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Instruments;
Carrier Gas
Flow regulators and meters
Sample injection system
Columns & ovens
Detectors
3
Schematic Diagram of Gas
Chromatograph
4
H2 inlet
(detector) N2 inlet
Air inlet
(make-up gas)
(detector)
He inlet
(carrier gas)
Process Flow Schematic
Detector (flame
Sample injection ionization
detector or FID)
Carrier gas
Air
(nitrogen or
helium) Hydrogen
Pack column
Column Temperature
Temperature too high, causes co-elution: poor resolution but faster separation
Temperature too low, longer elution times: compromise temperature or program
The Stationary Phase
requirements are:
Ideal detector:
High sensitivity to even small concentration
linearity, ie, less response to low concentration &proportional
response to high concentration
Large linear dynamic range
Compatible with the column, carrier gas, solvent, etc.
Useful at a range of temperatures
Good stability and reproducibility
Rapid response time
Easy to use
Stable, Predictable response
Inexpensive
operation from RT to 400 oC
Types of detectors
1. Thermal Conductivity Detector(TCD)
2. Flame Ionization Detector(FID)
3. Atomic Emission Detector(AED)
4. Electron Capture Detector(ECD)
5. Nitrogen Phosphoroes Detector(NPD)
6. Photo Ionization Detector(PID)
7. Flame Photometric detector(FPD)
8. Electrolytic conductivity detector (Hall detector)
9. Absolute Mass Detector(AMD)
10.Thermionic Detector(TD)
Flame Ionization Detector (FID)
Most widely used, Air-H2 flame
Number of ions depends on
number of reduced (methylene)
carbons in molecule
The positive ions will be attracted to the
cylindrical cathode.
Negative ions and electrons will be attracted to
the jet anode.
Organic compounds Produces ions and
electrons pyrolyzed(temp of flame) burner
tip and electrode
Ions &electrons move to ward the collector
less sensitive for non-hydrocarbon groups
Insensitive to noncombustible gases(CO2, SO2,
NO2 and H2O)
Insensitive to functional group Adv: High sensitivity, low noise ,wide
(carbonyl, alcohol, halogen and amine) linear range, easy to use, fast response
D.Adv: Destroy the sample
Thermal Conductivity Detector (TCD)
Element (platinum, gold or tungsten wire) is
electrically heated at constant power
– Temperature depends on thermal
conductivity (He & H)of surrounding gas.
Hydrogen and helium have higher thermal
conductivity and carrier gas provide best Thermal conductivity detector
sensitivity cell
Calibration curves:
standards of varying concentration are used determine peak areas
Separation of two polyaromatic hydrocarbons on a wall-coated open tubular column with different carrier gases.
Resolution, R, increases and analysis time decreases as we change from N2 to He to H2 carrier gas.