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mixture
SEPARATION
Dr. Nagappa L. Teradal
M.Sc., M.Phil., Ph.D., Post-Doc.(Israel)
Assistant Professor,
Department of Chemistry,
JSS Arts, Science and Commerce College,
Gokak 591307, Karnataka, India
CONTENTS:
Solvent Extraction: Types – batch, continuous, efficiency,
selectivity, distribution coefficient, factors affecting the partition,
relationship between % extraction and volume fraction. Numerical
problems on solvent extraction. Solvent extraction of iron and
copper.
Introduction:
Immiscible liquids are ones that cannot get mixed up together
and separate into layers when shaken together. These liquids are
usually water and an organic solvent.
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What is Solvent Extraction ?
• Solvent Extraction or liquid – liquid extraction is process for
separating components in solution by their distribution between
two immiscible liquid phases. Such process is referred to as
solvent extraction or liquid extraction.
• Three stages are involved in the process:
(i) bringing the feed mixture and the solvent into intimate contact
(ii) separation of the resulting two phases and
(iii) removal and recovery of the solvent from each phase
Distribution or Partition Coefficient
• The partition of a solute between two immiscible phases is an
equilibrium process that is governed by the distribution law,
known as Nernst Distribution Law.
If the solute specie A is allowed to distribute itself water and
organic phases, the distribution of solute is an equilibrium process,
ie., Aaq ⇋ Aorg
When equilibrium has established, the ratio of the activities of
solute A in both phases at particular temperature will be constant
and independent of the total quality of A. This constant is called
distribution or partition coefficient, represented by the term Kd
[A]org
Kd =
[A]aq
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Distribution or Partition Coefficient
• The distribution of solute (when there is interaction between
solute and solvent) between two immiscible solvents can be
described by the distribution coefficient, “Kd”:
[A]1 organic phase
Kd =
[A]2
[A]org association A
Kd = dissociation
[A]aq A
aqueous phase
Efficiency of Extraction or Percentage of Extraction
The distribution of acetic acid between benzene and water may serve as
an illustration of the effect of chemical interactions of the solute. The
distribution of acetic acid itself may be described as follows
(CH3COOH)aq (CH3COOH)org
[CH3COOH]org
Kd =
[CH3COOH]aq
However, acetic acid dissociate in
And form a dimer in benzene
aqueous phase
CH3COOH CH3COO- + H+ 2 CH3COOH (CH3COOH)2
[CH3COO-][H+] [CH3COOH)2]org
Ka = Kd =
[CH3COOH] [CH3COOH]2aq
The overall distribution of acetic is described by ‘D’, which is
[CH3COOH]org [(CH3COOH)2]
D= =
[CH3COOH]aq [CH3COO-] + [CH3COOH]
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Extraction Efficiency or Percentage of Extraction
• The percentage of solute that moves from one phase to the other.
Efficiency of extractions depends upon (i) Distribution ratio (D) &
(ii) Relative volume of two liquids
D
E= x 100
Vaq
D+
Vorg
where,
E = efficiency of extraction
D = distribution ratio
Vaq = volume of the aqueous phase
Vorg = volume of the organic phase
Selectivity in Solvent Extraction
The selectivity depends upon separation factor. If the solution to be
extracted consists of two solutes A and B, and we have to separate A
from B, then we will use extracting solvent which will dissolve
more quantity of A and very less quantity of B. This is called
selectivity of extraction.
Effectiveness of separation is expressed in terms of separation
coefficient or separation factor (). It is the ratio of distribution
coefficient of two solutes A and B.
KdA
E=
KdB
should be very high to separate two solutes by solvent extraction,
otherwise clear separation will be difficult.
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Uses of Solvent Extraction
Terminology in Solvent Extraction
• In the extraction process, the feed, which contains the first
solvent (or the diluent) and the solute. Another solvent
(commonly called the solvent) is also fed into the extractor,
with the purpose to remove the solute from the diluent.
• Normally, the diluent + the remaining solute is called the
raffinate phase, the second solvent + the solute is called
the extract phase.
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Solvent Extraction Process
Solvent Extraction Process
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Solvent Extraction Process
Types or Methods of Solvent Extraction
Batch Extraction
Continuous Extraction
Countercurrent Extraction
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Batch Solvent Extraction
This method is used for larger KD values.
The apparatus used for solvent extraction
is the separating funnel. Usually solute is
extracted from an aqueous solution into
an immiscible organic solvent. The
aqueous solution containing the solute is
shaken with the immiscible organic
solvent for a few minutes and the phases
are allowed to separate. The denser
solvent occupies the bottom layer and is
withdrawn by opening the stopcock.
Continuous Solvent Extraction
When the organic compound to be extracted has nearly the same
solubility in water as well as in the organic solvent i.e., distribution
coefficient between the organic solvent and water is very small.
Large quality of organic solvent is employed to obtain even a moderately
efficient extraction or multiple extraction is performed. But these will
create a number of complications and also tedious job.
This can be avoided by continuous extraction using the apparatus known
as continuous extractor where relatively small volume of solvent is
required.
The organic substance can be extracted from an aqueous solution with a
solvent which is
(a) Heavier than water
(b) Lighter than water
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Continuous Extraction: (a) When extracting solvent is lighter than water
The organic substance in aqueous phase is
placed in the extraction vessel fitted with reflux
condenser. A portion of extractant is placed in
the heated tube reservoir and vaporized. The
vapors are passed into the extraction vessel
which go up to the condenser and condensed
into liquid state. The liquid drops are passed
downwards with the help of bubbler funnel but
as it is lighter than water so it ascends through
aqueous phase containing the organic solute
and doing so they carry certain amount of
solute. The causes the organic solvent to flow
over into the reservoir. As the process continues, the organic solute
concentration in aqueous phase is gradually depleted as it concentrates in
reservoir. The organic solute is thus continuously extracted by the organic
solvent and accumulates in the reservoir.
Continuous Extraction: (b) When extracting solvent is heavier than water
The organic substance in aqueous phase is
placed in the extraction vessel fitted with reflux
condenser. The extraction solvent (immiscible
with water) is adjusted to the level of solvent
return tube. A portion of extraction solvent is
placed in the heated tube reservoir and
vaporized. The vapors are passed into the
Organic phase Aqueous phase
extraction vessel which go up to the condenser
and condensed into liquid state. The liquid drops
are passed downwards through aqueous phase
containing the organic solute and doing so they
carry certain amount of solute. The causes the
organic solvent to flow over into the reservoir.
As the process continues, the solute
concentration in aqueous phase is gradually
depleted as it concentrates in reservoir. The
solute is thus continuously extracted by organic
solvent and accumulates in the reservoir.
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Amount remain un-extracted
• From equilibrium coefficient it is clear that some quantity
of a compound will remain unextracted in aqueous
phase.
• In single extraction, quantitative separation of a
compound from aqueous phase into organic phase is not
possible.
• Thus for quantitative extraction of a compound from
aqueous phase into organic phase, aqueous phase must
be extracted again or number of times.
Amount remain un-extracted
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Amount remain un-extracted
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Factors affecting solvent extraction
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Factors affecting solvent extraction
Factors affecting solvent extraction
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Solvent Extraction of Iron (Fe)
Solvent Extraction of Copper (Cu)
CuCl2 •2H2O
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