α-B-Keggin型杂多化合物K_5H[Co_4(VW_9O_(33))_2]·5H_2O的合成和结构

合成了新化合物K_5H[Co_4(VW_9O_(33))·5H_2O,并运用IR,UV-ViS,DTA和单晶X射线衍射对其结构进行了表征.测定结果证实标题化合物具有α-B-Keggin型结构,两个(VW_9O_(33)~(7-)结构单元由四个Co(Ⅱ)O_6 八面体连接.杂多化合物属单斜晶系P2_(1/n),a=1.2307(3)nm,b=2.1250(4)nm,c=1.5817(3)nm,β=91.86(3)°,V=4.1343(14)nm~3,R=0.0895,R_w=0.2180.

Polymerization of ethylene by zirconocene-B(C6F5)(3) catalysts with aluminum compounds

Ethylene polymerization by zirconocene-B(C6F5)(3) catalysts with various aluminum compounds has been investigated. It is found that the catalytic activity depended on zirconocenes used, and especially on the type of aluminum compounds. For Et(H(4)Ind)(2)ZrCl2 (H(4)Ind : tetrahydroindenyl), the activity decreases in the following order: Me3Al > i-Bu3Al > Et3Al much greater than Et2AlCl. While for Cp2ZrCl2(Cp : cyclopentadienyl), it varies as follows: i-Bu3Al > Me3Al much greater than Et3Al. Furthermore, the activity is significantly affected by the addition mode of the catalytic components, which may imply that the formation of active centers is associated with an existing concentration of catalytic components. Results of thermal behavior of polyethylene (PE) studied by differential scanning calorimetry(DSC) show that crystallinity of the polymer prepared with Et3Al is higher than that with Me3Al or i-Bu3Al. It is also found that the number-average molecular weight ((M) over bar) of the polymers prepared with Me3Al or i-Bu3Al is much higher than that with Et3Al. H-1-NMR studies substantiate that i-Bu3Al is a more efficient alkylation agent of Cp2ZrCl2 in comparison with Me3Al. (C) 1997 John Wiley & Sons, Inc.

Study on the Property of Vitamin B-12-Modified Electrode and its Electrocatalysis for the Reduction of Oxygen

It was found that vitamin B-12 could be strongly adsorpted on the anodized glassy carbon electrode to form a vitamin Thy-modified glassy carbon electrode. The modified electrode is stable in a wide pH range. The electrochemical characteristics of the modified electrode were studied in details. In addition, it was found that the reduction of oxygen could be catalyzed by the modified electrode to form H2O2. An EC mechanism was suggested for the process, and the follow up chemical reaction might he the rate determined step.

Electrochemical studies on vitamin B-12 and its derivatives

The electrochemical studies on vitamin B-12 and its derivatives were reviewed in this paper. The importance of electrochemical studies for explaining the mechanism of B-12 coenzyme in body was discussed. The latest results of electrochemical studies on vitamin B-12 and its derivatives was reviewed. A prospect for the electrochemical studies in vitamin B-12 and its derivatives was suggested.

乙基罗丹明B－磷钼杂多酸－PVA体系超高灵敏显色反应的研究

本文详细研究了乙基罗丹明Ｂ－磷钼杂多酸－ＰＶＡ超高灵敏显色反应，提出了高灵敏测量痕量磷的新的分光光度法。缔合物的最大吸收波长位于５８４ｎｍ处，其表观摩尔吸光系数为１．３×１０￣６Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。并研究了缔合物的组成和红外光谱。本法直接用于钢样及试剂中痕量磷的测定，获得满意的结果，检测下限达６×１０￣（－７）％。

碱性染料杂多酸多元络合物显色反应的研究——IX.乙基罗丹明B-锗钼杂多酸-聚乙烯醇体系

本文研究了乙基罗丹明B-锗钼杂多酸-PVA显色体系,提出了测定痕量锗新的高灵敏分光光度法.缔合物最大吸收位于584nm,表观摩尔吸光系数ε为3.8×10~5L·mol~(-1)·cm~(-1).缔合物的组成比为Ge(Ⅳ):ERB~+=1:4.红外光谱研究表明,染料阳离子的结构未受缔合物形成的影响.本法用于人参中痕量锗的测定,得到满意结果.

Crystallization Behavior of Poly(tetrahydrofuran-b-methyl methacrylate) Diblock Copolymer

Crystallization behavior of a series of newly synthesized poly (tetrahydrofuran-b-methyl methacrylate) diblock copolymer has been studied by differential scanning calorimetry (DSC) and X-ray scattering and diffraction techniques. The results show that the

THE YELLOW-TO-BLUE INTENSITY RATION (Y/B) OF DY-3+ EMISSION

Various borates, vanadates, niobates, antimonates, titanates, zirconates and CaS doped with Dy3+ were prepared. Factors which have an effect on the yellow-to-blue intensity ratio (Y/B) of Dy3+ emission are reported. Y/B increases with decreasing Z/r or electronegativity of the next-neighbour element M in the complex oxides Dy-O-M. The greater the degree of covalency between Dy3+ and O2-, the greater Y/B is. When Dy3+ is located at a site with an inverse centre and high symmetry, Dy3+ displays no luminescence. It seems that Y/B of Dy3+ located at a site deviated from an inverse centre is greater than that of Dy3+ located at a site without an inverse centre. Y/B does not vary much with the variation in concentration of Dy3+ when Dy3+ is substituted for an element with the same valency, but it does depend on the concentration of Dy3+ when Dy3+ is substituted for an element with a different valency in the matrix, because defects are formed in this case.

THE COMPATIBILITY AND CRYSTALLIZATION OF THE MIXTURES OF POLY (TETRAHYDROFURAN-b-METHYL METHACRYLATE) DIBLOCK COPOLYMER WITH POLYVINYL CHLORIDE HOMOPOLYMER

The compatibility and crystallization behaviour of the mixtures of poly (tetrahydrofuran-methyl methacrylate) diblock copolymer (PTHF-b-PMMA) with polyvinyl chloride has been studied. We found that the compatibility of these blends, in which there is special interaction between the homopolymer and the PMMA block of the copolymer, is much better than that of the AB/A type blends; and that the crystallization rate and crystallinity of PTHF microdomain changed greatly due to the swollen by PVC homopolymer. In this paper, these changes in cryatallization are well explained according to the theories of block copolymer blends and the density gradient model presented by JIANG Ming.

碱性染料杂多酸多元络合物显色反应的研究Ⅷ.乙基罗丹明B分光光度法同时测定痕量磷和砷

本文利用乙基罗丹明B(ERB)和磷钼酸(PMo)或砷钼酸(AsMo)缔合物吸光度具有加和的特性,建立了在同一显色条件下,用ERB同时测定痕量磷和砷的水相光度法,方法具有灵敏、简便和快速的优点,已成功地用于钢和试剂中痕量磷和砷的同时测定,试剂中磷和砷的测定下限分别为2×10~(-6)％(1g)和5×10~(-6)％(1g)。

高灵敏分光光度法测定食品中痕量硒——硫氰酸盐-罗丹明B-Tween20体系

本文研究了Se(Ⅳ)-SCN-RhB-吐温20高灵敏显色反应体系。Se(Ⅳ)与SCN~-和RhB~+形成三元离子缔合物,并吸附了染料琉氰酸盐,表观摩尔吸光系数2.0×10~6L·mol~(-1).cm~(-1),是碱性染料类分光光度法中最灵敏的。Se含量在0～2μg/25ml范围内遵从比尔定律。利用巯基棉分离干扰离子,选择性高。测定了食品中总硒,结果满意。

PTHF-b-PMMA/PVC共混体系的相容性和结晶行为

研究了具有焓效应的聚四氢呋喃-聚甲基丙烯酸甲酯两嵌段共聚物与聚氯乙烯PTHF-b-PMMA/PVC)共混体系的相容性和结晶行为.结果表明,其相容性比AB/A 型嵌段共聚物共混体系的相容性要好得多;与PTHF 部分相容的PVC 对PTHF 微区的结晶行为可产生很大的影响.应用有关理论和模型很好地解释了结晶行为的这种变化.

ELECTROCATALYTIC OXIDATION AND FLOW DETECTION OF HYDRAZINE COMPOUNDS IN LIQUID-CHROMATOGRAPHY AT A VITAMIN-B-12 ADSORBED GLASSY-CARBON ELECTRODE

A vitamin B-12 chemically modified electrode (CME) was constructed by adsorption of vitamin B-12 onto a glassy carbon surface. The electrode catalyzes the electrooxidation of hydrazine compounds over a wide pH range. The electrocatalytic behavior of hydrazines is elucidated with respect to the CME preparation conditions, solution pH, operating potential, mobile phase flow rate, and other variables. When applied to liquid chromatographic detection of the analytes, the vitamin B-12 CME yielded a linear response range over 2 orders of magnitude, and detection limits at the picomole level. The vitamin B-12 CME offers acceptable catalytic stability in both batch and flow systems.

RELATIONSHIP BETWEEN CRYSTALLIZATION OF THE PDMS BLOCK AND MORPHOLOGY OF POLY(BUTADIENE-B-DIMETHYLSILOXANE)

Studies using transmission electron microscopy, differential scanning calorimetry, and X-ray diffraction showed correlations between the crystallization behavior of the polydimethylsiloxane (PDMS) block and the morphology of the block copolymer poly (butadiene-b-dimethylsiloxane) (PB-PDMS). When the PDMS component existed as spheres dispersed in a PB matrix, the crystallization rate of the PDMS block was lower than when the PDMS phase existed in rod or cylinder form.

超高灵敏显色反应及其应用的研究Ⅷ.铅-乙基罗丹明B-碘化物体系

本文研究了在聚乙稀醇-阿拉伯胶共存下,乙基罗丹明B和PbI_4~(2-)的超高灵敏显色反应并制定了新的光度法。缔合物最大吸收为605nm,ε值为1.0×10~6·L·mol~(-1)·cm~(-1)。经巯基棉分离、富集,本法成功地用于硫酸镁、硫酸锌和硫酸亚铁铵等试剂中痕量铅的测定。