Supercritical Fluids Extraction

SUPERCRITICAL FLUIDS EXTRACTION
INTRODUCTION
• SUPERCRITICAL FLUID EXTRACTION (SFE) IS THE PROCESS OF SEPARATING

ONE COMPONENT (THE EXTRACTANT) FROM ANOTHER (THE MATRIX)
USING SUPERCRITICAL FLUIDS AS THE EXTRACTING SOLVENT.
• EXTRACTION IS USUALLY FROM A SOLID MATRIX, BUT CAN ALSO BE

FROM LIQUIDS.
EXTRACTION AND SCF EXTRACTION
SUPER CRITICAL FLUIDS
• AT A CERTAIN TEMPERATURE AND PRESSURE CONDITION (CRITICAL CONDITION), LIQUID AND

VAPOR PHASES OF A SUBSTANCE BECOME INDISTINGUISHABLE. A SUBSTANCE WHOSE
TEMPERATURE AND PRESSURE ARE HIGHER THAN ITS CRITICAL POINT IS KNOWN AS
SUPERCRITICAL FLUID (SCF).
• IT CAN DIFFUSE THROUGH SOLIDS SUCH AS GAS AND DISSOLVE LIQUIDS
• SUPERCRITICAL FLUIDS ARE SUITABLE AS A SUBSTITUTE FOR ORGANIC SOLVENTS IN A

RANGE OF INDUSTRIAL AND LABORATORY PROCESSES
IMAGE
PROPERTIES OF SUPERCRITICAL FLUIDS
• SUPERCRITICAL FLUIDS HAVE HIGHLY COMPRESSED GASES, WHICH COMBINE PROPERTIES OF

GASES AND LIQUIDS IN AN INTRIGUING MANNER.
• SUPERCRITICAL FLUIDS CAN LEAD TO REACTIONS, WHICH ARE DIFFICULT OR EVEN
IMPOSSIBLE TO ACHIEVE IN CONVENTIONAL SOLVENTS.
• SCF HAVE SOLVENT POWER SIMILAR TO LIGHT HCS FOR MOST OF THE SOLUTES.
• SOLUBILITY INCREASES WITH INCREASING DENSITIES.
• THE FLUIDS ARE COMMONLY MISCIBLE WITH PERMANENT GASES AND THIS LEADS TO MUCH
HIGHER CONCENTRATIONS OF DISSOLVED GASES THAT CAN BE ACHIEVED IN CONVENTIONAL
SOLVENTS.
SIMILARITIES WITH LIQUIDS AND GASES
(i) LIQUID LIKE DENSITIES.

(ii) REDUCTION IN SURFACE TENSION
(iii) GAS LIKE VISCOSITY
(iv) GAS LIKE COMPRESSIBILITY PROPERTIES
(v) DIFFUSIVITIES HIGHER THAN LIQUIDS
SOME COMMONLY USED SCF
SOME COMMONLY USED SUPERCRITICAL SOLVENTS ARE

• CARBON DI OXIDE
• NITROUS OXIDE
• ETHYLENE
• PROPYLENE
• PROPANE
• N-HEPTANE
• ETHANOL AND AMMONIA.
 AMONG THESE, CO2 IS WIDELY USED AS A SUPERCRITICAL SOLVENT.
WHY CO2 ?
(I) LOW CRITICAL PRESSURE (74 ATM) AND LOW CRITICAL TEMPERATURE (320 C)
(II) RELATIVELY NON-TOXIC
(III) NON-FLAMMABLE
(IV) AVAILABLE AS HIGH PURITY
(V) LOW COST
(VI) EASILY REMOVABLE FROM EXTRACT
(VII) IT HAS POLARITY LIKE LIQUID PENTANE AT SUPERCRITICAL CONDITIONS AND THUS,
BEST SUITED FOR LIOPHILIC COMPOUNDS.
SCF CO2 PREPARATION
• THE SUPERCRITICAL CO2 CONDITION WAS ACHIEVED BY USING DRY ICE. IT IS A

SOLID PHASE OF CO2 WHEN FROZEN.
• IF DRY ICE IS PUT IN AN ENCLOSED VESSEL, IT WILL SUBLIMATE TO BECOME A

GAS AND THE PRESSURE WILL INCREASE DEPENDING ON THE MASS OF DRY ICE
UNTIL THE DESIRED PRESSURE (SUPERCRITICAL PRESSURE) IS ACHIEVED.
SCHEMATIC DIAGRAM OF SCF EXTRACTIONS
COMPONENTS OF SCF EXTRACTION
• 1. FLUID RESERVOIR (GAS CYLINDER IN CASE OF CO2 ) .

• 2. PUMP – RECIPROCATING PUMP – SYRINGE PUMP (PULSE-FREE FLOW AT LARGE RANGE OF
FLOW RATES) .
• 3. EXTRACTION CELL/COLUMN (STATIONARY PHASE) – USUALLY STAINLESS STEEL CHAMBER
OR VESSEL IN COMPARTMENT – CAPABLE OF WITHSTANDING HIGH PRESSURE (300-600 ATM)
[FOR SOLIDS] – OPEN TUBULAR CAPILLARY COLUMNS OR PACKED COLUMNS [LIQUIDS].
• 4. RESTRICTOR – MAINTAINING PRESSURE CHANGE INSIDE THE EXTRACTION VESSEL .
• 5. COLLECTOR (TRAPPING SYSTEM).
• 6. DETECTORS (FLAME IONIZATION DETECTOR OF GAS CHROMATOGRAPHY).
WORKING OF SCF EXTRACTION
• STEP 1: INTRODUCTION OF FEED INTO EXTRACTOR (SOLID FEED) OR EXTRACTOR

IN MODIFIED COLUMN EITHER CO-CURRENTLY OR COUNTER CURRENT.
• STEP 2: MIXING OF SOLUTES WITH SUPERCRITICAL FLUID.
• STEP 3: EXPOSURE OF MOBILE PHASE TO PRESSURES (50-500 ATM) AND
TEMPERATURES (AMBIENT TO 300°C) NEAR OR ABOVE THE CRITICAL POINT FOR
ENHANCING THE MOBILE PHASE SOLVATING POWER.
• STEP 4: ISOLATION OF DISSOLVED SOLUTE BY PRECIPITATION.
MODES OF SCF EXTRACTION
STATIC EXTRACTION MODE DYNAMIC EXTRACTION MODE

• IT IS ALSO CALLED AS STEADY STATE • IT IS ALSO CALLED NON STEADY
MODE. STATE MODE
• SAMPLE MATRIX IS SOAKED IN A • SUPERCRITICAL FLUID
FIXED AMOUNT OF SUPERCRITICAL CONTINUOUSLY PASSES THROUGH
FLUID. THE SAMPLE MATRIX.
• CAN BE COMPARED TO A TEABAG IN A • ANALOGOUS TO COFFEE MAKER.
CUP OF WATER.
MODELS OF SCF EXTRACTION
• DIFFUSION CONTROLLED/LIMITED EXTRACTION

• SOLUBILITY LIMITED EXTRACTION
APPLICATION OF SCF EXTRACTION
1. REMOVAL OF FAT FROM FOODS

2. EXTRACTION OF VITAMIN E FROM NATURAL RESOURCES
3. REMOVAL OF ALCOHOL FROM WINE AND BEER
4. EXTRACTION OF PESTICIDES
5. EXTRACTION OF POLYAROMATIC HYDROCARBON, POLY-CHLORO BENZENE
6. MAJOR APPLICATION IS DECAFFEINATION OF COFFEE BEANS

ADVANTAGES
• ELIMINATION OF ORGANIC SOLVENTS I.E. REDUCES THE RISK OF STORAGE.

• RAPID (DUE TO FAST BACK-DIFFUSION OF ANALYTES IN THE SCF REDUCES THE
EXTRACTION TIME SINCE THE COMPLETE EXTRACTION STEP IS PERFORMED IN ABOUT 20
MIN) .
• SUITABLE FOR EXTRACTION AND PURIFICATION OF COMPOUNDS HAVING LOW VOLATILITY
PRESENT IN SOLID OR LIQUID.
• SUSCEPTIBLE TO THERMAL DEGRADATION (LOW OPERATING CONDITIONS).
• COMPLETE SEPARATION OF SOLVENT FROM EXTRACT AND RAFFINATE.
• SOLVENT RECOVERY IS EASY
DISADVANTAGES
• PROLONGED TIME (PENETRATION OF SCF INTO THE INTERIOR OF A SOLID IS

RAPID, BUT SOLUTE DIFFUSION FROM THE SOLID INTO THE SCF).
• MODELING IS INACCURATE
• SCALE IS NOT POSSIBLE (DUE TO ABSENCE OF FUNDAMENTAL, MOLECULAR-
BASED MODEL OF SOLUTES IN SCF)
• EXPENSIVE
REFERENCES
• DAS, S. SUPERCRITICAL FLUID EXTRACTION, MODULE 10. NPTEL

• SUPER CRITICAL FLUID EXTRACTION – WIKIPEDIA
• JONIN, T.M., ADJADJ, L. P AND RIZVI, S.S. FOOD ENGINEERING. VOL III.
ENCYCLOPEDIA OF LIFE SUPORT SYSTEM (EOLSS).
• SAPKALE, G. N., PATIL, S. M., SURWASE, U. S., & BHATBHAGE, P. K. (2010).
SUPERCRITICAL FLUID EXTRACTION. INT. J. CHEM. SCI, 8, 729-743.
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SUPERCRITICAL FLUIDS EXTRACTION

• SUPERCRITICAL FLUID EXTRACTION (SFE) IS THE PROCESS OF SEPARATING

• EXTRACTION IS USUALLY FROM A SOLID MATRIX, BUT CAN ALSO BE

• AT A CERTAIN TEMPERATURE AND PRESSURE CONDITION (CRITICAL CONDITION), LIQUID AND

• IT CAN DIFFUSE THROUGH SOLIDS SUCH AS GAS AND DISSOLVE LIQUIDS

• SUPERCRITICAL FLUIDS ARE SUITABLE AS A SUBSTITUTE FOR ORGANIC SOLVENTS IN A

• SUPERCRITICAL FLUIDS HAVE HIGHLY COMPRESSED GASES, WHICH COMBINE PROPERTIES OF

(i) LIQUID LIKE DENSITIES.

SOME COMMONLY USED SUPERCRITICAL SOLVENTS ARE

• THE SUPERCRITICAL CO2 CONDITION WAS ACHIEVED BY USING DRY ICE. IT IS A

• IF DRY ICE IS PUT IN AN ENCLOSED VESSEL, IT WILL SUBLIMATE TO BECOME A

• 1. FLUID RESERVOIR (GAS CYLINDER IN CASE OF CO2 ) .

• STEP 1: INTRODUCTION OF FEED INTO EXTRACTOR (SOLID FEED) OR EXTRACTOR

STATIC EXTRACTION MODE DYNAMIC EXTRACTION MODE

• DIFFUSION CONTROLLED/LIMITED EXTRACTION

1. REMOVAL OF FAT FROM FOODS

6. MAJOR APPLICATION IS DECAFFEINATION OF COFFEE BEANS

• ELIMINATION OF ORGANIC SOLVENTS I.E. REDUCES THE RISK OF STORAGE.

• PROLONGED TIME (PENETRATION OF SCF INTO THE INTERIOR OF A SOLID IS

• DAS, S. SUPERCRITICAL FLUID EXTRACTION, MODULE 10. NPTEL

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