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SUPER CRITICAL FLUID CHROMATOGRAPHY. BY ABIJAH 08171S0417 MPAQA. SUPER CRITICAL LIQUID CHROMATOGRAPHY. Def Introduction Principle Instrumentation Applications. Definition. Chromatography: It is a method of separation of complex mixtures .

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super critical fluid chromatography

SUPER CRITICAL FLUID CHROMATOGRAPHY

BY ABIJAH

08171S0417

MPAQA

super critical liquid chromatography
SUPER CRITICAL LIQUID CHROMATOGRAPHY
  • Def
  • Introduction
  • Principle
  • Instrumentation
  • Applications
definition
Definition
  • Chromatography: It is a method of separation of complex mixtures .
  • Super critical liquid chromatography: It is a type of column chromatography in which super critical fluid is used as a mobile Phase for the separation of mixtures.
  • Super critical fluid: A super critical fluid is that which contains temperature and pressure above its critical temperature and pressure.
slide4
The critical temperature of a substance is the temperature above which a distinct liquid phase cannot exist regardless of pressure.
  • The critical pressure is that the vapour pressure at its critical temperature.
  • No matter how much temperature and pressure is applied the substance cannot exists as a liquid.
introduction
Introduction
  • This technique is a hybrid of Gas and High performance liquid chromatography.
  • It is relatively a recent chromatographic technique which is commercially available since 1982.
  • Advantages such as rapid separation without the use of organic solvents, faster separation than HPLC, high resolution chromatography than GC thereby faster analysis of thermo labile compounds.
slide6
Super critical temperature and pressure are the defining boundaries for a pure substance.
  • Beyond these boundaries the properties of a substances are intermediate between a liquid and gas.
  • In this region the fluid has a good solvating power and high diffusivity.
slide9
An HPLC like setup with two reciprocating pumps designed to provide a mixed mobile phase with a packed analytical column placed in an oven followed by an optical detector in which the pressure and flow rates can be independently controlled .
  • A GC like setup with a syringe pump followed by a capillary column in a GC oven with a restrictor followed by a flame ionization detector, where the pressure is controlled by the flow rate of the pump.
slide10
In SFC the mobile phase is initially pumped as a liquid and is brought into the super critical region by heating it above super critical temperature before it enters the analytical column.
  • It passes through an injection valve where the sample is introduced into the super critical stream and then into the analytical column.
slide11
It is maintained supercritical as it passes through the column and into the detector by a pressure restrictor placed either after the detector or at the end of the column.
  • Restrictor prevents clogging
  • Mobile phase: Carbon dioxide, ethane, butane, nitrous oxide, dichlorodifluoromethane, diethyl ether, ammonia and tetrahydrofuran.
slide12
Reciprocating pumps
  • Syringe pumps
  • LC Injection valve (Pneumatically driven valves)
  • Conventional GC or LC ovens
  • Capillary, stainless, Open tubular columns.
  • Stationary phase: Fused silica
slide13
Detectors: Optical, Flame ionization detector, Spectroscopic detectors.
  • The results of a run in SFC are a chromatogram.
  • Example: Chromatogram of separation of polymers. It is schematically shown as follows.
applications
Applications
  • Purification of thermo labile compounds.
  • Characterization of polymers.
  • Complex distributions can be resolved, low temperatures can be used
  • Oligomers can be detected.
  • Solute diffusivities
  • Separation of enantiomers
slide16
Metabolites of estrogens are separated by SFC .
  • Separation of chiral and Achiral mixtures.
  • Natural products, drugs, foods, Pesticides and herbicides, surfactants, fossil and propellants.