chapter2-气相色谱分析.ppt

Chapter 2 Gas Chromatography(GC);●Mobile phase Stationary phase（流动相与固定相): Chromatographic separation involving partition of different species in a mixture in two phases, among which one phase (solid or liquid) does not move (stationary phase) , the other phase (gas or liquid) takes the sample mixture to pass through the stationary phase packed in the column( mobile phase) Separations are affected due to the differences of substances’ affinities for a mobile phase and a stationary phase(分离原理）. ;;;皂膜流量计;;Chromatogram of xylene isomers on a polar column ;Y;GC;Nomenclature of Chromatographic separation;●Baseline(基线) Chromatographic curve under the experimental operation conditions, no components of materials flow out after the column(在实验操作条件下，色谱柱后没有样品组分流出时的流出曲线称为基线，反映检测器系统噪声（Noise) 随时间的变化情况。稳定的基线应该是一条水平直线。);Nomenclature of Chromatographic separation;●Retention value 表示试样中各组分在色谱柱中滞留时间的数值。通常用时间或用将组分带出色谱柱所需载气的体积来表示。 ■ Rely on component partition on two phases (or absorption) ■Thermodynamic controlled (Properties of stationary phase operation conditions) ■ Qualitative Base ;●Rotention time tR The time at which the maximum of the peak appears after sample injection 见图;Nomenclature of Chromatographic separation;●Dead Volume VM 指色谱柱在填充后，柱管内固定相颗粒间所剩留的空间、色谱仪中管路和连接头间的空间以及检测器的空间的总和。当后两相很小可忽略不计时，死体积可由死时间与色谱柱出口的载气流速F0（cm3·min-1）计算。 VM = tMF0 式中 F0为扣除饱和水蒸气压并经温度校正的流速。 仅适用于气相色谱，不适用于液相色谱;●Rotention volume VR 指从进样开始到被测组分在柱后出现浓度极大点时所通过的流动相的体积。保留时间与保留体积关系： VR= tR F0 = tM F0 ;The ratio of adjusted rotention value of the second component to that of the first component r21= tR(2) ? / tR(1)′= VR(2)? / VR(1)? ? tR(2) / tR(1) ?VR(2) / VR(1) 由于相对保留值只与柱温及固定相性质有关，而与柱径、柱长、填充情况及流动相流速无关，因此，它在色谱法中，特别是在气相色谱法中，广泛用作定性的依据。; 在定性分析中，通常固定一个色谱峰作为标准（s），然后再求其它峰（i）对这个峰的相对保留值，此时可用符号?表示，即 ? = tR ?(i) / tR ? (s) 式中tR ?(i)为后出峰的调