GAS CHROMATOGRAPHY

Gas chromatography (GC) is an analytical

technique used for separating compounds based primarily on
their volatilities. Gas chromatography provides both qualitative
and quantitative information for individual compounds present
in a sample. Compounds move through a GC column as gases,
either because the compounds are normally gases or they can
be heated and converted into gaseous state. The compounds
are partitioned between a stationary phase, which can be either
solid or liquid, and a mobile phase (gas). The differential
partitioning into the stationary phase allows the compounds to
be separated in time and space.

The particular advantage of using a gas as a

mobile phase is that high flow rates are possible often with long
columns. Another important practical advantage is that several
methods of detecting components in a flowing gas stream are
available. A further advantage is that it is relatively easy to find
a chemically innocuous gas which acts as no more than a
carrier of various vapours, though this can also be regarded as
a disadvantage in that the mobile phase cannot be used to
identify discrimination between materials.

In its simplest form, gas chromatography can be

regarded as a multiple distillation process, with separations
determined by relative volatilities, i.e. differences in the liquid
vapour equilibrium in various materials. Temperature variation
is the obvious way of controlling volatility and this is chemically
why temperature control is an important aspect of the
operation of gas chromatograph. Volatility is, however, not the
only factor of importance, since specific interactions with the
stationary phase, which is usually a liquid adsorbed on a solid
but which can be simple solid. The separation of simple gases
such as O2, N2, CH4 and CO2, for example, can be achieved on a
molecular sieve column, where in the size of pores within the
stationary phase determines whether or not a molecule enters
and diffuses within the solid, so being retarded additive to the
carrier gas.

One of the recent advances in gas

chromatography, in fact, has been a change to capillary glass
columns rather than the sometimes chemically reactive
stainless steel columns that were originally dominant. This use
of glass capillaries can be regarded as an offshoot of the
development of the optic technology. Another recent
development has been the use of open tubular rather than
wrecked columns. In these, the stationary phase is present as a
very thin film on the walls of only column rather than being
adsorbed on a finely divided solid which fills the column void.
The open column allows high flow rates and the thin film allows
very efficient mass transfer, so that extremely small values of
H result.

Basic Parts of a Gas Chromatograph

The basic parts of a gas chromatograph are shown in figure (a).

It consists of the following parts:
Carrier gas supply along with pressure regulator and flow
monitor,
Sample injection system,
Chromatographic column,
Thermal compartment or thermostat,
The detection system, and
Recorder.

The carrier gas, normally N2, Ar or He, is usually available

in a compressed form in a cylinder fitted with a suitable
pressure regulator. The gas is conducted from the cylinder
fitted regulator, to a sample injection port maintained at a
certain temperature T1, which is such that it ensures rapid
vaporization, but not thermal degradation of the solute.
Gas and liquid samples are almost always injected by
syringe through a self-sealing silicon rubber diaphragm in
the injection port. The solute vapour mixes almost
instantaneously with the flowing carrier gas and is swept
into chromatographic column, which is the heart of the
chromatograph. It is there that the different solutes in the
vaporized sample are separated from each other, by virtue
of their different interaction with the column packing. The
column is maintained at another temperature T 2. In
column packing temperature determines the time for the
passage of the solutes and to some extent, the resolute
and efficiency obtained with a particular column. At the
end of the column, the solutes emerges, individually enter
the detector, which produces an electrical signal
corresponding to the quantity of the solute leaving the
column. The detector signal is supplied to a recorder and a
plot of the thin signal amplitude called chromatograph is
obtained. This record is used to determine the
identification of the components in the mixture and their
respective concentrations.
The various parts of the gas
chromatographic system are described below:

In this detector, the effluent from the column is taken into

an oxy-hydrogen flame. An electric potential is applied
across two electrodes placed in a stainless steel housing.
The hydrogen flame burns at the tip of a capillary, which
also functions as the cathode and is insulated from the
body by a ceramic seal. The collector electrode consists of
a loop of platinum and is located at about 6mm above the
burner tip.
 The current across the electrodes
remains constant when only the inert carrier gas passes
the flame. However when the vapour of a compound
emerging from the column passes the flame, the vapour
molecules are broken into ions by the hot flame. These
ions result in the ionisation current and there would be a
consequent change in the current flowing across the
electrodes. The magnitude of the variation in the current
would be directly proportional to the number of ions or
electrons formed in the flame gases, which, in turn, would
be proportional to the carbon content of the organic
molecules in the vapour.
The flame ionisation detector has a
high out impedance similar to that obtained with glass
electrode when making pH measurements. Commercial pH
metres can, therefore, be easily adopted for use with this
detector. A vibrating reed electrometer is often used in
input stage of the amplifier to attain sensitivities up to 5 x
10- 13A. By placing a set of high resistors across the flame
and changing their resistances enables the sensitivity to
 be varied. The sensitivity is high, because of the
inherently low level of the detector.

A current amplifier with which a flame

ionisation detector can be used at all practicable
sensitivity levels. The amplifier makes use of the metal-
oxide silicon transistors in the input stage. The amplifier
gives a high degree of stability. The amplifier has a
sensitivity of 100mV pA- 1 and a noise output equivalent.
An rms at the input, thermal drift is typically 1 mV/ 0C. The
input stage of the amplifier consists of a matched pair of
MOSFETs, which is followed by a matched pair of p-n-p
transistors. The output stage is an emitter follower, while
the first stage is a long-tailed pair.
There are certain limitations in the use of
the flame ionisation detector. They are:
The FID does not respond to inert gases and inorganic
compounds.
The emerging components get destroyed in the flame.
The response to sample weight has to be separately
determined for each component.