Structure and magnetic properties of diaqua(4,4′-bipyridine) terbium(III) and the zinc(II) carboxylate dimer [Tb2Zn2(CH2C(CH3)COO)10(bipy)(H2O)2]2

A novel heteronuclear complex, [Tb₂Zn₂L₁₀(bipy)(H₂O)₂]₂ (HL = -methylacrylic acid, bipy = 4,4-bipyridine), was synthesized and characterized by elemental analysis and i.r. absorption spectra. Its structure, determined by X-ray diffraction, is a discrete octanuclear molecule, in which two Zn^II ions are linked by a bipy molecule and between Tb^III ions, or Tb^III and Zn^II ions are bridged by bidentate -methylacrylato groups. The temperature dependence of the magnetic susceptibility of the complex shows strong ferromagnetic interaction between the terbium atoms.     

Aggregate manganese Schiff base moieties by terephthalate or acetate: dinuclear manganese and trinuclear mixed metal Mn2/Na complexes

A reaction system consisting of terephthalic acid, NaOH, inorganic Mn(II) or Mn(III) salt, and salicylidene alkylimine resulted in dinuclear manganese complexes (salpn)(2)Mn(2)(mu-phth)(CH(3)OH)(2) (1, salpn = N,N'-1,3-propylene-bis(salicylideneiminato); phth = terephthalate dianion), (salen)(2)Mn(2)(mu-phth)(CH(3)OH)(2) (2, salen = N,N'-ethylene-bis(salicylideneiminato)), (salen)(2)Mn(2)(mu-phth)(CH(3)OH)(H(2)O) (3), and (salen)(2)Mn(2)(mu-phth) (4), while the absence of NaOH in the reaction led to a mononuclear Mn complex (salph)Mn(CH(3)OH)(NO(3)) (5, salph = N,N'-1,2-phenylene-bis(salicylideneiminato)). In addition, a trinuclear mixed metal complex H[Mn(2)Na(salpn)(2)(mu-OAc)(2)(H(2)O)(2)](OAc)(2) (6) was obtained from the reaction system by using maleic acid instead of terephthalic acid. Five-coordinate Mn ions were found in 4 giving rise to an intermolecular interaction and constructing a one-dimensional linear structure. Antiferromagnetic exchange interactions were observed for 1-3, and a total ferromagnetic exchange of 4 was considered to stem from intermolecular magnetic coupling. (1)H NMR signals of phenolate ring and alkylene (or phenylene) backbone of the diamine are similar to those reported in the literature, and the phth protons are at -2.3 to -10.1 ppm. Studies on structure, bond valence sum analysis, and magnetic properties indicate the oxidation states of the Mn ions in 6 to be +3, which are also indicated by ESR spectra in dual mode. Ferromagnetic exchange interaction between the Mn(III) sites was observed with J = 1.74 cm(-1). A quasireversible redox pair at -0.29V/-0.12V has been assigned to the redox of Mn(2)(III)/Mn(III)Mn(II), implying the intactness of the complex backbone in solution.     

Charge-transfer hybrids containing covalently bonded polyoxometalates and ferrocenyl units

Two new charge-transfer hybrids with one or two ferrocenyl units covalently attached to a hexamolybdate cluster through an extended pi-conjugated bridge have been prepared using Pd-catalyzed coupling reactions on monoiodo- or diiodo-functionalized cluster substrates in over 60% yields. These hybrids have been characterized by (1)H NMR, FTIR, electrospray ionization mass spectrometry, and X-ray diffraction. The electronic spectra of these hybrids show a broad absorption tail extending beyond 550 nm, indicating the existence of charge-transfer transition from the ferrocenyl donor to the cluster acceptor. The observation of the clear charge-transfer transition indicates the contribution of charge-transfer resonance to the ground state in both 2a and 2b even though the donor-acceptor separation distance of 11.29 A is rather long, signaling a through-bond charge-transfer nature made possible by the organic pi-conjugated bridge. Cyclic voltammetry studies reveal a one-electron oxidation wave and a one-electron reduction wave for the hybrid with one ferrocenyl unit. For the one with two ferrocenyl units, a lower reduction potential and a two-electron oxidation wave are observed, indicating negligible electronic interactions between the two ferrocenyl units.     

Determination of the residue of quizalofop-p-tefuryl in soybean by HPLC

A HPLC method was developed for the analysis of quizalofop-P-tefurylof in soybean. The samples were extracted with methanol-water (volume ratio), The extracts were cleaned up with a column of silica gel. The final residue was detected by HPLC, using a UV detector. The recoveries from the analytical method for soybean were 84.32%–89.25%. Variable coefficients were 0.49%∼1.51%. This method proved to be simple, reliable and accurate. __________ Translated from Chinese Journal of Chromatography, 2005, 23(2)(in Chinese)     

用理学3064X荧光仪分析碳

在理学３０６４Ｘ荧光仪上采用十八烷基马来酸（ＯＨＭ）晶体作为色散单元，通过改造电路，调整晶体倾角，获得对碳分析的良好线性，在流气正比计数器（ＦＰＣ）窗膜分别为５μｍ和０．６μｍ条件下，碳元素的峰背比分别达到３８．９１和５４．０４。作者分析了白口铸铁和碳化硅中的碳，结果表明在理学３０６４Ｘ荧光仪上定量分析碳是可行了，具有快速、简便、准确、多元素同时分析的特点，可用于日常分析     

影响双(2-丁氧羰基-3,4,6-三氯苯基)草酸酯化学发光体系的因素

过氧草酸酯类化学发光是一类以多氯代水杨酸酯与草酰氯反应生成的草酸酯、过氧化氢和荧光剂为主要组成的化学发光体［１，２］．它除了具有发光效率高，强度大，寿命长的特点外，还可以通过选择荧光剂调节发光的颜色．采用这类发光体系可制成多种化学光源．在草酸酯和荧光...     

Aqueous two-phase extraction as an effective tool for isolation of geniposide from gardenia fruit

Natural products are normally obtained by organic solvent extraction and many subsequent chromatographic separations. Compounds of interest are often isolated with very low yield and limited purity. An aqueous two-phase extraction process combined with a simple ethanol treatment, for removing excess inorganic salt, has been developed for preparation of geniposide from gardenia. The system was comprised of PE62, a random copolymer composed of 20% ethylene oxide and 80% propylene oxide, KH2PO4 and ethanol. To find optimal conditions, the partition behavior of geniposide under an aqueous two-phase system was investigated. Various factors were considered, including the concentration of salt, the concentration of polymer, the sample loading, and the addition of ethanol. The experimental results demonstrated that increasing salt concentration or decreasing PE62 concentration results in enhancement of the geniposide partition in the salt-rich phase. The addition of ethanol and higher sample loading also promoted the partition efficiency of geniposide. Based on this study, an optimized system containing 5% PE62, 7.5% KH2PO4, and 10% ethanol was tested on a large-scale extraction. A 39.0-g aliquot of final product (in powder form) with 77% purity of geniposide can be effectively extracted from 500 g of gardenia fruit. This process is proved to be useful for industrial application of geniposide preparation.     

线性低密度聚乙烯在与丁苯橡胶的共混体系中的结晶行为

本工作采用DSC、X-射线衍射、小角激光光散射、偏光显微镜等手段,研究了线性低密度聚乙烯/丁苯橡胶共混体系中聚乙烯的结晶结构、平衡熔点和结晶动力学。     

Preparation of Co3O4 Nanofibers via an Electrospinning Technique

Thin PVA/cobalt acetate composite fibers were prepared by using sol-gel processing and electrospinning technique.After calcination of the above precursor fibers,Co3O4 nanofibers with a diameter of 50-150 nm could be successfully obtained.The fibers were characterized by SEM,FT-IR,WAXD,respectively.