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Date : 24/07/2020

Experiment No. 1
Aim : To Prepare a Pure Sample of Potash Alum (Fitkari), [K2SO4.Al2 (SO4)3. 24H2O]
(Fitkari).

Theory :
Potash alum is a double salt and is prepared by crystallization of a solution of
equimolar mixture of hydrated Aluminum Sulphate (Al2(SO4)3.18H2O) and Potassium
Sulphate in minimum amount of water containing a little of sulphuric acid, on
crystallisation colourless transparent octahedral crystals of potash alum separate out.
K2SO4 + Al2 (SO4)3. 18H2O + 6H2O K2SO4.Al2 (SO4)3. 24H2O
-1 -1 -1
(174gmol ) (666 gmol ) (948 gmol )

Requirements :

1. Two beakers, porcelain-dish, funnel, filter-stand, filter paper, glass-rod, wash bottle,
watch glass, bottle, tripod stand, wire-gauze, Spirit lamp or Bunsen burner with tripod
stand and waire gauze or a electric heating plate, and a chemical balance or digital
weighing balance.

2. Potassium sulphate (2.5) , Aluminium Sulphate(10g) and conc. sulphuric acid and
distilled water.

Procedure :

1. 2.5g of Potassium Sulphate is dissolved in minimum quantity of distilled water by


warming and stirring the mixture.

2. 10g Aluminium Sulphate is mixed with 4-5 drops of conc. H2SO4 or 1ml of
dil.H2SO4 and dissolved in minimum quantity of distilled water by warming and
stirring the mixture. Then the solution is filtered and clear filtrate is taken.
Sulphuric Acid is added first to prevent hydrolysis of aluminium sulphate into
aluminium hydroxide.

3. Now both the solutions are mixed in a porcelain dish and concentrated by heating
till crystallization point is attained.

4. Crystallization point is checked from time to time. To do so the tip of a glass rod is
soaked in the hot solution and cooled by blowing at the tip, if any crystal deposit is
found at the tip, means crystallization point is reached and heating must be
stopped.

5. When crystallization point is reached , heating is stopped and the solution is


poured onto a watch glass placed over a filter paper made wet with cold water and
allowed to stand for crystallization.

6. Soon the colourless crystals of potash alum separate out. Decanting off the
mother liquor crystals are collected and washed with a small quantity of very cold
water and then dried by soft pressing between blotting or filter paper.

7. Finally the crystals are weighed to find its yield.

Observations

Expected yield = about 14g

Actual yield obtained = 12g

Color of the Crystal = Colourless transparent.

Precautions

1. Cool the solution slowly to get good crystals.


2. Do not disturb the solution while it is being cooled.

Youtube Video link :Preparation of Potash alum


https://www.youtube.com/watch?v=JTZ8u4NMAlg
Date : 25/07/2020
Experiment No. 2
Aim : To Prepare a Pure Sample of Mohr’s Salt FeSO4 . (NH4)2 SO4. 6H2O

Theory :
Mohr’s salt is a double salt and is prepared by crystallization of a solution of equimolar
mixture of green vitriol ( hydrated Ferrous Sulphate FeSO4.7H2O ) and Ammonium
Sulphate (NH4)2SO4 in minimum amount of water containing a little of dil sulphuric acid ,
on crystallisation, very light green octahedral crystals of Mohr’s salt separate out.
FeSO4.7H2O + (NH4)2 SO4 FeSO4 . (NH4)2 SO4.6H2O + H2O
-1 -1 -1
(278gmol ) (132 gmol ) (392 gmol )

Requirements :

1. Two beakers, porcelain-dish, funnel, filter-stand, filter paper, glass-rod, wash bottle,
watch glass, bottle, tripod stand, wire-gauze, Spirit lamp or Bunsen burner with tripod
stand and waire gauze or a electric heating plate, and a chemical balance or digital
weighing balance.

2. 4g Green vitriol FeSO4.7H2O and 2g Ammonium Sulphate (NH4)2 SO4 and 2ml dil.
sulphuric acid and distilled water.

Procedure :
4g Green vitriol and 2g Ammonium Sulphate are mixed with 2ml dil. H2SO4 in a
porcelain dish. H2SO4 prevents hydrolysis of FeSO4 .

8. 30ml distilled water is taken in a beaker and boiled for about 5 minutes to expel
dissolved oxygen from it. This prevents oxidation of Fe(II) into Fe(III).

9. Now the mixture in porcelain is stirred with optimum quatity of boiled water to
dissolve the content. The solution so obtained is filtered and filtrate is taken in the
porcelain dish and the solution is concentrated by heating till crystallization point
is attained.

10. Crystallization point is checked from time to time. To do so the tip of a glass rod is
soaked in the hot solution and cooled by blowing at the tip, if any crystal deposit is
found at the tip, means crystallization point is reached and heating must be
stopped.

11. When crystallization point is reached , heating is stopped and the solution is
poured onto a watch glass placed over a filter paper made wet with cold water
and allowed to stand for crystallization
12. Soon the light green crystals of Mohr’s salt separate out. Decanting off the mother
liquor crystals are collected and washed with a small quantity of very cold water
and then dried by soft pressing between blotting or filter paper.

13. Finally the crystals are weighed to find its yield.

Observations

Expected yield = 5.7g

Actual yield obtained = 4.2g

Color of the Crystal = Light green.

Precautions

1. Cool the solution slowly to get good crystals.


2. Do not disturb the solution while it is being cooled.

Youtube Video link : Preparation of Moh’s Salt


https://www.youtube.com/watch?v=Zrl2SXE0CUs
Possible Viva Questions :

1. What are double salt and complex salt.

Ans.
Double Salt :
A double is a salt usually produced by crystallization of equimolar mixture of two normal salts.
Double salts can retain its identity only in solid state but splits into original normal salts in
aqueous solution from which it was obtained and produces ions of original salts.
Example . Potash alum K2SO4.Al2(SO4)3.24H2O is a double salt and is obtained by
crystallization of equimolar solutions of K2SO4 and and hydrated Aluminium sulphate Al2(SO4)3
.18H2O .
In aq. Solution potash alum will produce K+, Al3+, and SO42- ions.
Another example of double salt is Mohr’s salt FeSO4.(NH4)2SO4.6H2O which is obtained by
crystallization of equimolar solutions of hydrated ferrous sulphate FeSO4.7H2O .
In aq. Solution Mohr’s salt will produce Fe2+, NH4+ , an SO42- ions.

Complex Salt : A complex salt contains complex ions and is produced by crystallization of
equimolar mixture of two normal salts. A Complex salt can retain its identity both in solid and
liquid state and produces chrateristic +ve cations and –ve complex ion in aq. solution.
Example . Potassium ferrocyanide K4[Fe(CN)6] is a complex salt and is obtained by
crystallization of equimolar solutions of potassium sulphate K2SO4 and and ferrous cyanide
Fe(CN)2. The IUPAC name of K4[Fe(CN)6] is Potassium hexacyanoferrate(II) .
In aq. Solution this salt will produce potassium ion K+, and ferrocyanide ion Fe(CN)64- ions.
here Fe(CN)64- is the complex ion. Any corordination compound is a complex salt.
Another example of complex salt is potassium tioxalatochromate(III) sulphate K3[Cr(C2O4)3]SO4.

2. Mention the ions produced by


(a) potassium ferrocyanide and (b) potash alum in aq. Solution of each

Ans. Try yourselves


3. What are alums ? Mention two examples
Ans. Alums are double salts with general formula M2+SO4 . M23+(SO4)3 . 24H2O wher M+ is a
monovalent metal or cation and M3+ is a trivalent metal ion .
Example :
(i) Potash alum K2SO4.Al2(SO4)3 . 24H2O
(ii) Chrome alum K2SO4.Cr2(SO4)3 . 24H2O
4. What is a crystallization point.
Ans. The saturated stage of a concentrated solution which when cooled undergoes
crystallization is known as crystallization point.
5. What is a mother liquor ?
Ans. The liquid left behind after separation of crystals from a saturated solution is called the
mother liquor.
6. Name some uses of potash alum.
Ans. After shave antiseptic and styptic , water purification, mordant in dying and calico
printing.
7. Why do you use H2SO4 in the preparation of potash alum
Ans. Try yourselves
8. Why do you use H2SO4 in the preparation of Mohr’s salt
Ans. Try yourselves
9. Why the distilled water to be used to dissolve FeSO4 in the preparation of Mohr’s salt has
to be boiled for some time.
Ans. Try yourselves
10. Why is Mohr’s salt preferred over normal FeSO4 in volumetric analysis ?
Ans. Fe(II) in Mohor’s salt is not easily oxidized into Fe(III) as that in normal FeSO4.

11. Mention formulae of Green Vitriol, White vitriol and Blue vitriol
Ans. Geen vitriol FeSO4. 7H2O
White vitriol ZnSO4. 7H2O
Blue vitriol CuSO4. 7H2O
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