顶空气相色谱法测定延生护宝液中甲醇残留量

本文用顶空气相色谱法，以ＧＤＸ－１０１为固定相，测定了延生护宝液中甲醇残留量，方法的回收率在８５．９％－１０１．６％之间，变异系数０．３％，最小检出量１．０ｍｇ／Ｌ。     

Iodine catalyzed efficient synthesis of symmetrical diaryl sulfoxides from arenes and thionyl chloride under solvent-free conditions

Synthesis of symmetrical diaryl sulfoxides from arenes and thionyl chloride in the presence of a catalytic amount of iodine at room temperature under solvent-free conditions is described.Mild reaction conditions,easy workup,high yield,and easily available catalyst are important features of this method.     

N—BOC—8—氨甲基—2—萘甲酸的改进合成法

以２－萘甲酸为原料，经硝化，酯化，重氮化，选择性催化氢化，ＢＯＣ酸酐保护等六步反应，完成了Ｎ－ＢＯＣ－８氨甲基－２－萘甲酸（１ａ）的合成，为化合物１的合成提供了新的合成途径。     

还原温度对超细K－Co－Mo催化剂合成低碳醇性能的影响

 用溶胶－凝胶法合成了K－Co－Mo催化剂．样品经不同温度还原后，用于低碳醇的合成．XRD和HRTEM结果表明，样品是超细粒子，粒子尺寸为2～5nm．考察了催化剂的还原温度和反应条件对催化剂性能的影响．实验结果表明，还原温度对催化剂的活性有较大的影响，最佳还原温度为500℃．最佳反应温度范围为310～330℃．升高压力和空速可以提高醇的收率和选择性．在空速14400h－1，压力6．0MPa和温度310℃的条件下，醇的选择性为55．8％，收率为520．0g／（kg·h），MeOH／C2＋OH为0．27．催化剂稳定性良好，在200h的寿命实验中，活性基本不变．与文献中催化剂相比，超细K－Co－Mo催化剂对合成醇具有较高的活性和选择性，尤其是对C2＋OH的合成明显高于其他合成醇催化剂体系．     

REDUCTION OF C=C DOUBLE BOND WITH BOROHYDRIDE EXCHANGE RESIN-TRANSITION METAL COMPOUND SYSTEMS

Borohydride exchange resin-transition metal(Co,Ni,Cu,)compoundsystems reduced C=C double to C-C single bond in ethanol.     

毛细管电泳安培检测扑热息痛及其水解物

研究了各种电化学预处理条件下碳纤维电极对扑热息痛及水解物的电化学行为。确定该体系最佳预处理条件为０．２Ｖ电位下阳极化１ｍｉｎ，再于－２．０Ｖ下阴极化１０ｓ。预处理后的碳纤维伏安响应得到明显提高。运用最佳条件并在支持电解中加入添加剂后，扑热息痛及其水解物在毛细管电泳上获得很好的分离和检测。其中扑热息痛的检测下限为２．７８ｐｇ；对氨基酚为１．８４ｐｇ。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

合成1，3－二（3－羟丙基）四甲基二硅氧烷的新方法

用二乙氧基二甲基硅烷与３－氯丙醇反应，合成了新化合物３－氯丙氧基乙氧基二甲基硅烷，然后用格氏反应代替Ｗａｌｔｅｒ的钠缩合反应，最后经水解制备了１，３－二（３－羟丙基）四甲基二硅氧烷，总收率为４２．０％。     

二价氯化稀土催化丁二烯聚合的活性

<正> 稀土催化聚合双烯烃的研究表明,不同稀土元素的催化活性极不一样,对此虽有不同的解释,但通常公认Sm、Eu等活性骤低,可归之于它们在制备催化剂过程中极易被烷基铝从三价还原到二价,又根据大部分具活性的其它稀土元素在催化体系中总是三价的事实,进而推断:只有在体系中能保持三价的稀土化合物方有产生活性的可能,二价化合物则不具活性。然而,由于二价稀土化合物,特别是除Sm、Eu之外的二价化合物难以制得,迄今为止并无直接的实验事实来判断这些推断是否正确。     

八配位钇(Ⅲ)-反式-1,2-环己二胺四乙酸配合物NH4[Y(trans-CYDTA)(H2O)2]·4.5H2O的合成及分子结构

In this paper, the molecular and crystal structures of the NH₄[Y(trans CYDTA)(H₂O)₂]·4.5 H₂O(trans-CYDTA=trans 1,2-cyclohexanediaminetetraacetic acid) are reported. The crystal data are as follows: Triclinic system, P1space group,a=0.8599(6)nm,b=1.0021(7)nm,c=1.4370(9)nm,α =88.095(13)°,β =75.559(1)°,γ =88.344(12)°,V=1.1981(14)nm³,Z=2, M=708.68,D_c=1.570g· cm^-3, μ =2.506mm^-1 and F(000)=590. The final R₁ and wR₂ are 0.0571 and 0.1350 for 4205 [I >2.0σ (I)] unique reflections and 0.1007 and 0.1615 for all 4981 reflections, respectively. In the title complex, the anion [Y(trans-CYDTA)(H₂O)₂]^- has an eight coordination structure with distorted square antiprism. The trans CYDTA which acts as a hexadentate ligand with four Oatoms and two Natoms and two H₂O molecules directly coordinate to central metal Y(Ⅲ) ion. It can be known that the Y(Ⅲ) ion can form an eight coordinate compound with aminopolycarboxylic acid ligands in addition nine coordination structure.