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GC. Schematic of a GC. Typical GC. Computer Controls for Method and Output . Carrier gas/ Regulator. Varian 3350 Gas Chromatograph. Separation. Flow of Mobile Phase. Injector. Detector. T=0. T=10’. T=20’. Most Interaction with Stationary Phase Least. GC – Peak Broadening.
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Typical GC Computer Controls for Method and Output Carrier gas/ Regulator Varian 3350 Gas Chromatograph
Separation Flow of Mobile Phase Injector Detector T=0 T=10’ T=20’ MostInteraction with Stationary PhaseLeast
GC – Column Efficiency Capillary Packed
GC – Sample Capacity Effect 0.53 mm 0.25 mm
GC – Film Thickness Effect 0.25mm 1.0mm 3.0mm 5.0mm
GC – Isothermal and Programming 500C 3min To 1400C at 100C/min 1050C 500C
GC – van Deemter Plots/Curves N2 He H2
GC - Injectors • SPLIT INJECTOR • Advantage - Limitations • Injected zone narrow • Small sample aliquot avoids overloading • Mass discrimination of sample components (different range of volatility) • Systematic errors for quantitative analysis • In trace analysis: only part of analytes to detector
GC- Injectors • SPLITLESS INJECTOR • Advantage - Limitations • Avoids large tailing of solvent peak • Allows transfer of main part of sample components into detector • Trace analysis: favourable technique for insertion of diluted samples • Recondensation of solvent at top of capillary: possible damaging stationary phase • Only columns with chemically bonded phases • Necessary wettability of stationary phase for condensed solvent (droplets)
Injection Technique and Peak Discrimination Filled Needle Hot Needle Cold On-Column
GC - Injectors • Advantage of on-column injector: • avoids mass discrimination effects • trace analysis: enables quantitative insertion of sample into column (and detector) • labile components not stressed thermally
Chromatography – Sampling Rate and Accuracy 2 Hz 25 Hz