GAS CHROMATOGRAPHY

PRESENTED BY:
RUPALI PRASHANT YEVALE.
 TYPES
• Gas-Solid adsorption Chromatography (GSC)
• Gas-Liquid partition Chromatography, (GLC)
• Liquid-Solid adsorption Chromatography (LSC)
• Liquid-Liquid partition Chromatography (LLC)
 INTRODUCTION
• The mobile phase is a gas and the components are
separated as vapors.
• To separate and detect small molecular weight
compounds in the gas phase.
• The sample is either a gas or a liquid that is vaporized
in the injection port.
• Helium because of its low molecular weight and being
chemically inert.
• The pressure is applied and the mobile phase moves
the analyte through the column.
• The separation is accomplished using a column coated
with a stationary phase.
 PRINCIPLE
• Adsorption effects-i.e., when the prepared
column consists of particles of adsorbent only
• Partition effects-i.e., when the particles of
adsorbent are coated with a liquid that forms
stationary phase
 ADVANTAGES
• High frequency of separation and even complex
mixtures may be adequately resolved into
constituents,
• Very high degree of sensitivity in detection of
components i.e., only a few mg of sample is
enough for complete analysis,
• Speed of analysis is quite rapid,
• Gives reasonably good accuracy and precision,
• The technique is fairly suitable for routine
analysis
 THEORIES
(a) Plate theory

(b) Rate theory

(c) Random walk and nonequilibrium theory.

Plate theory
Rate theory
Random walk and Nonequilibrium theory.
EDDY DIFFUSION :
LONGITIDINAL DIFFUSION:
RESISTANCE TO MASS TRANSFER
INSTRUMENTATION
 CARRIER GAS PRESSURE REGULATOR
AND FLOW METER
Various carrier gas used in GC

H2 : It has a distinctly better thermal conductivity and lower density.

He : It has an excellent thermal conductivity, low density, inertness and it

permits greater flow rates.

N2 : It offers reduced sensitivity and is inexpensive

Air : It is employed only when the atmospheric O2 is beneficial to the

detector separation.
.
 SAMPLE INJECTION SYSTEM
• Liquid Samples :

• Solid Samples :

• Gas Samples :
 TYPES OF SAMPLE INJECTION
1. DIRECT INJECTION
2.LOOP INJECTOR
3. HEADSPACE ANALYSIS:
 HEADSPACE ANALYSIS:
• Vial Size: Headspace vials are available in 6, 10
and 20ml sizes..
• Bottom Profile: Headspace vials may be
round-bottomed or flat-bottomed.
• Correct Crimping: Ensure the crimper is not worn
and is adjusted correctly.
• Septa Choice: Use septa suitable for the
temperature of the system..
• Cleanliness of Vial: Vials should be clean.
 1.Static Headspace analysis

2. Dynamic Headspace analysis

 COLUMNS
• PACKED COLUMN

• CAPILLARY/OPEN TUBULAR COLUMN

1.FSOT (Fused silica coated open tubular)
2.WCOT(Wall coated open tubular)
3.SCOT ( Support coated open tubular)
 COLUMN OVEN/THERMAL
COMPARTMENT

•system that is sensitive enough to changes of 0.01°C and that

maintains an accurate control to 0.1°
•programmes are also available that features both in linear and
non-linear temperature programming as sample and reference
columns.
•The compartment temperature can also be raised at various rates
upto a maximum of 60 °C min–1 in the lower-temperature ranges
and about 35 °C min–1 at higher temperatures.
 DETECTORS

There are in all six different kinds of detectors

used in ‘Gas Chromatography’, namely
(i) Thermal conductivity detector (TCD)

(ii) Flame ionization detector (FID)

(iii) Electron capture detector (ECD)

1.Thermal Conductivity Detector (TCD)
2. Flame Ionization Detector (FID)
3.Electron Capture Detector (ECD)
 RECORDING OF SIGNAL CURRENT

The following important points should be noted

before operating a recorder, namely :
(i) Its ‘zero’ must be adjusted (or synchronized)
with the ‘input zero’
(ii) The amplifier gain must also be adjusted duly.
(iii) A recorder with inadequate shielding from
AC circuits would display shifting of its zero
point.
(iv) A reasonably good recorder having quality
performance must be employed
 APPLICATIONS
• Gas liquid chromatography (GLC) or gas chromatography
(GC) finds its abundant applications in
The accurate and precise analysis of plethora of official
pharmaceutical substances covering a wide range as
enumerated below :
(i) Assay of Drugs,
(ii) Determination of specific organic compounds as impurities in
official pharmaceutical substance,
(iii) Determination of related substances in official drugs,
(iv) Determination of water in drug, and
(v) Determination of chloroform with head-space
chromatography.
LIMITATIONS:
THANK YOU…