先进材料表征技术-(I).ppt

Capillary chromatographic column Capillary columns are a thin fused-silica (purified silicate glass) capillary (typically 10-100 m in length and 250 μm inner diameter) that has the stationary phase coated on the inner surface. Capillary columns provide much higher separation efficiency than packed columns but are more easily overloaded by too much sample. How to select a column? GC is a mature science; it is highly probable that GC has already been applied to your type of sample as there are already over 100,000 GC publications. With ready access to Chemical Abstracts on-line, an experienced literature scientist should be able to come up with suggestions to help you. Handbook of GC Some examples will help to illustrate the effects of polarity on selectivity. To be effective as a stationary phase, the liquid chosen should interact with the components of the sample to be analyzed. The chemists rule of thumb like dissolves like suggests that a polar liquid should be used to analyze polar analytes and a nonpolar liquid for nonpolar analytes. nonpolar polar 三氯杀螨醇 硝苯硫磷酯 The polarity is crucial for the choice of stationary phase! (A) (B) Effect of stationary phase polarity on a 4-component separation: (a) Carbowax20Milll (polar); (b) DC-200 (nonpolar). Samples and their boiling points: (1) n-heptane (98); (2) tetrahydrofuran (64); (3) 2-butanone (80); (4) n-propanol (97). Reprinted with permission of the GOW-MAC Instrument Co., Bethlehem, PA, U.S.A. A large change in column polarity may result in a change in elution order. Thermal conductivity detector (TCD); Hydrogen flame ionization detector (FID). Detectors of GC: TCD detector: Principle: This detector senses changes in the thermal conductivity of the column effluent and compares it to a reference flow of carrier gas. Since most compounds have a thermal conductivity much less than that of the common carrier gases of helium or hydrogen, when an analyte elutes from the column the effluent thermal conductivity is redu