水杨醛亚胺镍/MMAO催化降冰片烯加成聚合

用水杨醛亚胺镍 / MMAO催化降冰片烯聚合获得了热稳定、高分子量、可溶性的加成聚合产物 . Al、Ni摩尔比、单体浓度、反应温度与时间对催化剂的活性和聚合物分子量均有较大影响 .在优化条件下 ,催化剂的活性达 1 3 t/ (mol· h) ,聚降冰片烯的粘均分子量达 1× 1 0 6.

Simultaneous determination of 2-aminothiazole, 2-aminobenzothiazole and 2-mercaptobenzothiazole by capillary electrophoresis with end-column amperometric detection

Capillary electrophoresis with amperometric detection is evaluated for the simultaneous determination of 2-aminothiazole (A), 2-amino-benzothiazole (AB), 2-mercaptobenzothiazole (AM). The cyclic voltammogram, hydrodynamic voltammogram, effect of pH, concentration of buffer and separation voltage on the separation and the detection were studied. The conditions were optimized as follows: 50 mM phosphate buffet; pH 6.0, 2s at 17.5 kV sample injection, separation at 17.5 kV, 1.2 V as detection potential. The method provided low detection limit as 0.5 mu M, 0.05 mu M and 0.01 mu M, wide linear range 2-200 mu M, 10-200 mu M and 0.025-100 mu M for A, AB, and AM, respectively. The variations in peak current and migration time for 15 consecutive injections of a standard containing 5 mu M each compound were 3.7, 2.1, and 3.9%, and 1.2, 0.8, and 1.2%, for A, AB and AM, respectively. This method was employed to analyze river water.

Syntheses and properties of thermotropic copolyesters of p-hydroxybenzoic acid

Two series of thermotropic copolyesters of p-hydroxybenzoic acid (HBA) were synthesized by direct thermal polycondensation. One comprised aromatic copolyesters from HBA, terephthalic acid, bis(4-hydroxyphenyl) ketone (BHP) and resorcinol. The other comprised semi-aromatic copolyesters from HBA, terephthalic acid, BHP and alpha,-diols with carbon atom number of 4, 6, 8, 10. The properties of the two series were characterized by polarized light microscopy, differential scanning calorimetry and wide angle X-ray diffraction. Most of the resulting copolyesters could form a nematic phase over a wide temperature range above their melting points. The effects of Variation in composition and monomer structure on the properties of copolyesters were discussed. (C) 2001 Elsevier Science Ltd. All rights reserved.

Investigation on moleculare and crystal structures of metal complexes with aminopolycarboxylic acids (VII) - Syntheses and structure determination of Na-3[Hg (I) (edta) C1] center dot 6H(2)O

In this paper we describe the moleculare and crystal structures of the Na-3[Hg( II )(edta)Cl] . 6H(2)O (edta=ethylenediamine-N,N,N',N'-tetraacetate). The crystal data are as follows: orthorhombic, a=8. 083 (2) Angstrom , b=13. 870(3) Angstrom , c=38. 617(5) Angstrom , v=4329. 4 (13) Angstrom(3) , Z=8, Dc= 1. 798 g . cm(-3), mu=5. 564 mm(-1), P(000)=2280, R=0. 0317 and R-w=0. 0731 for 3883 unique reflections. In complex, the complex anion [Hg ( II ) (edta)Cl](3-) has a seven-coordination structure like a mono-capped trigonal-prism (C-2v-MTP) in which the edta(4-) acts as a hexadentate ligand with four O atoms and two N atoms and a Cl- caps a quadrilateral face as a seventh ligand. It can be known that the Hg2+ which has a d(10) electronic structure can form a high-coordinate compound with a hexadentate ligand (edta) because it has a big ionic radius.

Synthesis of novel cyclic aryl ether thioether ketone (Sulfone) oligomers

Two kinds of macrocyclic oligomers containing aromatic sulfide linkages have been synthesized by the solution polycondensation in high yield. The cyclic compounds were characterized by H-1 and C-13 NMR, by and MALDI - TOF MS.

(NH4)(3)[PMo12O40]center dot 21H(2)O

The determination of the crystal structure of the title compound, triammonium hexatriacontaoxo(tetraoxophosphato)dodecamolybdate(3-) henicosahydrate, shows that the polyanion has a pseudo-Keggin structure with m (3) over bar m symmetry. The central PO4 group is disordered with P-O distances of 1.55 (3) Angstrom. The Mo-O distances range from 1.617 (14) to 2.414 (14) Angstrom.

Synthesis, characterization and catalytic activity for H2O2 decomposition of tetrabasic tungstovanadophosphate heteropoly rare earth element complexes with Dawson structure

Nine tetrabasic tungstovanadophosphate heteropoly rare earth element complexes with Dawson structure were synthesized. Their general molecular formulas are K15H4[Ln . (P2W16VO61)(2)] . xH(2)O(Ln = La3+, Pr3+, Nd3+, Sm3+, Eu3+, Gd3+, Dy3+, Yb3+). Their structures and properties were investigated by IR, UV, NMR, ESR, XRD, TG-DTA. The results showed that the series of complexes have the same structure as K-16[Ce(P2W17O61)(2)] . 50H(2)O. At the same time, the catalytic activity of the complexes for H2O2-decomposition was also investigated.

镧系元素Dawson结构钨钒磷四元杂多配合物的合成、表征以及对H_2O_2分解的催化活性

合成了通式为Ｋ_（１５）Ｈ_３［Ｃｅ（Ｐ_２Ｗ_（１６）ＶＯ_（６１））_２］·６１Ｈ_２Ｏ、Ｋ_（１５）Ｈ_４［Ｌｎ（Ｐ_２Ｗ_（１６）ＶＯ_（６１））_２］·ｘＨ_２Ｏ（Ｌｎ＝Ｌａ￣（３＋），Ｐｒ￣（３＋），Ｎｄ￣（３＋），Ｓｍ￣（３＋），Ｅｕ￣３＋，Ｇｄ￣（３＋），Ｄｙ￣（３＋），Ｙｂ￣（３＋））的９种镧系元素Ｄａｗｓｏｎ结构的钨钒磷四元杂多配合物，并用ＩＲ、ＵＶ、ＮＭＲ、ＥＳＲ、ＸＲＤ、ＴＧ－ＤＴＡ等对其结构和性质进行了研究。该类配合物具有与Ｋ_（１６）［Ｃｅ（Ｐ２Ｗ（１７）ＶＯ（６１））２］·５０Ｈ２Ｏ类似的结构，对Ｈ２Ｏ２分解有较高的催化活性。

BIS(ETA-HEPTYLAMMONIUM) TETRACHLOROZINCATE

The crystal structure of (C7H18N)(2)[ZnCl4] is composed of alternating layers of inorganic ions and paraffinic chains. It differs from the structures of analogous compounds that have a hydrocarbon chain containing an even number of C atoms. This may explain the odd-even effects observed in differential scanning calorimetry (DSC) measurements on these compounds.

EPITAXIAL CRYSTALLIZATION OF TRANS-1,4-POLYBUTADIENE ON HIGHLY ORIENTED ISOTACTIC POLY(PROPYLENE) FILMS

Epitaxial crystallization of trans-1,4-polybutadiene (PBD) on highly oriented isotactic poly(propylene) (iPP) has been investigated at different crystallization temperatures and rates. From electron microscopy and electron diffraction, it is confirmed that epitactic growth of the low-temperature modification (monoclinic) with microcrystals of PBD on the iPP films takes place with their chain directions about +/- 50-degrees apart. No epitaxial relationship occurs between the high-temperature modification (hexagonal) of PBD and the iPP substrate. Thermal analyses of PBD-PP layered films indicate that the epitaxy has an important effect on the formation of the high-temperature modification of PBD.

SYNTHESES AND CRYSTAL-STRUCTURES OF TRIINDENYLLANTHANIDE COMPLEXES (ETA-5-C9H7)3LN.OC4H8 (LN=ND,GD,ER)

The complexes named in the title (eta-5-C9H7)3Ln.OC4H8 (Ln = Nd, Gd, Er) were synthesized by the reaction of anhydrous lanthanide trichlorides with indenyl potassium and cyclooctadienyl potassium (1:2:1 molar ratio) in THF. The complexes were characterized by elemental analysis, infrared and H-1-NMR spectroscopy, and mass spectrometry. In addition, the crystal structures of (eta-5-C9H7)3Nd.OC4H8 (1) and (eta-5-C9H7)3Gd.OC4H8 (2) were determined by an X-ray diffraction study. Complexes 1 and 2 belong to hexagonal space group P6(3) with unit cell parameters a = b = 11.843(3), c = 10.304(4) angstrom, V = 1251.7(9) angstrom-3, D(c) = 1.49 g.cm-3, Z = 2 for 1, and a = b = 11.805(2), c = 10.236(2) angstrom, V = 1235.4(6) angstrom-3 D(c) = 1.54 g.cm-3, Z = 2 for 2. The structures were solved by Patterson and Fourier techniques and refined by least-squares to final discrepancy indices of R = 0.049, R(w) = 0.053 using 925 independent reflections with I greater-than-or-equal-to 3-sigma(I) for 1, and R = 0.023, R(w) = 0.025 using 1327 independent reflections with I greater-than-or-equal-to 3-sigma(I) for 2. Coordination numbers for Nd3+ and Gd3+ are 10; the average bond lengths Nd-O and Gd-O are 2.557(21) and 2.459(13) angstrom, respectively. The structural studies showed the complexes to have 3-fold symmetry, but the THF molecule has no such symmetry; consequently the arrangement of carbon atoms in the THF molecule are disordered.

用ESR方法研究Sn-Mo氧化物固溶体形成的机理

本文研究了Sn-Mo混合氧化物催化剂的活性与焙烧温度的关系。对Sn_(0.975)Mo_(0.025)催化剂进行了不同焙烧温度的ESR研究,跟踪观察了Sn-Mo混合氧化物固溶体随焙烧温度变化的形成过程。结果表明,焙烧温度在100—300℃之间,钼以钼酸铵微晶高度分散在氧化锡表面;300—550℃时,随温度升高钼逐渐向氧化锡体相扩散;550℃时可能形成嵌入型固溶体,催化活性最好;600℃开始形成置换型固溶体,Mo以Mo~(5+)形式取代氧化锡晶格中的Sn~(4+),此时ESR信号gzz>gxx>gyy。

LB膜修饰电极

本文对 LB 膜修饰电极特点、电化学行为及其在光电化学,电催化,传感器等方面的应用进行了综述。

The statistic inversion algorithms of water constituents for the Huanghai Sea and the East China Sea

A group of statistical algorithms are proposed for the inversion of the three major components of Case-H waters in the coastal area of the Huanghai Sea and the East China Sea. The algorithms are based on the in situ data collected in the spring of 2003 with strict quality assurance according to NASA ocean bio-optic protocols. These algorithms are the first ones with quantitative confidence that can be applied for the area. The average relative error of the inversed and in situ measured components' concentrations are: Chl-a about 37%, total suspended matter (TSM) about 25%, respectively. This preliminary result is quite satisfactory for Case-H waters, although some aspects in the model need further study. The sensitivity of the input error of 5% to remote sensing reflectance (Rrs) is also analyzed and it shows the algorithms are quite stable. The algorithms show a large difference with Tassan's local SeaWiFS algorithms for different waters, except for the Chl-a algorithm.

黄海太平洋磷虾种群生态学研究

太平洋磷虾（Euphausia pacifica Hansen）作为目前已开发利用的6种主要磷虾资源之一，广泛分布于北太平洋北部及其临近近岸海域。在黄海，太平洋磷虾是黄海海洋生态系统中大型浮游动物的优势种和重要功能群的组成种类，它还是黄海生态系统中鱼类等上层营养级生物的重要饵料。太平洋磷虾的种群组成以及数量变化会直接影响到黄海经济鱼类的资源动态，从而影响到整个黄海海洋生态系统的变化。 本论文依托国家重点基础研究发展计划项目（973-II）——“我国近海生态系统食物产出的关键过程及其可持续机理”和国家自然科学基金40306021号——“黄、东海太平洋磷虾种群补充机制研究”，在2006年4月到2007年8月的八个黄海调查航次中，通过网采固定样品和现场培养实验相结合的方法，对黄海海域太平洋磷虾的种群生态分布和补充、繁殖和发育策略、以及成体的摄食、代谢进行了较为全面、细致的研究。 种群生态分布：本文根据2006年4月（春季）和10月（秋季）两次黄海大面调查和2006年9月－2007年8月六次黄海断面调查所获得的样品，研究了太平洋磷虾在南黄海的种群生态分布和补充机制，并探讨了其生态分布与环境因子的关系。 春季，南黄海太平洋磷虾种群主要分布在33 °N－36 °N、50 m-75 m等深线之间的海域，种群总丰度（不包括卵）为152.90 ind. m-3，卵丰度非常高，成体丰度较低，仅占种群总数量的8.72%。调查海域的平均成体丰度为0.35 ind. m-3。种群组成以幼体为主，占到种群的90.85%。春季是太平洋磷虾种群补充的高峰期。秋季，种群主要分布在黄海冷水团海域，种群总丰度（不包括卵）为335.38 ind. m-3，成体丰度显著高于春季，调查海区成体的平均丰度为7.73 ind. m-3。成体和未成体以99.5%的总比例在种群中占绝对数量优势，卵和幼体都非常少。秋季太平洋磷虾种群处于稳定期。春季成体的体长显著大于秋季，春季成体全长以13-18 mm为主，而秋季成体的全长主要是9-13 mm。 春季，太平洋磷虾成体具有昼夜垂直迁移行为，白天主要停留在底层水域，夜间少部分成体会上升到中上层水域，但是大部分成体仍然停留在深层。幼体从C3期开始就具有一定昼夜垂直迁移行为，F2—F5期幼体的昼夜垂直迁移行为已经非常明显。由于从表层到底层叶绿素a浓度逐渐降低，因此，太平洋磷虾的昼夜垂直迁移行为可能与摄食有关。 太平洋磷虾成体的分布是与海水温度紧密相关，南黄海太平洋磷虾成体比较适宜生活的水温是8-16 °C。春、冬季水温较低，成体分布范围较广。夏、秋季表层水温急剧升高到20 °C以上，太平洋磷虾成体主要分布在黄海冷水团海域，丰度也达到一年中的最高值。另外，秋季在近长江口的北部海域有大量成体分布。 繁殖和发育：自2006年9月到2007年8月的一年内，在黄海进行了七个航次的太平洋磷虾现场培养产卵实验，结果表明：在南黄海，太平洋磷虾在3月—6月份都具有产卵行为，4月份达到产卵高峰期。单个雌体的最大产卵量为617 egg female-1，出现在4月份。8月、9月和12月在南黄海均未发现太平洋磷虾的产卵行为。太平洋磷虾具有二次产卵行为，并且第一次产卵量要高于第二次。太平洋磷虾的产卵行为与其干湿重紧密相关。成体干重低于5.0 mg，湿重低于26.0 mg，均不具有产卵能力。在产卵高峰期，太平洋磷虾的干湿重达到一年中的最高值。 在南黄海，太平洋磷虾的幼体发育主要遵循下面的发育途径：卵 → 无节幼体 → 后期无节幼体 → 原溞状幼体 → 溞状幼体F1（0' 7, 1' 7） → 溞状幼体F2（1' 4'' 7, 3' 1'' 7） → 溞状幼体F3（5'' 7） → 溞状幼体F4（5'' 5） → 溞状幼体F5（5'' 3） → 溞状幼体F6（5'' 1）。太平洋磷虾在15 °C下的幼体发育速度明显快于4 °C。15 °C下幼体发育到C1期只需5.6 d，而4 °C下则需要16.1 d。 摄食和代谢：2006年9、10、12月和2007年3、8月，在南黄海的五个断面调查航次中，在S1-4站进行了太平洋磷虾成体摄食实验，结果表明：太平洋磷虾在8月和9月份对水体中浮游植物的摄食率比较低，主要摄食水体中的微型浮游动物，从而由于营养级级联作用，致使水体中叶绿素a浓度升高。12月和3月，太平洋磷虾对水体中浮游植物有着很强的摄食活动，使得水体的叶绿素a浓度大量降低，当然太平洋磷虾也可能会同时摄食水体中微型浮游动物。 2006年9、12月和2007年3月，在南黄海的三个断面调查航次中，在S1-4站进行了太平洋磷虾现场耗氧率和排氨率实验，结果表明：太平洋磷虾在3月份的耗氧率是172.92 μg ind.-1 d-1，是9月份和12月份的6倍还要多。太平洋磷虾在9月和12月的耗碳率和体碳日损耗量相近，且都较低。3月份太平洋磷虾的代谢非常旺盛，体碳日损耗量达到2.70 % d-1，每日的耗碳率为62.9 µg C ind-1 d-1。9月和12月份太平洋磷虾代谢的氧氮比都较低，分别是11.3和7.0，太平洋磷虾成体的主要代谢基质是蛋白质。3月份的氧氮比为35.1，太平洋磷虾成体代谢主要以脂肪及碳水化合物为主。