Hii..
in which slide we are involving what is Gas chromatography there History, Theory & principle, Introduction, Phases, Types, Instrumentation, Application etc.
9. The mobile phase used gas is used to
transport the sample components through the column, it is also
called as carrier gas. They are compressible gases that expand with
increasing temp.
the commonly used carrier gases are
hydrogen helium, argon & nitrogen.
The gases should be inert.
Will not react with stationary phase.
It should be comfortable.
t should be easily available & not much expensive.
Carrier Gas
• Hydrogen
• Helium
• Nitrogen
•Argon
10. 1) Gas solid chromatography :
In which stationary phase are
solid adsorbent. The analyte is adosrbed on surface of
solid adsorbents.
2) Gas Liquid chromatography :
In which stationary phase are
liquid supported by solid. Liquid phase coated over
solid support & analytes distributed between gas &
liquid.
11. Gas liquid chromatography:
This techniques
introduced by Martin & Synge in 1941. In which
Principle involved is Partition. The components of
sample to be analyzed is partitioned between inert gas
(mobile phase) & Liquid Phase .
Gas solid chromatography: This technique
was developed by G.D. Kolher & K. Thiele in 1943. in
which principle involved in gas solid chromatography is
adsorption.
12. 1. Gas source 4. Temp. control
2. Sample injection system 5. Detector
3. Column 6. Read out device
13. 1. Gas source: It is consist of gas cylinder & generator to
produce carrier gas. Is controlled by pressure
regulator. The pressure regulator also help in
process to read pressure of gas.
i. Air/ Oxygen : These can oxidize sample components &
liquid stationary phases.
ii. Hydrocarbons : These will affect detector performance
and produce constant background signals.
iii. Water Vapour : It can affect some solid & bounded liquid
stationary phases & performance of some detectors.
2. Sample injection system :
There are different method of
sample injection system . Packed column application
mostly direct injection system using Hypodermis syringe
is employed.
In which sample is vaporized and carried onto column.
14. This is used with capillary
column to prevent over loading column with sample. It
consist of hollow needle which is placed centrally that
permits only small part of sample column.
15. ii) Splitless Injection system :
This is used When the
sample contain very low level of some
component (ppb) to be analysed.
iii) Special Injection Techniques :
It includes head space
sampling, purge , trap & pyrolysis.
Sampling useful for analysis of gases &
low viscosity & volatile liquid such as
Wine, food product, blood & water.
16. 3. Column
Two types of column
1. Packed column
2. Capillary column :
I) Packed column with solid particle
ii) Open tubular column :
a) wall coated Open tubular column
b) Supported coated Open tubular column
c) porous layer Open tubular column
In gas chromatography column are made up of glass & metal
tubing. Diameter of column in range of 2-10mm & usually 4.8
mm for analytical purpose. It is U tube column Shaped or coiled
column shape.
17. Packed column
It is used for gas solid liquid chrom. Stationary
phase is packed in glass, stainless steel &
nickel tubing to produce packed column. The
Length is 3 meter & Diameter range from 1.6 to
9.5 mm.
The pure diameter range from 2-9µm. The
particle size should be100/120 mesh (149-125
µm ) for 2 mm pore column.
Capillary column : It is usually made up of
fused silica which is a very high purity glass.
The outer wall of column is coated with
polyamide to protect the wall from scratches.
The column is 1 mm or less.
18. Packed column with solid particle
It is called as micropacked column. These column are
packed with solid particles.
Open tubular column : These column are made
up of stainless steel , copper , nylon & glass.
4.Temp. control program :
It control regulate the increase of temp. during
analysis. In this system a lower temp. is
selected initially & it is used to resolve the early
peaks.
The initial temp. is maintained for 10 min.
19. 5. Detector
a)Thermal conductivity detector
b) Flame ionization detector
c) Electron capture detector
d) Flame photometric detector
e) Electrolyte conductivity detector
f) Other detectors
a)Thermal conductivity detector : This is called as
Differential thermal detectors. Principle
involved based on thermal conductivity of gas
which controls the temp. Resistance of wire.
20. Construction :
A tightly coiled filament made up of tungsten
rhenium with gold placed inside & metal block.
The detector consist of four filament placed
within one metal block.
TCD can be constructed with thermistor which
is metal oxide lead with electrical load attached.
21. b) Flame ionization detector
The principle involved in detector is electrical
conductivity of gases.
The change of conductivity is recorded in
electric current.
Construction : To electrodes flame jet
collector electrode. Is a capillary can
produce flame.
The collector is placed about the type of
flame.
Inlet such as hydrogen gas, air, & column
effluents.
23. APPLICATION
Qualitative Analysis
Quantitative Analysis
Determination of pesticide
In pharmaceutical analysis
In food industry
In forensic science
In air monitoring
In natural product in volatile mixture separation
In petroleum industry
In biochemical & clinical
In cosmetic & perfume field.