Applications of ethylammonium and propylammonium nitrate solvents in liquid-liquid extraction and chromatography

Ethyl- and propylammonium nitrate are novel ionic solvents, liquid at room temperature, suitable for use as selective solvents for the isolation of analytes containing proton donor functional groups (alcohols, amines, phenols, carboxylic acids, etc.) by liquid-liquid distribution. These solvents form immiscible solvent pairs with non-polar aliphatic and aromatic hydrocarbons, ethers and alkyl halide solvents (e.g., methylene chloride, chloroform). Analytes can be recovered from the ionic solvents by back-extraction into ah organic solvent after dilution with water or pH buffer or, preferably, by extractive derivatization when gas chromatography is used for the analyses, avoiding the accumulation of salt on the column that results in poor baseline stability. Alkylation, acylation and particularly silylation are suitable methods for extractive derivatization using standard reaction conditions. Applications are presented for the isolation of polar analytes from an urban dust, shale oil and urine samples and for the determination of low-molecular-weight alcohols in gasahol and glycerol in soap. Liquid-liquid chromatographic systems with the liquid organic salt as stationary phase can be used to predict distribution constants for a particular separation and for the separation of polar solutes, particularly isomeric compounds possessing a proton donor functional group.     

Automated at-line solid-phase extraction-gas chromatographic analysis of micropollutants in water using the PrepStation

A fully automated at-line solid-phase extraction-gas chromatography procedure has been developed for the analysis of aqueous samples using the PrepStation. The sample extract is transferred from the sample preparation module to the gas chromatograph via an autosampler vial. With flame-ionization detection, limits of determination (S/N=10) of 0.05–0.13 μg/l were obtained for the analysis of HPLC-grade water when modifying the PrepStation by: (i) increasing the sample volume to 50 ml, (ii) increasing the injection volume up to 50 μl, and (iii) decreasing the desorption volume to 300 μl. The HP autosampler had to be modified to enable the automated “at-once” on-column injection of up to 50 μl of sample extract. The amount of packing material in the original cartridge had to be reduced to effect the decrease of the desorption volume. The total set-up did not require any further optimization after having set up the method once. The analytical characteristics of the organonitrogen and organophosphorus test analytes, i.e. recoveries (typically 75–105%), repeatability (2–8%) and linearity (0.09–3.0 μg/l) were satisfactory. The potential of the system was demonstrated by determining triazines and organophosphorus pesticides in river Rhine water at the 0.6 μg/l level using flame-ionization and mass-selective detection. No practical problems were observed during the analysis of more than 100 river water samples.     

The preparation of thick-film glass capillary columns

A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible.     

一种含5-硝基间苯二甲酸和菲咯啉配体的超分子化合物：结构表征，光致发光和电化学性能

采用水热法合成了含混合配体的铜配合物[CuClPhen]⁺·[HL]^-·2H₂O（HL=5-硝基间苯二甲酸,Phen=1,10-菲咯啉）,其结构由单晶X射线晶体学确定。标题化合物在三斜空间群P-1的晶体化合物。标题化合物的晶体数据：C₃₂H₂₄ClN₅CuO₈,M_r = 704.54,a = 10.4044(5),b = 12.3912(9),c = 12.4632(9)Å,α = 73.859(6),β = 85.036(5),γ = 78.202(5)^°,V = 1510.09(17) ų,Z = 2, T = 293(2) K,D_c = 1.549 g/cm³,μ(MoKα) = 0.874 mm^-1,F(000) = 720.0,R = 0.0554,wR = 0.1434,GOF = 1.098。当用作超级电容器电极材料时,所制备的配合物具有高比电容、良好的循环稳定性和优良的倍率性能。在1mol/L KOH溶液中,最大比电容可达到69 F/g。在2 A/g电流密度下,10000次循环后比电容保持率为72%。标题化合物是一种潜在的红色光致发光材料。     

Titantetrafluorid – Eine überraschend einfache Kolumnarstruktur

Titanium Tetrafluoride – a Surprising Simple Column Structure For the first time single crystals of TiF₄ have been obtained by solvothermal decomposition of (O₂)₂Ti₇F₃₀ in anhydrous HF. The colourless, transparent needles crystallize orthorhombic in spacegroup Pnma–D (No. 62) with a = 2 281.1, b = 384.8, c = 956.8 pm, Z = 12. The new type of structure is dominated by isolated columns of corner-linked TiF₆-octahedra.     

山西省古县野生资源综合开发利用对策

持续性农业将是２１世纪农业生产的主要模式,其基本特征是在强调农业发展的同时,重视自然资源的合理开发利用和环境保护。本文结合山西省古县丰富的野生资源现状,对其合理开发利用提出相应的对策     

Preparation of enantiomerically pure 1,1′-bi-2-naphthols from 85% cinchonine and 1,1′-bi-2-naphtholboric anhydride

A possibility of preparation of enantiomerically pure 1,1′-bi-2-naphthols using an impure cinchonine has been examined. The solid and the mother liquor formed from the reaction of 1,1′-bi-2-naphtholboric anhydride and 85% cinchonine in toluene could give optically pure (S)-(−)- and (R)-(+)-1,1′-bi-2-naphthol after acidification and kinetic crystallization, the overall yields were 40% and 28%, respectively. Supported by the National Natural Science Foundation of China (2937206) and the Natural Science Foundation of Hubei Province (93J27) Xiong Ying, born in 1971, Graduate student     

纳米结构硅研究的发展动态*

本文综合归类了目前制备纳米结构硅的主要方法：等离子体化学气相沉积．激光诱导化学气相沉积和热蒸发法（制纳米晶硅）及电化学腐蚀法（制多孔硅）,给出各种方法的典型参数及其对纳米硅结构的影响,分析了纳米硅结构特征,比较分析了各种方法制备的纳米硅的光学性能,如光学能隙Ｅｏｐｔｇ,光致／电致发光谱峰位波长、半高宽及影响因素等,并对纳米硅研究的发展前景进行展望．     

干湿循环法制备抗菌性 5A 沸石

本文探索了制备抗菌性沸石的新方法———干湿循环处理法,采用５Ａ沸石分别与抗菌性离子Ｚｎ２＋、Ａｇ＋、Ｃｕ２＋的溶液进行干湿循环处理,制备抗菌性５Ａ沸石。研究了反应条件,如温度、浓度、循环次数对沸石中抗菌性离子含量的影响,找出了最佳反应条件。测试了抗菌性５Ａ沸石的耐洗涤性能和抗菌性５Ａ沸石对黑曲霉菌、大肠杆菌及嗜热脂肪芽胞杆菌的抗菌效果。研究结果表明,干湿循环法制备抗菌性沸石,具有抗菌性离子含量多,抗菌性能好,方法简便,反应时间短,节约原料等优点。     

Preparation and characterization of Fully stoichiometric SrCoO3 by electrochemical oxidation

A nearly stoichiometric SrCoO₃ phase had been prepared up to now only using high oxygen pressure. A new method for preparing fully stoichiometric SrCoO₃ has been proposed using electrochemical oxidation. Brownmillerite-type SrCoO_2.50 is oxidized into a completely stoichiometric perovskite at a potential of 500 mV for 180 hours at room temperature in alkaline media (1 M KOH). The oxidized phase has a cubic unit cell (a=383.5 pm). It is metallic and, at temperatures below T=280 K, it shows ferromagnetic behavior. The magnetic moment at 0 K is 2.1 μ_B. The physical properties of SrCoO_3.00 have been explained in terms of partial occupancy of a σ*e band.