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SUPERCRITICAL FLUID
CHROMATOGRAPHY
BY
Abhishek Pradhan
CONTENTS
 Introduction
 Definition
 Principle
 Instrumentations
 Advantages
 Dis advantages
 Applications
 conclusion
INTRODUCTION
 Supercritical fluid chromatography(SFC) was first
proposed in 1958 by J.LOVELOCK .
 First used in 1962 by klesper.
 It is used for the analysis and purification of low
moderate molecular weight, thermally liable
molecules.
DEFINITION
A supercritical fluid chromatography is a material that can be either
liquid or gas used in state above critical temperature or critical pressure
where gasses or liquid can co exist . supercritical fluid chromatography is
a form of normal phase chromatography that uses a supercritical fluid
such as carbon dioxide as the mobile phase.
PRINCIPLE
Principles are similar to those of high performance liquid
chromatogray (HPLC), However SFC typically utilizes carbon dioxide
as the mobile phase ; therefore the entire chromatography flow path
must be pressurized, because the supercritical phase represents a
state in which liquid and gas properties converge , supercritical fluid
chromatography is sometime called convergence chromatography.
INSTRUMENTATION
 STATIONARY PHASE
 MOBILE PHASE
 PUMPS
 INJECTORS
 OVENS
 COLUMNS
 DETECTOR
STATIONARY PHASE
 Both packed and open tubular columns are used .
 Packed columns can provide more theoretical plates and handle
large volume than open tubular columns .Because of low viscosity of
supercritical media .
 The column length is 10 to 20m. And inside the diameter is 50 to
100mm Common is open tubular columns.
 For difficult separation column 60m or large have been used .
 Paked column uslly made up of stainless steel , 10 to 25 cm.
 more than 100,000 plates have been achived in plate column .
 Many of column coating used in LC have been applied to SFC as well
MOBILE PHASE
 The mobile phase is composed primarily of supercritical carbon
dioxide ,but since carbon dioxide on its own is too non polar to
effectively elute many analytes , co-solvents are added to modified
the mobile phase polarity.
 Co solvents are typically simple alcohols like methanol ,ethanol or
isopropyl alcohol .other solvents such as acetonitrile, chloroform or
ethayle acetate can be used as modifiers .
 Modify valves for analytes , ethane ,pentane, diethayl-ether,
ammonia.
 Pressure maintain is 72.9atm temperature is 35ºc.
PUMPS
Here mainly flow control is necessary so syringe pumps are used for
capillary SFC for consistent pressure and for packed columns for
easier blending of the mobile phase or introduction of modifier
fluids reciprocating pumps are used.
INJECTORS
 In capillary SFC small sample should be quickly injected
into the column and so pneumatically driven valves are
used.
 For packed SFC a typical injection valve is commonly used.
OVENS
Conventional GAS chromatography and liquid chromatography
ovens are used.
COLUMNS
 Two types of analytical columns are used in SFC i.e. packed
and capillary.
 Packed columns contain small deactivated substances to which
the stationary phase adheres. These are conventionally
stainless steel.
 Capillary columns are open tubular columns made of fused
silica which have small internal diameter.
DETECTORS
Flame ionization detectors and photometry detector, liquid-phase
detectors like refractive index detector, ultraviolet-visible
spectrophotometric detectors and light scattering detectors have
been employed for SFC.
ADVANTAGES
 SFC is emerging as a separation technique that is superior to both gas
chromatography and liquid chromatography for analysis of thermal
liable or non volatile compounds.
 Low viscosity.
 Lower operating temperature.
 High diffusion co efficient.
 High resolution at low temperature.
DISADVANTAGES
 SFC is pressure operating conditions. High-pressure vessels are
expensive and bulky.
 Maintaining pressure in SFC is difficult.
 Supercritical fluids are highly compressible and their physical
properties change with pressure.
 Cleaning will be time consuming.
APPLICATIONS
 SFC is used in industry primarily for separation of chiral
molecules.
 SFC now commonly used for chiral separation and purification
in the pharmaceutical industry.
 SFC technique has been applied to wide verity of materials,
including natural products, drugs, food and polymers etc.
CONCLUSION
 In overall ranking of chromatography techniques it can be
judges that SFC falls somewhere between HPC and GC.
 In field of pharmaceutical chemistry and bioanalytical
applications SFC gained its applications.

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Supercritical fluid chromatography

  • 2. CONTENTS  Introduction  Definition  Principle  Instrumentations  Advantages  Dis advantages  Applications  conclusion
  • 3. INTRODUCTION  Supercritical fluid chromatography(SFC) was first proposed in 1958 by J.LOVELOCK .  First used in 1962 by klesper.  It is used for the analysis and purification of low moderate molecular weight, thermally liable molecules.
  • 4. DEFINITION A supercritical fluid chromatography is a material that can be either liquid or gas used in state above critical temperature or critical pressure where gasses or liquid can co exist . supercritical fluid chromatography is a form of normal phase chromatography that uses a supercritical fluid such as carbon dioxide as the mobile phase.
  • 5. PRINCIPLE Principles are similar to those of high performance liquid chromatogray (HPLC), However SFC typically utilizes carbon dioxide as the mobile phase ; therefore the entire chromatography flow path must be pressurized, because the supercritical phase represents a state in which liquid and gas properties converge , supercritical fluid chromatography is sometime called convergence chromatography.
  • 6. INSTRUMENTATION  STATIONARY PHASE  MOBILE PHASE  PUMPS  INJECTORS  OVENS  COLUMNS  DETECTOR
  • 7.
  • 8.
  • 9. STATIONARY PHASE  Both packed and open tubular columns are used .  Packed columns can provide more theoretical plates and handle large volume than open tubular columns .Because of low viscosity of supercritical media .  The column length is 10 to 20m. And inside the diameter is 50 to 100mm Common is open tubular columns.  For difficult separation column 60m or large have been used .  Paked column uslly made up of stainless steel , 10 to 25 cm.  more than 100,000 plates have been achived in plate column .  Many of column coating used in LC have been applied to SFC as well
  • 10. MOBILE PHASE  The mobile phase is composed primarily of supercritical carbon dioxide ,but since carbon dioxide on its own is too non polar to effectively elute many analytes , co-solvents are added to modified the mobile phase polarity.  Co solvents are typically simple alcohols like methanol ,ethanol or isopropyl alcohol .other solvents such as acetonitrile, chloroform or ethayle acetate can be used as modifiers .  Modify valves for analytes , ethane ,pentane, diethayl-ether, ammonia.  Pressure maintain is 72.9atm temperature is 35ºc.
  • 11. PUMPS Here mainly flow control is necessary so syringe pumps are used for capillary SFC for consistent pressure and for packed columns for easier blending of the mobile phase or introduction of modifier fluids reciprocating pumps are used.
  • 12. INJECTORS  In capillary SFC small sample should be quickly injected into the column and so pneumatically driven valves are used.  For packed SFC a typical injection valve is commonly used.
  • 13. OVENS Conventional GAS chromatography and liquid chromatography ovens are used.
  • 14. COLUMNS  Two types of analytical columns are used in SFC i.e. packed and capillary.  Packed columns contain small deactivated substances to which the stationary phase adheres. These are conventionally stainless steel.  Capillary columns are open tubular columns made of fused silica which have small internal diameter.
  • 15. DETECTORS Flame ionization detectors and photometry detector, liquid-phase detectors like refractive index detector, ultraviolet-visible spectrophotometric detectors and light scattering detectors have been employed for SFC.
  • 16. ADVANTAGES  SFC is emerging as a separation technique that is superior to both gas chromatography and liquid chromatography for analysis of thermal liable or non volatile compounds.  Low viscosity.  Lower operating temperature.  High diffusion co efficient.  High resolution at low temperature.
  • 17. DISADVANTAGES  SFC is pressure operating conditions. High-pressure vessels are expensive and bulky.  Maintaining pressure in SFC is difficult.  Supercritical fluids are highly compressible and their physical properties change with pressure.  Cleaning will be time consuming.
  • 18. APPLICATIONS  SFC is used in industry primarily for separation of chiral molecules.  SFC now commonly used for chiral separation and purification in the pharmaceutical industry.  SFC technique has been applied to wide verity of materials, including natural products, drugs, food and polymers etc.
  • 19. CONCLUSION  In overall ranking of chromatography techniques it can be judges that SFC falls somewhere between HPC and GC.  In field of pharmaceutical chemistry and bioanalytical applications SFC gained its applications.