LABORATORY REPORT

Course Code: SKT3023 INORGANIC CHEMISTRY II

Semester 2 Session 2020/2021

ID NUMBER AND NAME 1. YUVARANI SELVAKUMAR (D20191088473)

2. NUR FATIHAH BINTI MOHD NASIR

(D20191088501)

LECTURER DR. SITI MUNIRAH BINTI SIDIK

EXPERIMENT NO. 3

TITLE SYNTHESIS OF PENTAAMMINECHLOROCOBALT(III)

CHLORIDE
DATE & DAY 8/04/2021- THURSDAY

CHECK LIST (Please tick) Marks

Title 5
Objective(s) 5
Methods 10
Results (Observation, Data, 30
Calculation, etc.)
Discussions and questions & 35
answers (if appropriate)
Conclusion(s) 10
References (at least 2) 5
TOTAL MARKS 100

Department of Chemistry
Faculty of Science and Mathematics
UNIVERSITI PENDIDIKAN SULTAN IDRIS
EXPERIMENT 1: SYNTHESIS OF PENTAAMMINECHLOROCOBALT(III)
CHLORIDE
1.1 OBJECTIVES
Upon completion of this experiment, students should have learned how to:
1. Synthesize pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2

1.2 INTRODUCTION
A coordination compound is formed between electron pair donors, ligands and electron pair
acceptors, the metal atoms. There are many possible ligands that can bond to the central
atom. For instance, in the formation of [Co(NH3)5Cl]Cl2, each NH3 atom donates one pair
of electrons to form coordinate bond to cobalt metal. Ligand exchange occurred by
introduction of hydrochloric acid to the ion. Ammonia is a better ligand than Cl- , so when
it is present, it replaced the Cl in the complex. Again, due to the greater electronegativity
of NH3 than Cl-, the Cl- associated with the cobalt is replaced by the ammonia. When HCl
is added back into the solution of [Co(NH3)5(OH2)]3+ to give the desired product.

Chemicals
Ammonium chloride (NH4CI)
Concentrated ammonia (NH3)
Cobalt(II) chloride hexahydrate (CoCl2.6H2O)
Hydrogen peroxide (H202, 30 % v/v)
Concentrated hydrochloric acid (HCI)
Methanol
Ice

Apparatus
Erlenmeyer flask
Beaker
Dropper
Filter funnel
Watch glass
Hot plate
 Magnetic stirrer
Filter paper
Buchner funnel

1.3 PROCEDURE
5g of ammonium chloride (NH4CI) is dissolved in 30 ml of concentrated ammonia
(NH3) solution in an Erlenmeyer flask. Combination of NH4CI and NH3 guarantees a
large excess of the NH3 ligand. The solution was stirred well and continuously. Then,
10 g of cobalt(II) chloride hexahydrate (CoCl2.6H2O) is added slowly. It was stirred
well and continuously until all CoCl2.6H2O dissolve. Next, 30% hydrogen peroxide
(10ml) is dropped wisely to the slurry by using a dropper. PRECAUTION, the peroxide
cannot be added too quickly because ammonia may be oxidized. After that, it was
stirred thoroughly after each addition of the peroxide. PRECAUTION, the hydrogen
peroxide is a strong oxidizing agent that will cause severe burns and bleaching of skin
and clothing. The solution is continuously stirred until all the Co(II) ammine dissolves
to form a deep red solution. More H2O2 is added if the solution is not a deep red until
the colour change is completed. Then, the effervescence or bubbles had been virtually
ceased. Then, concentrated HCI (30 ml) is added drop by drop and it was continuously
stirred. PRECAUTION, it must be conducted in fume hood since fumes of ammonium
chloride will be produced during the neutralization. Next, the mixture is heated on water
bath (75° - 85°C) for 20 min. the solution was stirred periodically to avoid the fumes
above the reaction beaker. The reaction contained a deep purple solid in a beautiful
indigo solution. After that, the mixture is cooled to room temperature in a cool water
bath, consisting of a 400 ml beaker filled with approximately 150 ml of cool water.
Once the beaker is no longer hot, it was transferred to an ice bath. The Erlenmeyer flask
was put in an ice bath when the temperature drops below 10°C. Vacuum filtration is
used to collect the product. The product is washed with cool water (30 ml, 0- 10C),
then with HCl solution (30 ml, 6M), with 10 ml of ice cold methanol. The sample was
let to dry and the product is weighed. Mass of product must be more than 3.0 g. The
physical properties (colour and melting point) was recorded. The sample is kept in
desiccator to be used in Experiment 5.
1.4 RESULT

Mass of ammonium chloride (g) 5.0012g

Mole of ammonium chloride 0.09349 mol
Mass of cobalt(II) chloride hexahydrate (g) 10.0073g
Mole of cobalt(II) chloride hexahydrate 0.04206 mol
Mass of filter paper (g) 38.3746g
Mass of filter paper + product 45.7866g
Mass of product (g) 7.412g
Mass of [Co(NH3)5Cl]Cl2 7.412g
Physical properties

Compound Colour Melting point (0C)

CoCl2.6H2O Dark reddish 86 oC
purple
[Co(NH3)5Cl]Cl2 Pinkish purple 303 oC
Write a balanced equation involved for the formation of [Co(NH3)5Cl]Cl2

2CoCl2 • 6H2O + 4 NH4Cl + 8 NH3 + H2O2 2 [Co(NH3)5Cl)]Cl2 + 14 H2O

Using calculation, clearly indicate which ingredient you conclude to be the limiting reagent
(between NH4CI OR CoCl2.6H2O).

𝟓.𝟎𝟎𝟏𝟐𝒈
No. of mol of NH4CI =
𝟓𝟑.𝟒𝟗𝟏𝒈/𝒎𝒐𝒍
= 0.09349 mol

𝟏𝟎.𝟎𝟎𝟕𝟑𝒈
No. of mol of CoCl2.6H2O =
𝟐𝟑𝟕.𝟗𝟑𝒈/𝒎𝒐𝒍

= 0.04206 mol

mol of CoCl2.6H2O (0.04206 mol) < mol of NH4CI (0.09349 mol)

Thus, CoCl2.6H2O is limiting reagent
Calculate the theoretical yield (g) for the formation of [Co(NH3)5Cl]Cl2

2mol of CoCl2.6H2O = 2 mol of [Co(NH3)5Cl]Cl2

Mol ratio = CoCl2.6H2O : [Co(NH3)5Cl]Cl2 = 2:2
mol of [Co(NH3)5Cl]Cl2 = 0.04206 mol

molar mass of [Co(NH3)5Cl]Cl2 = 58.93 + 5(14.00 + 3(1.00)) + 35.45 + 70.90

= 250.44 g/mol

Mass of [Co(NH3)5Cl]Cl2 = no. of mol x molar mass

= 0.04206 mol x 250.44 g/mol
= 10.53 g

𝒂𝒄𝒕𝒖𝒂𝒍
% yield of [Co(NH3)5Cl]Cl2 = x 100%
𝒕𝒉𝒆𝒐𝒓𝒊𝒕𝒊𝒄𝒂𝒍
𝟕.𝟒𝟏𝟐
= x 100
𝟏𝟎.𝟓𝟑
= 70.39%
1.5 DISCUSSION

In this experiment, in order to synthesis the pentanaaminechlorocobalt(iii) chloride, 5.0 g

of ammonium chloride, NH4Cl is added to 30 ml of concentrated aqueous ammonia in an
Erlenmeyer flask. This combination of NH4CI and NH3 guarantees a large excess of the
NH3 ligand. At this stage, the solution formed was clear and colourless. The dissolving
ammonium chloride, NH4Cl in concentrated aqueous ammonia, NH3 made the flask cold
as the reaction was endothermic.

10 g of cobalt(II) chloride hexahydrate, CoCl2.6H2O was then added slowly in small

portions with continuous and vigorous stirring. This addition of cobalt(II)
chloridehexahydrate, CoCl2.6H2O to the mixture of ammonium chloride-ammonia
caused the formation of dark brown solution with some precipitate that corresponds to
the formation of the pentaammineaquacobalt(III) salt. This was due to the displacement
of aqua ligands by ammine and chloride ligands. When hydrogen peroxide was added, a
brown-yellowish solution of cobalt(III) complex is produced. Thus, the addition of HCL
produce a dark maroon pentaaminechloro cobalt(III) chloride precipitate. The equation is
as below:

2CoCl2 • 6H2O + 4 NH4Cl + 8 NH3 + H2O2 2 [Co(NH3)5Cl)]Cl2 + 14 H2O

The mass of product obtained was 7.412 g while the theoretical mass of the product is
10.53 g. The yield is 70.39%. The actual mass is less than the theoretical mass. The product
form is less pure, but still suitable for future synthetic work. These might occur because of
certain errors during the experiment. The possible loss of precipitate when washing or left
in the stirring rod and glassware can attribute a smaller percent yield. There might be lost
of product during the transferring process. Therefore, the final mass product obtained is
lesser. The colour of the product was pinkish purple and its melting point was 303 oC.

Throughout running this experiment, there were several precautions that must be taken.
First, wear a proper a safety attire; lab coat, safety goggles, aprons, and gloves were worn
in the laboratory. Then, during the addition of hydrogen peroxide, it cannot be added too
 quickly because ammonia may be oxidized. Hence, the hydrogen peroxide is a strong
oxidizing agent that will cause severe burns and bleaching of skin and clothing. If spilled
on the skin, the affected area must be wash immediately with water. Then, the step of
addition the concentrated HCl, it must be conducted in fume hood since fumes of
ammonium chloride will be produced during the neutralization.

1.6 CONCLUSION

In summary, two cobalt (III) complexes, cobalt (II) chloride hexahydrate (CoCl2.6H2O) and
Pentaamminechlorocobalt (III) Chloride [Co(NH3)5Cl]Cl2, were synthesized with the aim
of characterizing them by means of infrared spectroscopy, melting point and conductivity
assays. At the end of the synthesis, 7.412 g of fine light pinkish purple crystal of
[Co(NH3)5Cl]Cl2 were obtained, giving 70.39% of yield. The melting point of
[Co(NH3)5Cl]Cl2 is 303oC.

REFERENCES

Alexandra Galetova, Nekane Medrano. (2019). Reasearchgate: Preparation and

Characterization of Cobalt Coordination Complexes. Retrieved from
https://www.researchgate.net/publication/339052052_Preparation_and_Characterizatio
n_of_Cobalt_Coordination_Complexes

Husna Assaedah Bain. (2020). Youtube: Synthesis of Pentaaminechlorocobalt(iii) chloride.

Retrieved from https://www.youtube.com/watch?v=KGpBdl5ExH0

Nada K. Abbas, Majeed Ali Habeeb, Alaa J. Kadham Algidsawi. (2015). International Journal
of Polymer Science: Preparation of Chloropentaaminecobalt(iii) Chloride. Retrieved
from https://www.hindawi.com/journals/ijps/2015/926789/