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Contents

Introduction
Basic Principle Of GC
Schematic Diagram of GC
Components of GC
Advantages & Disadvantages
Applications
Introduction
Gas chromatography (GC)
Analytical Technique
Developed by Martin and Synge in 1941
They suggested the use of gas-liquid partition chromatograms for
analytical purposes.
It is a process of separating component(s) from the given crude
by using a gaseous mobile phase.
Two major types:
Gas-solid chromatography
(stationary phase: solid)
Gas-liquid chromatography
(stationary phase: immobilized liquid)
Basic Principle of GC
It involves a sample being vaporized and injected onto the
head of the chromatographic column. The sample is
transported through the column by the flow of inert, gaseous
mobile phase. The column itself contains a liquid stationary
phase which is adsorbed onto the surface of an inert solid.
Schematic diagram of a gas
chromatograph
Components of Gas
chromatography
Carrier gas
- He (common), N2, H2, Argon
Sample injection port
- micro syringe
Columns
2-50 m coiled stainless steel/glass/Teflon
Detectors
-Flame ionization (FID)
-Thermal conductivity (TCD)
-Electron capture (ECD)
-Nitrogen-phosphorus
-Flame photometric (FPD)
-Photo-ionization (PID)
Carrier gas

The carrier gas must be chemically inert.

Commonly used gases include nitrogen, helium, argon, and


carbon dioxide.

The choice of carrier gas is often dependant upon the type of


detector which is used.

The carrier gas system also contains a molecular sieve to


remove water and other impurities.
Sample injection
Direct Injection:
into heated port (>T oven)
using micro syringe
Columns
There are two general types of column:
1. packed and
2. capillary (also known as open tubular).

Packed columns contain a finely divided, inert, solid support material


( diatomaceous earth) coated with liquid stationary phase. Most packed
columns are 1.5 - 10m in length and have an internal diameter of 2 - 4mm.

Capillary columns have an internal diameter of a few tenths of a


millimeter. They can be one of two types;
1. wall-coated open tubular (WCOT) or
2. support-coated open tubular (SCOT).
Common Stationary phases
DETECTORS
Detectors can be grouped into:
1. concentration dependant detectors and
2. mass flow dependant detectors.
The signal from a concentration dependant detector is
related to the concentration of solute in the detector, and does
not usually destroy the sample Dilution of with make-up gas
will lower the detectors response.
Mass flow dependant detectors usually destroy the sample,
and the signal is related to the rate at which solute molecules
enter the detector. The response of a mass flow dependant
detector is unaffected by make-up gas.
Flame Ionization Detector
(FID)
It operates by the principle that by change in
conductivity of the flame as the compound is burnt.

The change in conductivity of the flame does not


arise by simple ionization of the compound , it is
partial or complete stripping of the compound to give
charged hydrogen-deficient polymers or aggregates
of carbon of low ionization potential.

Sensitive (10-13 g/s) ;


Wide dynamic range (107) ;
Signal depends on # C atoms in organic analyte-
mass sensitive;
not concentration sensitive;
Weakly sensitive to carbonyl, amine, alcohol, amine
groups;
Not sensitive to non-combustibles - H2O, CO2, SO2,
Nox;
Destructive
Thermal Conductivity
Detector (TCD)
It is based upon the alteration of the thermal
conductivity of the carrier gas in the presence of an
organic compound.

The platinum wires are heated electrically and


assume equilibrium conditions of temperature and
resistance when carrier gas alone passes over them.

They are mounted in a wheatstone bridge


arrangement and when a compound emerges, the
thermal conductivity of the gas surrounding wire
alters, and hence the temperature and resistance of
the wire change with a concomitant out of balance
signal which is amplified and recorded.

Wide dynamic range (105);


Nondestructive;
Insensitive (10-8 g/s) - non-uniform
Electron Capture Detector
(ECD)
The ECD ionizes the carrier gas by means of a
radioactive source.

The potential across two electrodes is adjusted


to collect all the ions and a steady saturation
current, is therefore, recorded.

Electrons from b-source ionize carrier


molecules capture electrons and decrease current

Simple and reliable ;


Sensitive (10-15 g/s) to electronegative groups
(halogens, peroxides) ;
Largely non-destructive ;
Insensitive to amines, alcohols and
hydrocarbons ;
Limited dynamic range (102)
Advantages & Disadvantages

Advantages:
The technique has strong separation power and even complex mixture can be
resolved into constituents
The sensitivity of the method is quite high
It gives good precision and accuracy
The analysis is completed in a short time
The cost of instrument is relatively low and its life is generally long
The technique is relatively suitable for routine analysis

Disadvantages:
Limited to volatile samples
Not suitable for samples that degrade at elevated temperatures (thermally
labile)
Not suited to preparative chromatography
Applications of Gas Chromatography

Separation and identification of volatile materials, plastics,


natural and synthetic polymers, paints, and microbiological
samples
Miscellaneous-analysis of foods like carbohydrates, proteins,
lipids, vitamins, steroids, drug and pesticides residues, trace
elements
Pollutants like formaldehyde, carbon monoxide, benzene,
DDT
Inorganic compound analysis
Dairy product analysis- rancidity

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