超微粒分子筛多孔层毛细管气相色谱柱的初步研制

探讨了以超微粒分子筛成功地沉积于玻璃毛细管内壁制备出新型ＰＬＯＴ柱的方法。实验证明,这种ＰＬＯＴ柱具有快速、高效、稳定和选择分离等独到特性。     

分子筛改性气—液毛细管柱及其性能考察

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。     

超微粒介孔分子筛Ti-MCM-41的合成及应用

超微粒分子筛;苯乙烯;催化氧化;超微粒介孔分子筛Ti-MCM-41的合成及应用     

硫酸钡微晶改性毛细管柱的制备及其分离性能的研究（Ⅰ）

本文提出利用硫酸钡微晶对玻璃毛细管内表面进行改性,成功地将中、强极性固定液涂溃在这种改性表面上,制备出高效毛细管色谱柱。文中较详细地给出了硫酸钡微晶的制备方法以及微晶层的沉积方法,并对这种毛细管色谱柱的性能进行了考察。     

原位合成分子筛气-液改性毛细管柱的制备与评价

 用原位合成方法成功地制备了一类新型NaA分子筛毛细管柱 ,与传统柱型相比 ,原位合成柱的分子筛层更加均匀与致密、分离效果更佳。在此柱上涂敷不同极性的固定液制备了一类新型气 液分子筛改性SCOT柱 ,测试表明该柱型分离效果较佳、热稳定性好 ,其中超短柱及大口径柱的成功应用更显示该柱型具有很高的实际应用价值 ,值得推广。     

用改进的涂敷法考察模板剂对分子筛毛细管色谱柱分离性能的影响

1　引　　言传统分子筛柱的制备以静态涂敷或以水、甲醇为悬浮液的动态涂敷为主 ,两种方法耗时耗力、成功率低、重复性均匀度差。与此相比 ,本文发展的以一缩二乙二醇为悬浮剂的改进涂敷法简便易行、重复性好、柱效高 ,极大地拓展了分子筛柱的应用范围。利用该涂敷法 ,本文制备了ＺＳＭ 5分子筛柱 ,重点考察了模板剂四丙基溴化胺 (ＴＰＡＢｒ)在ＺＳＭ 5分子筛毛细管柱色谱分离中的作用。2　实验部分2 .1　仪器与试剂　ＧＤＭ 1Ｂ玻璃毛细管柱拉制机 (日本岛津公司 ) ,1 0 0型超声波振荡器 (美国ＮＥＹ公司 ) ,ＭＣＴ 1Ａ玻璃毛细管动态涂敷…     

直热式毛细管柱对直馏汽油组成的分析

采用柱内电阻丝加热升温的直热式１３Ｘ分子筛薄层毛细管填充柱分析汽油的族组成。分析时间比炉温加热短５０ｍｉｎ,定量分析结果与炉温加热和多孔层开管柱基本相同。保留时间的相对偏差小于３％,直馏汽油中绝大部分组分定量结果的相对偏差小于５％。     

改性5分子筛吸附剂从含氟水中除氟研究

研究了以5A分子筛为骨架吸附材料,经在含AI^3 或Fe^3 溶液中离子交换改性处理,获得了一种可吸附除氟的改性分子筛。实验表明,该种分子筛对水溶液中的低含量氟有良好的吸附性能。静态饱和吸附容量可达28．98和21．4mgF/g分子筛（分别对含AI^3 或Fe^3 分子筛）。含氟水经分子筛柱处理后,除氟率可达99％。吸附氟后的分子筛可用柠檬酸盐洗脱氟,洗脱率接近安全。洗脱后的分子筛可重复使用。得到一种新的效果显著的除氟方法。     

交联SE-54弹性玻璃毛细管柱研究

弹性玻璃毛细管柱的出现为毛细管色谱技术提供了一种新型柱。最近我们应用硅膜改性法成功地惰化了弹性玻璃毛细管柱而不损害其强度,使这种柱型有了良好的发展基础。关于交联弹性石英柱的制备巳有不少研究,但在硅膜改性玻璃毛细管柱上进行交联的工作尚未见报道。本文介绍SE-54弹性玻璃毛细管交联柱的制备和性能研究。在拉制好的     

甲基丙基酸丁酯/SiO_2/TiO_2有机-无机杂化毛细管整体柱的制备及其应用

采用溶胶-凝胶法制备了SiO2/TiO2杂化材料,并通过双官能团试剂3-(甲氧基硅烷基)甲基丙烯酸丙酯(γ-MAPS)对其进行改性;改性溶胶与甲基丙基酸丁酯(BMA)作为功能单体,在毛细管中进行原位聚合反应,制备了新型的有机-无机杂化毛细管整体柱。采用扫描电子显微镜观察了整体柱柱床的形貌。以硫脲为电渗流标记物对所制备的整体柱进行了柱性能评价,考察了柱的稳定性和重现性,获得了88000plates/m的柱效;考察了中性物质在柱上的的保留行为,得出该柱具有反相电色谱保留性能。通过对2种短肽(磷酸肽和非磷酸肽)洗脱测试,实现了对磷酸肽的有效富集与分离。     

原位合成分子筛膜毛细管色谱柱的研制

吸附型多孔层毛细管柱既耐高温又对气体及烃类异构体有选择性，同时又具有毛细管色谱快速、高效等优点，是解决难分离组分的重要柱型．常用作气一固吸附色谱固定相的有强极性的硅、中极性的氧化铝、非极性的碳质及特殊吸附作用的分子筛．其中分子筛以其独特的吸附作用，在永久性气体和烃类碳数族组成分析中有重要地位．Pruecell和Soulages[1，2]等制备了涂渍型5A和13X型分子筛的毛细管柱，对低碳烃类化合物显示了良好的分离能力，分析柱温较填充柱降低约100℃．邹乃忠等[3～5]也先后制备了分子筛层的毛细管柱用来作直馏汽油的分析．由于通…     

A new type of capillary column for gas chromatography

A new type of capillary column for gas chromatography was proposed. A sorbent layer (for example, stationary liquid phase) is supported on the internal capillary surface, and the internal (interstitial) volume is packed with nonporous large particles of a sorbent (particle diameter is 0.1—0.6 of the capillary internal diameter). The external surface of the particles can also be coated with the sorbent layer (for example, stationary liquid phase). The specific separation efficiency (number of separation) on the new type column is by 1.6—2.3 times higher than that of the initial classical capillary column.     

Quantitative gas chromatographic analysis on support-coated open tubular capillary columns : I. Analysis of isomeric ethylphenols

Gas chromatographic methodology has been developed for quantitative analysis of samples of o-, m-, and p-ethylphenols. Samples are dissolved in a dichloromethane solution of the internal standard, anisole, and are then derivatized with N-trimethylsilylimidazole to form the silyl ethers. The samples are chromatographed with similarly prepared standards on a stainless-steel OV-17 support-coated open tubular (SCOT) column.Specificity, linearity, precision and stability of the samples are discussed, and chromatograms obtained on the SCOT column are compared to those obtained on a packed analytical column.This report describes one of the first quantitative gas chromatographic analytical methods to use a SCOT (capillary) column.     

Dual column gas chromatographic system for use in mass spectral determination of nitrosamines.

A packed gas chromatographic column and a support coated open tubular (SCOT) column are connected in series. Between the columns are two micro-volume switching valves, one enabling solvent to be vented. Short retention nitrosamines are passed through both columns, whereas longer retention nitrosamines by-pass the SCOT column by means of the other switching valve.     

Evaluation of Packed GLC Columns for Nanomolar Analysis of Unknowns Lincluding a New Type of Packed Column

Abstract

Fatty acid methyl esters, 2,6-dimethylaniline, and 2,6-xylenol were used for rapid evaluation of the usefulness of packed GLC columns for analysis of unknowns at the nanomolar level. Three types of column construction with three liquid phases of widely varying polarity were tested by the above procedure. A new type of GLC column, a dynamically coated packed column prepared with a surface active agent, was found to yield better overall performance for less polar liquid phases than packed silanized glass or packed stainless steel columns.     

Glass capillary SCOT columns by a single-step coating method

A single-step coating method for the preparation of glass capillary SCOT columns is described. It is reproducible and less time-consuming than the well-known two-step coating procedures. Other methods attempted are discussed briefly. Both the flame ionization and electron capture detectors could be used in conjunction with temperature programming. The separations achieved with an “activity mixture”, phenols and phenolic acids, illustrate the resolution obtained. The columns are suitable for quantitative determinations and a comparison is made with a conventional packed column.     

超细NaY分子筛的深度脱铝

通过优化和组合不同脱铝补硅方法,依次经氟硅酸铵处理、600oC水热处理、硅溶胶+草酸处理和800oC水热处理过程,成功实现了200nm超细NaY分子筛的深度脱铝,最终产品骨架硅铝比高达27.3,比表面积为581.9m2/g,分子筛结晶度保持在65%以上.结果表明,对于超细NaY分子筛脱铝,第一步采用氟硅酸铵进行部分缺陷修补尤为重要.根据分子筛晶粒尺寸不同,需严格控制氟硅酸铵用量和处理次数.当晶粒为200nm时,氟硅酸铵与分子筛骨架铝的摩尔比为0.16,处理一次较为适宜.在连续脱铝过程中及时补修脱铝产生的缺陷是保障超细NaY分子筛成功脱铝的关键,而采用氟硅酸铵、硅溶胶、800oC高温水热处理,可有效实施这种骨架修正作用.