FACULTY OF APPLIED SCIENCES

(AS1205C)

CHM361

EXPERIMENT 5

Title : Synthesis of Chloropentaamminecobalt (III) Chloride

Name : Dayang Nor Shafiqah Binti Awang Shukeran

Student ID : 2017296442

Laboratory partner :

Name Student ID

1. Amira Nasirah Binti Jemat 2017403616

2. Nur Syasya Farzana Binti Mohd Taib 2017441662

Lecturer’s name : Mdm. Rabuyah Binti Ni

Date of experiment : 17 October 2019

Date of submission :
TITLE

Synthesis of Chloropentaamminecobalt (III) Chloride

OBJECTIVE

1. The purpose is to synthesize cloropentaamminecobalt (III) chloride. It raises the

question of wether the chloride atom is coordinated to cobalt or not.

INTRODUCTION

The equations for the preparation of cholopentaamminecobalt (III) chloride can be written as
follows:

Co2+ + NH4+ + ½ H2O2 → [Co(NH3)5H2O)3+

[Co(NH3)5H2O)3+ + 3Cl- → [Co(NH3)5Cl]Cl2 + H2O

The cobalt +2 ions are more stable than the cobalt +3 ion for simple salts of cobalt. Only
a few salts of Co (II) such as CoF3 are known. However, complexation stabilizes the higher
oxidation state, and a number of very stable octahedral coordinated complexes of cobalt (III)
are known.

APPARATUS

1. Goggles
2. Fume hood
3. 100 mL graduated cylinder
4. Electronic balance
5. Filter paper
6. Magnetic stirring plate
7. Burner
8. Funnel
9. Aluminium Foil
10. Erlenmeyer flask
CHEMICALS

1. Ammonium chloride
2. Concentrated aqueous ammonia
3. CoCl2.6H2O
4. 30 % hydrogen peroxide
5. Conc. HCL
6. Ethanol
7. Distilled water

PROCEDURE

1. In a fume hood, 5 g of ammonium chloride was added to 30 mL concentrated aqueous

ammonia in a 250 mL Erlenmeyer flask. (The combination of NH 4Cl and NH3 (aq)

guarantees a large excess of the NH3 ligand).

2. The ammonium chloride solution was stirred vigorously using a magnetic stirring
plate while adding 10 g finely divided CoCl2.6H2O in small portions.
3. 8 mL of 30% hydrogen peroxide was added to the brown Co slurry. Excessive
effervescence was avoided in this exothermic reaction. (If the reaction shows signs of
excessive effervescence, turning off the magnetic stirrer momentarily will usually
prevent overflow of the solution).
4. When the effervescence has ceased, 30 mL conc. HCl was added with continuous
stirring, pouring about 1-2 mL at a time. At this point, the reaction may be removed
from the hood.
5. A hot plate with 60°C temperature was used to heat the solution with occasional
stirring for 15 min; this incubation period is necessary to allow complete displacement
of all aqua ligands.
6. 25 mL of distilled water was added, and the solution was allowed to cool at room
temperature.
7. The purple product was collected by filtration through the Buchner funnel; it was
washed with 7.5 mL of cold distilled water and 7.5 mL of ice-cold ethanol. (The
solution must be cold to prevent undue loss of product by redissolving).
8. The product was transferred to crystallizing dish, it was loosely covered with
aluminium foil, and was allowed it to dry.
RESULTS

1. Mass of CoCl2.6H2O used 10.12 g

2. Moles of CoCl2.6H2O used 0.0425 mol

Theoretical yield of [Co(NH3)5Cl]Cl2

3. 10.65 g
(mass)

Theoretical yield of [Co(NH3)5Cl]Cl2

4. 0.0448 mol
(moles)
5. Mass of [Co(NH3)5Cl]Cl2 obtained 2.65 g

6. Percent yield of [Cu(NH3)4]SO4.H2O 24.9 %

CALCULATIONS

2. Moles of CoCl2.6H2O used

mass
moles =
molar mass

10.12 g
=
237.93 g /mol

= 0.0425 mol

3. Theoretical yield of [Co(NH3)5Cl]Cl2 (mass)

Balanced chemical equation:

2 CoCl2.6H2O(s) + 2 NH4Cl(s)+8 NH3(aq) + H2O2(aq) → 2 [Co(NH3)5Cl)]Cl2(g) + 14H2O(l)
(10.12 g) (2.65 g)

Theoretical yield:
10.12 g CoCl 2.6 H 2O 1mol CoCl 2 .6 H 2 O 2 mol ¿ ¿ Cl 2 ¿
x x 2 mol CoCl 2.6 H 2 O x
1 237.93 g

250.4 g
Cl 2 ¿
1mol ¿ ¿

= 10.65 g
4. Theoretical yield of [Co(NH3)5Cl]Cl2 (moles)

Theoretical yield:

1mol CoCl 2 .6 H 2 O 2 mol ¿ ¿ Cl 2 ¿

10.65 g x x 2 mol CoCl 2.6 H 2 O = 0.0448 mol
237.93 g

5. Mass of [Co(NH3)5Cl]Cl2 obtained

Mass of filter paper + precipitate 4.61 g

Mass of filter paper 1.96 g

Mass of precipitate 2.65 g

6. Percent yield of [Cu(NH3)4]SO4.H2O

actual yield
% yield = x 100%
theoretical yield
2.65 g
= x 100%
10.65 g
= 24.9 %
DISCUSSION
In this experiment, the synthesis of chloropentaamminecobalt(III) chloride,
[Co(NH3)5Cl)]Cl2 occurred in a few steps. Firstly, 5 g of ammonium chloride, NH 4Cl(s) was
added to 30 mL of concentrated aqueous ammonia, NH 3 in a 250 mL Erlenmeyer flask. A
large excess of the NH3 ligand was guaranteed with the combination of NH4Cl and NH3. At
this stage, the solution formed was clear and colorless. Dissolving ammonium chloride,
NH4Cl in concentrated aqueous ammonia, NH3 made our flask cold as the reaction was
endothermic.
10 g of finely divided cobalt (II) chloride hexahydrate, CoCl 2.6H2O was then added
slowly in small portions with continuous and vigorous stirring. This addition of cobalt (II)
chloride hexahydrate, CoCl2.6H2O to the mixture of ammonium chloride-ammonia caused the
formation of dark brown solution with some precipitate. This was due to the displacement of
aqua ligands by ammine and chloride ligands. In addition, heat also was generated after
addition of concentrated HCl.

The result of the experiment that we obtained was 2.65 g

chloropentaamminecobalt(III) chloride, [Co(NH3)5Cl)]Cl2 which is the actual mass, while the
theoretical yield calculated was 10.65 g. Thus, the percent yield that we get after the
calculation was 24.9% There are a few reasons why we were unabled to get 100% of
percentage yield plus the percentage can never be 100%. One of the reasons is because there
may be had some products remained at the Buchner funnel when we collected the product
after the filtration. Besides that, the product may dissolve when we washed the product with
alcohol. Other than that, the graduated cylinder used to measure the alcohol also might be the
cause to contaminate.

So there is some precaution that we must take care while we are doing an experiment.
First, we need to make sure our conical flask is cleaned before we are using it, this is
important because there may be other substance left in the conical flask and causing
contaminated products. Besides that, we have to wear gloves while handling with filter paper
weighing apart from handling concentrated solution. This is important so that there would be
no fingerprints left on the filter paper.
CONCLUSION

In conclusion, we can conclude that we have synthesized a coordination compound,

[Co(NH3)5Cl)]Cl2. We have learned the different techniques in synthesizing. The possible
sources of error in this experiment were: the inability to completely transfer all of the
reagents from the weight boats in to containers. The actual mass obtained of
chloropentaamminecobalt(III) chloride was 2.65 g, while the theoretical mass is 10.65 g. The
theoretical yield in moles is 0.0448 moles. The actual yield is lower than the theoretical yield.
Thus, the percent yield of the precipitate obtained was 72.4 %.

REFERENCES

Abbas, Habeeb, Ali, M., Algidsawi, Kadham, A. J. and Nada, K. (2015). Preparation of
Chloro Penta Amine Cobalt(III) Chloride and Study of Its Influence on the Structural and
Some Optical Properties of Polyvinyl Acetate. Retrieved October 26, 2019 from
https://www.hindawi.com/journals/ijps/2015/926789/.

CHM361 notes.

University of Engineering and Technology. (2018). Synthesis of

Chloropentaamminecobalt(iii) chloride. Retrieved October 26, 2019 from
https://www.slideshare.net/saimkhalid04/synthesis-of-chloropentaamminecobaltiii-chloride.