Synthesis and Crystal Structure of RE[CH_2(CH_2)_4CONC_4H_9]_3(NO_3)_3(RE=Dy,La)

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＲＥ［ＣＨ２（ＣＨ２）４ＣＯＮＣ４Ｈ９］３（ＮＯ３）３（ＲＥ＝Ｄｙ，Ｌａ）ＷａｎｇＨａｎｚｈａｎｇ（王汉章），ＸｕＱｉｎｇｆｅｎｇ（徐庆锋），ＱｉａｎＰｕ（钱朴）ＳｕｎＪｉａｎｐｉｎｇ（孙建...     

仲辛醇-HF-H2SO4体系制取超高纯氧化钽和超高纯氧化铌

研究了超高纯氧化钽和超高纯氧化铌试验与生产的工艺技术条件，进行了超高纯氧化钽和超高纯氧化铌的基础试验、中试和工业性生产试验，介绍了项目产品的技术指标和用户使用情况。     

乙酸铵介质中金属锰与水反应制备高纯氢氧化锰

研究了乙酸铵介质中金属锰与水的反应，考察了反应过程中有关参数对反应速度的影响。研究证明，在乙酸铵介质中，金属锰可与水反应制备高纯氢氧化锰。实验结果表明：随着乙酸铵浓度的增加，反应速度加快，随着反应温度的升高反应速度反而减慢；锰粉单位表面积上的反应速度随反应时间的延长基本不变。     

稀土配合物[REL3(4-picNO)H2O]的合成与表征

合成了2,3-二氯异丁酸根和4-甲基吡啶氮氧化物稀土三元配合物(RE=La、Ce、Pr、Nd、Sm、Eu).通过元素分析、红外、紫外、荧光、X射线粉末衍射、XPS、热分析以及摩尔电导等分析手段,确定了配合物的组成为[REL3(4-picNO)H2O](L= CH3C2H2Cl2COO -),并对它们的性质进行了讨论.     

Preparation of Lanthanum Nickel Oxide-Coated Ni Sheet Anodes and Their Application to Electrolytic Production of (CF3)3N in (CH3)4NF·4.0HF Melt

A new process for electrolytic production of a perfluorinated compound, (CF3)3N, using lanthanum nickel oxide-coated Ni sheet anode in the (CH3)4NF·4.0HF melt at room temperature, was developed. Thin films of the lanthanum nickel oxides were prepared on Ni sheets by sol-gel coating method using polyvinlylpyrrolidone(PVP). The main components of the thin films were La2O3, LaNiO3, and La2NiO4 at 500, 750 and 1000 ℃, respectively. The anode performance in the (CH3)4NF·4.0HF melt depends greatly on the main component of the thin film, and the LaNiO3-coated Ni sheet anode gives the best anode performance. The potential of LaNiO3-coated Ni sheet anode remains constant at 5.9 V during electrolysis at 20 mA·cm-2 in the (CH3)4NF·4.0HF melt for 100 h. This is because LaNiO3 and NiF3 and/or Ni2F5, the latter of which was formed during electrolysis, in the film give a high electronic conductivity to the surface film during electrolysis. The maximum mole fraction of (CF3)3N (21.4%) was obtained at 20 mA·cm-2 in (CH3)4NF·4.0HF melt using the LaNiO3-coated Ni sheet.     

Synthesis of Hexp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1-->O) (CH2)7 CH3 probes for exploration of the substrate specificity of glycosyltransferases: Part II, Hex = 3-O-methyl-beta-D-Gal, 3-deoxy-beta-D-Gal, 3-deoxy-3-fluoro-beta-D-Gal, 3-amino-3-deoxy-beta-D-Gal, beta-D-Gul, alpha-L-Alt, or beta-L-Gal

Seven analogues of the trisaccharide beta-D-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1-->O)(CH 2)7CH3 have been synthesized as potential substrates for glycosyltransferases involved in the chain-termination of N-acetyllactosamine-type N-glycans. These compounds include: 3-O-methyl-beta-D-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp -(1-->O) (CH2)7CH3, 3-deoxy-beta-D-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1 -->O) (CH2)7CH3, 3-deoxy-3-fluoro-beta-D-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-M anp- (1-->O)(CH2)7Ch3, 3-amino-3-deoxy-beta-D-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Ma np- (1-->O)(CH2)7CH3, beta-D-Gulp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1-- >O)(CH2)7CH3, beta-L-Galp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1-->O)(CH 2)7CH3, and alpha-L-Altp-(1-->4)-beta-D-GlcpNAc-(1-->2)-alpha-D-Manp-(1- ->O) (CH2)7CH3. All trisaccharides were obtained by condensation of suitably modified glycosyl donors based on imidates or thioglycosides with the same disaccharide acceptor, octyl 3,4,6-tri-O-benzyl-2-O-(3,6-di-O-benzyl-2-deoxy-2-phthalimido-beta-D- glucopyranosyl)-alpha-D-mannopyranoside, followed by deprotection.     

35Cl NOR and 19F NMR relaxation studies of CClF2 group dynamics in N(CH3)4H(ClF2CCOO)2

Although schedule-dependent cytotoxicity of etoposide has been reported, its mechanisms have not been elucidated fully. In this study, we attempted to clarify what concentration, time or exposure dose (ED, concentration of drug x time) of etoposide result in the antitumor effect on human ovarian cancer cells from the standpoint of cell cycle perturbation. The different ED were produced by different drug treatment schedules: 10 microgram/ml x 4 h (ED 40), 1.66 microgram/ml x 24 h (ED 40), 5 microgram/ml x 4 h (ED 20), 0.83 microgram/ml x 24 h (ED 20), 10 microgram/ml x 0.8 h (ED 8), 5 microgram/ml x 1.6 h (ED 8), 2 microgram/ml x 4 h (ED 8), 0.33 microgram/ml x 24 h (ED 8). Cell cycle perturbation on day 5 and the suppression of cell growth were dependent on the drug concentration at the lowest exposure dose (ED 8), but were dependent on ED at the higher EDs (20 or 40). The percentage of cells in the G2/M fraction significantly decreased from day 5 to day 7 in BG-1 cells treated at ED 20 or treated with higher concentrations (10 and 5 microgram/ml) at ED 8, but not in those treated at ED 40 or treated with lower concentrations (2 and 0.33 microgram/ml) at ED 8. Therefore, the cytotoxic mechanism of etoposide may not be explained by simple schedule dependency.     

Y(C_(16)H_(16)N_2O_2)(NO_3)_3(CH_3SOCH_3)的合成和晶体结构

合成了硝酸钇（Ⅲ）与双希夫碱Ｎ，Ｎ′－二亚水杨基乙二胺、二甲基亚砜的配合物〔Ｙ（Ｃ６Ｈ４ＯＨＣＨＮＣ２Ｈ４ＮＣＨＣ６Ｈ４ＯＨ）（ＮＯ３）３（ＣＨ３ＳＯＣＨ３）〕。ｘ—射线单晶结构分析表明该晶体属单斜晶系、空间群为Ｐ２１／ｎ，ａ＝０．９６３１（２）ｎｍ，ｂ＝１．６４１４（５）ｎｍ，ｃ＝１．６２０９（３）ｎｍ，β＝１０２．９８（２）°，Ｚ＝４，Ｄｘ＝１．６５３Ｍｇ·ｍ－３。Ｙ（Ⅲ）配位数为９，配位几何为畸变的单帽四方反棱柱，所有的配位原子均为氧原子，分别来自三个硝酸根，一个二甲基亚砜和二个双希夫碱，中心离子被双希夫碱桥联，组成一维无限长链。     

Thermoanalysis of the combined Fe3O4-reduction and CH4-reforming processes

The chemical equilibrium composition of the system Fe₃O₄ + 4CH₄, at 1300 K and 1 atm consists of solid Fe and a 2:1 gas mixture of H₂ and CO. Thermogravimetric (TG) analysis combined with gas Chromatographic measurements was conducted on the reduction of Fe₃O₄ (powder, 2-μm mean particle size) with 2.3, 5, 10, and 20 pct CH₄ in Ar, at 1273, 1373, 1473, and 1573 K. The reduction proceeded in two stages, from Fe₃O_{4 to FeO, and finally to Fe. CR}, conversion and H₂ yield increased with temperature, while the overall reaction rate increased with temperature and CH4 concentration. C (gr) deposition, due to the cracking of CR,, was observed. By applying a topochemical model for spherical particles of unchanging size, the reaction mechanism was found to be mostly controlled by gas boundary layer diffusion. The apparent activation energy reached a maximum at 30 pct reduction extent and decreased monotonically until completion. When compared with the results using instead either H₂ or CO as reducing gas, the reduction achieved completion faster using CH₄, at temperatures above 1373 K.     

大口径毛细管柱气相色谱法分析乙硫氨酯

选用SE-30大口径毛细管色谱柱和氢火焰离子化检测器(FID),使用N2000色谱工作站,采用峰面积归一法,建立了气相色谱分析乙硫氨酯的方法。当乙硫氨酯的体积分数为95%~98%时,采用该方法与《YS/T 357—1994乙硫氨酯的技术条件》中硝酸汞滴定法的分析结果进行比较,相对标准偏差为0.04%~0.06%。该气相色谱分析方法适用于以异丙基黄药、氯乙酸、纯碱和一乙胺为原料而合成的乙硫氨酯分析。