铕掺杂BaPbO3的EXAFS研究

采用扩展Ｘ射线吸收精细结构方法，研究了铕掺杂ＢａＰｂＯ３多晶粉末中Ｅｕ，Ｐｂ两种原子的近邻结构。Ｅｕ的掺杂，导致八面体中金属Ｐｇ，Ｅｕ的配位数降低。     

安培检测芯片毛细管电泳及其初步应用

An end-channel amperometric detector with a guide tube for working electrode was designed and integrated on a home-made glass microchip. The guide tube was directly patterned and fabricated at the end of the detection reservoir, which made the fixation and alignment of working electrode relatively easy. The fabrication was carried out in a two-step etching process. A 30 μm carbon fiber microdisk electrode and Pt cathode were also integrated onto the amperometric detector. The baseline separation of dopamine (DA), catechol (CA) and epinephrine (EP) was achieved within 80 s. Relative standard deviations of not more than 5.2% were obtained for both peak currents and migration times of DA and CA (n=5). Using standard adding method, DA in tLrine and plasma samples was detected. The recoveries were in the range of 83%—103%.     

Synthesis of Lanthanide Coordination Polymers with Benzophenone-4,4′-dicarboxylate： Effect of Lanthanide Contraction on Structures

Four lanthanide coordination polymers with benzophenone‐4,4′‐dicarboxylic acid (H₂bpndc) and 1,10‐phenanthroline (phen), [Ln₂(bpndc)₃(phen)] (Ln=La (1), Pr (2) and Tb (3)), [Yb(bpndc)₁₅(phen)].05H₂O (4) were obtained through solvothermal synthesis. The crystallographic data show that 1, 2, and 3 are isostructural, the Ln(III) ions in 1, 2 and 3 are all eight‐ and ten‐coordinated, respectively, and thus the Ln(III) ions are connected by bpndc ligands, resulting in an interpenetrating 3D structure. While in 4, the Yb(III) ions are eight‐coordinated and connected by bpndc ligands into a 3D structure with 1D rhombic channels, which result from the effect of lanthanide contraction from La(III) to Yb(III) ions, and the bpndc ligands in 1, 2, 3, and 4 display three types of coordination modes.     

3—（p—甲苯基）磺酰氨基—2，6—哌啶二酮（C12H14O4N2S）的晶体结构和分子

采用X－射线单晶衍射和INDO量子化学计算法研究了标题化合物的晶体和分子结构，标题化合物的分子式C12H14O4N2S，Mr=282.31，三斜晶系，空间群P1，a=7.229(2),b=8.7922(9),c=11.242(1)A;A=70.339(8),β＝71。15（2），γ＝87．88（2）°，V=634.8(7)A^3,Z=2,Dc=1.476g/cm^3,R=0.037,Rw=0.037(W=1),分子的哌啶二酮环中C＝0和C－N键与多肽分子和相应键长相一致，根据INDO计算结果讨论了标题化合物的水解反应活性。     

反-1,2-双[2'-(5'-苯基恶唑基)]乙烯的晶体结构

用X射线单晶衍射法测定了反-1,2-双[2'-(5'-苯基恶唑基)]乙烯(POEOP)的晶体结构,POEOP晶体属单斜晶系, 空间群为P2~1/C, a=0.8268(2), b=0.5977(2), c=1.6292(3)nm;β=100.55(2)°; v=0.7915nm~3; Z=2; d~x=1.319g/cm~3。POEOP分子具有中心对称性,它的两个苯环和两个恶唑环是彼此平行的, 但整个分子却稍有些扭曲成螺旋浆式构型。键长数据表明POEOP分子中苯环与恶唑环以及恶唑环与C'=C双键间均有很大程度共轭。     

Chemical Liquid Phase Deposition of Thin Aluminum Oxide Films

Introduction Inorganic oxide films have attracted a lot of interest in the last several decades. Among them, silicon dioxide films are widely used in modern microelectronics, optics and mechanics. This material has been grown by various methods including thermal oxidation, chemical vapor phase deposition, plasma-enhanced chemical vapor phase deposition, and so on.1,2 Recently, Nagayama et al.3 have reported that SiO2 thin films could be produced by a new chemical method of liquid phase depos…     

用X-射线衍射法测定聚对苯二甲酸乙二醇酯/聚对苯二甲酸丁二醇酯共混体系的结晶度

Based on Hermans and Weidinger postulate that the crystalline fraction is proportional to crystalline intensity Ic and that the amorphous fraction is proportional to amorphous intensity Ia, it is. Suggseteet that for PBT/PET blends we assume that the intensity at 18. 2° is completely originated from amorphous scattering. The separation between the peaks at 17. 2° and 20. 8° is 3. 6°m, which is regarded as large enough to justify this assumption. Thus , it is possible to draw an acceptable demaraction line between the crystalline and amorphous scattering. The degree of crystallinity Xc is given by X_c-I_c/(I_c+KI_a),coefficient K is available by the values of Ic plotted against the values of Ia.For PBT/PET blends,we obtain that K is 0.95 and that correlation coefficient is 0.92 According to the method revieved above,we investi-gated the crystallinity of PBT/PET blends prepared by different ways.     

PEO／PBHE共混体系X射线散射研究

在聚环氧乙烷(PEO)/聚双酚A羟基醚(PBHE)共混体系中PEO是一个强质子受体,而PBHE是一个强质子给体,两者极易形成氢键,十分有利于形成互容对。笔者研究了PEO/PBHE共混体系的相容性,等温及非等温结晶动力学,本文根据Vonk提出的一维电子密度相关函数,分析了PEO/PBHE的SAXS现象,求得了共混体系的结晶度,片晶层厚度,过渡层厚度及长周期等结构参数。     

醋酸乙烯酯基桥连铁硫配合物(σ,π-μ-CH3CO2C=CH2)(μ-RS)Fe2CO)6的制备及结构鉴定

乙酰氯同Fe_3(CO)_(12),RSH,Et_3N所形成的盐[(μ-CO)(μ-RS)Fe_2(CO)_6]Et_3NH相作用,生成一类含醋酸乙烯酯基配体的桥连铁硫配合物(σ,π-μ-CH_3CO_2C=CH_2(μ-RS)Fe_2(CO)_6[R=Et,tert-Bu,Ph)。除用碳氢分析,IR,~1HNMR及X衍射技术表征这类配合物的结构和构象外,还对形成此类产物的过程进行了初步讨论。R=Ph配合物单晶的空间群为PI,晶胞参数a=7.087(3),b=8.824(2),c=15.740(3),α=76.20(1),β=88.15(2),γ=86.28(2)°,D_x=1.65g·cm~(-3),Z=2。醋酸乙烯酯基配体中带有醋酸根的硫与一个铁原子发生σ相互作用,而碳-碳双键与另一个铁原子则发生π相互作用。Fe—Fe键长为2.553(1))苯基与硫桥原子以e键相连。     

Crystal Structures and Magnetic Studies of Naphthalene Derivatives Containing Nitronly Nitroxides

Crystal structures of new nitronyl nitroxide derivatives 1, 2 and 3 were determined with X‐ray diffraction analysis: 1, monoclinic, C₂/c, a = 1.2404(5) nm, b = 0.9730(5) um, c = 2.7049(10) ran, β = 98.189(15)°, V = 3.2315(24) nm³, Z = 8; 2, or‐thorhombic, Pbca, a = 0.61262(2) nm, b = 1.11426(6) nm, c = 2.30543(13) nm, V = 1.57373(13) nm³, Z = 4; 3, monoclinic, P2(1)/n, a=0.64253(4) nm, b=2.55003(17) nm, c = 1.15497(6) nm, β = 95.000(3)°, V = 1.8852(2) nm³, Z = 4. Their magnetic properties were measured with SQUID and analyzed based on their crystal structures with simple singlet‐triplet, modified one dimensional antiferromagnetic chain and modified singlet‐triplet models respectively: 1, J/k_b= ?2.5 K; 2, J/k_b = 7.8 K, θ = 2.8 K; 3, J/k_b = ?0.96 K, θ = 0.21 K.