6.

Determination of distribution coefficient of iodine between organic and

inorganic layer

Aim

To determine the distribution coefficient of I2 between the organic and inorganic layer (CCl4/
CHCl3 and distilled water)

Principle:

When iodine (solute) is shaken with two immiscible solvents, it gets partitioned between the
solvents. This distribution of solute in two solvents depends upon the solubility of the solute
in two solvents. At equilibrium, the ratio of concentrations of solute in both solvents will be a
constant at given temperature. The constant is called the partition coefficient (K) or the
distribution coefficient of the solute between the two solvents.

𝑁1
𝐾=
𝑁2

N1 is the concentration of iodine in organic layer

N2 is the concentration of iodine in the aqueous layer

Chemicals and apparatus required:

Chemicals Apparatus
Distilled water Separating funnel
Iodine crystals Conical flask
CCl4 or CHCl3 Pipette
0.01 N Na2S2O3 Burette
Starch Reagent bottles

Procedure

Prepare 100 mL saturated solution of iodine in carbon tetrachloride and use it as the stock
solution.

Prepare three sets of solutions in three different separating funnels

Set I: 50 ml water + 40ml stock solution + 10 ml of CCl4

Set II: 50 ml water + 30ml stock solution + 20 ml of CCl4

Set III: 50 ml water + 20ml stock solution + 30 ml of CCl4

Set IV: 50 ml water + 10 mL stock solution + 40 mL CCl4

Shake the mixture in separating funnel for about 30 minutes for the iodine to get distributed
between the two solvents and to reach the distribution equilibrium. Then, let the flasks to
stand for about 10 minutes so that two clear layers are separated. Now remove stopper of the
separating funnel and keep its mouth open during this period to facilitate the separation.
Collect the lower layer which is aqueous into a dry bottle. Discard the intermediate layer
between both the phases. Let the organic layer stay in the separating funnels. Using a dry
pipette, withdraw 10 ml of organic layer to a conical flask and titrate it against 0.1N Na2S2O3.
Starch is used as an indicator. End point is the disappearance of blue colour. Then, withdraw
10 ml of the aqueous layer using a dry pipette and titrate it against 0.01N Na2S2O3 solution
using starch as an indicator. End point is the disappearance of blue colour. Repeat the same
process for all the set of mixtures.

Remember: While titrating the non-aqueous layer, the titration flask must constantly be
shaken, otherwise the equivalence point may pass without the disappearance of purple colour
of nonaqueous layer. The addition of about 5mL of 10% KI solution also helps. KI facilitates
extraction of iodine into aqueous solution during titration due to the formation of unstable
complex I3-ion as;

I-+ I2 I3-
Observation

Set Vorg Vaq Norg Naq 𝑁𝑎𝑞 log Norg log Naq
𝐾=
𝑁𝑜𝑟𝑔

I
II
III
IV

Mean distribution coefficient, K =

Plot the graph of log Naq Vs log Norg

Distribution coefficient, K = Naq/(Norg)(1/n)

log Naq = (1/n) log Norg + log K (y = mx+c)

Results from graph:

Slope (m) =

Therefore, n is nearly =

log K =

K=

Calculations:

Set I:

At aqueous layer,

N1V1 (thio) = N2V2 (iodine)

0.01 N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

At organic layer,
N1V1 (thio) = N2V2 (iodine)

0.1 N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

Set II:

At aqueous layer,

N1V1 (thio) = N2V2 (iodine)

0.01N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

At organic layer,

N1V1 (thio) = N2V2 (iodine)

0.1 N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

Set III:

At aqueous layer,

N1V1 (thio) = N2V2 (iodine)

0.01N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

At organic layer,

N1V1 (thio) = N2V2 (iodine)

0.1 N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

Set IV:

At aqueous layer,
N1V1 (thio) = N2V2 (iodine)

0.01N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

At organic layer,

N1V1 (thio) = N2V2 (iodine)

0.1 N×-------ml = N2× 10 ml

N2, concentration of iodine in the aqueous layer = --------- N

Result:

Distribution coefficient of iodine in distilled water and CCl4 = -------- by calculation and ------
by graph.