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Biplabendu

Study the distribution of iodine between immiscible solvents


As a chemist, many times you face with complex mixtures of several
components. When you make a synthesis almost always, you need to separate the
main product reaction byproducts. At other times, you require separating an active
ingredient from a natural product from a plant or animal tissue, or recover a metal of
interest from a leached from a mineral; therefore, the processes of separation and
purification are important tasks for Chemistry professionals.
Solvent extraction is a process by which a solute is distributed between two
different phases. The liquid-liquid extraction consists of a solute transfer of a liquid phase
to another, the process therefore requires that the two phases are immiscible with each
other and are generally water and an organic solvent. It is known to extract and separate
phase, generally containing organic compound to the extracted.
When a substance is brought into contact with two immiscible liquids, it tends
to distribute between the two phases in a proportion, which depends on its chemical for
each affinity. In the laboratory, the liquid-liquid extractions are performed using
separatory funnels through which can be mixed and separating immiscible liquids.
The solubility of solutes can vary widely from one solvent to another and
depends on various factors such as the physicochemical nature of the solvent and
solute, ionic strength, temperature and pressure. Based on this property, it is possible to
design methods of separating solutes, if allowed to distribution equilibrium is
established thereof, between two phases consisting of solvents considered as
immiscible, and mechanically separating the two phases after equilibrium established.
The corresponding technique is called liquid-liquid extraction.
When a solute M is partitioned between an aqueous phase and another
consisting of an immiscible liquid phase, the ratio of the concentrations of M in both
phases is a constant that depends on temperature and is independent of the volume
ratio of the two phases in contact:

KD It is called distribution constant. It refers to the same chemical species M


present in both phases to equilibrium.

Biplabendu

Often the solute to be extracted is involved in chemical equilibrium


reactions and the additional distribution, either in the aqueous phase in the
organic phase or both. Species involving the solute in such equilibrium can
have very different affinities with the aqueous and organic phases. In such
cases the analyte distribution depends on the chemical composition of the
system.
According to the IUPAC, the distribution ratio is defined, DM, as equal to the
ratio between the total analytical concentration (CM) organic solute M in the
organic phase (regardless of the chemical form in which it is present) and total
analytical concentration (CM) aqueous phase in the aqueous:

Aqueous phase
Organic phase
Iodine is a sparingly soluble substance in water (10-3 M). In order to increase
its solubility in water, potassium iodide in excess, which reacts with molecular iodine
to give an adduct, triiodide anion is added (these solutions are known as iodized
iodine):
I 2 + I - = I 3 - (Triiodide)

Biplabendu

STANDARDIZATION A. A solution of sodium thiosulfate by iodometry


a solution of sodium thiosulfate (Na 2S203) was standardized by a back-titration
oxidation reduction using a solution of potassium iodate (KlO 3) 0.015 mol / Lt. One
milliliter of the above solution was transferred to a 125 mL Erlenmeyer flask, they were
added 50 mL of distilled water and 0.10 g solid potassium iodide (KI). Once he
dissolved the KI was added 1 mL sulfuric acid (H 2SO4) 1:10. By adding the sulfuric
acid solution becomes red-brown (explain why and the reaction that occurs).
Immediately after the solution was titrated with sodium thiosulfate being spent
volumes reported in Table 1 using starch as an indicator of the endpoint. Obtain the
average concentration of the solution of sodium thiosulfate.

Approach for the solution:

Biplabendu

Table 1. Standardization of sodium thiosulfate


Mass KI
Vol. H2SO4
Flask Vol. KI03
0015 M (mL) (G)
1:10 (mL)
1
1.0
0.10
1.0
2
1.0
0.10
1.0
3
1.0
0.10
1.0
4
1.0
0.10
1.0
5
1.0
0.10
1.0
6
1.0
0.10
1.0

Vol. Overspent
16.5
16.4
16.7
17.1
16.2
16.8

B. Determination of Iodine solubility in hexane.


Saturated iodine (I2) in hexane, this saturated solution was prepared were taken
10 mL and brought to a final volume of 1000 mL with pure hexane (working solution),
10 mL of working solution were taken and They were added 30 mL of distilled water
and 0.5 g of KI. This solution was titrated with sodium thiosulfate solution, standardized
in the previous step, spending volumes reported in Table 2, with data reported
calculate the concentration of iodine in the working solution and the saturated solution.
Table 2. Determination of the solubility of iodine in hexane.
Vol.
KI mass Vol. Overspent
solution of
Flask
work (mL)
(g)
Na2S203 (mL)
1
2
3
4
5
6

10.0
10.0
10.0
10.0
10.0
10.0

0.50
0.50
0.50
0.50
0.50
0.50

17.7
17.7
17.9
18.2
17.0
19.0

Biplabendu

Approach for solution to (B)

Biplabendu

C. STUDY OF DISTRIBUTION BETWEEN IODINE hexane and water.


10 mL of working solution are taken and mixed in a stirring funnel with aqueous solutions
containing varying concentrations of potassium iodide. After stirring and having reached
equilibrium distribution of iodine between the two phases, the aqueous phase from the
organic phase is separated and the concentration of iodine is determined in the aqueous
phase by iodimetric titration with the thiosulfate solution standardized sodium in the point
a worn volumes for each funnel are presented in Table 3.
Using expressions distribution constant and distribution ratio to find a
mathematical expression relating the inverse of the distribution ratio to the
concentration of free iodine in water (Iodine (aqueous) and allow calculating the
distribution constant of iodine in hexane and the formation constant of triiodide in water.

Table 3. Study the distribution of iodine between hexane and water.

Funnel
1
2
3
4
5
6
7

Vol. 0.1 M KI Vol. 1:10


(mL)
H2SO4 (mL)

0.0
0.5
1.0
2.0
3.0
4.0
5.0

50.0
50.0
50.0
50.0
50.0
50.0
50.0

Vol. Water
distilled (mL)

10.0
9.5
9.0
8.0
7.0
6.0
5.0

Vol.
Vol. Overspent
Dissolution Na2S2O3 (mL)
Working 12
(mL)
10.0
2.10
10.0
3.45
10.0
4.10
10.0
6.10
10.0
7.40
10.0
8.20
10.0
9.20

Biplabendu

Approach to solve the last part: