Chapter2stationaryphase.pptVIP

GC分类（P24-33） The most important factor in GC is the selection of the proper column stationary phase for the particular separation to be attempted. The nature of the liquid or solid phase will determine the exchange equilibrium with the sample components; depend on the solubility or adsorbability of the sample, the polarity of the stationary phase and sample molecules, the degree of hydrogen bonding, and specific chemical interactions. empirically; quantitative 气固色谱固定相的特点 表P25-26 填充柱气液色谱担体一览表 Liquid stationary phase 固定液 Over a thousand stationary phases have been proposed for GC, and numerous phases are commercially available. Hundreds of phases have been used for packed columns, necessitated by their low overall efficiency, and stationary-phase selection is critical for achieving selectivity. Several attempts have been made to predict the proper selection of liquid immobile phase without resorting exclusively to trial-and-error techniques. 例如 根据麦氏常数选择能分离下面样品 的合适固定相：（1）苯乙酮和苯 甲醇；（2）乙醇中痕量苯。 答：（1）两者沸点接近，都是极性物质，前者，中等极性，后者，可以发生氢键作用，极性大。如果要使苯乙酮先流出柱子而苯甲醇在后，选择Y ??（发生氢键相互作用）较大、Z ?（接受氢键能力）较小的固定液，Y ??与Z ?比值大，如聚乙二醇-2000等。 答：（2）要分析乙醇中痕量苯，苯应先出峰（为什么？）。两者极性不同，苯非极性物质，但易被极化；乙醇可以发生氢键作用，极性大。选择X ??小（与苯等易激化物质相互作用弱）、 而Y ?（氢键作用）较大的固定液，Y ??与X ?比值大，如SE-30等。当有多种固定液可选择时，考虑固定液的使用温度、黏度等性质。 Phases are selected based on their polarity, keeping in mind that “like dissolve like.” A polar stationary phase will interact more with polar compounds, and vice versa. 色谱柱及使用条件的选择 ? 固定液配比（涂渍量）的选择 Thermal conductivity detector TCD 热导检测器 Electron capture detector ECD 电子俘获检测器 Flame Photometric Detector FPD 火焰光度检测器 最低检测限 最小检测量 ： Qualitative and quantitative measurements 定性定量方法 By measuring the retention time and comparing this time with that of a standard of the pure substance, it may be possible to identify the peak agreement of retention times of two compounds does not guarantee the compounds are identical . 举例 测某一样品组分的保留时间分别为： 测某样品（甲苯）的保留时间分别为： The area under the peak is proportional to the