顺磁性聚酯金属配合物的合成及其驰豫性能的研究

本文通过二乙三胺五乙酸（ＤＴＰＡ）或乙二胺四乙酸（ＥＤＴＡ）的双酸酐与二元醇或二元酚进行聚合反应，制备了两个系列共１５种新的聚酯型大分子配体及其顺磁性金属配合物，用核磁、红外光谱以及元素分析表征了配体和配合物的结构。初步试验结果表明，与相应的小分子金属配合物相比，聚酯金属配合物具有较高的弛豫性能。     

不同介质凝胶体系中草酸钙结晶的研究

研究了五种不同介质（水、氯化钠、合成尿、正常人尿液和尿石患者尿液）的凝胶体系中草酸钙（CaC2O4）晶体的生长,及各种体系中防石药物柠檬酸钾（K3cit）对CaC2O4生长的影响.没有加K3cit时,CaC2O4晶体以一水草酸钙（calcium oxalate monohydrate, COM）为主要物相,但在氯化钠和合成尿的凝胶体系中同时出现了二水草酸钙（calcium oxalate dihydrate, COD）和三水草酸钙（calcium oxalate trihydrate, COT）,肾结石患者尿液中出现COD,而正常人尿液中没有COD和COT生成.加入K3cit后,水、氯化钠和合成尿介质的凝胶体系中,COT的含量显著增加,患者尿液中产生大量COD,而正常人尿液中出现了少量的COD和极个别的COT.COT的增加与低温、体系中高的离子强度及金属离子等因素有关.K3cit具有诱导COD和COT的生成、减小COM晶体比表面积的作用,从而有利于防治草酸钙结石的形成.     

二(三氟乙酸)氯化钕的合成及其对双烯聚合的催化活性

1976年F.Dawans在研究丁二烯定向聚合时,曾引入三氟乙酸氯化镍类型的乙醚络合物,对聚合机理作了令人满意的解释并已得到实际应用。但迄今为止,稀土催化剂作为定向聚合催化剂,在三烷基铝低用量条件下,均系非均相的三元体系。这在理论研究和实际应用上都存在一定困难。     

Complexes formed between nitrilotris(methylenephosphonic acid) and M(2+) transition metals: isostructural organic-inorganic hybrids

Nitrilotris(methylenephosphonic acid) (NTP, [N(CH(2)PO(3)H(2))(3)]) recently has been found to form three-dimensional porous structures with encapsulation of templates as well as layered and linear structures with template intercalation. It was, therefore, of interest to examine the type of organic-inorganic hybrids that would form with metal cations. Mn(II) was found to replace two of the six acid protons, while a third proton bonds to the nitrilo nitrogen, forming a zwitter ion. Two types of compounds were obtained. When the ratio of acid to Mn(II) was less than 10, a trihydrate, Mn[HN(CH(2)PO(3)H)(3)(H(2)O)(3)] (2) formed. Compound 2 is monoclinic P2(1)/c, with a = 9.283(2) A, b = 16.027(3) A, c = 9.7742(2) A, beta = 115.209(3) degrees, V = 1315.0(5) A(3), and Z = 4. The Mn atoms form zigzag chains bridged by two of the three phosphonate groups. The third phosphonate group is only involved in hydrogen bonding. The metal atoms are octahedrally coordinated with three of the sites occupied by water molecules. Adjacent chains are hydrogen-bonded to each other through POH and HN donors, and the additional participation of all the water hydrogens in H-bonding results in a corrugated sheet-like structure. Use of excess NTP at a ratio to metal of 10 to 1 yields an anhydrous compound Mn[HN(CH(2)PO(3)H)(3)] (1), P2(1)/n, a = 9.129(1) A, b = 8.408(1) A, c = 13.453(1) A, beta = 97.830(2) degrees, V = 1023.0(2) A(3), and Z = 4. Manganese is five coordinate forming a distorted square pyramid with oxygens from five different phosphonate groups. The sixth oxygen is 2.85 A from an adjacent Mn, preventing octahedral coordination. All the protonated atoms, three phosphonate oxygens and N, form moderately strong hydrogen bonds in a compact three-dimensional structure. The open-structured trihydrate forms a series of isostructural compounds with other divalent transition metal ions as well as with mixed-metal compositions. This is indicative that the hydrogen bonding controls the type of structure formed irrespective of the cation.     

Ab initio studies of small AlmFen clusters

The equilibrium geometrical structures of small Al_mFe_n clusters have been determined through ab initio calculation of the cluster total energy at the UB3LYP/Lanl2dz level. For dimers of iron and aluminum, the dissociation energies, the equilibrium atomic distances, and the vibrational frequencies were calculated. The agreement between calculations and experiments is reasonable. The ground stable geometrical structures of Fe₄, FeAl₃, Fe₃Al and Fe₂Al₂ clusters favor three-dimension configurations, but Al₄ tetramers are planar structures. The Al-rich tetramers are more stable than the other two composition tetramers. This is different from that of bulk alloys.     

Aculeoside I, a novel 18,19-seco-ursane saponin isolated from Ilex aculeolata

A novel 18,19-seco-ursane saponin, aculeoside I (1), in addition to four known saponins were isolated from the leaves of Ilex aculeolata Nakai and identified by using spectroscopic and chemical methods. The structure of the new saponin was established as 3,19-dihydroxyl-16,21-epoxy-18,19-seco-13(18)-urs-ene-28-oic-acid-19-O-alpha-L-rhamnopyranosyl-(1 --> 2)-alpha-L-arabinopyranoside.     

微波合成SrTiO3的工艺、结构与性能研究

应用微波会成这一材料合成新方法制备SrTiO3，研究了不同工艺条件下微波合成产物的结构，确定出制备纯净SrTiIO。的合成条件．对微波合成的工艺及其影响因素进行详细的探索，从合成产物的显微结构、粒度分布、比表面积、烧结性能等方面比较了微波合成与常规固相合成的差别，结果表明微波合成与各种常规方法相比有合成时间短、合成工艺简单、合成产物性能好等特点，是一种有发展潜力的材料合成技术．     

光化学-荧光分析法研究——Ⅲ.片剂及注射液中安定的测定

本文提出了测定安定的光化学—荧光分析新方法。安定在含有十二烷基硫酸钠的稀硫酸介质中,经紫外光照射后,产物能发射荧光(=368nm,=476nm)。安定浓度在0～2.5μg/ml范围内,荧光强度与浓度成良好的线性关系。方法的相对标准偏差为1.5％,检出限为0.044μg/ml,可用于片剂及注射液中安定含量的测定。