2020

M.BILAL

ROLL # 43
DETERMINATION OF ACETIC ACID BETWEEN TWO IMMCIBLE
SOLVENT BY BATCH EXTRACTION:

Theory :
separate compounds based on their relative solubilities in two different immiscible
liquids. 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. LLE is an
extraction of a substance from one liquid into another liquid phase. The most common use of the
distribution principle is in the extraction of substances by solvents, which are often employed in
a laboratory or in large scale manufacturing. Organic compounds are generally much more
soluble in organic solvents, like benzene, chloroform, and ether, than in water and these solvents
are immiscible with water. Organic compounds are then quite easily separated from the mixture
with inorganic compounds in aqueous medium by adding benzene, chloroform, etc. Upon
shaking, these separate into two layers. Since organic compounds have their distribution ratio
largely in favor of the benzene phase, more of them would pass into a non-aqueous layer. Finally
this non-aqueous layer is removed and distilled to obtain the purified compound.

Principle of solvent extraction:

When the solute (liquid or solid) is add to a heterogeneous system of two immiscible liquids (in
both of which the solute is soluble), the solute distributes between the two liquids. This
distribution governed by Nernst distribution law.
According To Distribution law:
“When a substance is added in excess quantity in two immiscible solvents, it distributes itself
between two liquid phases so that each becomes saturated. The distribution or partition of a
solute between immiscible liquids is known as Nernst's distribution law or simply distribution
law or partition law.”
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑜𝑟𝑔𝑎𝑛𝑖𝑐 𝑝ℎ𝑎𝑠𝑒
k=
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑎𝑞𝑢𝑒𝑜𝑠 𝑝ℎ𝑎𝑠𝑒

Apparatus required:
Separating funnel, beaker, burette, burette stand, pipette, conical flask, measuring cylinder.

Chemicals required:
Distilled water (25ml), acetic acid (5ml), carbon tetrachloride (25ml), (1M )sodium hydroxide,
phenophthaein as a indicator.
Procedure:
First of all, we take separating funnel and wash it, with distilled water and then clean it
with dryier.
Now 25ml of water and 5ml of acetic acid was taken in separating funnel and it was
shaken for 2-3 times and then resting time was given to have solute in aqueous phase.
Then 25ml of carbon tetrachloride was added in separating funnel and separating was
shaken for some time and then allowed to settle for for 15-20 mint and pressure was
released from time to time.
After some time organic and aqueous phase was separated and visible.
Then organic phase and aqeuos phase was taken into two different beaker.
Both layer are separated and then was titrated against 1M NAOH (which is prepared by
adding 20g of NAOH in500 ml of distilled water ) by using phenolphthalein as a
indicator.
 Calculation:
For aqueous phase:

𝒗𝟏 = 5.5 𝒗𝟐 = 32

𝑴𝟏 = 1 𝑴𝟐 = ?

𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.172
𝑽𝟐

For organic phase:

𝑽𝟏 = 1.2ml 𝑽𝟐 = 17ml

𝑴𝟏 = 1 𝑀2 = ?

𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.07
𝑽𝟐

Distribution constant:

[𝟎.𝟎𝟕 ]𝑶
𝑲𝑫 = [ 𝑲𝑫 = 0.41
𝟎.𝟏𝟕𝟐 ]𝑨𝑸

Result:
As the concentration of acetic acid is higher in aqueous phase so acetic acid
is more soluble in aqueous phase than in organic phase.
DETERMINATION OF ACETIC ACID BETWEEN TWO IMMCIBLE
SOLVENT BY BATCH EXTRACTION :

Theory:
separate compounds based on their relative solubilities in two different immiscible
liquids. 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. LLE is an
extraction of a substance from one liquid into another liquid phase. The most common use of the
distribution principle is in the extraction of substances by solvents, which are often employed in
a laboratory or in large scale manufacturing. Organic compounds are generally much more
soluble in organic solvents, like benzene, chloroform, and ether, than in water and these solvents
are immiscible with water. Organic compounds are then quite easily separated from the mixture
with inorganic compounds in aqueous medium by adding benzene, chloroform, etc. Upon
shaking, these separate into two layers. Since organic compounds have their distribution ratio
largely in favor of the benzene phase, more of them would pass into a non-aqueous layer. Finally
this non-aqueous layer is removed and distilled to obtain the purified compound.

Principle:
When the solute (liquid or solid) is add to a heterogeneous system of two immiscible liquids (in
both of which the solute is soluble), the solute distributes between the two liquids. This
distribution governed by Nernst distribution law.
According To Distribution law:
“When a substance is added in excess quantity in two immiscible solvents, it distributes itself
between two liquid phases so that each becomes saturated. The distribution or partition of a
solute between immiscible liquids is known as Nernst's distribution law or simply distribution
law or partition law.”
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑜𝑟𝑔𝑎𝑛𝑖𝑐 𝑝ℎ𝑎𝑠𝑒
k=
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑎𝑞𝑢𝑒𝑜𝑠 𝑝ℎ𝑎𝑠𝑒

Apparatus required:
Separating funnel, beaker, burette, burette stand, pipette, conical flask, measuring
cylinder.
Chemical required :
Distilled water , acetic acid , carbon tetrachloride , (1M ) sodium hydroxide, phenophthaein as a
indicator.
Indicator: 10% Phenolphthalein

Procedure:
First of all, we take separating funnel and wash it, with distilled water and then clean it
with dryier.
Now 30 ml of water and 5 ml of acetic acid was taken in separating funnel and it was
shaken for 2-3 times and then resting time was given to have solute in aqueous phase.
Then 10 ml of carbon tetrachloride (ccl4) was added in separating funnel andit was
shaken virgorsly and then it was allowed to stand for 10 mint, so that the two phase are
separated.
Organic phase was appeared from bottom.
Then again 15 ml of carbon tetra chloride was added in separating funnel and extraction
was again carried out twice adopting the same procedure, so that whole of the 50ml of
𝑐𝑐𝑙4 are utilized.
Both the aqueous and organic layer is titrated against 1 M NaOH (which is prepared by
adding 20g of NaOH in 500ml of distilled water) using phenolphthalein as an indicator
and note the volume.
By using molarity formula, we can find the molarity and then we can find the value of
distribution constant.
 Calculation:
For aqueous phase:

𝒗𝟏 = 3.1𝑚𝑙 𝒗𝟐 = 34𝑚𝑙

𝑴𝟏 = 1

𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.0912
𝑽𝟐

For organic phase:

𝑽𝟏 = 1.2 𝑽𝟐 = 24

𝑴𝟏 = 1 𝑴𝟐 = ?

𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.05
𝑽𝟐

Distribution constant:

[𝟎.𝟎𝟗 ]𝑶
𝑲𝑫 = [ 𝑲𝑫 = 0.6
𝟎.𝟎𝟓 ]𝑨𝑸

Result: As the concentration of acetic acid is higher in aqueous phase so acetic acid is more
soluble in aqueous phase than in organic phase.
 DETERMINATION OF POTISSIUN IODOIDE (KI) BETWEEN TWO
IMMCIBLE SOLVENT BY BATCH EXTRACTION :

Theory:
separate compounds based on their relative solubilities in two different immiscible
liquids. 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. LLE is an
extraction of a substance from one liquid into another liquid phase. The most common use of the
distribution principle is in the extraction of substances by solvents, which are often employed in
a laboratory or in large scale manufacturing. Organic compounds are generally much more
soluble in organic solvents, like benzene, chloroform, and ether, than in water and these solvents
are immiscible with water. Organic compounds are then quite easily separated from the mixture
with inorganic compounds in aqueous medium by adding benzene, chloroform, etc. Upon
shaking, these separate into two layers. Since organic compounds have their distribution ratio
largely in favor of the benzene phase, more of them would pass into a non-aqueous layer. Finally
this non-aqueous layer is removed and distilled to obtain the purified compound.

Principle of solvent extraction:

When the solute (liquid or solid) is add to a heterogeneous system of two immiscible liquids (in
both of which the solute is soluble), the solute distributes between the two liquids. This
distribution governed by Nernst distribution law.
According To Distribution law:
“When a substance is added in excess quantity in two immiscible solvents, it distributes itself
between two liquid phases so that each becomes saturated. The distribution or partition of a
solute between immiscible liquids is known as Nernst's distribution law or simply distribution
law or partition law.”
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑜𝑟𝑔𝑎𝑛𝑖𝑐 𝑝ℎ𝑎𝑠𝑒
k=
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑎𝑞𝑢𝑒𝑜𝑠 𝑝ℎ𝑎𝑠𝑒
Apparatus required :
Separating funnel, beaker, burette, burette stand, pipette, conical flask, measuring
cylinder.
Chemicals required :
Distilled water , acetic acid , carbon tetrachloride , (0.1M ) HCL.

INDICATOR:
Methyl orange

PROCEDURE:
First of all, we take separating funnel and wash it, with distilled water and then clean it
with dryier.
Now 30 ml of water and 5 g of pottissum iodide (KI) was taken in separating funnel and
it was shaken for 2-3 times and then resting time was given to have solute in aqueous
phase.
Then 10 ml of carbon tetrachloride (ccl4) was added in separating funnel andit was
shaken virgorsly and then it was allowed to stand for 10 mint, so that the two phase are
separated.
Organic phase was appeared from bottom.
Then again 15 ml of carbon tetra chloride was added in separating funnel and extraction
was again carried out twice adopting the same procedure, so that whole of the 50ml of
𝑐𝑐𝑙4 are utilized.
After separating newly formed organic layer then add 10ml CCl4 and repeat the same
process.
Hold all separating organic phase in singular glassware and aqueous layer in another
glassware.
Both the aqueous and organic layer is titrated against 1 M HCl (which is prepared by
adding 5ml of HCl in 500ml of distilled water) where Methyl orange using as an
indicator and note the volume.
 Calculation:
For aqueous phase:

𝒗𝟏 = 4𝑚𝑙 𝒗𝟐 = 32𝑚𝑙

𝑴𝟏 = 0. 1 𝑴𝟐 = ?

𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.125
𝑽𝟐

For organic phase:

𝑽𝟏 = 3𝑚𝑙 𝑽𝟐 = 27𝑚𝑙

𝑴𝟏 = 0.1
 𝑴 𝟏 𝑽𝟏
𝑴𝟐 = 𝑴𝟐 = 0.111
𝑽𝟐

Distribution constant :

[𝟎.𝟏𝟏𝟏 ]𝑶
𝑲𝑫 = [ 𝑲𝑫 = 0.88
𝟎.𝟏𝟐𝟓 ]𝑨𝑸

Result: The concentration of KI is higher in organic phase so potassium iodide is more soluble
in organic phase than in aquas phase.