CHAPTER 3

Gas Chromatography
 It encompasses all chromatographic techniques which use gaseous mobile
phase.

 We can use liquid stationary phase which is held in solid support material.
 The type of interaction is the partitioning of solute particles between the liquid
stationary phase and gas mobile phase.
 We can use also solid stationary phase.
 Separation takes place due to the difference in the degree of adsorption of
solute particles on the solid stationary phase.
 It is entirely column chromatographic technique.
 We can`t use stationary phase coated in paper or flat plate.

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 Instrumentation

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 Important components of GC
1. Mobile Phase (Carrier gas supply)
 He, H2, N2 are most common mobile phases in GC
 They are chemically inert toward both the sample and stationary phase.
 They interact weakly (no) with both the sample and stationary phase.
 Their only purpose is to transport the sample across the stationary phase.
 This is why they are usually called carrier gas.
 The choice of mobile phase in GC is based on the type of detector used.
 The best suitable gas for the detector used is selected as mobile phase.
Example. When we use thermal detectors, He is used as mobile phase
because it is more suitable as a mobile phase for thermal detectors than
other gases. This depends on the thermal conductivity of the carrier gas.

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2. Sample Introduction
 Three considerations determine how samples are introduced to the gas
chromatograph.

all constituents injected into the GC must be volatile or made to be volatile.

 By chemical derivatization or by heating. For example, amino acids which
are not sufficiently volatile can be made volatile by reacting it with 1-
butanol and acetyl chloride which produces an esterfied amino acid and
subsequent treatment with trifluoroacetic acid gives the amino acid’s volatile
Ntrifluoroacetyl-n-butyl ester derivative.
 Solutes of low volatility may be retained by the column and continue to
elute during the analysis of subsequent samples.

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3. Chromatographic columns
 A chromatographic column provides a location for physically retaining
the stationary phase.
 The column’s construction also influences
 the amount of sample that can be handled
 the efficiency of the separation,
 the number of analytes that can be easily separated,
 the amount of time required for the separation.
 Both packed and capillary columns are used in gas chromatography.
Selectivity in gas chromatography is influenced by the choice of stationary
phase.
Elution order in GLC is determined primarily by the solute’s boiling point
and, to a lesser degree, by the solute’s interaction with the stationary phase.

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 The following are criteria which are considered while selecting a stationary phase.
The stationary phase
a. must be chemically inert
b. must be thermally inert
c. low volatility (i.e. mostly the boiling point of the stationary phase must be
100 oC greater than the optimum temperature)
d. must have an appropriate polarity for the solutes being separated
 Usually the column is housed in a thermostat, which is used to adjust the
temperature of the column.
 This temperature is used for temperature programming purpose.
 The optimum temperature for the separation depends on the boiling point of
the stationary phase and degree of separation.

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 4. Detectors

 There is a detector at the end of the column which signals the change in the
nature of the gas flowing out of the column.

 Recall that helium is the carrier gas and will have a specific thermal
conductivity, for example. Other compounds have their own thermal
conductivities.

 The elution of a compound other than helium will cause a change in

conductivity and that change is converted to an electrical signal.

 The detector, in turn, sends a signal to a strip chart recorder or to a computer.

 Detectors come in several varieties, for example, thermal detectors, flame-
ionization and electron capture detectors.

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