Instructions-
• Dear students note down the following practicals in your lab manual.
• Write Chemical equation in left side.
• Write result, yield and calculation part with pencil.
• Do not mention any date .
• Do neat and clean work.
• In case of any doubt feel free to ask.
Experiment- 1
Aim - To Prepare a Pure Sample of Ferrous Ammonium
Sulphate (Mohr’s salt), [FeSO4 . (NH4)2 SO4.6HO20]
Theory
Mohr’s salt is prepared by dissolving an equimolar mixture of hydrated ferrous sulphate
and ammonium sulphate in water containing a little of sulphuric acid, and then
subjecting the resulting solution to crystallisation when light green crystals of ferrous
ammonium sulphate. FeS04 . (NH4 )2S04.6H20 separate out.
Requirements
Two beakers (250 ml), china-dish, funnel, funnel-stand, glass-rod, wash-bottle, tripod
stand and wire-gauze. Ferrous sulphate crystals, ammonium sulphate crystals, dilute
sulphuric acid and ethyl alcohol.
Procedure
1. Take a 250 ml beaker and wash it with water. Transfer 7.0 g ferrous sulphate and
3.5 g ammonium sulphate crystals to it. Add about 2-3 ml of dilute sulphuric acid
to prevent the hydrolysis of ferrous sulphate.
2. In another beaker boil about 20 ml of water for about 5 minutes to expel dissolved
air.
3. Add the boiling hot water to the contents in the first beaker in small instalments at
a time. Stir with a glass rod until the salts have completely dissolved.
4. Filter the solution to remove undissolved impurities and transfer the filtrate to a
china-dish.
5. Heat the solution in the china-dish for some time to concentrate it to the
crystallisation point.
6. Place the china-dish containing saturated solution over a beaker full of cold water.
On cooling crystals of Mohr’s salt separate out.
7. Decant off the mother liquor quickly. Wash the crystals in the china-dish with a
small quantity of alcohol to remove any sulphuric acid sticking to the crystals.
8. Dry the crystals by placing them between filter paper pads.
Observations
Weight of crystals obtained =……….. g
Expected yield = ………..g
Colour of the crystals = …………..
Shape of the crystals =……
Experiment-2
Aim- To Prepare 2-Naphthol Aniline or Phenyl-azo-β-
Naphtholdye
Theory
2-Naphthol aniline dye or Phenyl-azo-β-naphthol is an orange-red dye. It belongs to a
large class of azo-compounds, all of which contain the characteristic grouping
Azo compounds are all coloured compounds. For the preparation of this dye, aniline is
diazotised and then diazonium salt thus obtained is subjected to coupling reaction with
2-naphthol.
Apparatus
One 100 mL conical flask, one 100 mL beaker, one 250 mL beaker, ice-bath, glass-rod,
buchner funnel, water pump.
Chemicals Required
Aniline = 4.5 ml
Sodium nitrite = 4g
2-Naphthol = 7 g
Cone, hydrochloric acid = 10 ml
Glacial acetic acid = 40 ml
Procedure
1. Take a 100 ml conical flask and add 4.5 ml of aniline, 10 ml of cone. HCl and 20
ml of water. Cool this solution to 5°C by placing the conical flask in a trough
containing ice- cold water.
2. In a 100 ml beaker dissolve 4 g of sodium nitrite in 20 ml of water and cool this solution
also to 5°C.
3. Now slowly add sodium nitrite solution to the solution of aniline in cone. HCl.
4. Dissolve 7.0 g of 2-naphthol in 60 ml of 10% NaOH solution taken in a 250 ml beaker and
cool this solution to 5°C by placing in an ice bath. Some crushed ice may be added
directly to fecilitate cooling.
5. Now add the diazotised solution very slowly to the naphthol solution with constant
stirring. The mixed solutions immediately develop a red colour and the phenyl-azo-β-
naphthol rapidly separates as orange-red crystals.
6. When the addition of diazo solution is complete, allow the mixture to stand in ice-salt
mixture for 30 minutes, with occasional stirring. Filter the solution through a buchner
funnel under suction from the pump. Wash the phenyl-azo-β-naphthol with water and dry
the crystals obtained by pressing between the folds of filter paper.
7. Recrystallise the product from glacial acetic acid. Filter the crystals obtained at the
pump. Wash with a few ml of ethanol to remove acetic acid. Phenyl-azo-β-naphthol is
obtained as orange-red crystals. Expected yield is 3 g and melting point is 133°C.
Result
Weight of phenyl-azo-β-naphthol obtained as orange-red crystals = …….g.
Precautions
1. The solution of the aniline hydrochloride should be cooled to 5°C, and this
temperature should be maintained throughout the addition of the sodium nitrite
solution.
2. Addition of sodium nitrite should be very slow because the reaction is exothermic
and may cause the temperature to rise.
3. Always add diazonium chloride solution to β-naphthol solution for dye formation
and not vice-versa.
