Introduction

 Chromatography is used in analytical chemistry for analyzing and separating the compounds from
a sample mixture.
 Gas Chromatography is used to separate and analyze compounds that can be vaporized without
decomposition.
 Here the volatile mixture is separated by using a gaseous mobile phase.
 Another term given to Gas Chromatography is “Vapor-Phase Chromatography (VPC)”, or Gas–
Liquid Partition Chromatography (GLPC)”. Mobile phase in GC is a carrier gas, which is inert in
nature such as helium, hydrogen or nitrogen.
 Stationary phase can be either a microscopic layer of liquid or polymer layered on the inert solid
support, inside a column made up of metal or glass. The liquid material used for stationary phase
should have high boiling point like that of silicone grease or wax.
 Types of Analysis
Gas chromatography can be used for:

1) Qualitative analysis
The identification & separation is done by comparing the volume of the sample or
retention time to the standard or by collection of the individual components as they
emerge from the chromatograph and later on identifying them by other methods.
2) Quantitative analysis
In Quantitative analysis parameters of the chromatogram are determined by Gas
Chromatography in relation to the amount of the corresponding component of the injected
sample. It is necessary to measure the peak area or peak height of each component to analyze
the components quantitatively. For the well resolved peaks, both peak
height and area are proportional to the concentration of the component.

3) Checking the purity of a compound

In preparative chromatography purity of a compound can be checked by comparing the
chromatogram of the standard & the sample.
 On the basis of mobile phase and stationary phase used, Gas Chromatography can be broadly
classified into two:
1. Gas-Liquid Chromatography (GLC)

 The name of the technique refers to the mobile phase (gas) and stationary phase (liquid) respectively and GLC
is often referred to as gas chromatography which is based on the principle of partition co-efficient.

 The non-volatile liquid is coated on the inert solid powder (solid support) as a thin layer or along the inner wall
of capillary tubing and this liquid film helps in partitioning of the sample components between stationary phase
(liquid layer) and mobile phase (carrier gas)

 The solid support used in GLC includes materials like glass powder, diatomaceous earths, powdered Teflon,
crushed firebricks, carbon black etc while the liquid layer applied over solid support should generally have low
volatility and high decomposition temperatures e.g. polyethylene glycol, dimethyl silicone, diethylene glycol
succinate (DEGS) etc.

 Length of these capillary columns range from 30 m of 100 meters with internal diameter of 0.1 mm – 0.53 mm.
2. Gas-Solid Chromatography (GSC)

 The name of the technique refers to the mobile phase (gas) and stationary phase (solid)
respectively.
 The basic principle of Gas solid chromatography is physical adsorption
 In general, the column length is up to 10m with internal diameters ranging from 2-4mm
ADVANTAGES OF G.L.C OVER G.S.C

a. Shorter analysis time and better resolution between the peaks.

b. GLC can be used for both, quantitative and qualitative analysis.
c. Large concentration range of samples can be evaluated in GLC.
d. Wide range of stationary phase i.e. liquid coating is available for large number of
separations.
 INSTRUMENTATION
The equipment generally consists of
1. Supply of carrier gas
2. An injector
3. Temperature regulated oven,
4. Column,
5. Detector (at a short distance from the column)
6. Recorder
 CARRIER GASES: SUPPLY AND CONTROL
 Carrier gas or the mobile phase is an important component in Gas Liquid Chromatography and
should be inert in nature such as helium, hydrogen or nitrogen.
 Pressurized cylinder or bottled gas supply are the most common gas source that readily supplied by
vendors as steel tank with pressure regulator. The pressure regulator regulates the gas supply so that
correct pressure is fed to the required part of the instrument.
 In 90% of the GC systems, extremely pure Helium is used. Helium gas entering the separating
column is passed through at least a resin trap that removes oxygen, hydrocarbons, trace analytes,
and/or water vapor which might interfere with the analysis part, or degrade the column or interfere
with the detection system.
 Special attention should also be given to the purity of tubing which connects the source (cylinder)
and the gas chromatograph (machine).
 INJECTORS
 After passing through the resin trap, purified helium enters the injector where it acts like the
mobile phase by pushing the analytes through the separation column.
 Numerous types of injectors are available like on column injector, split-splitless injector, cryogenic focusing
injector etc., but split-splitless injector is the most commonly used.
 This type of injector operates in two modes, split and splitless-split modes. If the sample solution is containing
highly concentrated levels of analytes (parts per thousands), the injector is operated in the split mode.
 In split mode, only a small fraction of sample injected truly enters the separation
column and the rest is vented to the atmosphere.
 TEMPERATURE REGULATED OVEN
 Samples of gas chromatography must be converted into and maintained in vapor state
throughout the separation process.
 In general, temperature of the separating column in GC is controlled with the help of oven, it
keeps the column at temperatures from 40 °C to 400 °C.
 Oven heats rapidly, however the temperature can be brought down using a fan that removes the
hot air from the back of oven, thereby providing thermal control for better separation of analyte.
 The column is provided a supported system to prevent it touching the oven walls that
might damage the column.
 The connections of injector and detector are also within this oven.
 Depending on the operations, GC can be performed either isothermal or temperature
controlled.
 COLUMNS FOR GC

 Column is the important component of analytical gas chromatograph, the quality of

separation can be only by this.
 Early GC used to have a typically 1–5 m long and 1–5 mm internal diameter, however, micro-
packed columns used later on had <1 mm internal diameter.
 The column is coiled to fit the temperature regulated oven (column oven) and is connected with the
injector and detector inlets.
 DETECTORS

 Detection of analytes in gas chromatography plays an important role in separation process as

the whole idea of analysing the sample will be wasted if the analyte is not detected.
 Detector detects sample components/analytes on the basis of their physiochemical properties.
 It amplifies the response and generates an electronic signal thereby generating the
chromatogram.
 As the sample gas stream comes out from the column, the detector monitors the separated
components of the gaseous sample and signals are interpreted after data acquisition.
 Mainly used detectors in Gas chromatography are Thermal Conductivity Detector (TCD),
Flame Ionization Detector (FID), and Electron Capture Detector (ECD).
 DATA SYSTEM

 Data system accepts analogue signal from detector and digitalizes to record it as
separated peaks in the form of chromatogram due to chromatographic separation.
 It automatically reports peak retention times, peak areas, etc and the software
displays the result in automated manner.
 Pharmaceuticals

Food/Flavors/
Environmental Fragrances
Analysis

APPLICATION

Forensic
Science

Chemical/
Industrial
 Pharmaceuticals

• With the development of complex pharmaceuticals, high-tech

delivery systems and advanced formulations, accurate
analysis is needed to provide safe and effective drugs. In the
pharmaceutical industry Gas Chromatography technique is
used to analyze residual solvents in both raw materials (drug
substance) and finished products (drug product)
 Food/Flavors/Fragrances

• Analysis of foods like carbohydrates, lipids, proteins, steroids, vitamins, drug and
• pesticides residues, trace elements
• Quantification of volatile organic food products
• Food adulteration
• Detecting toxic components
• Monitoring of legislation for food products
• Controlling diet formulation
• Controlling formulation during product expansion.
• Recognizing changes in food during storage and processing
• Alcohol beverages analysis.
• Solvents analysis in food preparation.
• Analysis of dairy products such as milk, cheese, butter etc - rancidity
• Analysis of herbicides, residual pesticides etc.
• Assessing of fragrances and flavors
• Fatty acids depicting of fats and oils
 Environmental
• Environmental Gas Chromatographic operations include determination of
pollutants such as fungicides, pesticides, purgeable aromatics, herbicides,
chlorinated compounds in water, air and soils etc. The applications viz,
industrial environmental conservation include stack and waste emissions
and water discharges.
• Monitoring of ambient air and stack emissions
• Quantification of pollutants in drinking and waste water.
• Remaining pesticide in agricultural produce, soils, fruits, vegetables and
drinking water
• Analysis of environmental toxins like dibenzofurans, dioxins, polychlorinated
biphenyls (PCB’s), polynuclear aromatic hydrocarbons, etc
• Identification of unknown organic compounds in hazardous waste dumps.
 LIMITATION

 First and the foremost limitation of gas chromatography is that the substance
which is being analysed must be volatile so that a finite fraction of it gets
distributed in the gaseous phase.
 Volatility of organic substance having molecular weight more than 500 is rarely
adequate.
 Although high temperature (up to 300°C) increases the volatility but can result in
decomposition of the substance.