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Lab Manual Final 12-13

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12 views

Lab Manual Final 12-13

Uploaded by

pranavxkiller
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Experiment No.

12
Aim: To prepare double salts of ferrous ammonium sulphate (Mohr’s salt).

Theory
When a mixture containing equimolar proportions of ferrous sulphate and ammonium sulphate is
crystallised from its solution, a double salt is formed. The formation of double salt may be shown as
follows:

FeSO4 + (NH4)2SO4 + 6H2O FeSO4.(NH4)2SO4.6H2O


Ferrous ammonium sulphate (Mohr’s salt)

Fe2+ and Al3+ ions undergo hydrolysis, therefore, while preparing aqueous solutions of ferrous
sulphate and aluminium sulphate in water, 2-3 mL dilute sulphuric acid is added to prevent the
hydrolysis of these salts.

Material Required: Beaker (50 mL), Conical flask (50 mL), Trough, Glass rod, Tripod stand,
Funnel, Wire gauze, Ferrous sulphate, Ammonium sulphate, Dilute sulphuric acid, Ethanol

Procedure:

(i) Dissolve 3.5 g of ferrous sulphate and 1.7 g of ammonium sulphate (weighed separately), in 5
mL of distilled water contained in a 50 mL conical flask by heating. Add about 0.5 mL of
dilute sulphuric acid to the flask and concentrate the solution by heating till the crystallization
point is reached.
(ii) Allow the mixture to cool to room temperature slowly.
(iii) On cooling, light green crystals of ferrous ammonium sulphate separate out.
(iv) Decant the mother liquor and wash the crystals by shaking with very small amounts of 1: 1
cold water and alcohol mixture to remove sticking mother liquor.
(v) Separate the crystals by filtration wash with alcohol, dry between the folds of a filter paper
and record the yield.

Result:

Yield of Mohr’s salt is _________ g.

Precautions:

(a) Cool the solution slowly to get good crystals. Avoid rapid cooling.
(b) Do not disturb the solution while cooling.
(c) Avoid prolonged heating while preparing crystals of ferrous ammonium sulphate, as it may
oxidise ferrous ions to ferric ions and change the stoichiometry of the crystals.
Experiment No 13
Aim: To prepare potassium trioxalatoferrate(III).

Theory:
When hydrated ferric chloride is dissolved in aqueous solution of oxalic acid containing potassium
hydroxide, green crystals of potassium trioxalatoferrate(III) are obtained. The reaction involved in the
formation of these green crystals is as follows:

FeCl3 + 6KOH + 3H2C2O4 K3[Fe(C2O4)3] + 3KCl + 6H2O

Material Required: Beaker (50 mL), Porcelain dish, Water bath, Glass rod, Funnel, Ferric chloride,
Potassium hydroxide, Oxalic acid, Ethanol

Procedure:
(i) Prepare a solution of 3.0 g of oxalic acid in 12.5 mL of hot water contained in a clean 50 mL
beaker.
(ii) To the above solution, add 3.8 g of potassium hydroxide gradually in lots, with stirring so that
it dissolves completely.
(iii) Add 2.5 g of ferric chloride into the above solution with constant stirring till it is completely
dissolved.
(iv) Filter the solution and concentrate the green filtrate by heating in a porcelain dish over a water
bath and cool the mixture slowly.
(v) Filter the crystals so formed, wash with 1:1 mixture of cold water and alcohol and dry them
by pressing between the folds of a filter paper.

Result:
Yield of potassium trioxalatoferrate(III) is _________ g.

Precautions:
(a) Do not evaporate the entire solvent when the solution is being concentrated.
(b) Weigh the desired quantities of different substances accurately.
(c) Maintain the temperature of hot water around 40°C.
(d) Add potassium hydroxide to oxalic acid solution in small lots.

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