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Experiment Number: 02

Name of the Experiment:

DETERMINATION OF DISTRIBUTION
COEFFICIENT OF I2 BETWEEN TWO
IMMISCIBLE SOLVENTS .
Date of Performance: 05.04.16
Temperature: 32°C

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Objective:
This experiment is based on NERNST’S distribution law. Here we determine the distribution
coefficient of I2 between two immiscible solvents. Distribution co-efficient has a wide range of
application in industrial field. We need to know the value of distribution co-efficient for solvent
extraction, which is much needed in chemical process industries. It has other applications in
partition chromatography, recovery of gold and silver from impure lead by the parkes process,
organic synthesis operation- thus there is wide use of distribution coefficient in both organic and
inorganic field.

In this experiment , our main purposes are to –

 Determine the distribution coefficient of I2 with respect to two different immiscible


solutions-CCl4-H2O and H2O-Ethyl Acetate systems
 Observing the distribution phenomenon.
 Learn about the process of measuring distribution coefficient.
 Get introduced with separating funnel
 Observe the temperature dependency of distribution coefficient.

Theory:
The distribution coefficient Kd for a component (A) between two immiscible solvents is given by
the following Nernst equation

Kd= [A]org/ [A]aq=constant

Kd is known as Distribution coefficient or Partition coefficient. The equation is applicable only if


the species (A) is soluble in both layers and the species is in same molecular condition in two
solvents. The relation is a direct consequence of the Nernst’s Distribution Law which states

“When a solution is shaken up with two liquids which are immiscible with each other, but in both
of which the solute is soluble, then the solute distributes itself between the two liquids in such a
way that the ratio of the concentration of the solute in the two liquids is a constant at a constant
temperature provided the solute is in the same molecular condition in the two liquids.”

The distribution law can be derived from the kinetic theory and the rate law. Since the solute is at
equilibrium in both the liquids, the rate at which it leaves one phase must be equal to the rate at
which it leaves the other phase, i.e., dynamic equilibrium is established. Consequently

Solute (in solvent 1) ⇌ Solute (in solvent 2)

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At equilibrium k1 [A]org=k2 [A]aq

Or [A]org/ [A]aq= k2/ k1=Kd

Where k1 and k2are rate constants of the solute in the two phases.

In this experiment, for the same solute, I2, in different arrangements the distribution coefficient
can be calculated in different manners:

a) In case of mixing H2O with the organic solution of I 2 and CCl4, the distribution coefficient, KD,
can be calculated as follows:
KD = [I2]CCl4 /[I2]H2O

b) When ethyl acetate is mixed with the aqueous solution of I 2, then KD can be calculated as
follows:
KD = ([I2]H2O - [I2]E.A.)/ [I2]E.A.

Distribution coefficient for a particular system changes with temperature as the influence of
temperature on the solubility of the solute is different for the two solvents.

Figure: Separating Funnel

Apparatus and Chemicals:


1. Burette
2. 5ml & 10ml pipette
3. Separating funnel
4. Conical flasks
5. Saturated solution of iodine in CCl4& Ethyl acetate
6. Standard thiosulphate solution (0.1)

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7. Starch
8. Iodine Solution

Data Collection:
Set-1

TABLE 1 : Determination of the concentration of I 2 CCl4 layer :

No. of observation Volume of CCl4soln Burette reading (ml) Volume of


(ml) Initial final Na2S2O3
(ml)
1. 10 0 18.4 18.4

Strength of I2 in CCl4 solution is determined by:

V1 * S1 = V2 * S2 , where S is expressed as normality

S2 = (v1 *s1 )/v2

= (18.4*0.05)/10

= 0.092 N

TABLE 2 :Determination of the concentration of I2 aqueous layer :

No. of observation Volume of Burette reading (ml) Volume of


aqueous soln Initial final Na2S2O3
(ml) (ml)
1. 100 1 12.6 11.6

Strength of I2 in aqueous solution is determined by:

V1 * S1 = V2 * S2 , where S is expressed as normality

S2 = (v1 *s1 )/v2

= (11.6*0.01)/100

=0.0016 N

KD = 0.092/0.0016 = 79.31

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SET 2

Table 3 : Determination of the concentration of I2 solution by standard Na2S2O3 solution :

No. of observation Volume of CCl4 soln Burette reading (ml) Volume of


(ml) Initial final Na2S2O3
(ml)
1. 20 2.8 41.8 39

Strength of I2 solution is determined by:

V1 * S1 = V2 * S2 , where S is expressed as normality

S2 = (v1 *s1 )/v2

= (39*0.05)/20

= 0.0975 N

Table 4 : Determination of the concentration of I2 in aqueous layer in addition of ethyl acetate :

No. of observation Volume of Burette reading (ml) Volume of


aqueous soln Initial final Na2S2O3
(ml) (ml)
1. 20 12.6 16.9 4.3

Strength of I2 in aqueous layer in addition of ethyl acetate is determined by:

V1 * S1 = V2 * S2 , where S is expressed as normality

S2 = (v1 *s1 )/v2

=(4.3*0.01)/20

=2.15*10^-3 N

KD= [.0975-(2.15*10^-3)]/(2.15*10^-5)

=44.34

Result:
1. Distribution co-efficient of Iodine in CCl4and aqueous layer is 79.31

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2. Distribution co-efficient of Iodine in Ethyl acetate and aqueous layer is 44.34

Discussion:
Iodine remains dissolved in carbon tetrachloride layer. But the titration is done in aqueous layer.
To bring the iodine back to aqueous layer some potassium iodide is added. This forms tri iodide
which is soluble in aqueous layer. The aqueous layer is first done to avoid contamination.
Our observed value of KD 79.31 and 44.34 has varied from the original value of 80 and 26
respectively. The reasons behind that are stated below:
 There is time constraint during we perform experiment in lab. Sufficient time is
required for the two phases to become separated completely.
 During determining initial concentration of set 2 we mistakenly used a very lower
concentration solution of Thiosulphate. As a result comparatively large initial value
obtained which is the reason for huge deviation from original value of 26.
 Two phases should be separated carefully. But some solution had lost during
separation. This is the vital reason for the error.
 The strengths of Thio-solncould have varied from the values we used as they were
prepared formerly and we did not standardize them.
 The titration was done only for one time. So it is natural to have some error. We
should do the titration for more than once.
 Some solutions may have been introduced somehow in the solution. It may cause the
error.

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