Faculty of Chemistry of

Santiago de Compostela
3-3-2021

Laboratory report
of Analytical
Separation
Techniques

Pablo López Cortés

L7I GROUP
 EXPERIMENT 1: LIQUID-LIQUID EXTRACTION (LLE): SINGLE AND
MULTISTAGE PARTITION EQUILIBRIUM OF I2 IN AQUEOUS SOLUTION TO
HEXANE
General questions - Introduction
1.- Can acetone be a good solvent for the extraction of a solute form an aqueous
solution?
No, because acetone is miscible with water and for LLE we need two immiscible phases
where the solute is distributed.
A good solvent for LLE must be immiscible with the aqueous phase. It also must not be
too viscous for the extraction and it ought to be stable at work conditions (In this case,
not having a low boiling point at room temperature).
2.- In the example of I2 partitioning between water and carbon disulfide. Why is
iodine much more soluble in the organic phase?
I2 (solute) is a diatomic molecule with net total dipole equal to 0 (it is nonpolar). On
the other hand, we have two solvents, one polar (water) and one nonpolar (carbon
disulfide).
As we know, polar substances tend to dissolve in polar solvents, and nonpolar
substances dissolve in nonpolar solvents. For this reason, I2 is more soluble in CS2 than
H2O.
3.- If instead of I2, we would like to extract acetic acid, how would the pH influence
the extraction yield?
The acetic acid is a weak base that in water can be in the neutral and the ionic specie
depending on the pH. If we have and acid media, the concentration of protons [H+] will
increase, and the ionic specie of acid will be lower (to remain constant Ka) than in a
basic media, where the concentration of protons would be lower.

Questions related to the experiment – Part 1:

1.- In step 5, why is agitation needed?
It is necessary the agitation to extract as much as possible solute to the organic phase
(hexane). With higher dipersion of the particles of solute higher efficiency in the extraction.
2.- Which color changes have you observed? Why do this color
changes occur? Clearly identify the phases in the funnel,
which phase is the less dense?
The organic phase will have a orangish color due to the
presence of the iodine in the organic phase after the agitation
while the aqueous phase will be lighter due some I2 is
extracted to the aqueous phase.
The density of hexane is 0.6593, and for water it is 0.9982. Due to hexane is less dense
than water it will be at the top and water at the bottom. (As the picture shows)
3.- Describe your observations during the starch test.
During the starch test we can see that there is a formation of a dark blue complex that
occurs when there is iodine remaining. This is because the single extraction is not
enough to extract most of the iodine to the hexane due to the partition coefficient k is
lower than 100. Then a multistage extraction will be performed.

Questions related to the experiment – Part 2:

1.- Assuming that K= 35 when iodine is extracted with hexane. What would be the
recovery in the case of single and multistage extractions?
In a single extraction:

[ I 2 ] h ex (n ¿ ¿ T −n eq )/V hex ( n ¿ ¿ T −neq )V eq 3.33(n ¿ ¿ T −neq )

35= = = = → ¿¿ ¿
K= [ I 2 ] aq neq neq V h ex neq
V eq
Kneq+3.33neq=3.33nT
3.33n T neq /V aq n eq 0.087 nT
neq= =0.087 nT α= = = =0.087
K +3.33 n T /V aq nT nT

The extraction efficiency=100-8.700=91.130%

In a multistage extraction:
n
1
α =( )
V hex =¿= 0.0109
1+ K
V aq

The extraction efficiency =100-1.098=98.902% It is better a multistage extraction.

2.- Is the partition coefficient the same in single and multistage extractions?
Yes, the partition coefficient does not depend on the type of the extraction. It depends
on the relative solubility of the product in two immiscible phases that are the same in
both extractions.
Notes:
-I2 is a solute that dissolved generates brownish aqueous solutions. When the
concentration is higher the solution is more brownish.
-We have to take care of hexane vapors that are toxic.
EXPERIMENT 2: SEPARATION OF FE & AL FROM AN AQUEOUS SAMPLE BY
SELECTIVE EXTRACTION WITH OXINE
Results on Fe determination:
Calibration curve
ml Fe 100 mg/l µg Fe absorbance
0 0 0
0,2 20 0,211
0,4 40 0,375
0,6 60 0,540
0,8 80 0,693
Linear regression
Intercept: 0,0208
Slope: 0,0343
Linear equation: y=0,0343x+0,0208
R2=0,9962

Response
0.8
0.7
f(x) = 0.03 x + 0.02
0.6 R² = 1
0.5
Response

0.4
0.3
0.2
0.1
0
0 5 10 15 20 25
Conc

Sample:
Replicate absorbance µg Fe µg Fe/ml
number
1 0,516 14,437 3,610
2 0,548 15,371 3,843
Concentration in the sample:
14,904± 0,660438 µg/mL Fe
Notes:
Equilibrium between chloroform with oxine and the aqueous solution
containing 80 micrograms of Fe(III).