UNIVERSITY OF MALAWI

CHANCELLOR COLLEGE
FACULTY OF SCIENCE
DEPARTMENT OF CHEMISTRY

TO : DR. E. VUNAIN

FROM : Ambrose Gumbwa

REGISTRATION # : BSc/12/15

COURSE CODE : BIO421

EXPERIMENTAL TITLE : SYTHESIS AND ITERPRETATION OF CONDUCTANCE DATA

FOR AMMINECHLOROCOBALT(III) COMPLEXES

EXPERIMENTAL No. : ONE

DUE DATE : 02nd October, 2020.

0
TABLE OF CONTENTS

Abstract---------------------------------------------------------------------------------------------------------2

Introduction----------------------------------------------------------------------------------------------------3

Methodology---------------------------------------------------------------------------------------------------5

Results----------------------------------------------------------------------------------------------------------7

Discussion------------------------------------------------------------------------------------------------------8

Conclusion-----------------------------------------------------------------------------------------------------9

References----------------------------------------------------------------------------------------------------10

Appendix -----------------------------------------------------------------------------------------------------11

1
ABSTRACT

Coordination compounds of Co(III) have been of particular interest because their complexes
undergo ligand exchange very slowly compared with other complexes of many other transition
metal ions. For example, [Ni(NH 3)6]2+ reacts virtually instantaneously with H 2O to form
[Ni(OH2)6]2+. Under the same conditions, the analogous reaction of [Co(NH 3)6]3+ occur very
slowly. This difference in behavior of complexes of different metal ions has been accounted for
by ligand field theory and molecular orbital theory. The slow reactivity of Co(III) complexes has
made them suitable for extensive investigations. The focus of this practical was to synthesize and
interpret (particularly conductivity measurements) of complex (1) and complex (2) coordination
compounds. The percentage yield for the complex 1 and complex 2 were 42.59% and 26.09%
respectively.

2
INTRODUCTION

Coordination compounds or metal complexes are metal ions surrounded by ligands. Ligands are
either anions or molecules that can donate electrons into the d-orbitals of the metal ion and form
a bond. Examples of common ligands are chloride ion, cyanide ion, ammonia, ethylenediamine,
and ethylenediaminetetraacetate ion (EDTA). The metal ions that form coordination compounds
are from a group of metals known as transition metals. These metals have more than one
oxidation state. This property allows the transition metals to act as Lewis acids (Wulfsberg,
2000). A central metal atom is electron-deficient species (electrophile) which can use its empty
orbitals for the bond and this was well articulated by Alfred Werner (Cotton, 1972).

He was the first to propose correct structures for coordination compounds containing complex
ions, in which a central transition metal atom is surrounded by neutral or anionic Ligands. For
example, it was known that cobalt forms a complex hexamminecobalt (III) chloride, with
formula CoCl3.6NH3, but the nature of the association indicated by the dot was mysterious.
Werner proposed the structure [Co(NH3)6]Cl3, with the Co3+ ion surrounded by six NH3 at the
vertices of an octahedron. The three Cl- are dissociated as free ions, which Werner confirmed by
measuring the conductivity of the compound in aqueous solution, and also by chloride anion
analysis using precipitation with silver nitrate. Later, magnetic susceptibility analysis was also
used to confirm Werner's proposal for the chemical nature of CoCl3.6NH3.

For complexes with more than one type of ligand, Werner succeeded in explaining the number
of isomers observed. For example, he explained the existence of two tetrammine isomers,
"Co(NH3)4Cl3", one green and one purple. Werner proposed that these are two geometric
isomers of formula [Co(NH3)4Cl2]Cl, with one Cl- ion dissociated as confirmed by conductivity
measurements. The Co atom is surrounded by four NH3 and two Cl ligands at the vertices of an
octahedron. The green isomer is "trans" with the two Cl ligands at opposite vertices, and the
purple is "cis" with the two Cl at adjacent vertices.

The practical exercise was to prepare the complexes (1) and (2) of the type Co(NH 3)xCly where x
and y values have been evaluated from conductance measurements of complex (1) and (2). A
study of the molar conductance will provide information as to the number of ions
produced per mole of a given complex. The number of ions released by solutions of
complexes (1) and (2) will total one complex cation, [Co(NH 3) Cl6 – x ]n+ and a number,

3
x-3, of counter chloride ions. The conductance will increase with the number of aqueous
chloride ions that the complex yields in solution and so will be different for equimolar
solution of each complex.

4
METHODOLOGY

A. Preparation of Complex 1

A hot solution of ammonium chloride (2g) plus water (2ml) in 250ml reaction beaker was
prepared, cobalt chloride crystals (3g) which are purple in color were added and allowed to
dissolve. In the same mixture, activated charcoal about 0.3g was added. (The activated charcoal
serves as a catalyst for the reaction that forms the bonds between NH3 and Co. Conveniently, it
also catalyzes the transformation of Co2+ into Co3+ by the H2O2!) The solution was allowed to
cool at room temperature and the first beaker which contained cobalt was washed with 6ml conc.
Ammonia after which it was added to second beaker then containing the mixture. The solution
(purple in color) was cooled in an ice bath. While shaking, 6ml of 20 vol. Hydrogen peroxide
solution was added after which it was heated at 60 oC for about 15 minutes. Crystals formed
which were filtered using suction pump and recrystallized with a mixture of 20ml hot water and
5ml HCl. The mixture was filtered while hot and, in the filtrate, 4ml of HCl was added and
allowed to cool in an ice bath. The crystals formed (golden brown) were filtered and washed
with propanone.

B. Preparation of Complex 2

Warm water (7.5ml) was prepared in conical flask and 8.6g of [CoCl 2. 6h2O] was dissolved in
completely. The solution was cooled in an ice bath before adding and suspension of ammonium
chloride (12.5g) in aqueous ammonia about 30ml. The flask was set on a magnetic stir and in it
15ml Hydrogen peroxide was added in a drop wise manner. Further 17.5ml of same solution was
added to the mixture from a dropping funnel. After few minutes, conc. HCl about 10ml was
added to neutralize the mixture. The pH was checked using litmus paper to make sure reaches
pH 7. Another 6.5ml of the acid was added and then the mixture was boiled. After few minutes,
it was removed from boil and in it, a mixture 2M HCl (15ml) and 30ml water was then added.
The solution was cooled in an ice bath and filtered. Another beaker was prepared, in the same
90ml of 2M ammonia plus 90ml water was added. The purple precipitates obtained above was
dissolved while warming the mixture. The solution was filtered while still hot and 7ml HCl was

5
added before setting it to boil again. After boil, the mixture was cooled in an ice bath to come up
with a fine purple precipitate of the complex.

6
RESULTS

The third molecular formula with consistent y value equal to 3 is, [Co (NH 3)4Cl2] Cl the name of
the compound is tetramminedichlorocolbalt(III) chloride. The calculations of percentage yield
and others are in the appendix section.

Part 1: preparation of complex (1): [Co (NH3)6] Cl3 (hexamminecobalt(III) chloride)

Mass of filter paper 0.55g

Mass of filter paper + sample 1.99g

Mass of sample(crystals) 1.44g

Percentage Yield (%) 42.59%

Part 2: preparation of complex (2): [Co (NH3)5Cl] Cl2 (pentamminechlorocobalt(III) chloride)

Mass of filter 0.55g

Mass of filter paper + sample 2.898g

Mass of sample(crystal) 2.348g

Percentage Yield (%) 26.09%

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DISCUSSION

The synthesis of each complex was successful though its percentage yield could be result of the
several factors. There are two common factors that contribute to yields of less than 100%. One is
simply the employment of a synthetic reaction step whose kinetics or equilibrium prevent
complete
reaction, or encourage side reactions that lead to the generation of products other than the one
desired. The other common factor is the physical loss of reaction materials during the
synthesis. However, the results obtained shows that a large percentage was lost for the product
meaning that these two factors in one way or another both contributed to the loss. The complex 1
has four ions and has a higher conductance value as compared to complex 2 which has three ions
and this is so because number of ions is directly proportional to the conductance. The names of
complex 1 and 2 are Hexaminecobalt (III) chloride and Pentamminechlorocobalt (III) chloride
respectively and their molecular formular are [Co (NH3)6] Cl3 and [Co (NH3)5Cl] Cl2 respectively.
The y values were found to be 3 in the both complexes that’s to include the third complex. The
third complex molecular formula was [Co(NH3)4Cl2]Cl named as Tetramminedichlorocobalt (III)
chloride and its molar conductivity is within a range of 96-150 cm2 /mol. The percentage yield
for the complex 1 and complex 2 were 42.59% and 26.09% respectively.

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CONCLUSION

To sum up with, the experimental results indicates the succuss and achievement of the purpose of
the practical exercise. However, the yield percentage is low for both complexes and it can be
achieved once the flaws aforementioned in discussion section are improved. Finally, we were
able to figure out the complex formula as well the coordination, molecular formula of the
complexes.

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REFERENCES

G. Wulfsberg, Inorganic Chemistry, University Science Books, 2000.

Chemistry 111 Laboratory. Experiment 6: Synthesis of a Coordination Compound.

Retrieved on 1st April, 2019. From www.slideshare.net

Chemistry 36. Lab: Synthesis of Cobalt complex. Retrieved on 28th March, 2019.

From www.slideshare.net

Chemistry laboratory manual, (2020). Synthesis and Interpretation of Conductance Data for

Amminechlorocobalt (III) complexes. Chancellor College: Faculty of science.

Department of Chemistry

Cotton, F. A. Welch, A.R & Wilkson, G. (1972). Advanced Inorganic Chemistry.

A comprehensive text. Third edition. Canada: John Wiley & Sons Inc

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APPENDIX
Assigning the respective formula to complexes (1) and (2)

Table 1: Range of molar conductivities for various ion conductors in aqueous solution

⇒ The formula: [Co(NH3)xCl6-x]Clx-3 becomes;

⇒ [Co(NH3)4Cl6-4]Cl5-4 = [Co(NH3)4Cl2]Cl

But [Co (NH3)4Cl2] Cl = [Co (NH3)4Cl2]3+ + Cl-

It implies that the value of y remains 3.
From the table 1 above of conductance it shows that the conductance of [Co (NH3)4Cl2] Cl
compound is within the range of 96-150 Ω-1cm2mol-1.
i. Calculating percentage yield of complex 1 and 2.
Complex 1
Reaction equation for formation of [Co (NH3)6] Cl3 :

charcoal 2[Co(NH3)6]Cl3(S) + 1/2O2(g)

2CoCl2.6H2O(s) + 2NH4Cl(s) + 10NH3(aq) + H2O2(aq) + 3H2O(l)

Molar mass of CoCl2⋅6H2O(s) = 238.889 g/mol

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 m 3g
number of moles= = 0.0126 moles
M 238.889 g /mol
Molar mass of [Co(NH3)6]Cl3(s) = 268.33g/mol
The stoichiometric ratio of CoCl2⋅6H2O(s) to [Co(NH3)6]Cl3(s) is 1:1, therefore the same number of
moles were produced for [Co(NH3)6]Cl3(s) which is 0.0126mol.
g
Theoretical mass of [Co(NH3)6]Cl3(s) = 268.33( )× 0.0126 mol=3.381 g
mol
Actual yield 1.44 g
Percentage yield= ×100 %= ×100 %=42.59 %
Theoretical yield 3.381 g
Complex 2
Reaction equation for formation of [Co(NH3)5Cl]Cl2

charcoal 2[Co(NH3)5Cl]Cl2(S) + 1/2O2(g)

2CoCl2.6H2O(s) + 2NH4Cl(s) + 10NH3(aq) + H2O2(aq) + 3H2O(l)
Still the molar mass of CoCl2⋅6H2O(s) = 238.889 g/mol
m 8.6 g
number of moles= = 0.036 moles
M 238.889 g /mol
Molar mass of [Co(NH3)5Cl]Cl2(s) = 250g/mol
The stoichiometric ratio of CoCl2⋅6H2O(s) to [Co(NH3)6Cl]Cl2(s) is 1:1, therefore the same number
of moles were produced for [Co(NH3)6Cl]Cl2(s) which is 0.036mol.
g
Mass of [Co(NH3)6Cl]Cl2(s) = 250( )× 0.036 mol=9 g
mol
Actual yield 2.348 g
Percentage yield= ×100 %= ×100 %=26.09 %
Theoretical yield 9g
Definition of the following terms:
(i) Conductance-the degree to which an object conducts electricity, calculated as the ratio of the

current which flows to the potential difference present

(ii) Molar conductance-is the conducting power of all the ions produced by dissolving one mole

of an electrolyte in solution

(iii) Specific conductivity-of an electrolyte solution is a measure of its ability to conduct

electricity.

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