消除夹带溶胀的新液膜操作法

消除夹带溶胀的新液膜操作法曹汉瑾，褚莹，何彦涛，吴子生，严忠（东北师范大学化学系长春１３００２４）关键词液膜，油／水乳液，溶胀，夹带，包裹消除液膜操作中的夹带溶胀对液膜的工业化具有重要意义，夹带溶胀分为包裹溶胀和再液化溶胀。前者是乳状液滴上浮时将水相...     

Drying agents for water-free introduction of desorption solvent into a GC after on-line SPE of aqueous samples

Summary A small cartridge containing a drying agent is inserted between a solid phase extraction (SPE) column and a gas chromatograph (GC) to enable the introduction of water-free desorption solvent into the GC in on-line liquid chromatography (LC)-type enrichment of trace-level analytes from water samples. Some characteristics of the drying agents, such as their capacity to retain water and their re-usability after heating, have been tested. Possible interactions of the drying agent with the analytes, e.g., irreversible adsorption or catalyzed degradation, have been checked for a wide range of alkanes, alkylbenzenes chlorobenzenes, chlorophenols and phthalate esters. Using the on-line SPE-GC system with flame ionization detection (FID) and spiked samples containing different levels of the test compounds, the repeatability was shown to be satisfactory (6–17%). For 10 mL samples, the detection limits were lower than 0.1 g/L. The on-line SPE-GC-FID system here presented can be used for the repeated analysis of water samples without exchange of the dyring cartridge. The technique is applied to the analysis of tap water.     

N-TiO2/ZnO复合纳米管阵列的掺杂机理及其光催化活性

以ZnO纳米柱阵列为模板, 采用溶胶-凝胶法制备出TiO2/ZnO和N掺杂TiO2/ZnO的复合纳米管阵列. 扫描电镜(SEM)、X射线光电子能谱(XPS)和紫外-可见漫反射吸收光谱(UV-Vis)的结果表明: 两种阵列的纳米管均为六角形结构, 直径约为100 nm, 壁厚约为20 nm; 在N-TiO2/ZnO复合纳米管阵列中, 掺入的N离子主要是以N-Ox、N-C和N-N的形式化学吸附在纳米管表面, 仅有少量的N离子以取代式掺杂的方式占据TiO2晶格O的位置; 表面N物种形成的表面态能级和取代式掺杂导致带隙的窄化, 增强了纳米管阵列的光吸收效率, 促进了光生载流子的分离. 光催化实验结果表明, N离子的掺杂有利于N-TiO2/ZnO复合纳米管阵列光催化活性的提高.     

Products active on mosquitoes,IV: Synthesis and biological activity of 8-propargyloxy-3,7-dimethyl-2,6-octadienyl/6-octenyl ethers

Summary A series of 8-proparglyoxy-3,7-dimethyl-2,6-octadienyl and 8-propargyloxy-3,7-dimethyl-6-octenyl ethers were prepared from 8-hydroxygeranyl and 8-hydroxycitronellyl ethers, respectively. Almost all compounds showed high toxicity toCulex quinquefaciatus larvae at 1 mgl^–1 dose level.

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Gegen Mücken aktive Produkte, 4. Mitt.: Synthese und biologische Aktivität von 8-Propargyloxy-3,7-dimethyl-2,6-octadienyl/6-octenyl-ethern

Zusammenfassung Eine Reihe von 8-Propargyloxy-3,7-dimethyl-2,6-octadienyl- und 8-propargyloxy-3,7-dimethyl-6-octenyl-ethern wurden aus 8-Hydroxygeranyl- bzw. 8-Hydroxycitronellyl-ethern hergestellt. Fast alle Verbindungen zeigten hoch Toxizität gegenüber Larven vonCulex quinquefaciatus in einer Dosierung von 1 mgl^–1.

     

A novel separation technique of diastereomeric esters of pyridylethanols by extraction: formal total synthesis of PNU-142721, HIV-1 reverse transcriptase inhibitor

The separation of diastereomeric esters derived from (±)-pyridylethanols and 3β-acetoxyetienic acid were achieved by an extraction technique using diethyl ether and aqueous hydrochloric acid. A formal total synthesis of PNU-142721 was effectively carried out to prepare the chiral, non-racemic synthon 1-furo[2,3-c]pyridin-5-yl-ethanol (1) by means of this technique. The structure optimized using MOPAC calculations on each diastereomer suggested the presence of intramolecular CH/π interaction in only the (S)-isomer of the diastereomers.     

MORPHOLOGIES AND GAS SEPARATION PROPERTIES OF MELT-SPUN ASYMMETRIC POLY(4-METHYL-1-PENTENE)HOLLOW FIBER MEMBRANES*

Poly(4-methyl-1-pentene) (PMP) hollow fiber membranes were prepared by the melt-spun and cold-stretch(MSCS) method. Scanning electronic microscopy (SEM) was used to characterize the section and surface structures of themembranes with special asymmetric structure. The preliminary results of gas permeation measurements indicated that the resultant hollow fiber membranes have the potential ability for oxygen/nitrogen separation.     

Promoting effect of sol-gel method and pre-treatment on the activity of SnO2/Al2O3 catalyst for NO reduction by propene

SnO₂/Al₂O₃ catalyst prepared by sol-gel method showed higher activity than those prepared by impregnation method, and their activity was significantly improved by pre-treatment in the reaction gas. The increased activity is closely related to the agglomeration of SnO₂ species and the re-exposure of Al₂O₃, which was previously covered by dispersed SnO₂ species. This revised version was published online in June 2006 with corrections to the Cover Date.     

Two New Xanthone Glycosides from Polygala tenuifolia

Two new xanthone glycosides,polygalaxanthone IV and V were isolated from the roots of Polygala tenuifolia Willd. Their structures were established as 6-O-[α-L-rhamnopyranosyl-(1→2)-β-D-glucopyranosyl]-1-hydroxy-3,7-dimethoxyxanthone(polygalaxanthone IV), and 6-O-[α-L-rhamnopyranosyl-(1→2)-β-D-glucopyranosyl]-1,3-dihydroxyl-7-methoxyxanthone (polyga-laxanthone V),respectively, on the basis of chemical and spectral evidence.     

Highly Efficient Pd/C-Catalyzed Suzuki Coupling Reaction of p-（un）Substituted Phenyl Halide with （p-Substituted phenyl） Boronic Acid

A highly efficient Pd/C-catalyzed ligandless, heterogeneous Suzuki reaction of p-（un）substituted phenyl halide with （p-substituted phenyl）boronic acid in DMF/H2O solvent in a short reaction time （0.5 h） at 75 ℃ was developed. The key for such a catalytic system was the addition of 1 equivalent of tetrabutylammonium bromide. A wide variety of substituents can be tolerated and high yields of cross coupling products were achieved. The palladium catalyst can be easily recovered and reused without significantly decreasing its efficiency.     

Effect of Addition of Base on Ceria and Reactivity of CuO/CeO2 Catalysts for Low-Temperature CO Oxidation

In this work, we have reported the influence of the addition of base (KOH) on the physicochemical property of ceria synthesized by alcohothermal process, and the alcohothermal mechanism was also put forward. Furthermore, the prepared CeO2 was used as the support to prepare CuO/CeO2 catalysts via the wet impregnation method. The samples were characterized by N2 adsorption-desorption, X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM), and temperature-programmed reduction by H2 (H2-TPR). The catalytic properties of the CuO/CeO2 catalysts for low-temperature CO oxidation were studied using a microreactor-GC system. The crystal size of CeO2-A was much smaller than that of CeO2-B, and the corresponding copper oxide catalysts exhibited higher catalytic activity than that of the CeO2-B-supported catalysts under the same reaction conditions. The alcohothermal mechanism indicated that KOH plays a key role in determining the physicochemical and catalytic properties of ceria-based materials.