常见饮料中痕量铝的分光光度法研究

新试剂5-溴水杨基荧光酮可在pH5.5～6.8的六次甲基四胺缓冲溶液中,与铝,溴化十六烷基吡啶形成稳定的红色三元配合物。最大吸收波长约为568nm,摩尔吸光系数高达1.7×10~5L mol~(-1)·cm~1,常见金属离子很少干扰。据此,建立了测定微量铝的方法。其线性范围为0～6μg/25ml回收率在96％～103％之间。本文测定了常见饮茶,饮料及饮水中的微量铝。     

Ferromagnetic ordering and metamagnetism in malonate bridged 3D diamond-like and honeycomb-like networks: [Cu(mal)(DMF)]n and [[Cu(mal)(0.5pyz)].H2O]n (mal = Malonate Dianion,DMF = N,N-dimethylformamide,pyz = Pyrazine)

Two three-dimensional (3D) malonate bridged networks, [Cu(mal)(DMF)](n) (1) and [[Cu(mal)(0.5pyz)].H(2)O](n) (2), have been synthesized in H(2)O-DMF solution. Compound 1 exhibits ferromagnetic ordering below 2.6 K (T(c)), and 2 displays a metamagnetic behavior below 3.2 K (T(N)).     

Rhenium-promoted diastereo- and enantioselective cyclopentannulation reactions: furans as 1,3-propene dipoles

The rhenium furan complexes TpRe(CO)(MeIm)(eta2-2-methylfuran) (1) and TpRe(CO)(MeIm)(eta2-2,5-dmethylfuran) (2) undergo Lewis acid-promoted cyclopentannulation reactions with enones and enals to generate 3-acetylcyclopentene complexes. During the reaction, a rearrangement occurs such that the alpha and beta carbons of the enone are incorporated into the new carbocycle. Treatment of these complexes with an oxidant (H2O2 or silver triflate) liberates the acetylcyclopentene. When a resolved form of the rhenium complex is used, the acetylcyclopentenes can be obtained enantioselectively.     

The grain-boundary-related optical and electrical properties in polycrystalline p-type ZnO films

Cathodoluminescence spectra and electrical properties of the N doped and N–Al codoped p-type ZnO films and the dependence of these two properties on the post-annealing were investigated. Spectral analyses show that the intensity of the green emission strongly depends on the annealing ambient and closely relates with the width of the electron depletion region at the particle boundary. The conducting type and electrical properties of N doped and N–Al codoped ZnO films are greatly affected by the annealing process. The grain boundary effect was proposed to explain the green emission behavior and the p-type conduction in polycrystalline ZnO based films.     

Fine structures of zeolite-Linde-L (LTL): surface structures, growth unit and defects

High-resolution electron microscopy (HREM) has been used to image the surface structure of nano- and micrometer-sized synthetic crystals of zeolite-Linde-L (LTL). Columnar holes and rotational, nano-sized, wheel-like defects were observed within the crystals, where the hole has a minimum size equal to that of the rotational defect. Predictions of surface structure from atomistic computer simulation concur with the observations from HREM and provide insight into the crystal growth mechanism of perfect and defective LTL. Analysis of the energetics of the formation of rotational defect structures reveals that the driving force for defect creation is thermodynamic and furthermore, the rotational defects could be created in high concentrations. Formation of a columnar hole is found to be slightly energetically unfavourable and therefore we speculate that the incidence of both rotational and nano-sized vacancy defects is strongly dependent on kinetic factors and reaction conditions. The morphology of nano- and microcrystalline LTL is contradistinct and we use insights from simulation to propose an explanation of the disparity in crystal shape.     

A study on postsplenectomy changes of serum tuftsin level using a radioimmunoassay protocol

In this article, postsplenectomy changes of serum tuftsin level were studied on both human subjects and rabbits by using a self-established radioimmunoassay protocol. Antituftsin antibodies were raised in rabbits and roosters.¹²⁵I-tuftsin was prepared through an Iodogen method. The characteristics of the RIA were satisfactory with a detecting range of 0.5–100 ug/ml and the lowest detection limit of 400ng/ml. Serum tuftsin levels of splenectomized subjects were measured and compared with control groups. The serum tuftsin level from 30 postsplenectomy human beings was 406±179 ng/ml ( ± s) while that from a control group of 40 healthy blood donors was 557±256 ng/ml; the serum tuftsin level of 10 postsplenectomy rabbits was found to be 206±75 ng/ml while that of a control group of 10 normal rabbits was 318±96 ng/ml. The results showed that serum tuftsin level decreased markedly after splenectomy.     

微分倒数示波计时电位法的研究—定量测试及滴定分析

首次利用微分倒数示波图定量测试微量金属离子并滴定分析药物，结果满意。     

Two salts of 5‐sulfosalicylic acid and 3‐aminopyridine

5‐Sulfosalicylic acid (5‐SSA) and 3‐aminopyridine (3‐APy) crystallize in the same solvent system, resulting in two kinds of 1:1 proton‐transfer organic adduct, namely 3‐aminopyridinium 3‐carboxy‐4‐hydroxybenzenesulfonate monohydrate, C₅H₇N₂⁺·C₇H₅O₆S⁻·H₂O or 3‐APy·5‐SSA·H₂O, (I), and the anhydrous adduct, C₅H₇N₂⁺·C₇H₅O₆S⁻ or 3‐APy·5‐SSA, (II). Both compounds have extensively hydrogen‐bonded three‐dimensional layered polymer structures, with interlayer homo‐ and heterogeneous π–π interactions in (I) and (II), respectively.     

硫氰酸甲基三烷基季铵盐萃取Co（Ⅱ）的动力学

有关Co(Ⅱ)、Ni(Ⅱ)萃取分离的研究一直受到人们的重视。Preston报导了硫氰酸季铵盐(Q~ SCN-)萃取Co(Ⅱ)、Ni(Ⅱ)的平衡研究,认为Co(Ⅱ)的萃合物组成为Q_2Co(SCN)_4.本文用上升液滴法技术考察了Co(Ⅱ)/0.10mol·L~(-1)SO_4~(2-)/QSCN-煤油体系在298±1K条件下萃取速率R与CoSO_4、SO_4~(2-)和QSCN浓度的关系,确定了正向初始萃取速率方程,拟定了速控步骤。