二-(2-乙基己基)二硫代磷酸萃取Tl~ 的研究

迄今,国内外萃取回收铊的工艺都是以三价形式进行的,这不论在经济上还是在技术上都不如萃取一价铊优越。国外已有人对用二-(2-乙基已基)二硫代磷酸(下文以D_2EHDTPA或HA代之)从水溶液中萃取Tl~ 进行了研究。为了更好地了解D_2EHDTPA萃取TI~ 的行为,我们也对D_2EHDTPA萃取Tl~ 进行了研究。     

微波常压法合成水杨酸酯

在浓硫酸催化下，采用微波常压法由水杨酸分别与正丁醇、异丁醇、正戊醇和异戊醇反应合成相应的水杨酸酯。结果表明：当水杨酸：醇：Ｈ２ＳＯ４＝１：５．５：０．３（摩尔比）时，采用５６０Ｗ微波辐射２２ｍｉｎ，水杨酸酯的产率可达８８．７％￣９６．４％，反应速度至少是常规反应的１４倍。     

一种新的烯烃环氧化催化剂MBC的合成及其催化作用的研究

为了克服以往许多烯烃环氧化催化剂发生严重沉积的缺点,我们首次合成了一种苯乙二醇氧钼螯合物(简称M BC,M为MoO_2,B为苯乙二醇,C为螯合物).将其用于丙烯环氧化新反应中,可以免去助溶剂,苯乙二醇配位体原料可重新由该过程获得,各反应指标均较满意,较好地消除了沉积,表明MBC是个良好的环氧化催化剂.     

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.     

4，4＇－偶氮二［4－氰基戊酰（对－二甲氨基）苯胺］作为引发剂的嵌段共聚物合成

his paper describes a new polyfimctional inihator, 4,4'-azobis[4-cyanopentanoyl (p-dimethylandno)anilide] (ACPDA), for the the radical polymerization. It was obtained by the rcaction of 4,4'-azobis(4-cyanopentanoyl chloride) with p-amino-N, N-dimethylaniline' ACPDA contains two reaction centres with different reactvities that are azo-group and N, N-dimethylaniline-group. By the controlled different conditions this initator can be utilized to make block polymers.     

绿原酸的极谱行为及测定

绿原酸(Chlorogenic acid)是著名中草药金银花的有效成份,它有清热解毒、抗菌等功能,其结构式为: 有人曾提出在3M的高氯酸底液中,在Ge(Ⅳ)的存在下进行催化极谱测定,但在NH_4OH-NH_4Cl底液中,绿原酸的极谱行为和测定方法尚未见报导,本文在NH_4OH-NH_4Cl底液中,对绿原酸的极谱行为和测定方法进行了研究。实验部分 883型笔录式极谱仪,滴汞电极为极化电极,在0.1MKCl溶液中,当汞柱高80cm时,汞流速为1.2mg,自由滴下时间为4.2s,汞池为阳极。XJP-821新极谱仪、pHS-2型酸度计、自装控时敲击器、通高纯氮气除氧,实验于室温下进行。     

溶液中非过渡金属混合配体配合物形成的热力学研究——Ⅱ.某些镉(Ⅱ)-联吡啶(邻菲咯啉)-氨基酸混配配合物中配体间疏水缔合作用的热力学

应用pH电位法测定水溶液中CdLA型混合配体配合物和相应的单配体配合物cdL,CdL_2,CdA,CdA_2在离子强度为0.10(KNO_3)、温度分别为15℃,25℃,35℃和45℃时的稳定常数,其中L为联吡啶或邻菲咯啉;A为丙氨酸、亮氨酸、苯丙氨酸和色氨酸。稳定性数据结合配体的结构表明,在含有亮氨酸、苯丙氨酸和色氨酸的混配配合物中存在着按上述配体顺序逐渐增强的配合物分子内的配体间疏水缔合作用。用温度系数法求出上述混配配合物形成反应的焓变△H,并进一步求出反应的自由能变化△G和熵变△S。热力学函数数据表明,较大的熵增加是上述混配配合物中配体间疏水缔合作用的主要推动力。     

包结物晶析法选择分离辛夷挥发油中1，8-枝叶素

We used 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol(A) as the host molecule to selectively recognize the component 1,8-cineole(B) in the volatile oil of Flos Magnoliae(Xin Yi). The inclusion com-pound (A B) was formed as crystalline, and the structure was confirmed by means of IR, ^1H NMR, and single crystal X-ray diffraction, with the 1:2 molar ratios of the host to the guest. The component 1,8-cineole(B) was selectively isolated from the inclusion compound(A B) by Kugelrohr vaccum technology, and then further characterized by IR, ^1H NMR and ^13C NMR. The whole components in the volatile oil of Flos Magnoliae (Xin Yi) and the isolation effect of 1,8-cineole isolated from inclusion crystals were analyzed by GC and GC-MS, respectively. The result indicate that the good isolation effect is given by the inclusion method, with purity and yield of the component 1,8-cineole(B) separated from the volatile oil of Flos Magnoliae are 100% and 85%, respectively.     

流通池光度滴定法应用—络合反应中的质子释放数测定

用具有流通池的分光光度计作测定装置,建立了由平衡移动法测定络合反应中质子释放数的新方法。方法简单、快速,仅用一个标准溶液,适于在变更pH值范围内金属离子不发生水解和没有其他副反应的体系。     

《分析化学》再次选入“CA”千种表

据美国《化学文摘资料来源索引季刊》（ChemicalAbstractsServiceS0urceIndex，QuarteHv，No·4，1995）公布资料，编纂年度为1994年7月至1995年6月中，我国（含台湾）有71种科技期刊被选入“CA”千种表中，其中《分析化学》居该干种表的第221位，为我国入选期刊第4名，人选期刊顺序、名称与名次见下表：1995年入选“CA”千种表中的71种中国期刊《分析化学》再次选入“CA”千种表@刘丽华$辽宁大学化学系资料室