为98.7%~102.2%,具有操作快速、简便,结果灵敏可靠等优点,应用该法直接测定补锌口服液葡萄糖酸锌含量,结果满意。     

一维链状锰配位聚合物[Mn(4-CPOA)(2,2-bipy)(H_2O)]_n的合成与晶体结构(英文)

0IntroductionThe solid-state chemistry of manganese!car-boxylate coordination polymers has received growingattention over the past few years,owing to their fasci-nating network topologies and potential application inthe field of molecular magnetism and bi…     

CdS/SiO2复合材料的低频Raman散射研究

对用溶胶凝胶法制备的ＣｄＳ／ＳｉＯ２复合材料进行低频Ｒａｍａｎ散射研究，结果表明可从其低频Ｒａｍａｎ散射峰位计算出ＣｄＳ微晶的粒径，两种不同的低频振动模式由激发光的两种偏振方向加以区分，低频Ｒａｍａｎ散射射的二级散射峰根据实验结果加以指认，所得平均粒径结果与透射电镜观察结果有较好的对应关系，复合材料吸收光谱吸收边蓝移与ＣｄＳ纳米子粒径之间存在着密切的关系，实验证明，样品吸收边能量与ＣｄＳ平均粒径的     

一阶导数吸光光度法测定碘酸钾碘盐中碘

采用一阶导数吸光光度法测定碘酸钾碘盐中碘 ,线性范围为 0～ 12 μg·ml-1,检出限为1.6μg·ml-1,对盐样进行重复测定 ,相对标准偏差≤ 1.9% ,对样品进行加标回收试验 ,回收率在 97.0 %～ 10 2 .5 % ,结果良好