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Gas chromatography & cc ms principles is2008-04-18
This document provides an overview of gas chromatography (GC) including its basic principles, instrumentation components, and detectors. GC separates molecules via vaporization and movement between a mobile gas phase and a stationary phase. Key components include the injector which introduces samples, the column for separation, the oven which houses the column, and various detectors for identifying molecules. Common detectors measure molecules via concentration-dependent or mass-dependent responses and can have universal or selective responses. The document also discusses GC-mass spectrometry which couples separation with identification capabilities.
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Gas chromatography & cc ms principles is2008-04-18
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- 2. What is chromatography • Separation Science • Organizing by size • Organizing by boiling point (vapor pressure) • Organizing by solubility Before After
- 3. What is GasChromatography • Performed in the vapor state • Requires a mobile phase, gas • Requires a stationary phase • Molecules migrate between the phases
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- 5. Gas Chromatographic Equipment AUTOSAMPLERS GC BASIC UNITS GC DETECTORS INTEGRATORS MS DETECTORS MS Detector Autosampler GC Detector Autosampler Data system GC Basic Unit Gaschromatog. DATA SYSTEMS SAMPLE PREPARATION SYSTEMS GC Basic Unit Data system SAMPLE PREPARATION AND INJECTION SYSTEMS CHROMATOGRAPHIC SEPARATION SYSTEMS DETECTION & IDENTIFICATION SYSTEMS DATA SYSTEMS GC/SA Benchtop GC/MS
- 6. GC Instrument :injector
- 7. Requirements for theideal injector • Capable to quantitative accept a broad volatility range of sample components – Low discrimination • To handle dirty and clean matrices – With dirty matrices reduces sample clean-up – With clean matrices boosts sensitivity • Extremely inert – Able to handle polar/active compounds • Provide optimum band shape
- 8. Vaporizing Injectors: SSL PPKD PKD PTV No-vaporizing Injectors: On-column Injection techniques
- 9. Injectors True coldon-column split/ splitless PTV Packed and wide-bore columns
- 10. General criteria forinjection system selection PTV PTV
- 11. PRIMARY COOLING SYSTEM SECONDARY COOLING SYSTEM SBP Room temperature Temp. Liquid sample droplets Liquid sample plug Liquid sample film 1 2 Carrier gas Primary cooling system Cooling fluid (secondary cooling) Oven temperature 3 Cold On-Column Injector
- 12. Split Injector Additional Insulating Carrier Septum Purge Split Line Glass Liner 5 mm ID Length of Column Inside Injector = 40 mm Capillary Column 7001-1417 970810 50 mm Syringe Splitting Point Liner Carrier Pathway Column Injector Chamber Terminal Fitting
- 13. Splitless Injector Carrier Septum Purge Split Line 80 mm Syringe Length of Column Inside Injector = 64 mm Capillary Column 77001-1416 970805 Additional Insulating Splitless Liner
- 14. PTV Injector Septum purge line Splitting line Carrier OVEN Liner Column Carrier gas inlet Septum Septum purge line Splitting line FORCED AIR COOLING Heating element
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- 16. GC Instrument :column oven
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- 23. Detectors Characteristics RESPONSEMECHANISM • Concentration dependent: TCD, ECD, PID • Mass rate dependent: FID, NPD, FPD NON DESTRUCTIVE DESTRUCTIVE • TCD, ECD, PID • FID, NPD, FPD RESPONSE TYPE • Universal: TCD, FID, (PID) • Selective: ECD, NPD, FPD, (PID)
- 24. FID : FlameIonization Detector Air Column effluent +Hydrogen
- 25. ECD : ElectronCapture Detector Radioactive source Outlet Column effluent + make-up gas
- 26. NPD : NitrogenPhosphorous Detector Collecting electrode Heated source Air Column effluent + Hydrogen
- 27. FPD : FlamePhotometric Detector Interference filter Photomultipier tube Air Column effluent + Hydrogen
- 28. PID : PhotoIonization Detector Heat sink Quartz cell UV lamp GC column Exit tube
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- 30. Coupling Chromatography to Mass Spectrometry Separation plus identification
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- 32. TRACE DSQ components Ion Source Analytical Quadrupole Curved Quadrupole Pre-filter Detector
- 33. Quadrupole Wiring •X Quadrupole Rod Pair • AC and pos DC Voltage • Y Quadrupole Rod Pair • AC and neg DC Voltage 0.5 1 1.5 2 Series1
- 34. Stability Regions APEX(0.706, 0.23699) YZ-stable XZ-stable
- 35. Mathieu Parameters RF= m r2 2 e 2qz DC = m r2 2 e 4az e = charge (constant =1) m = Mass in kg r = radius = distance between rod inner surface and center of quadrupole w = 2 * frequency (1100 kHz)
- 36. DSQ II SingleQuadrupole
- 37. Literature Available forDSQ II • Confirmation of Drugs of Abuse Application/Technical Notes Marijuana Cocaine PCP Amphetamines Opiates