SYNTHESIS AND STOICHIOMETRIC ANALYSIS OF

HEXAAMMINENICKEL(II)CHLORIDE
Abstract

In this experiment, we synthesize complex salt hexaamminenickel (II) chloride via crystallization
and purification methods. We also add a known excess quantity of an acid to neutralize the
ammonia hydroxide. This is to obtain the amount of ammonia present in the product. We start
the experiment by adding the green solution which is the nickel (II) chloride with the
concentrated ammonia. Then, the solution turns into purple colour. Based on the calculations,
average amount of N H 3 found in the product is 33.67% while for chloride ions is 19.84%.

1.0 Introduction

Hexaamminenickel (II) chloride, ¿]Cl 2, is a coordination compound whose nickel atom and
six ammonia molecules constitute the cation ; the anion is the chloride ion. In aqueous solution
nickel ion ( N i 2+¿¿ ; Ni(II)) is surrounded by six water molecules which are actually bonded to the
central metal ion. This complex is called the hexaquanickel(II) ion. When aqueous nickel
chloride is precipitated from solution, the nickel ions carry their six water molecules into the
crystals and so solid nickel(II) chloride is hydrated, has the formula [ ¿( H 2 O)6 ¿ Cl 2 , and is more
properly called hexaquanickel(II) chloride. If ammonia is added to a solution of this salt,
ammonia molecules compete with the water in bonding Ni 2+ and, because the ammonia forms
a stronger bond than water, the ammonia replaces the water according to:

[¿( H 2 O)6 ¿ Cl 2 (aq) +6 NH 3 (aq) → ¿]Cl 2 (aq) + 6 H 2 O (l)

Objective of this experiment is to synthesis a complex which is complex salt

hexaamminenickel (II) chloride via crystallization and purification methods. Other than that, to
quantify chemical component in a chemical complex via back titration method.

2.0 Experimental
2.1 Materials
Nickel(II)chloride, distilled water, concentrated ammonia, ethanol, acetone, standard
hydrochloric acid, bromocresol green, standard sodium hydroxide, bromophenol blue indicator,
nitric acid, diphenycarbazone, 2-propanol, standard mercury(II) nitrate solution were used in
this experiment.
2.2 Synthesis of hexaamminenickel(II) chloride
Nickel (II) chloride (4.413g , 0.030 mol) was dissolved in 6ml distilled water. In the fume
cupboard, 12ml concentrated ammonia was added to the above solution and the mixture was
warmed for about 10 minutes. The solution was cooled in an ice-bath, and 6ml ethanol was
added while stirring the solution with glass rod. The formation of solid was noted. When all of
the solid has formed, the solution was filtered under suction and washed with ethanol ,
followed by acetone. The weight of solid was recorded.
2.3 Analysis of ammonia
Hexaamminenickel(II) chloride ( 0.206g , 0.894 mmol ) was weighed and dissolved by adding
standard hydrochloric acid (25.0 ml, 0.28 M). 3-5 drops of bromocresol green was added to the
solution. The solution was titrated with standard sodium hydroxide solution until the colour of
the indicator changed to pale blue.
2.4 Analysis for chloride ion
Hexaamminenickel(II) chloride (0.209g , 0.894 mmol ) was weighed and dissolved in 10ml
distilled water. 2 drops of bromophenol blue indicator was added to the solution and nitric acid
(1M) was added using dropper until the color of the solution changes to green. 5 drops of
diphenycarbazone and 25 ml of 2-propanol was added to the mixture. The mixture was titrated
with standard mercury (II) nitrate solution until the colour of the indicator changed to pale
purple.

3.0 Results and Discussion

Table 1 : Weight of hexaamminenickel(II) chloride
 Weight/(g)
1 2
¿]Cl 2 + plastic 1.6880 1.3454
Plastic 0.9963 0.9655
¿]Cl 2 0.6717 0.3799

Green hydrated nickel (II) chloride [¿( H 2 O)6 ¿ Cl 2 was dissolved in water. When adding
concentrated ammonia, the solution turns purple colour. Violet crystals formed in the pale navy
blue solution, which was cooled in an ice bath. Then, violet crystals were filtered under suction.
The procedure to synthesis hexaamminenickel(II) chloride was repeated twice because the solid
of hexaamminenickel(II) chloride obtained is insufficient to proceed for analysis N H 3 and
Cl−¿¿.The data in table 2 show the average amount of NH 3 in the product is 33.67% which a bit
far from the theoretical value which is 44.42%. The theoretical value is calculated by dividing
the molar mass of 6 mole of N H 3 with molar mass of ¿]Cl 2 .

Table 2 : Analysis for N H 3

Weight of¿]Cl 2/g 0.2056 0.2181

Molarity of HCl 0.2803 M
Initial volume of HCl, V initial/ml 25.00 25.00
Molarity of NaOH 0.1009 M
Final burette reading/ml 36.71 30.34
Initial burette reading/ml 7.13 3.98
Volume of NaOH/ml 29.58 26.36
¿
Volume of excess HCl, V excess /ml 10.65 9.45
Volume of reacted HCl, V reacted /ml 14.35 15.55
Moles of NH 3# 0.004 mol 0.004 mol
Weight of NH 3 0.0685g 0.0742g
% NH 3 in ¿ ¿]Cl 2 33.32 34.02

*V (HCl , excess)=M (NaOH ) V (NaOH ) ¿ M (HCl)

# moles of ammonia = moles of HCl = M ( HCl) V (HCl)reacted /1000

Theoritical value of % NH 3 in ¿ ¿]Cl 2=(molar mass of 6 mole of NH 3 / molar mass of ¿ ¿]Cl 2 ) ×

100 %

% NH 3 ¿ ¿ ¿]Cl 2=(weight of NH 3/ weight of ¿ ¿]Cl 2) × 100

In table 3, the chloride analysis show that average amount of Cl−¿¿ in the product is
19.84%. This value was obtained when the chloride ions is titrated with standard mercury(II)
nitrate.
Table 3 : Analysis for Cl−¿¿ ion

Weight of ¿ ( N H 3 )6]Cl 2/g 0.1617 0.2093

Molarity of H g 2+¿¿ 0.0569 M
Final burette reading /ml 12.44 21.71
Initial burette reading /ml 3.35 12.89
Volume of H g 2+¿¿ /ml 9.09 8.82
Moles of Cl−¿ 0.001 mol 0.001 mol
Weight of Cl−¿¿ 0.03667 0.03558
% Cl−¿¿ in ¿ ( N H 3 )6]Cl 2 22.68 16.99

*moles of Cl−¿¿ = 2 moles of Hg 2+¿¿ = 2 M ¿¿ / 1000

% Cl−¿¿ in ¿ ( N H 3 )6]Cl 2 = (weight of Cl−¿¿/ weight of ¿ ( N H 3 )6]Cl 2) × 100%

The equation for the formation of ¿ ( N H 3 )6]Cl 2 is

NiCl 2 ( aq )+ 6 NH 3 ( g ) → ¿ ( N H 3 )6]Cl 2(aq)

NiCl 2 ( aq )+ 6 NH 3 OH ( aq ) → ¿ ( N H 3 ) 6]Cl 2 ( aq )+ 6 H 2 O(l)

4.413 g
n¿ CL = =0.03405 mole
2
129.5994 g /mol

12 ml ×14.5 M
n N H OH = =0.174 mole
3
1000

0.03 mole × 6=0.18 mole of NH 3 OH is needed when all amount of NiCl 2 is used for the
synthesis of hexaamminenickel(II) chloride, ¿ ¿]Cl 2. Ammonium hydroxide, NH 3 OH is the
limiting reactant in the reaction because of insufficient amount ammonium hydroxide to react
with all of the NiCl 2 .

To find theoretical yield of hexaamminenickel(II) chloride :

n 0.174 mole
[¿ ( N H3 )¿ ¿6 ]Cl 2= =0.029 mol ¿
6

Theoretical yield : 0.029 mol × 230.032 g/mol = 6.67g

Actual yield : 0.6717g
actual yield
Percentage yield = × 100 %
theoretical yield
0.6717 g
= ×100 %=10.07 %
6.67 g

molar mass of ∋ ¿ ¿
% Ni = 58.693
molar mass of [¿ ( N H 3 ) ¿ ¿ 6 ]Cl 2= ×100 %=25.51 % ¿
230.032
Average mass of ¿ ¿]Cl 2 is 0.199 g
25.51
Mass of Ni in ¿ ¿]Cl 2 = × 0.199 g=0.0508 g
100

Empirical formula :

¿2 +¿¿ NH 3 Cl−¿¿
Mass 0.0508g 0.07135g 0.036125g
Mol 0.0008 mol 0.004 mol 0.001 mol
Ratio 0.0008 0.004 0.001
=1 =5 =1
0.0008 0.0008 0.0008

The empirical formula obtained by the calculation is different from the theoretical
formula which is ¿ ¿]Cl 2. This error occurs because of a few error happens when conducting the
experiment. One of them is we overshoot the end point of the titration and we also need to
repeat the procedure of synthesis of hexaamminenickel(II) chloride because we did not get
enough hexaamminenickel(II) chloride to proceed with procedure to analysis the ammonia and
chloride ions.
4.0 Conclusion
In conclusion , hexaamminenickel(II) chloride is successfully synthesis via crystallization and
purification methods. The average amount of ammonia, Ni and chloride ions present in the
product are is 33.67% , 25.51% , 19.84%.

References
1. Rose, N. J., Elder, M. S., & Busch, D. H. (1967). Complexes derived from the reaction of
hexaamminenickel (II) ion with acetone. Inorganic Chemistry, 6(10), 1924-1926.

2. Wieder, G. M. (1986). Preparation and spectrophotometric analysis of hexaaminenickel(II)

chloride: A general chemistry experiment. Journal of Chemical Education, 63(11), 988. doi:
10.1021/ed063p988’

3. Wells, A. F. Structural Inorganic Chemistry, Oxford Press, Oxford, United Kingdom,

1984.

4. Zumdahl, Steven S. (2009). Chemical Principles 6th Ed. Houghton Mifflin Company.

p. A22.