超动态法快速制备毛细管色谱柱研究

涂渍毛细管柱常用的方法有静态法和动态法。恒温下自由蒸发溶剂和以液化的气体作固定液溶剂的静态法虽改进了静态法的涂渍速度,涂渍条件却要求苛刻。最近V.G.Berezkin和A.A.Korolev报道了超动态法制柱的方法,它比经典动态法有明显的改进。例如具有制柱速度快、柱效高、方法简便和重复性好等优点。本文用甲基乙烯基聚硅氧烷固定液     

交联键合型石英毛细管柱的研制及其应用

交联键合型石英毛细管柱,由于其突出的柔性和惰性,以及固定相经交联键合后固定相液膜的非萃取性和良好的热稳定性,故近年来在国内外引起了广泛的兴趣。 本工作通过交联键合型石英毛细管柱的研制,提出采用涂渍SE—54液相的交联键合型石英毛细管柱分析测定大庆油中宽馏程常、减压蒸馏馏份中的正构烷烃的分布。工     

高分子冠醚毛细管柱的性能研究

本文报道了3种新的聚硅氧烷侧链冠醚作气相色谱固定液,并涂渍成弹性石英毛细管柱,这种毛细管柱具有优良的色谱性能,它们具有柱效高,热稳定性好,选择性强的特点,适于分离各种异构体。     

一类新的毛细管气相色谱固定液—侧链液晶冠醚聚硅氧烷的研究

合成了一种新的毛细管气相色谱用固定液——侧链含冠醚液晶的聚硅氧烷,这种固定液易于涂渍在弹性石英毛细管柱上,柱效高,热稳定性好,极性中等,它具有高分子液晶和高分子冠醚固定液的双重保留性能,适于分离多种异构体。     

毛细管气相色谱法分离溴代烷氧基苯类位置异构体

比较了6种不同极性固定液色谱柱对溴代烷氧基苯类位置异构体的分离效果。采用SE-30毛细管柱50m×0.32mmi.d.,0.25μm)的分离效果最好,用该柱一次性同时分离了22种溴代烷氧基苯类化合物。     

侧链长短对全氧冠醚聚硅氧烷色谱性能的影响

设计合成了一种新型聚硅氧烷侧链全氧冠醚（丙烷氧甲基１５－冠－５），将其涂渍在示经处理的弹性石英毛细管柱上，其色谱柱具有高柱效，较宽的使用温度范围，高热稳定性和优异的选择性。并且通过与另一种氧烷侧链冠醚固定液涂渍柱的比较，考察了侧链脂肪间隔基的长短对冠醚固定液色谱性能的影响。研究了固定液对样品的分离机理。     

超动态法快速制备毛细管色谱柱的研究

用超动态法快速制出了几种非极性毛细管柱,柱效、涂渍效率分别为3000～4500理论塔板/m和65～85%。研究了超动态法中涂渍压力、涂渍液浓度与容量因子的关系;考察了制柱重复性和液膜厚度均匀性;给出了涂渍一般口径和试涂大口径厚液膜毛细管柱的部分结果。     

高效邻苯二甲酸二异癸酯毛细管色谱柱的制备

采用超细载体对毛细管柱内壁进行预处理,增加固定液在柱内壁的铺展性,然后将多种复配剂与邻苯二甲酸二异癸酯(DIDP)复配,配制质量浓度为5 mg/mL的固定液,通过加压装置,将固定液通入毛细管柱中,以间甲酚与对甲酚的分离度和对甲酚的理论塔板数评价了复配毛细管柱的分离性能。结果发现:DIDP与SE-54复配效果最好,对甲酚的每米理论塔板数可达3600。建立了快速、简便制备DIDP毛细管柱的方法。     

氨基酸光学异构体的气相色谱分离——光学活性毛细管柱与无阀柱切换技术的应用

应用双炉、双柱带无阀切换系统的气相色谱仪,建立了氨基酸光学异构体的分析方法。预柱是涂渍OV-101的玻璃毛细管柱,主柱是涂渍手性固定液——chiyasil-val的玻璃毛细管柱。具有溶剂切割、中心切割和反吹功能的二维无阀切换技术的应用,不仅能保护主柱。而且能缩短分析时间,同时大大提高柱分离能力,使更有利于体液中氨基酸的定性定量分析。     

表面分子印迹聚合物纳米线用于蛋白质的特异性识别

手性配体交换色谱是拆分手性化合物,特别是氨基酸和羟基酸对映体的一种有效方法,通常以光活性氨基酸或其衍生物为手性选择子,可通过键合及涂渍制备手性固定相,也可作为流动相添加剂来实现手性配体交换色谱分离分析,配体交换键合固定相需要完成载体和手性选择子之间的偶联,键合量因受到载体和制备条件的影响而较难控制,且柱效较低。     

Studies of open tubular micro capillary liquid chromatography. 1. The development of open tubular micro capillary liquid chromatography

Micro capillary columns were successfully applied to liquid chromatography by employing the principles used in micro high performance liquid chromatography. Fundamental investigations on the use of capillary columns in LC were performed for the various column parameters. Good separations of five aromatic hydrocarbons and four kinds of phthalic esters were obtained on a 62 μm I.D. capillary column, coated with SE-30.     

Gas chromatographic study of acetyl derivates of chlorinated guaiacols

Summary The gas chromatography of acetyl derivatives of guaiacol and all chlorinated guaiacols has been studied on SE-30, OV-351 and Carbowax 20M capillary columns. The retention order and relative retention times under isotermal and temperature-programmed conditions are discussed. Different retention times for all mono- and dichloro compounds have been observed on the SE-30 column. However, all trichloroguaiacol isomers were separated only on polar columns. The best overall temperature-programmed separations have been achieved on an SE-30 capillary column.     

Seperation of protein amino acids as their N(O)-Acyl alkyl ester derivatives on glass capillary columns

A comparison of the elution properties of the major protein amino acids as their N(O)-acyl alkyl ester derivatives (O-n-propyl, -n-butyl, -isopentyl; N(O)-trifluoroacetyl, -heptafluorobutyryl) on open-tubular glass capillary columns coated with SE-30, OV-17, OV-210 and EGA is described. A single-column separation to the baseline of the protein amino acids as their N(O)-heptafluorobutyryl n-butyl ester derivatives in less than 35 min was obtained on the SE-30 column. OV-210 columns have properties complementary to those of SE-30 columns and can be used as an aid to compound identification from retention time data. Separations of the amino acids from beer and dialysate from uremic patients are used to illustrate the practical posibilities of the method.     

单萜/顺丁烯二酸酐加成物及其酯类衍生物的气相色谱法分析

 摘要：研究了单萜/顺酐加成物及其酯化衍生物在OV-17和SE-30柱上的某些色谱性能和定量分析的线性相应关系。结果表明,这两种化合物在涂渍量为5％～10％的OV-17和SE-30柱上均能正常出峰;在峰形对称性和出峰时间上,OV-17柱具有优势。260℃以后,色谱峰面积与汽化温度无关。     

Evaluation of copper-1,3,5-benzenetricarboxylate metal-organic framework (Cu-MOF) as a selective sorbent for Lewis-base analytes

The metal-organic framework copper-1,3,5-benzenetricarboxylate (Cu-BTC) was evaluated for its ability to selectively interact with Lewis-base analytes by examining retention on gas-chromatographic columns packed with Chromosorb W HP that contained 3.0% SE-30 along with various loadings of Cu-BTC. Scanning electron microscopy images of the support material showed the characteristic Cu-BTC crystals embedded in the SE-30 coating on the diatomaceous support. The results indicated that the Cu-BTC-containing stationary phase had limited thermal stability (220 °C) and strong general retention for analytes. Kováts index calculations showed selective retention (amounting to about 300 Kováts units) relative to n-alkanes for many small Lewis-base analytes on a column that contained 0.75% Cu-BTC compared with an SE-30 control. Short columns that contained lower loadings of Cu-BTC (0.10%) allowed elution of nitroaromatics; however, selectivity was not observed for aromatic compounds (including nitroaromatics) or nitroalkanes. Observed retention characteristics are discussed.     

外标归一化气相法测定天然气组成

 对SP 6000天然气分析仪的气路系统作了改进,实现了仪器自身标定。采用填充柱和毛细管柱分离,热导检测器和火焰电离检测器双检测器检测,外标 归一化法定量,简易、快速地测定了天然气组成。方法的准确度及精密度均符合气相法定量分析的要求。     

Glass-capillary gas chromatography of chlorobenzenes on SE-30 and Carbowax 20M columns. Simultaneous determination of chlorobenzenes and chlorophenols

Summary Gas chromatography of benzene and all chlorobenzenes has been studied on SE-30 and Carbowax 20M glasscapillary columns under various operating conditions. The benzene isomers are eluted on both columns according to their boiling points. Separation of all components in a mixture is achieved on Carbowax 20M, whereas on SE-30 the peaks of closely related isomers overlapped. Also one partial overlapping is observed on a non-polar phase. The relative retention times for compounds are given and the retention order is discussed. The retention behaviour of chlorobenzenes and chlorophenols is compared. By using an SE-30 quartz-capillary column a mixture of 33 individual components gives 29 resolved peaks the analysis time being less than 26 minutes. A polar column proved to be unsuitable for the separation of polychlorophenols.     

Gas Chromatographic Analysis of DDT-Type Compounds

Abstract

Four columns have been used experimentally in combination with an electron capture detector, which allowed the determination of 25 DDT-type compounds, some of which have been reported as DDT breakdown products in many biological and nonbiological systems. The liquid phases were 5% QF-i, 5% Igepal, 5% Versamid 900, and 5% DC-11. The solid support for the 4 columns was 80 to 100 mesh Chromosorb W. Optimal temperatures (°C) for the columns were 190 (column), 210 (detector), and 230 (injector port). Optimal nitrogen flow rate was 35 ml/min., for all columns. The trimethylsilyl derivatives of the polar DDT-type compounds, DBH, DDOH, Dicofol, and DDA were successfully gas chromatographed on the column 5% QF-1 and the mixed column 2.5% QF-1 + 2.5% SE-30.     

Gas chromatographic – mass spectrometric analysis of compounds generated upon thermal degradation of some stationary phases in gas chromatography – Part II

The applicability of capillary columns for gas chromatography is often limited by stationary phase degradation at elevated temperatures. In order to achieve a better understanding of column thermostability, column bleed products have been analyzed qualitatively by gas chromatography-mass spectrometry (GC-MS). Three silicone stationary phases were studied: SE-52, SE-54, and OV-1701. Each of these was immobilized in the columns. The proportion of cyclics containing diphenyl in column bleed from SE-52 reflected to a large extent the composition of the polymer, while for SE-54 the proportion of such cyclics was unexpectedly high. The polar moiety of OV-1701, the cyanopropyl(phenyl)siloxy unit, was found to exert a highly destabilizing effect on the polymer, and the thermal degradation products consisted mainly of cyclosiloxanes containing this unit.     

C_5馏分及其羰化产物的毛细管气相色谱分析

石油裂解副产物C5馏分及其羰化产物是成分较为复杂的混合物,尤其是C5馏分中1,3-环戊二烯和顺-1,3-戊二烯的物性更为接近。用SE－54弹性石英毛细管柱和角鲨烷玻璃毛细管柱分别对C5馏分及其羰化产物进行了分析,使各组分达到了很好的分离。