GAS CHROMATOGRAPHY

Histo
1940s Martin establish chromatography
ry
1950s first publication by Martin and
James of gas-liquid chromatography
Mid 1950s first commercial gas
chromatograph (manufactured by Griffin
and George)
 Gas Chromatography
Distinct Feature: the use of a gas as a moving, or mobile
phase.
istinguished by the different times which they take
to pass through the column the retention times.
Retention Time - dictated by the position of its
distribution equilibrium between the two phases.
 Gaseous Mobile Phase
role in the separation to carry the components
through the system.

Stationary Phase
greatest contribution to a separation,
interactions between it (solvent) and the
components (solutes) are both strong and varied.
GC INSTRUMENTATION SYSTEM
 CARRIER GAS
little interaction between the sample molecules and
the mobile phase
serves as a carrier of the sample

INJECTION PORT
heated to a temperature at least 50C above
the boiling point of the lowest boiling sample
component
TYPES OF INJECTION
SYSTEM
1. Packed Column Injector
(PKD)
2. On column Injection System (OCL)
3. Split / splitless Injection
(S/SL)
4. Programmed
Temperature
Vaporization Injector
(PTV)

- This technique avoids the

selective vaporization of volatile
sample components from the
tip of the syringe needle
5. Headspace Analysis
Types of headspace
methods:

Static Method the volatile

liquid sample is contained in a
sealed, thermostated vessel.

Dynamic Methods include

gas phase stripping analysis
and purge and trap.
6. Autosamplers
commonly used to allow
unattended use of the
chromatograph

the samples are contained

within small vials loaded onto
the autosampler carousel.
compressed air is used to
inject the sample from the
autosampler syringe into the
GC.
GAS CHROMATOGRAPHY COLUMN
TWO TYPES OF GC
COLUMNS:
1. Packed
made from glass or stainless tube, coiled to fit
inside the column oven.

2. Open tubular (capillary)

made from fused silica;
have greater separation efficiency than packed
columns.
COLUMN OVEN
A temperature which is equal to or slightly above the average
boiling point of the sample will give the reasonable elution time.

TYPES OF TEMPERATURE CONTROL OF OVEN:

1. Isothermal elution
elution using a constant temperature

2. Temperature programmed elution

elution whereby column temperature increased as separation
proceeds.
DETECTORS
TYPES OF GC DETECTORS
Flame ionization detector (FID)

PRINCIPLE:
Effluent from the column is mixed with hydrogen and
air, then ignited.
The resulting gaseous cations (positive ions) are
attracted to a negatively charged collector electrode,
located above the flame.
FLAME IONIZATION DETECTOR (FID)
FLAME IONIZATION DETECTOR (FID)

APPLICATION:

commonly used for the analysis of most

organic samples;
does not respond to non combustible
gases, such as H2O, CO2, and SO2
ELECTRON CAPTURE DETECTOR
(ECD)
PRINCIPLE:
Effluent from the column passes between two electrodes within
the ECD;
One of the electrodes has on its surface a radioisotope such as
nickel-63 or tritium, which are emitters of -particles.
Bombardment of the carrier gas by these high energy electrons
results in the formation of a plasma of positive ions, radicals and
thermal electrons.
ELECTRON CAPTURE DETECTOR (ECD)
ELECTRON CAPTURE DETECTOR (ECD)

APPLICATION:
Selective towards molecules which contain
electronegative functional groups

Insensitive towards amines, alcohols and hydrocarbons