Gas Chromatography

Assignment of

Instrumental Methods of
Analysis
[PHS-CC-7101]

Supervisors: Submitted by:

Prof. Ashmita Gajbhiye Mehak Kesharwani
Dr. Adarsh Sahu [Y19150030]
B.Pharm ,VII semester

Department of Pharmaceutical Sciences

Dr. Harisingh Gour Vishwavidyalaya, Sagar (M.P)
(A Central University)
 CERTIFICATE

This is to certify that Mehak kesharwani, student of B.pharm ,Vll semester has
successfully completed the assignment on the topic “Gas Chromatography (introduction
and theory)” under the guidance of respected subject teachers during the year 2022-23.

Signature of teacher
 ACKNOWLEDGEMENT

I would like to express my special thanks of gratitude to Prof. Ashmita Gajbhiye, who gave
me the golden opportunity to do this assignment of Instrumental Methods of Analysis on Gas
chromatography (introduction & Theory).
I came to know about so many new things.
I would also like to thank my parents and friends who helped me a lot in completing this
assignment within the limited time frame.

Mehak Kesharwani
Y19150030
B.pharm, Vll semester
 CONTENT

o Introduction
o Gas chromatography
o Types of Gas Chromatography
o Principle of Gas Chromatography
o Criteria for compounds to be analysed by GC
o How a Gas Chromatography Machine Work’s
o Theories of Gas Chromatography
 Introduction

In early 1900s, Gas chromatography (GC) was discovered by Mikhail Semenovich Tsvett as
a separation technique to separate compounds. In organic chemistry, liquid-solid column
chromatography is often used to separate organic compounds in solution. Among the various
types of gas chromatography, gas-liquid chromatography is the method most commonly used
to separate organic compounds. The combination of gas chromatography and mass
spectrometry is an invaluable tool in the identification of molecules. A typical gas
chromatograph consists of an injection port, a column, carrier gas flow control equipment,
ovens and heaters for maintaining temperatures of the injection port and the column, an
integrator chart recorder and a detector. To separate the compounds in gas-liquid
chromatography, a solution sample that contains organic compounds of interest is injected
into the sample port where it will be vaporized. The vaporized samples that are injected are
then carried by an inert gas, which is often used by helium or nitrogen. This inert gas goes
through a glass column packed with silica that is coated with a liquid. Materials that are less
soluble in the liquid will increase the result faster than the material with greater solubility.
The purpose of this module is to provide a better understanding on its separation and
measurement techniques and its application. In GLC, the liquid stationary phase is adsorbed
onto a solid inert packing or immobilized on the capillary tubing walls. The column is
considered packed if the glass or metal column tubing is packed with small spherical inert
supports. The liquid phase adsorbs onto the surface of these beads in a thin layer. In a
capillary column, the tubing walls are coated with the stationary phase or an adsorbant layer,
which is capable of supporting the liquid phase. However, the method of GSC, has limited
application in the laboratory and is rarely used due to severe peak tailing and the semi-
permanent retention of polar compounds within the column.

The development of GC as an analytical technique was pioneered by Martin and Synge and
James 1941;

They suggested the use of gas-liquid partition chromatograms for analytical purposes.

Archer J. P. Martin Anthony James Richard L. M. Synge

 Gas Chromatography

Separation of gaseous & volatile substances. Simple & efficient in regard to separation.
In performing gas chromatographic separation, the sample is vaporized & injected onto the
head of a chromatographic column.

Elution is brought about by the flow of an inert gaseous mobile phase.

Gas chromatography is a term used to describe the group of analytical separation techniques
used to analyze volatile substances in the gas phase. In gas chromatography, the components
of a sample are dissolved in a solvent and vaporized in order to separate the analytes by
distributing the sample between two phases: a stationary phase and a mobile phase. The
mobile phase is a chemically inert gas that serves to carry the molecules of the analyte
through the heated column.
Gas chromatography is one of the sole forms of chromatography that does not utilize the
mobile phase for interacting with the analyte. The stationary phase is either a solid adsorbent,
termed gas-solid chromatography (GSC), or a liquid on an inert support, termed gas-liquid
chromatography (GLC).
 TYPES OF GAS CHROMATOGRAPHY

Based on stationary phase used in column, GC are of two types as follows:

i. Gas solid chromatography (GSC)

Mobile phase – gas
Stationary phase – solid

ii. Gas liquid chromatography (GLC)

Mobile phase – gas
Stationary phase – liquid

Stationary phase is liquid that is retained/coated on the surface of an inert solid by adsorption
or chemical bonding

GLC finds much greater application in the analysis of most of the organic compounds,while
GSC has limited application owing to:

a. Semi-permanent retention of active or polar molecules which reduces the available area.

b. Severe tailing of elution peaks (a consequence of nonlinear character of adsorption

process)

c. Difficulty in reproducing surface conditions

d. Surface catalyst also plays a restricting role

e. GSC finds application only in the separation & determination of low molecular mass gases
such as air components, hydrogen, sulphide, CO and nitrogen oxides.
  PRINCIPLE OF GAS CHROMATOGRAPHY

1.GSC principle is “Adsorption”.

Mobile phase – gas

Stationary phase – solid

When a carrier gas containing analytes is passed through a column containing solid SP the
analytes get adsorbed on to the solid SP & the separation is due to differences in their
adsorptive behaviour.

2. GLC principle is “Partition”

Mobile phase – gas

Stationary phase – liquid

 When a carrier gas containing analytes is passed through a column containing liquid
SP, the analytes get distributed themselves between the liquid SP & the carrier gas
phase according to their partition coefficients.

Partition co-efficient is the ratio of solubility of a substance distributed between two

immiscible liquids at a constant temperature

Compounds are separated by their different affinities to the column during the
stationary phase. Compounds with less affinity will elute from the column sooner;
compounds with greater affinity will elute later.
 Criteria for compounds to be analysed by GC

The criteria are as follows;

Volatility
Unless a compound is volatile, it cannot be mixed with mobile phase. Hence volatility is
important.
Thermostability

All the compounds will not be in the form of vapour. There will be solid as well as liquid
samples. Hence to convert them to a vapour form, they have to be heated to a higher
temperature. At that temperature, the compounds have to be thermostable.
Vapour pressure

The analyte should have a measurable vapour pressure at the temperature employed.

How a Gas Chromatography Machine Works

• First, a vaporized sample is injected onto the chromatographic column.

• Second, the sample moves through the column through the flow of inert gas.
• Third, the components are recorded as a sequence of peaks as they leave
the column.

Deals with both the stationary phase and the mobile phase.
Mobile – inert gas used as carrier.
Stationary – liquid coated on a solid or a solid within a column

Theories of Gas Chromatography

1.Gas solid chromatography technique follows the laws of Freundlich or Langmuir.

According to Freundlich or Langmuir law when a gas comes in contact with an adsorbent
certain amount of the gas is adsorbed on the surface of the adsorbent.

This phenomenon is explained by the following expressions.

Freundlich’s Law states: x/m = KC¹/n

Langmuir’s Law states: x/m = K₂C + K₂C

Where ; x = Mass of the gas absorbed

 C= Concentration of vapour in the gas phase
K, K, Ky=Constants

2.Gas liquid chromatography follows the Henry’s law of partition.

Henry’s law of partition states that ;

“At constant temperature, the mass of a gas dissolved in a given volume of a solvent is
directly proportional to its partial pressure in the gas phase in equilibrium with the solution”.
Thus when gas comes in contact with liquid certain amount of gas is dissolved in the liquid
according to;
x/m = KC
 REFERENCES

Sankar Ravi.S; “Textbook of Pharmaceutical Analysis”, Rx publication, Tirunelveli ; 5th

Edition ; 2018; 17.1-2

K. R. Mahadik, L. Sathiyanarayanan; “A textbook of instrumental method of analysis”, Nirali

Prakas, New Delhi; 2022;14.2-3

S. Malathi ,Pallavi Mangesh Pati, Sunil Kumar ; “ Instrumental Methods of Analysis”,

Thakur publications Pvt ltd, Lucknow ;2022; 210-12