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Gas Chromatograph

Sujeewa S. Palayangoda

Group meeting - 03/01/2006


What is chromatography?

• chromatography is a versatile technique for separating mixtures.

• strategy: flow the mixture over a material that retains some components more than
other different components flow over the material at different speeds.

• in chromatography, a mobile phase sweeps the sample over a stationary phase.


Advantages of chromatography

• can separate very complex mixtures such as drugs, foods, pesticides…………

• very small sample sizes can be used

• separated components can be collected individually

• analyses can be highly accurate and precise


General Classifications of Chromatographic Methods

• Column chromatography

• Paper chromatography

• Thin-layer chromatography

• Gas chromatography

• High pressure liquid chromatography

• Ion-exchange chromatography

• Gel filtration chromatography

• Supercritical fluid chromatography


History of Gas Chromatography

• The origin of gas chromatography can be dated back to 1905 when

W. Ramsey separated a mixture of gases and vapors from solid adsorbent

such as activated charcoal.

• Gas chromatography, where gas is used as a mobile phase, was first

introduced in 1952 by James and Martin. The technique was based on a

suggestion made 11 years earlier by Martin and Synge on partition

chromatography, for which they were presented the Nobel Prize in chemistry

in 1952.
Gas Chromatography is a versatile instrument in chemistry

• Testing the purity of compounds

• Determine relative amounts of compounds in chemical mixture

• Separation and analysis of chemical compounds

• Temperature of gas can be controlled


Schematic diagram of Gas Chromatograph

Filters/Traps Data system


H

RESET

Regulators Syringe/Sampler

Inlets

Detectors
Argon
Hydrogen
Oxygen

Column
Basic components of Gas Chromatograph

• Gas

• Flow control

• Injector

• Oven, Column

• Detector

• Eluents

• Recorder
• Gas

Three types of gasses are used 1. Ar or He or N2 – carrier gas

2. O2 – helps to burn column effluent

3. H2 – helps to burn column effluent

• Flow control

Helps to control gas flow


• Injector
• Column

Capillary column- 30m Packed column-3m

Cross-section of a column
These factors affect the separation

• Boiling points of components present in the sample

• Length of the column

• Flow rate of carrier gas

• Intermolecular interactions
1. Orientation interactions
The interactions between two permanent dipoles

2. Debye interactions
The interactions between a permanent dipole in one molecule
and the induced dipole in a neighboring molecule

3. Dispersion interactions
The forces arising out of synchronized variations in the
instantaneous dipole of the two interaction species
Commercially available GC detectors and their applications

Detector Application
Flame Ionization (FID) Carbon compounds
Thermal Conductivity Universal
(TCD)
Mass spectrometer (MSD) Variety of compounds

Electron capture (ECD) Halogenated compounds


Flame Photometric (FPD) S & P compounds

Atomic emission (AED) Metals, Halogen, C & O compounds


Radioactivity 3H & 14C compounds
Chemiluminescent Sulfur containing compounds
Photoionization (PID) Aromatic compounds
Nitrogen / Phosphorous N,P & halogen compounds
(NPD)
Electroconductivity (ECD) S & N compounds
• Detector

FID TCD

High temperature of hydrogen flame (H2 + O2) ionizes


compounds eluted from column into flame
Analysis

•The detector response is sent to a computer system where the progress

of the sample is monitored on the computer monitor in graphical form

that displays detector response as a function of run time.

•Each component of the mixture reaches the detector at a different time and

produces a signal at a characteristic time called a retention time.

•The area under a peak is related to the concentration of that compound.


Determination of Retention Time

Since Velocity = Distance


Time

Retention Time = Dist(cm)


Vel(cm/min)

Dist = Distance chart moves in cm


Vel = Velocity of chart in cm/min

Starting Point
On Chart

Distance
Peak Area by the
Triangulation Method

Peak Area
 Triangulation Method

Peak Area = h * w½

Where h = Peak Height

w½ = width of peak at
½ the Peak Height
Total Peak Area(TA) = A + B
Mole Fraction(MF) = A/TA, B/TA
Mole Percent = MF x 100
Recording

The detector information is sent to the printer that produces hard copy
of the chromatographic run.

Output from the printout


• The number of peaks correlates with the number of compounds in the sample

• The area under each peak correlates with the relative amount of each

components in the sample mixture


Acknowledgement

Dr. Daniel Berger

Thank you