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.     

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.     

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.     

锕系多重键金属有机化合物研究进展

多重键金属有机化合物在多种催化反应中已经得到广泛的应用, 并取得了很好的研究成果. 目前, 多重键金属有机化合物的研究已成为催化化学领域中一个引人注目的研究热点. 综述了锕系多重键金属有机化合物的研究进展. 根据化合物多重键的不同, 分别讨论了它们的合成及反应性能, 并定性讨论了多重键的性质.     

Coupling of thermal desorption in modified closeable sampling columns with wide-bore capillary gas chromatography and mass spectrometric detection

In contrast to usability of Curie-point pyrolysis at 700°C directly attached to gas chromatography-mass spectrometry (GC-MS) for determination of organic wood preservatives in waste wood samples the investigation method reported here consists of thermal desorption at temperatures about 260°C in connection with GC-MS for peak identification or GC with flame ionization detection for quantitative analyses. So-called “modified closeable sampling columns” are used as batch-reactor in thermal desorption experiments. Desorbed vapours can be introduced on capillary columns without sample discrimination and without a disturbing lost of resolution. In this manner a lot of individual polycyclic aromatic hydrocarbons were determinated in waste wood samples, especially in railway sleepers.     

Glass capillary gas chromatography of amino acid enantiomers

Glass capillaries coated with Chirasil-Val, a chirally functionalised polysiloxane, are capable in principle of resolving all protein amino-acid enantiomers in a single run and within a short analysis time, thus allowing for example the quantitative amino acid determination by enantiomer labelling. The elution characteristics of the individual amino acids however are also dependent upon the chemical nature of the capillary wall surface, and a surface pretreatment is found to be necessary if all protein amino acids are to be analysed. Of the various methods of pretreatment tested, etching of borosilicate glass with gaseous HCl followed by deposition of colloidal silicic acid is considered to be the most suitable.     

酰胺型萃取剂N-503的合成

酰胺型萃取剂N-503[N,N-二-(1-甲基庚基)乙酰胺]可以用甲庚醇或2-氯代辛烷为原料来合成。它的重要中间体二-(1-甲基庚基)胺的制备方法有二:一是从甲庚醇制备的方法,将甲庚醇用阮来镍催化,常压氨解,得率95～99％左右;二是从2-氯代辛烷制备,此法需要高压设备,得率35％左右。第一个方法在扩大试验中,产率和产品质量都比较好,是一个较好的制备长碳链仲胺的方法。     

Darstellung und Kristallstruktur von LnAl3Br12 (Ln = La,Ce, Pr,Nd, Sm,Gd) und thermischer Abbau zu LnBr3

Preparation and Crystal Structure of LnAl₃Br₁₂ (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr₃ LnAl₃Br₁₂ (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl₃Br₁₂, PrAl₃Br₁₂, and NdAl₃Br₁₂ were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3₁12, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl₃Br₁₂ (Ln = Nd) to the corresponding lanthanoide tribromide is described.     

葡萄糖氧化酶电极的制备

葡萄糖氧化酶电极的制备于秀娟，周定，郭京华（哈尔滨工业大学应用化学系哈尔滨１５０００６）关键词葡萄糖氢化酶，酶电极，制备酶与电极的连接即酶膜的形成是制备酶电极的关键步骤之一，有许多种方式［１～９］．葡萄糖氧化酶（ＧＯＤ）电极是研究较早和报道较多的一类...