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本文详述了以碳分子筛作为吸附剂时,多孔层毛细管柱的制备方法,并用它在不同条件下对永久性气体以及C_1~C_6烃类气体进行了分离及分析。这类色谱柱可以使C_6烃在350℃馏出,不同碳数的烃类严格按碳数分开,不存在不同碳数间交叉的现象。在4℃时还可使O_2、N_2、CO很好分离,但对C_4异构体的分离不理想.如以k′值来代替涂层厚度(df)作为柱参数时,对HEPT~k′的曲线分析显示:减小颗粒直径、增加涂层厚度,有助于提高涂层均匀性和多孔层色谱柱的柱效。 相似文献
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PLOT柱是用于永久性气体,低碳烃和挥发性化合物色谱分析的最有效的工具,经常用于替代经典填充柱,对多孔层开管毛细管柱(PLOT)吸附色谱的分离机理、PLOT柱制备方法和各类吸附剂的色谱特性及其特定应用进行了综述。 相似文献
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溶胶 凝胶气相色谱毛细管柱是一种新型的色谱柱。这种色谱柱分离效果佳[1,2],柱容量大,耐热性能好,制作工艺简单[3]。本文采用几种方法对自制溶胶 凝胶柱[1~3]的极性进行了探讨,并与传统柱作了比较。所用色谱仪为岛津17A型,配有火焰离子化检测器(FID);色谱柱尺寸为10m×0 25mmi d ;载气为He;气化室温度250℃;分流(100∶1)进样。1 极性评价方法与结果1.1 不同化合物流出顺序的测定 色谱条件:溶胶 凝胶柱,固定液为Ucon75 H 90000及端羟基聚二甲基硅氧烷(PDMS)毛细管柱;FID温度300℃;柱温,80℃6℃/min280℃。试液:含亚油酸甲酯… 相似文献
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合成了上缘特丁基脱去的杯[4]芳烃25,27-二丁氧基-26,28-二(ω-十一碳烯氧基)杯[4]芳烃(p-H-C[4]B)及其相应的聚硅氧烷化高分子(PSO-p-H-C[4]B),以有上缘用N,N-二乙基氨甲基取代的杯[4]芳烃5,11,17,23-四(N,N-二乙基氨甲基)-25,26,27,28-四(ω-十一碳烯氧基)杯[4]芳烃(p-DEAM-C[4]U),并首次将它们用作毛细管柱气相色谱固定液,涂制成色谱柱,考察了这些杯[4]芳烃色谱柱的性能。结果表明,研制的杯[4]芳烃柱对芳香位置异构体均有良好的分离能力。 相似文献
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南京师范大学化学与环境科学学院王东新等人采用溶胶-凝胶法制备用于分离极性有机化合物的毛细管气相色谱柱,其制备工艺简单,制柱时间较传统工艺大为缩短。该柱涂层与毛细管内壁间形成的化学键使毛细管柱具有很好 相似文献
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X. -M. Lu X. -Q. Yun C. -S. Zhang D. -M. Kou C. -X. Fu S. -H. Xiang H. -X. Li 《Chromatographia》1996,43(3-4):211-214
Summary The preparation of a zeolite membrane PLOT column by in-situ synthesis is described. The advantages of this new column are discussed. Some analytical applications to alkanes, arenes, esters, alkyl halides and ethers on the zeolite membrane PLOT column compared with those on a coated zeolite PLOT column are reported. 相似文献
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The separation features of a new type of PLOT U column are presented through many applications. This type of PLOT U column is coated with a divinylbenzene-ethylene glycol dimethacrylate copolymer. It has an increased polarity when compared with a conventional PLOT Q type column. The stationary phase of the PLOT U column is truly bonded, thus providing column rinsability and low column bleed. 相似文献
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分子筛改性气—液毛细管柱及其性能考察 总被引:1,自引:0,他引:1
以原位合成法制备的分子筛膜对玻璃毛细管内壁进行改性后,成功地制备了常规口径及大口径分配SCOT柱,并对毛细管柱的性能进行了评价。 相似文献
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以甲基丙烯酸缩水甘油酯(GMA)和乙二醇二甲基丙烯酸酯(EDMA)为前驱体制备了新型聚合物多孔涂层毛细管开管(PLOT)柱固定相。通过优化聚合反应时间、致孔剂比例及交联剂比例获得了色谱性能良好的PLOT柱,扫描电镜结果显示毛细管柱内的多孔涂层厚度适中且均匀。在毛细管电色谱模式下,PLOT柱以反相色谱分离机理有效分离了中性、酸性和碱性小分子。人血清白蛋白(HSA)共价结合的蛋白亲和PLOT柱对5对手性对映体实现了较好的分离,且其分离度远高于HSA修饰的单层聚合物毛细管开管柱。PLOT柱分离烷基苯的日内、日间和柱间的相对标准偏差分别小于1.7%、4.8%和7.8%。 相似文献
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A layer of elemental silicon has been deposited on the surface of stainless steel tubing by means of chemical vapor deposition (CVD). Two kinds of capillary column were prepared from the deactivated tubing: cross-linked, silanol-terminated polydime-thylsiloxane wall coated open tubular (WCOT) columns and molecular sieve 13X porous layer open tubular (PLOT) columns. Unlike fused silica capillary columns, stainless steel WCOT and PLOT columns can be operated at temperatures in excess of 400°C. High temperature simulated distillation has been performed successfully with a macro bore WCOT column and rapid PNA (paraffin, naphthene, and aromatic) analysis with a multidimensional gas solid chromatographic (GSC) system using PLOT columns. 相似文献
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A protein-bonded porous-layer open-tubular (PLOT) column has been synthesized and applied to the separation of amino acids by CEC. The porous layer was coated on the capillary inner wall by in situ polymerization of 2-hydroxyethyl methacrylate and 2-vinyl-4,4-dimethylazlactone in the presence of 1-decanol as a porogen inside a fused-silica capillary silanized with gamma-methacryloxypropryltrimethoxysilane. The azlactone functionalities at the surface of the porous polymeric support layer were allowed to react with BSA to yield a protein-bonded PLOT column. This porous layer was characterized by scanning electron microscopy and its thickness was about 1 microm. CEC on this column gave enhanced resolution of three amino acids (histidine, phenylalanine, and tryptophan), and baseline separation was achieved with 20 mM phosphate buffer, pH 8.0. 相似文献
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R. C. M. de Nijs 《Journal of separation science》1981,4(12):612-615
A method is described for the preparation of a Porous Layer Open Tubular (PLOT) fused silica column coated with submicron particles of aluminum oxide for the analysis of light hydrocarbons. The column is thermally stable and provides reproducible analytical data over a long period of time. The column can be operated at temperatures easily controlled by commercially available gas chromatographic apparatus. 1,3-Butadiene is retarded much more than its principal impurities: thus the polarity of aluminum oxide is extremely useful for butadiene analysis because none of the contaminants is obscured by the butadiene peak. The analysis of the 16 most common C1–C4 hydrocarbons is achieved within 5 min at 60°C with helium as the carrier gas. Conditioning of the carrier gas with water vapor from CuSO4.5H2O to decrease the activity of the aluminum oxide is described. Some applications of a 30 m × 0.32 mm aluminum oxide PLOT column are given. 相似文献
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Guohong-Zhao Xiaoqiang-Lei Zhonglai-Wang Chengke-Gong Hanqing-Wang Liren-Chen 《Chromatographia》2003,58(7-8):465-469
Summary A new method is described to prepare polymeric porous-layer open-tubular (PLOT) columns by using a two-step in-situ polymerization technology. The integrated method involves a straightforward in-situ polymerization of the monomer. By using -(trimethoxysilyl)propyl methacrylate as a bridge, the porous polymer is bonded to the columns inner wall, and this polymer is crosslinked so the whole polymer looks like a single moleculer. The new column avoids the defects of traditional polymer PLOT columns where particles are easily released and swept through the column, causing blockage or a spiking detection signal. The new type of PLOT column is coated with a divinylbenzene and ethylene glycol dimethyl acrylate copolymer and has an increased polarity when compared to a conventional polymer Q-type PLOT column. The retention characteristics of the new column were evaluated and found to be comparable with the commercially available HP PLOT-U column. The inertness of the porous polymer allows the elution of a range of apolar and polar compounds: even most active and polar compounds such as H2O and H2S eluted symmetrically. The new column possesses high stability and can withstand temperatures up to 210 °C. With this new type of capillary columns, significantly better mechanical stability, temperature endurance, reproducibility, strong separation power and good inertness are obtained in combination with short analysis times. 相似文献