Gas Chromatography

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GAS CHROMATOGRAPHY

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CONTENTS

o Introduction
o Types of GC
o Principle
o Instrumentation
o Applications
o References
GAS CHROMATOGRAPHY
Types of gas chromatography:

• GAS LIQUID CHROMATOGRAPHY: In this liquid is used as a stationary


phase and the principle involved is “PARTITION”.

• GAS SOLID CHROMATOGRAPHY: In this solid is used as a stationary phase


and the principle involved is “ADSORPTION”.
• GLC: Partition PRINCIPLE
• GSC: Adsorption
• The compounds which are more soluble
towards stationary phase travels slower
& elutes faster.
• The compounds which are less soluble
towards stationary phase travels fast &
elutes later, hence the compounds are
separated

Sample column separation Detection Peak

To measure a sample with an unknown concentration, a standard sample with known


concentration is injected into the instrument.
The standard sample peak retention time (appearance time) and area are compared to the test
sample to calculate the concentration.
INSTRUMENTATION
It consists of six components:
• A carrier gas
• A sample injection system
• Column
• Detectors
• Thermo stated chambers
• An amplification and recorded Schematic Diagram of GC
system
CARRIER GAS

• The most widely used


carrier gases are
o Hydrogen
o Helium
o Nitrogen
o Air
• It should be inert
• It should be suitable for
detectors employed and the
type of sample analysed
SAMPLE INJECTION SYSTEM
• Liquid samples are generally introduced by hypodermic syringe through a self –
sealing rubber septum into small inlet chamber, which may be heated to cause flash
evaporation.
• The temperature must not be so high they it decomposes the sample. Solid samples
must be dissolved in volatile liquids for introduction or may be introduced directly if
they can be liquefied.
COLOUMNS

The columns can be constructed of glass or metal tubing and for


analytical work it has 4.8mm diameter
1. Packed column
2. Open tubular column
3. Support coated open tubular columns
DETECTORS
1. Thermal conductivity detector
2. Flame ionisation detector
3. Electron capture detector

1. THERMAL CONDUCTIVITY DETECTOR: The principle of the detector is that the


temperature and thus the resistance of a wire through which a current is flowing is dependent upon
the 6thermal conductivity of the gas in which it is immersed
2. FLAME IONISATION DETECTOR:
The ionisation detectors are based on the electrical conductivity of gases.
At normal temperatures and pressure gases act as insulators but will become
conductive of ions if electrons are present.
•Sample is directed at an air-hydrogen flame
after exiting the column.
•At the high temperature of the air-hydrogen
flame, the sample undergoes chemical
decomposition
•Release ions and electrons that carry current.
•A high-impedance pico-ammeter measures this
current to monitor the sample's elution
2. ELECTRON CAPTURE DETECTOR:
The electron affinity of different substances can be used as the basis .For an
ionisation detector known as electron capture detector. It responds to only those
compounds whose molecules have an affinity for electrons
Eg- chlorinated compounds, alkyl lead etc.
•Highly selective detectors commonly used for detector. Device
selectively detects organic compounds with Moieties such as
halogens, peroxides, quinones and nitro groups
•High selectivity and sensitivity towards certain organic Species
with electronegative functional groups.
•Gives little to no response for all other compounds.
•Potentially dangerous owing to its radioactivity.
TEMPERATURE CONTROL

A temperature programing facilitates controlled of even temperature


during an analysis.
The latter peaks also become sharp and emerge quickly

Temperature programming is carried out in different modes:


1.Linear
2.Multi linear
AMPLIFICATION & RECORDED SYSTEM

• An integrator is employed for simultaneous measurement of


areas under chromatographic peaks by electronic or mechanical
means.
• Electronic integrators print out of the peak area digitally and
give highest precision but they are quite expensive.
ADVANTAGES OF GAS CHROMATOGRAPHY
 High resolution power compared to other methods.
 High sensitivity.
 High accuracy and precision.
 Analysis of sample very quickly (minutes even seconds)
 Small sample needed(ul-ug).

DISADVANTAGES OF CHROMATOGRAPHY
 Limited to volatile sample.
 Not suitable for thermally liable substances.
 Samples be soluble don’t react with the column.
 During injection of gaseous sample proper attention is required.
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APPLICATIONS
1. Miscellaneous: analysis of foods like carbohydrates ,proteins, lipids, vitamins, etc.
2. Pollutants like formaldehyde, carbon monoxide, benzene, DDT, etc.
3. Dairy product analysis- rancidity
4. Inorganic compound analysis
5. Separation &identification of volatile materials, plastics, natural&synthetic polymers, paints, and
microbiological samples.
6. Separation of fatty acids derived from fixed oils.
7. Gas chromatography is a physical separation method in where volatile mixtures are separated.
8. Pharmaceuticals, cosmetics and even environmental toxins are separated by GC.
9. Air samples can be analyzed using GC.
10. Determination of Organic Volatile Impurities by GC.
11. Determination of nicotine level during drugs formulation.
12. Biological and pesticides detections.
13. Food, beverage, flavour and fragrance analysis.
14. Determination of level of pollutants in air.
REFERENCES

• B. K .Sharma instrumental methods of chemical analysis Goel publishing


house, 180-224.
• Dr. S .Ravishankar textbook of pharmaceutical analysis IV edition, 17.1-17.20.
• Dr. K. R. Mahadik pharmaceutical instrumental methods volume II, 180-224.
• Gurdeep R. Chatwal instrumental methods of chemical analysis, 2.673-2.678
THANK YOU…

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