Techncal Specifications for the Xray Diffractometer用X射线衍射仪技术条件.docVIP

Lecture Notes Lecture 31 Chem. 4631 Gas Chromatography Introduction GC entails all chromatographic methods in which the mobile phase is gas. It may involve either a solid stationary phase or a liquid stationary phase retained on a solid solvent (packed column) or a column wall, such as in an open tubular column. Instrumentation Carrier Gas Carrier gas usually consist of He, N, H or a mixture of argon and methane. The function of the gas is to carry the sample through the system. The carrier gas must be: inert toward the sample dry thermally stable safe cost effective compatible with the detector This can be seen with the following van Deemter curve: To reduce deterioration of the stationary phase and to lessen detector noise – very high purity gas needs to be used. For this reason oxygen and moisture traps in the carrier gas lines are used. The flow of gas is described by two variables Carrier gas is regulated by a flow controller – older flow controllers were diaphragm types with a polymeric membrane, newer instruments use electronic programmable flow controllers. Sample Injection Peak widths are influenced by the efficiency of the injection process. The shorter the length of the column occupied by the injected sample, the shorter the band as it begins and completes the chromatographic process. The critical function of the injection process is to introduce the sample so that it occupies the shortest possible length of column. Syringe Technique Reproducibility with gas samples is poor since the volume of gas is temperature dependent. Several techniques are used to inject the sample. A vaporizing injection can retain the sample in the needle when introduced into the injection port. Hot needle - sample in barrel only Cold needle - sample in barrel only Filled needle - sample in barrel and needle. Solvent flush - solvent + sample + solvent or solvent + air + sample + air. Split Injection Sample is injected using solvent flush or hot needl