Crystal Structure and Characterization of a Large Polyoxotungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2O

The heteropolytungstate (NH4)₂₁{La(H₂O)₅[Ni(H₂O)]₂As₄W₄₀O₁₄₀}·53H₂O is obtained by the reaction of Na₂₇[NaAs₄W₄₀O₁₄₀]· 60H₂O with NiCl₂·6H₂O, La(NO₃)₃·6H₂O and NH₄Cl at pH‐4.5. The structure and chemical composition are determined by X‐ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are a = 1.9551(3) nm, b = 2.4156(4) nm, c= 3.7068(6) nm, β = 91.505(3)°, V = 17.500 (5) nm³, monoclinic crystal system with space group P2₁/n, Z = 4, R₁ = 0.0573, wR₂ = 0.0717 [I >2<s?(I)], R₁, = 0.2463 and wR₂ = 0.1199 (all data). [La(H₂O)₅] {Ni(H₂O)}₂AS₄W₄₀O₁₄₀ has C₂, symmetry. IR spectra of the ligand [NaAs₄W₄₀O₁₄₀]^27‐ and its three complexes were discussed.     

Synthesis of polypiperazine-amide thin-film membrane on PPESK hollow fiber UF membrane

A new interfacial polymerization (IP) procedure is developed in order to synthesize polypiperazine-amide thin-film membrane on the inner surface of poly(phthalazinone ether sulfone ketone) (PPESK) hollow fiber ultrafiltration (UF) membrane.A hollow fiber composite membrane with good performance was prepared and studied by FT-IR and scanning electron microscopy.     

C9‐Iridoids from Scrophularia buergeriana

Four new iridoids, buergerinins B–E ( 1 – 4 ), along with three known iridoids, were isolated from the roots of Scrophularia buergeriana. Their structures were identified on the basis of spectroscopic analysis.     

An Efficient Synthesis of Pyrazolo[3,4‐b]Pyridine Derivatives in Aqueous Media

A series of pyrazolo[3,4‐b]pyridines was synthesized by the reaction of 5‐aminopyrazole with benzylidenemalononitrile in aqueous media. The structures were characterized by IR, ¹H NMR, and elemental analysis and were further confirmed by X‐ray diffraction analysis.     

混合模式硅胶基质毛细管电色谱整体柱的制备及其电色谱性能研究

采用温和条件下的溶胶-凝胶技术,成功制备了阴离子交换-反相混合模式硅胶基质毛细管电色谱整体柱.通过调整反应液中不同前体的比例,优化了整体柱的制备条件.通过扫瞄电镜,对柱床进行了表征和分析.实验发现,所制备的整体柱电渗流的方向和大小可随流动相pH值的改变而改变,在酸性和中性条件下,具有从阴极流向阳极的电渗流;当流动相pH值升至约7.5时,电渗流方向发生了反转(由阳极流向阴极).在优化的实验条件下,用所制备的整体柱对所考察的酸性(中性)化合物实现了快速分离,并获得了高达160,000 N/m的柱效.     

A New Asterosaponin from the Starfish Culcita novaeguineae

A new asterosaponin named novaeguinoside A, along with a known saponin, asteronyl pentaglycoside sulfate, was isolated from the starfish Culcita novaeguineae. The new compound was identitied to be sodium 6α-O-{β-D-fucopyranosyl-(1→2)-β-D-fucopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-xylopyranosyl-(1→3)-[β-D-quinovopyranosyl}-5α-pregn-9(11)-en-20-one-3β-yl-sulfate by extensive spectral analysis and chemical evidence.     

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002     

双羟基极性键合固定相在氨基酸分析上的应用

我们曾报道了一类新型双羟基键合固定相(GDSB)的合成,研究表明这类固定相具有键合相浓度高,热和化学稳定性好的特点,可用于性质相似的有机化合物的分离。 本文以GDSB为色谱柱填料,含Cu~(2+)离子和烷基磺酸盐的HAc-NaAc缓冲溶液作流动     

Tris(2,2''''-bipyridyl)ruthenium(Ⅱ) electrochemiluminescence (ECL) enhanced by rutin on platinum electrode

Ru(bpy)_(3~(2 )) electrochemiluminescence (ECL) was applied to determination of rutin. ECL intensity of Ru(bpy)_(3~(2 ))could be enhanced in the presence of rutin in basic solution on platinum electrode. At pH 9.9, light emission intensity was found to be linear with rutin in the range of 1-50 mmol/L.     

稀土在鼠肝中的物种分布

采用 ICP-MS、微量蛋白层析分离技术 ,研究了长时间、低剂量混合稀土及短时间、高剂量硝酸镧分别对大鼠及小鼠作用后 ,稀土在鼠肝中的代谢累积及其物种分布 .结果表明 ,鼠肝中各稀土含量随给药剂量的增加而增大 ,其累积速度大小顺序为 La>Ce>Nd>Pr;经柱层析分离未得到与稀土特异结合的鼠肝蛋白 ;稀土可与多种鼠肝蛋白 (包括多种重要的酶 )结合 ,在一定条件下 ,稀土与其结合蛋白可发生解离