Supercritical Fluid Extraction 1

Supercritical fluid extraction (SFE)
Supercritical fluid extraction

(SFE, Supercritical Fluid Extraction)
=
extraction using the fluid in supercritical state as an
extraction agent - so-called supercritical fluid (SCF,
Supercritical Fluid)
Supercritical Fluid (SCF)
=
fluid, which is in the state above its critical point (CP), i.e. above its
critical temperature (Tc) and critical pressure (pc)
 it can be produced by warming a gas or liquid

on temperature higher than its critical
temperature Tc by simultaneous compression
on value higher than its critical pressure pc
 above the critical temperature and pressure is
the material in one condensed state with
properties between gas and liquid
 it is used in extraction and also in chromatography as
mobile phase – Supercritical Fluid Chromatography
(SFC)
Critical values of some substances
Critical values of some substances
Critical
Critical Critical pressure Critical density
Substance molecular
temperature(K) MPa (atm) (g.cm-3)
weight (g.mol )
-1
Carbon dioxide (CO2) 44.01 304.1 7.38 (72.8) 0.469

Water (H2O) 18.02 647.3 22.12 (218.3) 0.348
Methane (CH4) 16.04 190.4 4.60 (45.4) 0.162
Ethane (C2H6) 30.07 305.3 4.87 (48.1) 0.203
Propane (C3H8) 44.09 369.8 4.25 (41.9) 0.217
Ethylene (C2H4) 28.05 282.4 5.04 (49.7) 0.215
Propylene (C3H6) 42.08 364.9 4.60 (45.4) 0.232
Methanol 32.04 512.6 8.09 (79.8) 0.272
Ethanol (C2H5OH) 46.07 513.9 6.14 (60.6) 0.276
Acetone (C3H6O) 58.08 508.1 4.70 (46.4) 0.278
● Supercritical Fluids – some properties like gases,
others like liquids
– are compressible, its possible to change its density. The density of SCF is close
to density of liquids; the dissolving capability depends on density ⇒ by density
changes is possible to change dissolving properties
– viscosity of SCF is more than 1 place value lower than viscosity of liquids; it can
be achieved of fast mass transfer due to the favourable flow characteristic
– high diffusivity and absence of surface tension causes easily penetration of
SCF into the pores of solid phase, thereby the efficent extraction in SFE or the
fast analysis in SFC
Density (g ml-1) Viscosity (Pa s) Diffusivity (cm 2 s-1)

Gas 10-3 (0,5 – 3,5).10-5 0,01 – 1,0
Supercritical Fluid 0,2 – 0,9 (0,2 – 1,0).10-4 (3,3 – 0,1).10-4
Liquid 0,8 – 1,0 (0,3 – 2,4).10-3 (0,5 – 2,0).10-5
● Important property is the solubility of

material in supercritical liquids
● Solubility of material increases with
increasing of density (T=konst.)
● Near the critical point can the density
steeply decreases with minimum of
temperature increasing
● Solubility near the critical point often
decreases with increasing temperature
and then increases again
 Supercritical carbon dioxide
critical temperature Tc = 35 °C, critical pressure pc = 75 bar
40 °C : 72 bar → 0,22 g ml-1

400 bar → 0,96 g ml-1
80 °C : 72 bar → 0,14 g ml-1

400 bar → 0,82 g ml-1
note: triple point of CO2 lies by pressure 5,2 atm and temperature -57 °C. At pressure 1
atm passes the CO2 straight from solid to liquid phase (sublimes), at atmospheric
pressure the CO2 does not exist in liquid phase
● Advantages of CO2
– Tc and pc are relatively low and instrumentally achievable
– nontoxic
– nonflammable
– easy to clean
– Compatible with detectors (UV, IR , FID)
● Disadvantages CO2
– nonpolar
– for polar substances: necessary to use modifiers (most often methanol, acetonitrile,
water, THF in concentrations 1 - 20 % - similar to HPLC)
● Carbon dioxide in SFE

– Food Industry
● essential lipids extraction, removing of lipids from nuts, removing of
lipids from potato chips – using the corbon dixide as SCFthe fat
content is reduced to the half without loosing a taste
● Extraction of caffeine
– Other
● Extraction of pesticides and insecticides
note: Supercritical Fluid Chromatografy (SFC) – high cost – only

pharmaceuticals, dry cleaning, bio-diesel production, nano- and micro-
particles production, impregnation and dying
● Supercritical water
– Conditions for supercritical water are significantly harder:
H2O : 647,3 K at 22,12 MPa (CO2 : 304,1 K at 7,38 MPa)
– Synthesis of inorganic substances – biggest commercial success in
synthesis of silicon crystals for mobile phones
– At supercritical conditions is water very corrosive for all kinds of steel, a
lot of organic substances are not stable in supercritical water, this state
can be used by waste disposal - process is called supercritical water
oxidation (SWO)
– above 200 ˚C the water earns the properties of organic solvents, at
about 300 ˚C has properties similar to acetone, substitution of organic
solvents by supercritical water should be environment friendly
● Supercritical water
– Conditions for supercritical water are significantly harder:
H2O : 647,3 K at 22,12 MPa (CO2 : 304,1 K at 7,38 MPa)
– Synthesis of inorganic substances – biggest commercial success in
synthesis of silicon crystals for mobile phones
– At supercritical conditions is water very corrosive for all kinds of steel, a
lot of organic substances are not stable in supercritical water, this state
can be used by waste disposal - process is called supercritical water
oxidation (SWO)
– above 200 ˚C the water earns the properties of organic solvents, at
about 300 ˚C has properties similar to acetone, substitution of organic
solvents by supercritical water should be environment friendly
Instrumentation
Instrumentation
Extraction of plant oil, South Korea, 2 x 3800 liters, 550 bars
Rice Processing, Taiwan, 3 x 5800 liters, 325 bars
Supercritical CO2
Velmi dobře Dobře Velmi špatně
rozpustné rozpustné rozpustné
Fragrances Plant Oils Sugars
Esencial Oils Pigments Starches
Esters, alcohols Polyphenols Proteins
Aldehydes, ketons Waxes Mineral salts
Supercritical fluids in nature
● Sea volcano is a common element of the sea

ground, its presence is sometimes expressing
by explosion of steam and erosion of reef
● Some of them are situated in depth (greater
then 3 km); big pressure (over than 30 MPa)
gained from the weight of water is avoiding the
explosion of steam and gases, which are
warming the water to more more than 648 K,
i.e. the water is in supercritical state
Deep sea volcano

Supercritical fluids in nature
 Atmosphere of Venus consists of 96,5 % CO2 and 3,5 % N2; at there

founded temperature (735 K) and pressure (9,3 MPa) is the carbon
dioxide in supercritical state
Venus

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Supercritical fluid extraction (SFE)

Supercritical fluid extraction

 it can be produced by warming a gas or liquid

Carbon dioxide (CO2) 44.01 304.1 7.38 (72.8) 0.469

Density (g ml-1) Viscosity (Pa s) Diffusivity (cm 2 s-1)

● Important property is the solubility of

40 °C : 72 bar → 0,22 g ml-1

80 °C : 72 bar → 0,14 g ml-1

● Carbon dioxide in SFE

note: Supercritical Fluid Chromatografy (SFC) – high cost – only

● Sea volcano is a common element of the sea

Deep sea volcano

 Atmosphere of Venus consists of 96,5 % CO2 and 3,5 % N2; at there

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