ICP-AES法测定烟花爆竹中禁限用药物

以5%HNO3处理烟花爆竹内药物样品,以ICP-AES法测定样品中K、Na、P、Mg、Ba、Cu、B、Sr、Sb、Ga、Ge、Al、Ti、Mn、Pb、As 16种元素。比较了不同酸、不同浓度时样品的处理方法,5%HNO3为最佳样品处理条件。对4个不同厂家产品进行了测定和加标回收研究,测定结果的相对标准差小于5%(n=5),各元素的回收率在93.4%～114.3%之间。     

NEMATICIDAL,INSECTICIDAL, ANTIFERTILITY,ANTIFUNGAL AND ANTIBACTERIAL ACTIVITIES OF SALICYLANILIDE SULPHATHIAZOLE AND ITS MANGANESE,SILICON AND TIN COMPLEXES

A facile synthesis and studies on the stereochemistry and biochemical aspects of some organosilicon(IV), organotin(IV), and manganese(II) complexes derived from imine having N^∪N^∪O donor system is reported. The imine was prepared by the condensation of salicylanilide with sulphathiazole. This imine reacts with organosilicon(IV)chloride, organotin(IV)chloride, and hydrated manganese(II) chloride to yield compounds having M─O and M←N bonds. The structures of the compounds have been elucidated by physicochemical and spectral (IR, ¹H NMR, ¹³C NMR, ²⁹Si NMR, ¹¹⁹Sn NMR, and ESR) studies, which clearly point to a trigonal bipyramidal geometry around silicon(IV) and tin(IV), and tetrahedral geometry around manganese(II), as the active lone pair of the nitrogen is also included in the coordination sphere. In the search for better fungicides and bactericides, studies were conducted to assess the growth-inhibiting potential of the synthesized complexes against various pathogenic fungal and bacterial strains. These complexes are highly active against nematode (Meloidogyneincognita) and insect (Trogodermagranarium). The activity will be increased with increasing concentration. These studies demonstrate that the concentrations reached levels that are sufficient to inhibit and kill the pathogens. All compounds have also been found to act as sterilizing agents by reducing the production of sperm in male mice.     

冠醚与碱金属苦味酸盐在氯仿中形成络合物的电导

测定了氯仿中碱金属苦味酸盐——冠醚络合物的电导率及络合比。确定了体系中电导率、冠醚浓度和络合比之间的关系。讨论了这些结果的某些应用。     

以陶瓷纤维为基材的硅胶吸附材料的制备与性能

以陶瓷纤维纸为基材，经水玻璃浸泡，絮凝剂沉积，盐酸调节pH值得到陶瓷纤维基硅胶吸附材料：探讨水玻璃浓度、絮凝剂浓度，盐酸浓度等条件对硅胶吸附剂吸附性能的影响：采用扫描电镜(SEM)，多孔介质孔隙分析仪揭示吸附材料的表面形貌、比表面积及孔径大小。实验结果显示：当水玻璃浓度为26．67wt%，絮凝剂浓度为15wt％，盐酸浓度为0．5mol／L时，吸附剂具有较好的吸附性能：硅胶能较好分散在纤维表面及其空隙中，BET比表面积为347．4m^2／g，总孔容为0．20295cm^2／g，其中，微孔所占比例为50．54％，平均孔径为，微孔0．4939nm，中孔3．907nm。     

RECENT DEVELOPMENTS IN THE METALLOSUPRAMOLECULAR AND MOLECULAR STRUCTURES OF THE COBALT,IRON AND VANADIUM COMPLEXES OF THE DIANIONIC TETRADENTATE SCHIFF BASE LIGANDS OF SALICYLIDENEIMINE AND ACETYLACETONEIMINE

Abstract

Four different types of metallosupramolecular structures are distinguishable for the title complexes. These types are described as: (a) The metal complex could react with other metal ions as a ligand, (b) Dimerization occurs through Lewis acid and Lewis base interactions of the metal ion and the coordinated oxygen atom of the ligand with those of an adjacent molecule, (c) Dimerization and chain formation occur using the donor-acceptor behaviour of the oxovanadium (IV) ion, and (d) Molecular association occurs through the bridged fluoride. Types (b), (c) and (d) are self-assembly. Chemical understanding of those types could lead to designing, and establishing procedures for, the preparation of new metallosupramolecular structures of homo- and heterobinuclear (as well as polynuclear) metal complexes with similar or mixed ligands.     

希土离子单硫代二苯甲酰甲烷配合物的合成及性质研究

本文合成了单硫代二苯甲酰甲烷(HTDBM)和三价希土离子及路易斯碱(Q)的Ln(TDBM)_4QH型配合物(Ln=除Ce外的La～Lu,Q=二乙基胺)。测定了它们的摩尔电导值、红外光谱,可见—紫外光谱,核磁共振谱.观察到配合物是通过硫原子、氧原子同时与Ln~(3+)离子配位.Ln-O键强于Ln-S键。在Nd~(3+)、Pr~(3+)、Ho~(3+)、Er~(3+)离子的该类配合物的可见吸收光谱中发现超灵敏跃迁现象。讨论了题述配合物作为核磁共振化学位移试剂的可能性.     

希土离子单硫代二苯甲酰甲烷配合物的合成及性质研究

本文合成了单硫代二苯甲酰甲烷(HTDBM)和三价希土离子及路易斯碱(Q)的Ln(TDBM)₄QH型配合物(Ln=除Ce外的La～Lu,Q=二乙基胺).测定了它们的摩尔电导值、红外光谱,可见—紫外光谱,核磁共振谱.观察到配合物是通过硫原子、氧原子同时与Ln³⁺离子配位.Ln-O键强于Ln-S键.在Nd³⁺、Pr³⁺、Ho³⁺、Er³⁺离子的该类配合物的可见吸收光谱中发现超灵敏跃迁现象.讨论了题述配合物作为核磁共振化学位移试剂的可能性.     

丙酮酸·邻菲咯啉·稀土三元固体配合物的合成和表征

丙酮酸在生物体内具有生理功能,它与稀土的二元配合物巳有报导。近期的研究结果表明某些稀土的邻菲咯啉三元配合物有一定的抑菌能力。本文报道丙酮酸(pyr-H)、邻菲咯啉(phen)稀土三元固体配合物的合成与表征结果。 按硝酸稀土:邻菲咯啉:丙酮酸(摩尔比)=1:1:3,将一定量的硝酸稀土加入无水乙醇中,溶解完全后,加入计算量丙酮酸,加热搅拌半小时,然后慢慢加入含计算量邻菲咯啉的     

PREPARATION AND PROPERTIES OF DIAZENIDO,HYDRAZIDO(2-), AND HYDRIDO-HYDRAZIDO(2-) COMPLEXES OF TUNGSTEN. X-RAY PHOTOELECTRON SPECTROSCOPY OF DINITROGEN AND HYDRAZIDO(2-) COMPLEXES OF MOLYBDENUM AND TUNGSTEN

Abstract

Reactions of HBr with trans-[W(N₂)₂(dppe)PPh₂Me)₂] (1) (dppe = Ph₂CH₂CH₂PPh₂) result in protonation of coordinated N₂ but no formation of ammonia or hydrazine. The tungsten-containing product depends upon the reaction conditions: (i) in MeOH, the product formed is [WBr(NNH₂) (dppe)(PPh₂Me)₂]HBr₂ (2) which converts to the hydride, [WBr₂(H)(NNH₂(dppe)(PPh₂Me)](Br(3), with loss of phosphine in THF or CH₂Cl₂, (ii) in THF or CH₂Cl₂, the hydride (3) is formed directly. Reaction of 2 with Na₂CO₃ in MeOH results in the loss of HBr and the formation of the diazenido complex [WBr(NNH)(dppe)(PPh₂Me)₂] which reacts further with Na₂CO₃ in benzene under N₂ to lose HBr and form a mixture of 1 and trans-[W(N₂)(dppe)₂]. The reaction of 1 with aqueous HF forms [WF(NNH₂)(dppe)(PPh₂Me)₂]BF₄. The X-ray photoelectron spectra of trans-[M(N₂)₂ (dppe)₂], [MBr(NNH₂)(dppe)₂Br (M = Mo, W), [WCl(NNH₂)(dppe)₂]Cl, [WCl(N)(dppe)₂]Cl and [WCl(NH) (dppe)₂] are reported. In all of these complexes, nitrogen is in a highly reduced form.     

PREPARATION AND CYCLIZATION OF PHOSPHONYL CHLOROVINYLALDEHYDE

Abstract

β-Phosphonyl-β-chlorovinylaldehyde was synthesized through chloroformylation of the Vilsmeier reagent with acetylphosphonate, and reacted with hydrazine, oxyammonia, formamidine, and guanidine to give the corresponding phosphonyl heterocyclic compounds.     

8-羟基喹啉-邻菲罗啉-稀土三元固体配合物的合成和表征

近年来 ,稀土三元配合物的种类和数目增加很快 ,有关具有特殊性质和结构的稀土三元配合物的合成报道日益增多 ,这些研究促进了稀土配位化学的发展。稀土含氮杂环化合物的合成、结构、荧光性质的研究很多 ,其中以Ｐｈｅｎ的稀土配合物研究占有较大的比例。我们知道 ,稀土离子与氮的亲和力小于与氧的亲和力 ,因此在水溶液中 ,作为弱碱性的氮给予体 ,即有机含氮杂环配体难与水竞争而取代水 ,故难以得到稀土含氮杂环化合物。直到二十世纪六十年代 ,人们利用非水溶剂为介质 ,合成了稀土与Ｐｈｅｎ的配合物[1 ] 。由于Ｐｈｅｎ含有较大范围的的共…     

NEW DINUCLEAR ASYMMETRIC COMPLEXES OF RUTHENIUM AND RHENIUM

Abstract

New dinuclear asymmetric complexes of ruthenium and rhenium, of formula [(bpy)(CO)₃ Re^I(4,4′-bpy)Ru^II/III(NH₃)₅]^3+/4+ have been prepared and characterized by spectroscopic and electrochemical techniques. In the mixed-valent species [Re^I, Ru^III], the back electron transfer reaction Ru^II → Re^II, that occurs after light excitation, is predicted to be in the Marcus inverted region. This fact is consistent with the observed quenching of the luminiscence of the Re chromophore in [(bpy)(CO)₃Re^I(4,4′-bpy)Ru^III(NH₃)₅]⁴⁺, when compared to the parent complex [(bpy)(CO)₃Re^I(4,4′-bpy)]⁺. A theoretical treatment due to Creutz, Newton and Sutin has been successfully applied to predict the electronic coupling element in the mixed-valent complex.     

稀土元素-吡啶氧正离子硼氢配合物的XPS伴峰及其价带谱研究

在以往十多年中,XPS技术用于稀土元素氧化物与卤化物,探讨了稀土元素的内壳谱及其伴峰现象,但对稀土元素配合物的研究报导甚少。本文报导我们新合成的稀土元素-吡啶氧正离子硼氢配合物[Ln(PyO)_7]_2(B_(10)H_(10))_3的XPS及其价带谱结果,而这些研究尚未见文献报导。     

不对称五氮齿镉和铟大环配合物的合成及其光物理性质研究

近年来,含有22个共轭电子的五氮齿大环金属配合物的新物种不断被合成^[1~2],这类配合物的0-0跃迁吸收带已扩展至大于700 nm的近红外区,作为第二代光动力光疗试剂倍受人们的重视,已在细胞水平上及动物实体瘤的实验中获得肯定结果^[3~4].最近,又发现这类分子还具有多种非线性光学效应,诸如反饱和吸收和非线性折射等^[5],可开发成激光限辐材料和器件,在激光防护方面有重要的应用价值.本文合成的不对称五氮齿镉和铟配合物就是这样一类新型化合物,本文报导其合成方法和基本光物理性质.     

SYNTHESIS AND CHARACTERIZATION OF A SERIES OF LIPOPHILIC CISPLATIN ANALOGS WITH CIS-1,4-DIAMINOCYCLOHEXANE AS NONLEAVING AMINE LIGAND

Abstract

A series of lipophilic platinum(II) complexes of the type [Pt(cis-1,4-DACH)L₂] (where cis-1,4-DACH = cis-1,4-diaminocyclohexane and L = acetate, propionate, butyrate, valerate, hexanoate, heptanoate, octanoate, 2,2′-dimethyloctanoate, nonanoate, decanoate, undecanoate, laureate, tridecanoate, myristate, pentadecanoate, palmitate, heptadecanoate, stearate, nonadecanoate, or eicosanoate) has been synthesized and characterized by elemental analysis and by infrared, ¹³C, and ¹⁹⁵Pt nuclear magnetic resonance spectroscopic techniques.     

SYNTHESIS,CHARACTERIZATION AND SOLUTION CHEMISTRY OF NEW Re(V) DIOXO COMPLEXES

Abstract

In this work, we report the synthesis, characterization and potentiometric studies of new Re(V) complexes of general formula [ReO₂(amine)₂]⁺ (amine = 1,2-diaminopropane, 1,4-diaminobutane, N,N′-diethylethylenediamine, diethylenetriamine, triethylenetetramine and N-tris(2-aminoethyl)amine). Compounds were prepared starting from [ReO₂I(PPh₃)₂] and characterized by several techniques. The presence of different substituent groups in the diamines (including alkyl and amine groups) allows the presence of pendant arms. When these groups are free amino groups, they can react with acids such as H⁺ and M²⁺ cations and studied by potentiometry. The formation of very stable binuclear species was demonstrated.