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An Introduction to Chromatography

An Introduction to Chromatography. What is chromatography? The separation of a mixture by distribution of its components between a mobile and stationary phase over time mobile phase = solvent or gas stationary phase = column packing material. Purpose of Chromatography.

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An Introduction to Chromatography

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  1. An Introduction to Chromatography • What is chromatography? • The separation of a mixture by distribution of its components between a mobile and stationary phase over time • mobile phase = solvent or gas • stationary phase = column packing material

  2. Purpose of Chromatography • Analytical - determine chemical composition of a sample • Preparative - purify and collect one or more components of a sample

  3. Schematic of a Gas Chromatograph Detector Syringe Flow splitter Rotameter Two-stage pressure regulator Injector Flow controller Temperature controlled zones Carrier gas supply Column

  4. Carrier Gas Supply

  5. Injector and Detector 300Vdc

  6. 300Vdc

  7. Injection types

  8. A Capillary Column for GLC A thin layer of nonvolatile stationary phase is coating on the inner wall of the tubing (WCOT) • Polydimethylsiloxane (silicone) • Good for retaining and separating nonpolar solutes by boiling point Fused silica tubing dc 0.3 mm df 1 m L = 15 - 60 m

  9. OH OH OH OH O O O O Si Si Si Si CH3 CH3 Cl O Si Cl Cl Si OH + Si Si CH3 CH3 CH3 CH3 OCH3 O Cl + CH3OH Si O Si Si Si CH3 CH3

  10. 4 1 Isothermal at 45oC 2 3 5 0 10 20 30 5 6 Isothermal at 145oC 7 8 0 10 20 30 4 Programmed from 30o to 180oC 9 8 3 1 5 6 7 2 Time 0 10 20 30 Temperature(oC) 30 60 90 120 150 180 Effect of temperature on gas chromatograms

  11. Capillary GC-MS GC Data system Quadruple MS Transfer Line Fused silica Column

  12. Packed column GC-MS Interface Nozzel Jet separator From GC Skimmer To MS Carrier Sample To vacuum pump

  13. Components of a Mass Spectrometer 10-5 to 10-8 torr Gaseous ion sources Mass analyzer Ion transducer Ion inlet Vacuum pump Signal processor

  14. Sample inlet • batch inlet • direct probe inlet • chromatographic inlet

  15. Direct probe A sample probe for inserting a sample directly into an ion source Vacuum pump Heating coil Direct insertion probe Ionization chamber

  16. Shield Heater Filament Electron beam 2nd accelerating slit 1st accelerating slit Repeller To mass analyzer Focusing slit Molecular leak Anode

  17. Quadruple Mass Spectrometer Ions with stable trajectories Ions with unstable trajectories Ion source Dc and ac oltages

  18. Continuous Dynode Electron Multiplier Resistive conductive surface 2kV GND

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