Session 18

Gas Chromatography

1
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Gas Chromatography
Contents
Gas chromatography
Principle involved
Criteria for compounds

Practical requirements
Carrier gas
Flow regulators and flow meters
Injection devices
Columns

2
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Objectives

By the end of this session, students will be able to:

Explain the principle involved in Gas Chromatography

Outline the components of GC

State ideal characteristics of carrier gas

3
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Gas Chromatography
Consists of gas solid chromatography (GSC) and
Gas liquid chromatography (GLC)
In both types gas is used as mobile phase
Either solid or liquid as stationary phase

Gas Solid Chromatography (GSC)

Not widely used because of limited number of stationary phases available
Principle of separation is adsorption
Used for low solubility of solutes in stationary phase
It happens very rare
We discuss more about GLC

4
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Gas Chromatography
Gas Liquid Chromatography (GLC)
Principle involved is partition
Gas is used as mobile phase
Liquid which is coated on to a solid support is used as stationary phase
Mixture of components to be separated is converted to vapor and mixed with
gaseous mobile phase
Component which is more soluble in stationary phase travels slower and eluted
later
Component which is less soluble in stationary phase travels faster and eluted first
No two components have same partition coefficient for a fixed combination of
stationary phase, mobile phase and other conditions
Components are separated according to their partition coefficients

5
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Criteria for Compounds
Criteria for compounds to be analysed by gas chromatography

Volatility
Unless a compound is volatile, cannot be mixed with mobile phase

Thermostability
All the compounds will not be in the form of vapor
Will be solid or liquid samples
To convert them vapor, have to be heated to a higher temperature
At that temperature, compounds have to be thermostable
Only thermostable compounds can be analysed by GC

6
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Practical Requirements
Carrier gas
Flow regulators and flow meters
Injection devices
Columns
Temperature control devices
Detectors
Recorders and Integrators

7
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Carrier Gas
Choice of carrier gas determines the efficiency of chromatographic separation
Most widely used carrier gas are hydrogen, helium, nitrogen and argon
Hydrogen
It has better thermal conductivity, low density
Useful in case of thermal conductivity detector and flame ionization detector
Drawback- reacts with unsaturated compounds
It is inflammable

Helium
Has excellent thermal conductivity
It is expensive
Good carrier gas when used with thermal conductivity detector
8
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Carrier Gas
Nitrogen
Inexpensive but has reduced sensitivity

Requirements of carrier gas

Inertness
Suitable to the detector used
High purity
Easily available
Cheap
Less risk of explosion or fire hazards
Should give best column performance consistent with required speed of analysis

9
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Carrier Gas
Considering the requirements nitrogen and helium are the most commonly used
carrier gas
Carrier gases are compressible, stored under high pressure in cylinders

Flow regulators
Used to deliver the gas with uniform pressure or flow rate

Flow meters
Used to measure the flow rate of carrier of gas
Rotameter and soap bubble flow meter

10
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Flow Meters
Rotameter
Placed conveniently before column inlet
Has an ordinary glass tube (like burette) with a float held on to a spring
Level of float is determined by the flow rate of carrier gas
It is precalibrated

Soap bubble meter

Similar to rotameter
Instead of float, soap bubble indicates the flow rate
It has a glass tube with a inlet tube at the bottom through which gas comes in
Rubber bulb is used to store soap solution

11
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Flow Meters
Bulb is gently pressed for release of soap bubble by pressure of carrier gas and
travels up
Distance travelled upwards is a measure of flow rate of carrier gas
Graduations are precalibrated

Injection devices
Samples for introducing into the column can be of any type
Either gas, liquid or solid in nature
Gases can be introduced into column by valve devices
Liquids can be injected through loop or septum devices
Most GC instruments have high quality rubber septum through which sample
solution is injected

12
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Injection Devices
Solid samples are dissolved in a suitable solvent and injected through a septum

Columns
Important part of GC which decides separation efficiency
Made up of glass or stainless steel
Stainless steel columns have advantage of long life
Can be easily handled without the fear of fragility
But some samples react with them

In such cases glass columns are used (Example: steroids)

Have the advantage of inert
But highly fragile and difficult to handle
13
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Columns
Can be classified according to nature and use
Depending on its use

Analytical column
Have a length of 11.5 metres and outer diameter of 3-6 mm
Packed columns and are made up of glass or stainless steel
Only small quantity of samples can be loaded on to the column

Preparative column
Larger when compared to analytical columns
Large amount of samples can be loaded
Have a length of 3-6 metres and outside diameter of 6-9 mm

14
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences
 Summary
Consists of gas solid chromatography (GSC) and Gas liquid chromatography (GLC)
In both types gas is used as mobile phase
Liquid which is coated on to a solid support is used as stationary phase in GLC
Component which is more soluble in stationary phase travels slower and eluted
later
No two components have same partition coefficient for a fixed combination of
stationary phase, mobile phase and other conditions
Criteria for compounds to be analysed by gas chromatography- should be
volatile and thermostable
Choice of carrier gas determines the efficiency of chromatographic separation
Most widely used carrier gas are hydrogen, helium, nitrogen and argon
Flow meters- Rotameter and Soap bubble meter

15
Faculty
FacultyofofEngineering
Pharmacy & Technology M. S. Ramaiah University of Applied Sciences