流动注射在线微柱预富集火焰原子吸收光谱法测定痕量铂

研究了流动注射在线微柱分离 预富集火焰原子吸收光谱法测定痕量铂的新体系。以α 氨基吡啶树脂作预富集试剂 ,以 2mol·L-1HCl + 0 .3mol·L-1NaClO4 混合液作洗脱剂。当进样体积为 15 .2ml,洗脱液体积为 0 .2 7ml时 ,浓集效率达 30倍 ,采样频率 2 8次·h-1。该方法检出限 (3σ)5 .2 μg·L-1,RSD为 1.4 % (n =11,1μg·ml-1铂 )     

STUDY ON HIGHLY ACTIVE ZIEGLERNATTA CATALYSTS FOR POLYMERIZATION OF OLEFINS

In this paper, highly active Ziegler-Natta catalysts of MgCl_2 supported TiCl_4 for synthesis ofpolyolefins, using di-n-butyl phthalate (DNBP) as internal donor and diphenyl dimethoxyl silane(DPDMS) as external donor, have been prepared. The conditions controlling the treatment ofsupport were studied. The interactions of various components present in the catalysts and theirinfluences on catalytic performance were investigated. It is found that by using DNBP and DPDMSas internal and external donors together the polymer products with higher isotactic index can beobtained. Plausible structure model and mechanism were proposed.     

Ni的掺入对复合氧化物LaFeO3的结构及性质的影响

合成子Ｎｉ替代铁酸稀土复合氧化物ＬａＦ３１－ｘＮｉｘＯ３（ｘ＝０．１－０．６），对样品进行了ＸＲＤ、ＩＲ及Ｍｏｓｓｂａｕｅｒ谱测试，结果表明：ｘ＝０＼１，０＼２，０＼３的样品为正交相，ｘ＝０．５，０．６的样品为菱方相；伴随相结构从正交向菱方结构的转变，ＩＲ谱上Ｆｅ（Ｎｉ）－Ｏ键伸振动谱带向高频移动近２０ｃｍ＾－１，Ｍｏｓｓｂａｕｅｒ谱测试表明Ｆｅ均处于＋３自旋态，Ｎｉ离子以＋３价进入晶格。     

托里贝母中新生物碱的结构研究

托里贝母产于中国西北的新疆,我们从其鳞茎中分得五个生物碱成分, 其中一个新生物碱名为托贝辛, 另外四个已知成分为西贝素, 茄次碱, Delavinone和Tortifoline.它们的结构由IR, MS, ^1H NMR 和 ^1^3C NMR确定.     

矿泉水中总α、总β放射性的同时测量

对常规测定矿泉水中总α及总β放射性时须在两份样品中分别操作并测量的方法作了改进，即只取一份样品，同时测量其中的总α和总β。方法的主要改进在于将矿泉水样品（1～5L，预先用少量盐酸酸化）蒸发至干，使其中放射性物质浓集于残渣中。将在100℃烘干的残渣于450℃灰化2h，冷至室温准确称得其质量。残渣中的放射性源应满足厚于有效厚度和少于最大取样量的要求。测量时间对检出限和测定的相对偏差有明显影响的因素也进行了讨论。     

Highly Enantioselective Phenylacetylene Addition to Benzaldehyde Catalyzed by Chiral Tridentate Ligand

Development of new or improved methods for the asymmetric preparation of chiral propargylic alcohols has gained considerable significance during the past years because they are useful building blocks for the synthesis of many biologically active compounds and natural products.[1] A series of chiral tridentate ligands were conveniently synthesized from amino acids with good yields (Scheme 1).[2] A preliminary study of the enantioselective alkynylation of benzaldehyde catalyzed by this chiral tridentate ligand was carried out and up to 83% ee of chiral propargyl alcohols was obtained (Table 1 ). A further investigation of the tridentate ligand is currently underway.     

Characterization of Nested Hollow Inorganic Fullerene-like Tungsten Disulfide Nanoparticles Prepared by Solid-Gas Reaction

Non-carbon inorganic fullerene-like(IF) nanoscale materials have recently attracted intense interest due to their nested hollow and nanotube structures,In this letter,IF-WS2 nanoparticles prepared by solid-gas reaction were characterized by X-ray diffraction,Scanning electron microscopy and transmission electron microscopy.The results show that the IF-WS2 nanoparticles have a nested hollow closed spherical structure with diameter of 100-150mm.     

Synthesis and Crystal Structure of 1,7,7-Trimethyl- 4-（4-methoxyphenyl）-4,6,7,8-tetrahydroquinoline- 2,5（1H,3H）-diones under Microwave Irradiation

1 INTRODUCTION Various quinolone derivatives are known to dis- play interesting biological properties ranging from microbial activity to cytotoxicity[1]. They have been reported as antiviral (HIV-1)[2] and antitumor agents[3] as well as used as tubulin[4], topoisomerase[5] and thrombocyte inhibitors[6]. As a member of the quino- lone family, substituted N-phenyl-2-quinolones re-present the structural basis of many biologically active compounds, such as protein kinase inhibitors, immunodu…     

甲醇在Au(111)表面吸附的密度泛函研究

 采用基于第一性原理的密度泛函理论和周期平板模型相结合的方法,对CH3OH分子在Au(111)表面top, fcc, hcp和bridge位的吸附模型进行了构型优化、能量计算以及Mulliken布居分析,结果表明top位是较有利的吸附位. 吸附的CH3OH解离产生甲氧基CH3O和H, 对它们在Au(111)面的吸附进行的计算表明, bridge和fcc位分别是二者的最佳吸附位. 对过渡态的计算给出了CH3OH在Au表面解离吸附的可能机理: 首先发生 O-H 键的断裂,继而生成甲氧基中间体.     

生物可降解聚丁二酸/苯基丁二酸丁二醇酯系列共聚物的合成及其结晶行为

合成了一系列聚丁二酸/苯基丁二酸丁二醇共聚酯(PBSBS),利用DSC、1H-NMR和X射线等测试手段对共聚物组成、热力学性能、结晶性能、等温结晶行为进行了表征和研究.结果表明,含苯基的共聚单元的引入显著改变了聚丁二酸丁二醇酯(PBS)的热力学性能4,利用Hoffman-Week曲线得到的共聚物平衡熔点随共聚组分含量的增加显著降低,玻璃化转变温度则明显升高,结晶熔点符合无规共聚物的Flory方程.此外,利用Avrami方程对均聚物PBS以及共聚物PBSBS-10分别进行了等温结晶行为研究,结果表明共聚使结晶速率降低,PBS和PBSBS-10的Avrami指数分别介于2.8~3.0和2.7~2.9之间,结晶方式为三维生长异相成核,X射线测试结果表明共聚不影响晶体结构.