Inorganic Preparation

Experiment 1: Preparation of tris(thiourea)copper(I) sulphate
Aim:
To prepare tris(thiourea) copper (I) sulphate
Principle:
When a solution of copper sulphate and thiourea are shaken together they readily yield
the complex.
2Cu2SO4 + 7H2N–CS–NH2 ➔ [Cu(H2N–CS–NH2)3]2SO4+ H2N–CS–NH–HSO4
Chemicals required
Thiourea - 4g
Copper sulphate - 4g
Procedure
Dissolved 2g of thiourea in 12.5ml of hot water and then cooled the solution to room
temperature. Shaken the solution well while adding to it in portions a cold solution of
4g of copper sulphate in 20ml of water. Finally cooled thoroughly in running water
while the separated yellowish oil adheres to the walls of the flask. Decanted and
rejected the mother liquor. Shaken the oil vigorously with the solution of 2g of thiourea
in 12.5ml of water, untill crystallization is complete. Filtered and washed the crystals
with small amount of water. Recrystallised with 5% aqueous thiourea containing 2ml
of IN sulphuric acid. The recrystallisation temperature should not be allowed to rise
above 80°C. Noted the yield.
Result
The yield of tris(thiourea)copper (I) sulphate = ………………g.
PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

Experiment 2: Preparation of potassium trioxalatochromate(III)trihydrate
Aim:
To prepare potassium trioxalatochromate(III) trihydride complex
Principle:
The experiment is based on the following equation:
K2Cr2O7 + 7H2C2O4 + K2C2O4 ➔ K3[Cr(C2O4)3] + 6CO2 +H2O
Chemicals required:
Oxalic acid - 3g
Potassium dichromate - 1g
Potassium oxalate - 1.2 g
Ethyl alcohol - 2 ml
Procedure
To the solution of 3g of oxalic acid in 8ml of warm water, added in portions 1 g of
potassium dichromate. When the vigorous reaction has subsided, the resulting
solution was heated to boiling and in it 1.2 g of potassium oxalate was dissolved. The
whole solution was cooled to room temperature. Added 1.2 ml of ethanol and cooled.
The green crystals separated out from an almost black solution. Collected the
precipitate from Buchner funnel, washed with 1 % ethanol and finally with pure ethanol.
The yield was noted.
Result
The yield of potassium trioxalatochromate(III)trihydride complex = ………………g.

Experiment 3: Preparation of tetraaminecopper(II) sulphate
Aim:
To prepare tetraammine copper(II) sulphate complex
Principle:
Hydrated tetraammine cupric sulphate is obtained by
addition of liquid ammonia in the solution of copper
sulphate followed by the addition of ethyl alcohol in the
solution.
CuSO4+ 4NH3 +H2O [Cu(NH3)4]SO4.H2O
Chemicals required:
Copper sulphate - 2.5 grams
Liquid ammonia - 5.0 mL
Ethyl alcohol - 7.5 mL
Procedure:
Firstly dissolve 2.5 g of crystalline CuSO4.5H2O in minimum amount of H2O in 250 mL
beaker. Now add few drops of conc. H2SO4 to clear up the solution if necessary. Add
liquor ammonia to copper sulphate solution from dropping funnel with constant stirring
until the blue precipitate formed is dissolved to give a deep solution. Now add 20 mL
of ethyl alcohol slowly with constant stirring to the deep blue solution. And allow it to
stand to slow evaporation which gives long needle shaped brilliant dark blue violet
crystal of tetraamine cupric sulphate complex. Filter and wash it with ethyl alcohol and
dry in a desiccator.
Result
The yield of tetraamine copper(II) sulphate = …………………g.

Experiment 4 :Preparation of Reineck’s salt; NH4[Cr(NCS)4(NH3)2]·H2O
8 g of ammonium thiocyanate in a china dish is melted at temperature of 145–150°. At

this point an intimate mixture of 1.70 g of ammonium dichromate and 2.0 g of
ammonium thiocyanate is added in portions of 0.10 g with constant stirring. After about
ten such portions have been added a fairly vigorous reaction takes place with evolution
of ammonia and the temperature rises to 160°. The flames are extinguished, and the
remainder of the mixture is added at such a rate that the heat of reaction maintains
the temperature at 160°. Stirring is continued while the mass cools, and any lumps of
solid which form around thesides of the vessel are broken loose.The product, is finely
powdered and stirred with 7.5 ml of ice water in a large beaker. After fifteen minutes
the insoluble portion is filtered by suction, freed as completely aspossible from mother
liquor without washing (Note 5), and stirred into 2.5 l. of water previouslywarmed to
65°. The temperature is then rapidly raised to 60° (Note 6), the solution is filtered at
oncethrough a hotwater funnel, and the filtrate is placed in a refrigerator overnight.
The resulting crystals are collected and the mother liquor employed for a second
similar extraction of the residue at 60°. This yields a further crop of crystalline Reinecke
salt. The mother liquor is finallyconcentrated to 250–300 cc. by evaporation at 40–50°
under reduced pressure, when a small third crop (12–13 g.) is obtained. The total yield
of air-dried crystals is 250–275 g. (52–57 per cent of thetheoretical amount) (Note
7).The undissolved residue from the second extraction consists chiefly of Morland salt
(the guanidine salt of the Reinecke acid) and amounts to 130–135 g. (33–34 per cent
of the theoretical amount)
(Note8).

Experiment 5: Preparation of hexathioureacopper(I) chloride dihydrate*
Aim:
To prepare hexathioureacopper(I) chloride dihydrate
Principle:
2Cu + 2HCl + 6NH2-CS-NH2 ➔ [Cu(H2N-CS-NH2)3]2 + Cl2 + H2
Chemicals required:
thiourea - 5g
Copper turnings - 1g
Conc.HCl - 5ml.
Procedure:
Dissolved 5g of thiourea in 25ml of hot water in a conical flask with a funnel. To the
solution added lg of copper turnings and then 5ml of concentrated HCI. Heated on the
wire gauze while copper is dissolved with the liberation of hydrogen. After 5 minutes,
the solution is filtered while hot and then allowed the solution to cool slowly. The
crystals separated are filtered, washed with acetone and noted the yield.
Result:
Yield of tris(thiourea)copper(I) chloride = …………………g.

Experiment 6: Preparation of cis-potassium tri oxalate diaquachromate(III)
Aim:
To prepare cis-potassium tri oxalate diaquachromate(III)
Principle:
K2Cr2O7 + 7H2C2O4.2H2O➔2 K[Cr(C2O4)2(H2O)2].2H2O + 6CO2 + 13H2O
Weigh the oxalic acid and potassium dichromate and place them in their respective
mortars.
ii. Grind both separately and mix the two materials.
iii. Continue to grind until a frothing of CO2 is released. The reaction is started.
iv. Immediately pour ethanol in the mixture and heat until the syrup solidifies into dry
powder.

Experiment 7: Preparation of sodium tris(oxalato)ferrate(III) complex
Aim:
To prepare sodium tris (oxalato) ferrate (III) complex.
Principle:
Mixing of FeCl3 and KOH in minimum amount of water forms
hydrated ferric oxide slurry. And when this slurry is added to
the hot solution of sodium oxalate, a greenish-brown solution
of Iron (III) oxalate obtained, which on slow evaporation gives
greenish crystals of sodium tris (oxalato) ferrate (III).
FeCl3 +3NaOH  Fe(OH)3+ 3NaCl
Fe(OH)3+ 3H2C2O4 + 3NaOH  Na3[Fe(C2O4)3] + 6H2O
Required chemicals:
Ferric chloride - 2.50 g
Sodium hydroxide - 2.75 g
Oxalic acid - 3.00 g
Procedure:
i) Preparation of ferric hydroxide: Separately dissolve 2.5 g of FeCl3 and 1.75 g of
sodium hydroxide in 1-2 mL of water. Now add sodium hydroxide solution to ferric
chloride solution to make brown colour slurry with stirring. This slurry is the precipitate
of Fe(OH)3. Filter the precipitate of ferric hydroxide in Bruckner funnel and wash it with
small amount of hot water 2 to 3 times.
ii) Preparation of sodium tris (oxalato) ferrate (III): Dissolve 3g of oxalic acid in 10-
15 mL of hot water then add 1 g of NaOH. Transfer ferric hydroxide in this hot solution
with constant stirring. Dissolve Fe(OH)3 in hot solution, taking 3 moles of oxalic acid
per 1 mole of Fe(OH)3. This will produce dark greenish-brown solution of iron (III)
oxalate. Filter the solution and concentrate the green filtrate on water bath and obtain
green crystal of sodium tris (oxalato) ferrate (III)
Result
The yield of sodium tris (oxalato) ferrate (III) is …………………….g.

Experiment 8: Preparation of hexathiourealead(II) nitrate; [Pb{CS(NH2)2}6](NO3)2
Aim:
to prepare hexathiourealead(II) nitrate complex
Principle:
???
Chemicals required:
Lead nitrate - 0.25 g
Thiourea - 0.33 g
Procedure:
Dissolve (0.25 gr) of lead nitrate in (5ml) of distilled water in beaker then heat it.
Dissolve (0.33 gr) of thiourea in (5 ml) of distilled water and then heat it. Mix the two
solutions in one beaker and then cool the mix with ice bath; this will lead to produce
separated colourless crystals in the form of needles. Filter the solution, dry the crystals
and weight out them.
Result
The yield of hexathiourealead(II) nitrate complex = ………………….g.

Inorganic Preparation

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Experiment 1: Preparation of tris(thiourea)copper(I) sulphate

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

CuSO4+ 4NH3 +H2O [Cu(NH3)4]SO4.H2O

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

8 g of ammonium thiocyanate in a china dish is melted at temperature of 145–150°. At

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

ii. Grind both separately and mix the two materials.

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

to prepare hexathiourealead(II) nitrate complex

PARTHIBAN D | ASSOCIATE PROFESSOR, DEPT OF CHEMISTRY, RVGAC

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