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.     

三元配合物[RE(Gly)4(Im)(H2O)](ClO4)3(RE=La,Pr)的热化学研究

利用自行研制的新型恒温环境反应量热计,以2mol·L-1HCl做溶剂,分别测定了LaCl3·7H2O、PrCl3·6H2O、[La(Gly)4(Im)(H2O)](ClO4)3、[Pr(Gly)4(Im)(H2O)](ClO4)3、Im、NaClO4、Gly、NaCl在298.15K时的溶解焓,再通过设计的热化学循环求得化学反应的摩尔反应焓,利用这些结果和其它辅助数据,计算出两种配合物的标准摩尔生成焓分别为:ΔfH m{[Prm{[La(Gly)4(Im)(H2O)](ClO4)3,s}=-3459.3±0.2kJ·mol-1;ΔfH (Gly)4(Im)(H2O)](ClO4)3,s}=-3460.63±0.18kJ·mol-1。     

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。     

Preparation of La0.9RE0.1MnO3 Ultra-fine Particles Used for CH4 Oxidation

Ｐｅｒｏｖｓｋｉｔｅ ｔｙｐｅｏｘｉｄｅｓ (ｇｅｎｅｒａｌｆｏｒｍｕｌａＡＢＯ3 )ｈａｖｅｂｅｅｎａｔｔｒａｃｔｉｎｇｍｕｃｈａｔｔｅｎｔｉｏｎｆｏｒｍｏｒｅｔｈａｎｔｗｏｄｅｃａｄｅｓｄｕｅｔｏｔｈｅｉｒｐｏｔｅｎｔｉａｌｃｏｍｍｅｒｃｉａｌａｐｐｌｉｃａｔｉｏｎｓａｓｃａｔａｌｙｓｔｓｆｏｒｖａｒｉｏｕｓｒｅａｃｔｉｏｎｓ :ｏｘｉｄａｔｉｏｎｏｆＣＯ[1～ 3 ] ａｎｄｌｉｇｈｔｈｙ ｄｒｏｃａｒｂｏｎｓ[4～ 7] ,ｃｏｍｂｕｓｔｉｏｎｏｆｎａｔｕｒａｌｇａｓｏｒＣＨ4 [8～ 1 1 ] (ｔｏｃｏｎｔｒｏｌＮ…     

Research of Three-Dimensional Fluorescence Spectra of RE3+ (RE=Eu, Tb) and Na2WO4 Co-doped Silica Luminescence Materials

In the preparation of this precursor tetraethlortho silicate (TEOS), sodium tungstate, ethyl alcohol, HCl and RECl3 (RE=Eu, Tb) were mixed and then heated at 800℃ for 2h, leading to a luminescent compound. The structure of the materials was characterized by TG-DTA and IR analysis, and the results indicate that the materials were in SiO2 network structure. Three-dimensional fluorescence spectra was used to characterize the luminescent properties of the materials. The luminescence property of doped and un-doped Eu3 or Tb3 and Na2WO4 in silica materials were prepared and measured. The results show that good energy transfer from WO2-4 to Eu3 ion, sensitized the luminescence intensify of Eu3 remarkably. Tb3 ion incorporated silica materials expressed the inverse energy transition from Tb3 to WO2-4, however, we got the materials with homogeneous green blue fluorescent light. Finally, the energy transfer of WO2-4 and Eu3 , WO2-4 and Tb3 were expained by energy levels diagram.     

Effect of RE-Doped and RE Quantity of Ni-Based Catalysts on CH4/CO2 Reforming Reaction

RE-doped Ni-based catalysts were prepared by sol-gel method.These catalysts were applied to the reaction of CO2 reforming CH4 to syngas.The studies reveal that RE-doped ( RE = La, Ce, Sm, Yb) Ni-based catalysts show higher catalytic activity than undoped Ni-based catalyst, and with the increasing of RE-doped quantity, the catalytic activity of catalysts exhibits regular changes.When RE-doped quantity is 0.2% ( molar ratio), the catalysts show the best catalytic activity.     

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。     

Thermochemical Properties of the Complexes RE(HSal)3·2H2O (RE=La, Ce, Pr, Nd, Sm)

Five solid rare earth salicylate complexes were synthesized by low hydrated lathanide chloride and salicylic acid. The complexes in this experiment were identified as the general formula RE(Hsal)3·2H2O(RE=La, Ce, Pr, Nd, Sm) by elemental analysis and EDTA volumetric analysis. IR spectra of the complexes show that carboxyl of salicylic acid coordinates to RE3 ions. Electrochemical behaviors of the complexes on the glass-carbon electrode were researched with cyclic voltammetry (CV). It is indicated that the electrochemical process of the complexes is a one-electron redox process and the electrochemical reversibility of complexes is less than that of the lanthanide chlorides. The constant-volume combustion energies of complexes, ΔcU, were determined with a precise rotating-bomb calorimeter at 298.15 K. Their standard molar enthalpies of combustion, ΔcHθm, and standard molar enthalpies of formation, ΔfHθm, were calculated.     

Preparing of Nano-Sized Power RE2O3(RE = La,Y,Gd) by Pyrolying Precursors

The precursors RE (HSal) 3 ( RE = La, Y, Gd; HSal = C6 H4 (OH) COO) were synthesized by the rheological phase reaction method. The mechanism and products of thermal decomposition of precursors was studied by using TG,DTA, gas chromatography-mass spectrometry (GC-MS). Nano-sized RE2O3 ( RE = La, Y and Gd) power were obtained by thermal decomposition of the precursors in air at 800 ℃. TEM measurement indicates that RE2O3 are spherical particles. The middle level diameter ( d50 ) of the particles are 19.3 ( La2O3 ) , 53.8 ( Y2O3 ) and 28.6 nm( Gd2O3 ) respectively by means of laser particles size analyzer.     

用乳状液膜从硫酸铵型浸出液中浓缩稀土

在作者所做的＂用乳状液膜从氯化钠型浸出液中浓缩稀土＂的工作基础上，利用所获得的液膜体系和较佳工艺条件，继续进行了料液类型［即ＮａＣｌ型和（ＮＨ４）２ＳＯ４型浸出液的比较实验］、ＮａＡｃ用量、膜相中有无石蜡、膜回用等条件实验，获得了从（ＮＨ４）２ＳＯ４型浸出液中浓缩稀土的适用液膜体系Ｎ２０５－Ｐ５０７－煤油－ＨＣｌ乳状液膜浓缩稀土的浓度达１０２ｇ／Ｌ，稀土提取率达９３％。     

RE2(CoFe)17-xTix型合金的结构和磁性(RE=Nd,La)

用电子探针(EPMA)、 X射线衍射仪和20 T脉冲强磁场测试仪研究了RE2(CoFe)17-xTix(RE=Nd, La)的结构与磁性. 结果表明, Nd2Co17-xTix 经过1050 ℃×15 h均匀化处理, 在x=1时, Nd2Co17型化合物变成Nd(CoTi)12和Nd2(CoTi)7型化合物, 而呈现出单轴各向异性. 此时合金的饱和磁化强度为0.7 T, 各向异性场为2250.3 kA*m-1. 对La-Co-Fe-Ti 2∶17型合金的磁特性进行了研究. 随着铁含量的增加, 合金的饱和磁化强度明显增加, 但也明显地降低了各向异性场.     

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。     

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.