2. Introduction
It is one of the separation technique
Gas is used as the mobile phase, solid or liquid are used as the stationary phase
Solid is not mostly used, liquid stationary phase is used
GSC is not widely used
GSC: principle is adsorption
GLC: principle is partition
PRINCIPLE:
Partition, the liquid coated on solid support then used as stationary phase
The components are separated according to the solubilities
More soluble in stationary phase: elute latter
Less soluble in stationary phase: elute first
The components are separated according to partition coefficient
3. REQUIREMENT FOR COMPOUND ANALYSED BY GLC:
1. Volatility: the compound possible to convert volatile state then only it is mixed with mobile
phase
2. Thermo stability: All the compounds convert into vaporised state by using high temperature then
only used, so at high temperature the compound is stable
REQUIREMENTS:
Carrier gas
Flow regulator
Injection device
Column
Temperature control device
Detectors
Recorders
4.
5. CARRIER GAS:
Mostly used inert gases for mobile phase
Eg: hydrogen , helium, nitrogen and argon
Hydrogen:
Thermal conductivity is more, low density, very useful in case of thermal conductivity
and flame ionisation detector
Disadvantage: it reacts with unsaturated compounds
6. HELIUM:
Advantage: Thermal conductivity is more.
Disadvantage: Expensive
REQUIREMENTS OF CARRIER GAS
Inertness
Suitable to detector
High purity
Easily available and cheap
Less risk of explosion or fire hazards
FLOW REGULATORS AND FLOW METERS:
The carrier gas supplied at high pressure so to use flow regulator, to regulate the pressure
Flow meter to regulate the flow rate of the gas
Eg: rotameter, soap bubble flow meter
7. Rotameter:
It is appearing like glass tube containing spring
Fixed before the column inlet
To pass the gas
The spring is floated then measure the flow rate
Soap bubble meter:
Instead of spring to use soap solution
To pass the gas solution soap bubble is form then it travels particular pressure
INJECTION DEVICE:
To use gas, liquid or solid samples
Gases are introduced by using valve devices
Liquid are introduced by using septum device
Solid: dissolve in particular solvent then introduced in to column
8. COLUMNS:
Important part of the instrument
Made of glass or stainless steel
Two types
1. Depending on its use: Analytical column, Preparative column
2. Depending on its nature: Packed column, open tubular or capillary column
ANALYTICAL COLUMN:
Length:1-1.5m, diameter: 3-6mm
To use only small quantity of sample
PREPARATIVE COLUMN:
Length: 3-6m, Diameter: 6-9 mm
To use large amount of samples. Possible to loaded
9. PACKED COLUMN:
Commercially available
Available in polar and non polar nature
Eg: polydimethyl.siloxane, poly siloxane, poly alkylene glycol, polyethylene glycol
Temperature range 60-320ºC
CAPILLARY COLUMN:
Made of capillary tubing of 30-90m in length
Diameter(internal)0.025-0.075cm
Made of stainless steel in the form of coil
The inner wall is coated with stationary phase liquid of a thin film 0.5-1µ
These have least resistance to the flow of carrier gas
SCOT COLUMN:
Support coated open tubular column
10. It is improved type of capillary column
The supporting material is micron size in porus layer
The the lliquid stationary phase is coated so to get more sample holding
PREHEATERS:
For GC to convert the sample in to vaporised state
The preheaters are present along with injection device
THERMOSTATICALLY CONTROLLED OVEN:
To keep the column in thermostatically controlled oven by maintaining the temperature only to get
equal distribution between the solutes in mobile phase
Column is kept at high temperature oven
The columns are highly accurate and it maintains temperature to 0.1ºC
11. Two types of operations are possible:
1. Isothermal programming: to maintain the same temperature up to the process
2. Linear programming: the oven is heated linearly over a period of time. To fix the temperature
initially 150ºC but at the end of process it becomes 200ºC
DETECTORS:
To detect the component after separation mainly to detect the component present in the carrier gas
Applicable to wide range of sample
High sensitivity
Rapid response
Linearity
Not to destructive the sample
Simple to maintain
In expensive
12. THERMAL CONDUCTIVITY DETECTOR[KATHAROMETER]
Principle: to measure the thermal conductivity difference between carrier gas and that of
katharometer
Method:
It consist of two platinum wirs
Both connected to wheatstone bridge
One side pass only carrier gas other side to pass eluent from column
The two platinum wires heated electrically
To maintain temperature and electrical resistance
To measure the baseline
The compound eluted from column to get electrical resistance
It is amplified and recorded
Hydrogen and helium is most widely used carrier gas good thermal conductivity
Advantage:
It is used for wide range of compounds, good linearity and simple
14. Disadvantage:
Low sensitivity, affected by fluctuation in temperature and flow rateresponse is only relative
Biological samples cant be analysed
FLAME IONISATION DETECTOR:
The ionisation detectors are based upon the electrical conductivity of carrier gas
At normal temperature and pressure gasses act as insulators, but become conductive if ions are
present
Carrier gas: Hydrogen if used any other carrier gas to mix with hydrogen then use it
Advantage:
Extremly sensitive
Stable, organic compounds mostly used, linearity is excellent
To pass the carrier gas from the column
If only hydrogen or carrier gas no ionisation
Produce electrical pulse
Compound is present ionisation takes place
15.
16. ARGON IONISATION DETECTOR:
Argon atoms are excited by using alpha , beta particles
Meta stable state --------- pass carrier gas with effulent-------------argon are ionised------- then
produce electrical pulse
Argon treated with Radium.D or tririum, it goes to metastable state-------pass the carrier gas---
ionised, electric current pulse
Applications:
Qualitative: to identify the compounds, to check the purity, identification of impurities
Quantitative: %purity,
Direct comparison method
Calibration curve method
Internal standard method