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.     

Terminally functionalized polyisobutylene oligomers as soluble supports in catalysis

A new phase selective hydrocarbon soluble polymer support is described.     

Synthesis and in vivo study of metallofullerene based MRI contrast agent

Gd@C₈₂(OH)₄₀ has been developed as a new generation of MRI contrast agent. But recently, it was found that Gd@C₈₂(OH) _x with a larger number of OH (x>36) would lead to cage break and hence, release of highly toxic Gd ions. We synthesized the more stable Gd@C₈₂(OH) _x with less OH-number, Gd@C₈₂(OH)₁₆, and studied its proton relaxivity and MRI images. The results indicate that Gd@C₈₂(OH)₁₆ also gives high proton relaxivity, even higher than that of (NMG)₂-Gd-DTPA. The bio-distribution indicated that Gd@C₈₂(OH)₁₆ tends to be entrapped in the liver and kidney and remained in tissue for about 2 hours. The results suggest that the more stable metallofullerene derivative Gd@C₈₂(OH)₁₆ can be the potential candidate of the new MRI contrast agent.     

Study of the Complexation Behavior of Calixarene with Transition Metal Cations by UV—vis and Fluorescent Spectra

A new fluorescent compound based on calix[4] arene skeleton was synthesized.Its complexation ability with transition metal ions,such as Fe^3 ,Co^2 ,Ni^2 ,Cu^2 ,Zn^2 and Ag^ ,Was investigated by UV-vis and fluorescent spectra.     

机械球磨与反应烧结合成Sr2CeO4发光体的研究

Sr₂CeO₄ phosphor was synthesized by mechanical milling and reactive sintering in this work. The solid state reaction of SrCO₃and CeO₂ (2∶1) started at about 850 ℃ and completed at 1 000 ℃ for about 4 h. Two types of formation mechanism of Sr₂CeO₄ were proposed. When the starting powder mixture was fired above 1 000 ℃, the unstable intermediate phase SrCeO₃was developed, which then reacted with SrCO₃to form the final product Sr₂CeO₄, however, SrCO₃and CeO₂ converted directly to Sr₂CeO₄ at a lower temperature. The XRD results showed the crystal structure of Sr₂CeO₄ was orthorhombic. The emission spectra displayed a broad band with maximum at about 465 nm. The mechanical milling of starting power mixture and the sintering temperature had no effect on this emission spectra.     

呋喃甲醛缩二乙撑三胺希夫碱铜配合物的合成及结构(英)

A novel copper(Ⅱ) complex CuL(NO₃)₂(where L=N,N′-bis(furaldehyde)-diethylenetriamine) was synthesized and characterized by X-ray crystallography analysis. The crystal belongs to monoclinic, space group C2/c with cell parameters a=1.924 0(6) nm, b=0.792 8(3) nm, c=2.504 1(8) nm, β=111.163(5)°, and Z=8. The coordination geometry around Cu(Ⅱ) is a distorted trigonal-bipyramid，and one-dimensional chain is formed through intermolecular hydrogen bonds. CCDC: 255629.