GC气相色谱.pptVIP

毛细管柱气相色谱 毛细管柱的发明使得气相色谱分析发生了革命性的变化！ 毛细管的理论塔板数可达到300,000！ 把填充柱色谱分析试样的沸点上限提高了100oC以上,分析样品的量和检测下限降低了1-2个数量级 毛细管气相色谱仪器和填充柱色谱仪类似,只是: 在进样口增加了分流/不分流装置——解决了柱容量小的问题； 以及在柱后增加了一个尾气吹扫气路——减少了柱和检测器连结处的死体积过大的问题； 通常采用程序升温技术。 分类: 按固定液涂渍方法不同，可分为: 开管柱(WSOT): 管内壁经处理后，直接涂渍固定液 小内径毛细管柱：内径小于0.1mm的毛细管柱，主要用于快速分析。 大内径毛细管柱：内径在0.3-0.5mm的毛细管，往往在其内壁涂渍5-8μm 的厚液膜 载体涂渍开管柱(SCOT)：管内壁经处理后，先涂载体，再涂固定液——液膜厚，因而柱容量大。 多孔层开管柱: 管内壁涂渍一层多孔吸附剂颗粒，不涂固定液，实际上是毛细管气固色谱柱。 In the most basic level, a capillary column is composed of two parts - the tubing and stationary phase Fused silica and stainless steel are the primary tubing materials. There are numerous stationary phases. Most are high molecular weight, thermally stable polymers that are or gums. The most common liquids stationary phases are the polysiloxanes and polyethylene glycols. The next most common type of stationary phases are small, porous particles composed of polymers or zeolites (e.g., alumina, molecular sieves). 外涂聚酰亚胺保护层的熔融石英管, 管壁薄，因而不和待测物作用、柔韧性好、强度高、易弯曲 A capillary column is characterized by its dimensions (L, i.d.) and by the nature of the stationary phase. For GLC, a relatively thin stationary (liquid) phase film, with film thickness df , is coated directly on the inner wall (WCOT columns). The film thickness controls the retention factor and the sample capacity of a capillary column. Most of the applications ( 90 %) in capillary GC are performed on WCOT columns. The selection of a capillary column depends on the complexity of the sample to be analyzed. The column length, the internal diameter, the stationary phase, and its film thickness determine the separation power (resolution), the sample capacity, the speed of analysis, and the detectability or sensitivity. Guidelines for the selection of film thickness for the stationary phase methylsilicone 0.1μm high molecular mass compounds 500-1500 0.2μm Mr ? 300 – 500 0.3μm Mr ? 150 – 400 0.5μm Mr ? 50 – 200 1μm Mr ? 30 – 150 仪器特点： 分流器和尾吹气装置 毛细管柱 苯、甲苯、乙酸丁酯、乙基苯