EXPERIMENT 4 : Preparation of Double Salt and Complex Salt

OBJECTIVES:
1. Prepare complex and double salt
2. Differentiate between complex and double salt
3. Identify the bond character between complex and double salt

THEORY

In this experiment, we are preparing different salt that is double salt and complex
salt. For the first one, double salts containing more than one cation or anion. They form
when one salt and more dissolved in a liquid then together crystallize in a regular pattern.
They have their own crystal forms which need not be the same as that of either of their
component salts. This is a solid state phemnomenon where in solution they are
decomposed completely, or nearly so, into of their component salts. In this respect double
salt are distinguished from complex salts, which give complex ions of their own in
solution. Double salts are extremely numerous.

Complex salt is another type of salt. It is a salt that does not dissociate in solution.
When ammonia is added to a solution of a cupric salt, a light blue precipitate of cupric
hydroxide is first formed which dissolves in excess of ammonia to form a deep purplish-
blue solution. The colour is due to the complex ion Cu(NH 3)4+. The sulfate of this ion is
easily obtained in solid form as the hydrate Cu(NH3)4SO4. H2O.
METHODOOGY

Double salt, CuSO4.(NH4)2SO4.6H2O

0.03mole of copper sulfate + 0.03mole ammonium sulfate was added into a beaker
contain 15ml of hot water

Coll filter

Dry, weight

Observe

Complex salt, Cu(NH3)4SO4. H2O.

10ml [NH3] + 6ml H2O and 6.25g copper sulfate was put into a beaker

10ml ethyl alcohol was added

1 hour

Cool

Filter

Wash with 10ml alcohol + 10ml [NH3]

 ↓

Wash with 10ml ether

Dry in oven

weight

RESULT AND CALCULATION

A) Double salt

Sample Number of mole Mass of theory Mass used in

(mole) (g) experiment (g)
CuSO4.5H2O 0.03 7.49 7.49
(NH4)2.SO4 0.03 3.96 3.69

Mass of filter paper 1.12 g

Mass of filter paper + sample 7.89 g
Mass of sample 6.74 g

Calculation
Salt CuSO4.5H2O

No. of mole = 0.03 mole

Mass of relative molecule = [(63.546) + (32.066) + 9 (16) + 10 (1.0079)]
= 249.691
Mass = (0.03) (249.691)
= 7.49 g
Salt (NH4)2.SO4

No. of mole = 0.03 mole

Mass of relative molecule = [2 (14.007) + 8 (1.0079) + 32.066 + 4 (15.999)]
= 132.13292
Mass = 3.96 g

Reaction equation:

CuSO4.5H2O + (NH4)2.SO4 + H2O → CuSO4.(NH4)2SO4.6H2O

The mass of sample of CuSO4.(NH4)2SO4.6H2O from this experiment

= 6.74 g

From the theory, mass of CuSO4.(NH4)2SO4.6H2O

Mass = no. of mole x mass of relative molecule

Mass of relative molecule : (63.546) + 2 (32.066) + 14 (15.999) + 20 (1.0079)

+ 2 (14.007)
= 399.836 g/mole

Mass in theory : (0.08) (399.836)

= 11.005 g

% of sample from experiment

= experiment sample x 100
 Mass in theory

= 6.47 g x 100
11.005 g

= 61.24 %

% of error = (11.005 g – 6.74 g) x 100

11.005 g

= 38.76 %

B) Complex salt, Tetrammine Cupric Sulfate

CuSO4.(NH4)2SO4.6H2O

Sample Mass of theory Mass used in Volume

(g) experiment (g) (ml)
CuSO4.5H2O 6.24205 6.25 -

NH3 - - 10

Mass of filter paper 1.13 g

Mass of filter paper + sample 5.13 g
Mass of sample 4.00 g

Calculation :
Salt CuSO4.5H2O
No. of mole : 0.025 mole
Mass of relative molecular : [(63.546) + (32.066) + 9 (15.999) + 10 (1.0079)]
= 249.682 g/mole
Mass : (0.025) (249.682)
= 6.24205 g

The equation of reaction :

CuSO4.5H2O + 4NH3 → Cu(NH3)4SO4.H2O + 4H2O

From theory, mass of Cu(NH3)4SO4.H2O

= no. of mole x mass of relative molecule

Mass of relative molecule = 63.546 + 4 (14.007) + 32.066 + 5 (15.999) + 14 (1.0079)

= 245.7456 g/mole
Mass from theory = 0.025 x 245.7456
= 6.14364 g

% of sample from experiment

= mass from experiment x 100
Mass from theory

= 4.00 x 100
6.14364
= 65.108 %

% errors : (6.14364 - 4.00) x 100

6.14364

= 34.892 %

Observation :
Observation Double salt Complex salt
Homogeneous Homogeneous Heterogeneous
Appearances Sky blue Deep blue
- colour, crystal size Diamond shape Rod shape
Behaviour in solution Dissolve Cannot dissolve

DISCUSSION
Preparation of CuSO4.(NH4)2SO4.6H2O and Cu(NH3)4SO4.H2O show the difference in
constitution of structure and behaviour in solution between double salt and complex salt.
From the experiment, we found out that double salt can dissolve in water. Double salt
produce a homogeneous solution. The appearance are diamond shape. Formation of Cu2+
make the solution colour are sky blue.

From the experiment, double salt is CuSO4.(NH4)2SO4.6H2O. The formation of crystal is

observed in sky blue colour and has a shining and coarse surface. Do not stir during the
cooling process to get the right result. The salt is highly soluble to form homogeneous
solution. 6.74 g salt mass formed while the theory value is 9.9959 g. The percentage error
is 38.76%

Equation reaction:
CuSO4.5H2O + (NH4)2SO4 → CuSO4.(NH4)2SO4.6H2O
The mass of double salt that we get is very little compare to the theory value. This might
be happen because of not all the crystal is fully transferred into the filter paper by using
Buchner funnel. There might have many errors occur in the electrical balance that make
the reading not precise. The filtering process is not perfect and caused some crystal lose.

The complex salt is Cu(NH3)4SO4.H2O. The colour of the crystal formed is deep blue.
The structure are weak and not shining. Complex salt cannot dissolve in water. The
formation of Cu(NH4)44+ turn the solution into deep blue colour. It is more concentrated
and easy to formed Cu(NH4)4+4 complex ion by leaving the solution for 1 hour. To get
the best result the solution must be cooling in natural. The shape of crystal is small and
tiny like rod. Mass of complex salt is 4.00g while the theory is 6.14364g. the percentage
error is 34.892%

The reaction is :
CuSO4.5H2O + 4NH3 → CuSO4.(NH4)2SO4.H2O + 4H2O
The result that we get from experiment and theory are different due to some errors which
are, the cooling process is not complete, the error in the electrical balance during take the
weight value, some salt is still leaving on the glass when prepare the salt, the crystal lost
from the imperfect filtering process and only some the crystal is transfer into the filtering
paper by using Buchner funnel.

PRECAUTION
1. Weight CuSO4.5H2O and (NH4)2.SO4 approximately.
2. Do the mixture in fume cupboard.
3. Do the cooling process slowly and complete.

CONCLUSION
1. From this experiment we got the mass of double salt is 6.47 g while mass of
complex salt is 4.00g.
2. The double salt characteristics are homogenus, dissolve and its appearance is sky
blue and diamond shape.
3. The complex salt characteristics are heterogenus, cannot dissolve and its
appearance is deep blue and rod shape.

REFERENCES :

1. Shriver & Atkins , Oxford Inorganic chemistry, fourth edition

2. www.tutornext.com/difference-between-double-salt-complex/2461
3. www.britannica.com/eb/topic-129980/complex-ion

QUESTIONS

1. Name three double salts that are important in industry or in laboratory practice.
 • Potassium sodium tartrate-in the process of silvering mirror, an ingredient
of Fehling’s solution.
• Calcium double salt - additive in food product (such as French Fries and
potato chips)
• Alum - purify water and harden plaster of Paris.

2. Metallic cations form complex ions with ammonia.

• Cadmium,
• nickel
• argentum.

3. When the complex salt is dissolved in water, a slight precipitate appears. What is
this precipitate, and why is it formed?
Cu(OH)2, because Cu is bind to water molecule.

4. What is the difference in constitution between tetrammine cupric sulfate and

cupric ammonium sulfate?