聚己内酯和聚氧化乙烯共混体系中的两类片晶相间堆砌

对聚(ε-己内酯)(PCL)/聚氧化乙烯(PEO)共混物的相差显微镜、广角X-射线衍射(WAXD)、小角X-射线散射(SAXS)及示差扫描量热计(DSC)等的研究表明,只有当共混物中PCL(或PEO)的含量低于20％时,两组份是相容的.当PCL含量低于20％时,在共混物中形成了PEO片晶和PCL片晶相间堆砌的结晶形态,当PEO含量不超过20％时,PEO则完全以非晶形式混入PCL的非晶区,同时阻碍了PCL的结晶.可见在结晶过程中,相容的两组份对共混体系形态结构的影响却不尽相同.     

阴离子交换色谱-积分脉冲安培法测定鱼粉和玉米粉水解液中氨基酸

将高效阴离子交换色谱．积分脉冲安培直接检测法应用于鱼粉和玉米粉水解液中的氨基酸的分析测定。该方法使用Dionex AminoPac PA10阴离子交换柱为分析柱，控制柱温为35℃，以NaOH和NaAc的强碱性溶液为淋洗液，在合适的梯度条件下，可以实现对17种常见氨基酸的高效分离。在强碱性条件下，获得良好分离的各个氨基酸可在配有金工作电极的电化学检测器上以积分脉冲安培法获得高灵敏度的检测。在优化的测定条件下，该方法对这17种氨基酸的检出限在0．21—3．38pmol之间；峰面积校正曲线的线性范围为2—3个数量级；5次平行测定的峰面积的相对标准偏差RSD在0．32％—4．7％之间。该方法应用于玉米粉和鱼粉水解液中氨基酸含量的测定，结果良好。对玉米粉和鱼粉水解液标准加入的回收率分别在81．9％—108．0％和90．0％～108．0％之间。     

Synthesis of an optically active intermediate for A-ring of 19-nor- 1α,25-dihydroxyvitamin D3

An optically active intermediate 5 for A-ring of 19-nor-1a,25-dihydroxyvitamin D3 2 has been synthesized in five steps, starting from readily available, inexpensive D( )-xylose 6 with good yield.     

吸附丝富集化探样品中烃类的色谱—质谱检测

通过吸附丝富集样品中的游离烃，热解析后直接进行色谱－质谱分析，该法适用于土、岩石、水及油气样品，操作简便，灵敏度高，可检测至Ｃ１６的烃类，是油敢化探中行之有效的一种新方法。     

C_（60）的胺加成反应和电喷雾电离质谱（ESI－MS）检测

报道了Ｃ６０与１，３－丙二胺和Ｎ，Ｎ－二甲基－１，３－丙二胺的加合反应，反应产物未经预先离子化处理直接用ＥＳＬ－ＭＳ进行检测。由于反应产物从甲苯溶液中析出，避免了生成多胺基加合物，产物以单加成物为主。当加合反应在空气氛下进行时，有加合氧的产物Ｃ６０Ｏｎ（ＮＨ２—ＣＨ２ＣＨ２ＣＨ２ＮＲ２）ｍ（Ｒ＝Ｈ，ＣＨ３）存在。实验发现：Ｎ，Ｎ－二甲基－１，３－丙二胺比１，３－丙二胺更容易与Ｃ６０发生多胺基加成和氧加成反应。通过控制反应条件可制备Ｃ６０二胺的单加成产物。     

A High－efficiency Preparation, Properties and Structure of （R, S ）－and （ S, S）－Pyrrolidine－2－carboxylic Acid 3,5－Dioxa－4－boracvclo.hepta [ 2,1－α; 3,4－α′] dinaphthalen－4－yl Esters

A highly-efficient preparative procedure for ( R, S )- and ( S, S)-pyrroHdine-2-carboxyHc acid 3,5-dioxa-4-boracyclohepta[2, 1-α ; 3,4-α′] dlnaphthalen-4-yl esters [ namely ( R, S )-BNBAP and (S, S )-BNBAP] is described and the crystal structure of (R, S )-BNBAP was obtained. The data indicate that ( R, S )-BNBAP is a spirocyclic inner borate salt with almost normal te-trahedral configuration. This structural form may be the basic reason for their high chemical, optical and thermodynamic sta-bility.     

噻吩甲酰三氟丙酮和4，5-二氮芴-9-酮及4，5-二氮芴-9-酮连氮铕(Ⅲ)三元配合物的合成和表征

合成了Eu(TTA)₃L1(Ⅰ)和［Eu(TTA)₃］₂L2(Ⅱ)二种新的铕(Ⅲ)三元配合物(TTA=噻吩甲酰三氟丙酮一价阴离子、L1=4,5-二氮芴-9-酮、L2=4,5-二氮芴-9-酮连氮)。用元素分析、IR、UV和溶液荧光光谱对配合物进行了表征。探讨了溶剂对Eu(Ⅲ)三元配合物荧光光谱的影响，发现在CH₃CN中Eu(Ⅲ)三元配合物发光效果最好，而溶剂DMF会使配合物荧光减弱。     

Synthesis and electrochemical properties of 2,6-bis（6-aryl-[1,2,4]- triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines

By the condensation of 2,6-bis（4-amino-5-mercapto-[1,2,4]-triazoles-2）pyridine with aromatic acid in the presence of phosphorus oxychloride. Compounds of 2,6-bis（6-aryl-[1,2,4]-triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines were synthesized. Their structures were confirmed by IR, ^1H NMR spectroscopies and elemental analysis. Their electrochemical behavior and cyclic voltammogram also were be studied. The results showed that they have high ionization potentials and good affinity.     

(Y,Gd)VO_4∶Eu~(3+)的紫外-真空紫外发光特性

用高温固相法合成了Y1-xGdxVO4∶Eu3 (0≤x≤1)系列单相样品并研究了其发光特性。在254nm激发下,观察到最大强度位于619nm的红色发射峰且其强度在Y/Gd=0.4/0.6时达到最大。在147nm激发下的发射峰与紫外下的一致,发射强度也是在Y/Gd=0.4/0.6时达到最大,大约是商用(Y,Gd)BO3∶Eu3 荧光体的65%。619nm监控下的真空紫外激发光谱由峰值位于158nm,204nm,247nm以及300nm的系列激发带组成,归属于钒酸根的基质吸收以及Gd3 、Y3 和Eu3 的电荷迁移带吸收。相对(Y,Gd)BO3∶Eu3 中Eu3 占据中心对称格位,(Y,Gd)VO4∶Eu3 中Eu3 占据非中心对称格位,其真空紫外下光谱色纯度更好。色坐标分别为(0.632,0.355),(0.672,0.328)。     

异双桥二维镍(Ⅱ)配位聚合物 ∞2[Ni(μ-4，4′-bpy)2/2(μ-L)4/2](HL=2-indolyl-formic acid)的水热合成和晶体结构

The allo-bisbridge 2D coordination polymer _∞²[Ni(μ-4，4′-bpy)_2/2(μ-L)_4/2](HL=2-indolyl-formic acid) has been obtained by using hydrothermal synthesis, and the results of X-ray single crystal diffraction analysis show that the compound crystallizes in monoclinic system, space group C2/c (No.15) with a=2.300 2(5) nm, b=1.129 1(2) nm, c=0.974 0(2) nm, β=109.85(3)°, V=2.379 2(8) nm³, D_c=1.494 g·cm^-3, Z=4, F(000)=1 104, μ=0.860 mm^-1, R=0.032 2, wR=0.088 8. The crystal structure consists of the [Ni(μ-4,4′-bpy)_2/2(μ-L)_4/2] complex molecules, in which the Ni atom is octahedrally coordinated by two N atoms from two different 4,4′-bpy molecule ligands and four O atoms from four different L- anion ligands. TG analysis indicate that title coordination polymer possesses relatively high thermal stability. CCDC: 252833.