Name: Obada Subhi Mustafa

ID Number: 332156

Section Number: 2

Experiment Title:

1
The purpose for this experiment is preparing the following complexes: [Co(NH3)4(CO3)] NO3
& [Co(NH3)5Cl]Cl2,Calculate the theoretical & percent yield.

2
The Cobalt Ammines
the most extensively studied class of octahedral transition metal compounds are cobalt (III)
complexes in which ammonia (or other neutral molecules, closely related to ammonia, called
amines) occupies some or all of the six coordination positions. The (III) in the name is a way
of indicating the +3 oxidation state of the Co3+ ion. These complexes played a decisive role in
early formulations of the structure of transition metal compounds and they continue to be
important model systems for contemporary research into the properties of complex ions.

The first and simplest cobalt ammine complex ion, [Co(NH3)6]3+, was prepared in 1798. Alfred
Werner, a German chemist, studied the cobalt ammines extensively in the late 19th and early
20th centuries. He correctly interpreted his observations as requiring an octahedral geometry
of the ligands about the metal. Modern transition metal chemistry has evolved from his work
for which he was awarded the Nobel Prize in chemistry in 1913. The intensity of ongoing
research interest in cobalt ammine complexes is measured by the fact that a recent chemical
abstract cumulative index to the chemical literature has about 5000 entries referring to
articles on the subject over a five year period.

This laboratory experiment involves the preparation of aquapentaammine-cobalt(III) as a

nitrate salt, [Co(NH3)5(H2O)] [NO3]3:

Note the spelling of the complex name. There are molecules which, as a class, are called
amines, but the ammonia as a ligand is called ammine in the chemical's name. Water as a
ligand is called aqua (formerly aquo) in the name.
Once a successful synthesis has been carried out, a number of reactions of the complex will be
explored that will establish the purity of the product and characterize some of its chemical
behavior in weeks two, three, and four.

Complexes of amines with cobalt(III) are nearly always prepared from a cobalt(II) salt, the
amine, and a reagent which will convert cobalt(II) to cobalt(III). The procedure used here is
typical, with hydrogen peroxide serving as the reagent (called an "oxidizing agent" for its
ability to remove an electron) and ammonia as the amine. Here is the stoichiometric net
reaction for this synthesis:

2 HNO3 + 2 [Co(H2O)6] [NO3]2(s) + H2O2 + 10 NH3

2 [Co(NH3)5(H2O)] [NO3]3(s) + 12 H2O

The oxidation-reduction half-reactions consist of the oxidation of cobalt (II) to cobalt (III):

2 Co2+ 2 Co3+ + 2 e-

And the reduction of the hydrogen peroxide:

3
2H2O 2H++H2O2+2e-

The purpose of each reagent in the mixture is described below.

REFRENCES:

WWW.dartmouth.edu/chemlab/chem6/cobalt/full_text/chemistry.html

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 A: CHEMICAL USED:
PART ONE: [Co(NH3)4(CO3)]NO3

Formula Name Amount Molar

Mass
(NH4)2CO3 Ammonium carbonate 20g (0.21 mol) 96
H2O water 60 ml 18
NH3 Ammonia 60 ml 17
[Co(OH2)6] (NO3)2 Hexaaquacobalt(III) nitrate 15g(0.052 mol) 290.93
H2O water 30 ml 18
H2O2 Hydrogen peroxide 8 ml 34
CH3CH2OH+H2O Ethanol+water Few milliliters 46+18

PART TWO: [Co(NH3)5Cl]Cl2

Formula Name Amou Molar
nt Mass
[Co(NH3)4(CO3)] NO3 carbonatotetraaminecobalt(III) 3g 248.9
H2O water 30 ml 18
HCl Hydrochloric acid 6 ml 36.45
NH3 ammonia 5 ml 17
HCl Hydrochloric acid 40 ml 36.45

B: STRUCTURE:
[Co(NH3)4(CO3)]NO3

NH3
H3N O
NO3
Co C O
H3N O
NH3

Name: Carbonatotetraaminecobalt(III) nitrite

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 [Co(NH3)5Cl]Cl2

NH3
H3N NH3
Co Cl2
H3N Cl
NH3

Name: Chloropentaaminecobalt(III) chloride.

C: CHEMICAL EQUATION:
PART ONE: [Co(NH3)4(CO3)]NO3

2[Co(OH2)6] (NO3)2+2(NH4)CO3+8NH3+H2O2 [Co(NH3)4(CO3)]NO3+2NH4OH+2NH4NO3+12H2O

PART TWO: [Co(NH3)5Cl]Cl2

[Co(NH3)4(CO3)] +3HCl+NH3 [Co(NH3)5Cl]Cl2+CO2+3HNO3

D: DATA:

For the preparation 1st complex: [Co(NH3)4(CO3)]

The color of is : Red crystal.
The actual yield is7.00g
For the preparation 2nd complex: [Co(NH3)5Cl]Cl2
The color of is : Purple-Red crystals.
The actual yield is2.20g

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 PART ONE: [Co(NH3)4(CO3)]NO3

2[Co(OH2)6 ](NO3)2 + 2(NH4 )2CO3 [Co(NH3)4CO3]NO3

15g( 0.052 mol ) 20g(0.21 mol )

To determine the limiting reactant, we use the mole ratio between [Co(OH2)6(NO3)2 & (NH4)2CO3 and
the ratio is 1:1 then

[Co(OH2)6] (NO3)2 is limiting reactant

The mole ratio between [Co(OH2)6](NO3)2 and[Co(NH3)4CO3]NO3 is 1:1

# of mole [Co(OH2)6 ](NO3)2 = # of mole of [Co(NH3)4CO3]NO3

mole of [Co(NH3)4CO3]NO3 = 0.052 mol

The theoretical yield for[Co(NH3)4CO3]NO3 =

Mole of [Co(NH3)4CO3]NO3 M.wt [Co(NH3)4CO3]NO3
= 0.052 x 248.9 = 12.94g

The actual yield for[Co(NH3)4CO3]NO3 = 7.00g

% yield = (7.00 / 12.94) 100% = 54.1 %

PART TWO: [Co(NH3)5Cl]Cl2

[Co(NH3)4CO3]NO3 [Co(NH3)5Cl]Cl2

#of mole of [Co(NH3)4CO3]NO3 = 3g / M.wt = 3g /248.9

=0.0121mol
The ratio between [Co(NH3)4CO3]NO3 & [Co(NH3)5Cl]Cl2 is 1:1
Then # mol of [Co(NH3)5Cl]Cl2 = 0.0121 mol

The theoretical yield for [Co(NH3)5Cl]Cl2 =

Mol [Co(NH3)5Cl]Cl2 M.wt [Co(NH3)5Cl]Cl2
= 0.0121 mol 250.28 g\ mol = 3.03 g
The actual yield for[Co(NH3)5Cl]Cl2 = 2.20g

%yield = ( 2.20/ 3.03 ) 100% = 72.00 %

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 CoIII &CrIII have special properties due to react very slowly with ligand compared with other
transition metal like NiII which react very fast.

We added excess (NH4)2CO3 due to NH3 is volatile then keep NH3 in this reaction.

We added H2O2 as oxidizing agent due to convert CoII CoIII due to the ligand is weak as the
following:
CoII+L CoII-L+H2O2 CoIII-L when L: weak ligand
While if the ligand is strong:
CoIII+L CoIII-L when L: strong ligand

We used suction filtration to get rid of impurities that not soluble in water.

We must cool the product to give nice crystal.

We added water to remove impurities that soluble in water.

We used Ethanol to make the product dry by remove water.

We used strong acid (HCl) to expelled CO2

We added another HCl to make Cl as counter ion.

In 2nd part, if I use hot filtration ,then the complex will be removed.

Method for identity the complex:

i. Conductance
ii. Infrared Spectroscopy (IR)

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1-
By using AgNO3, such that number of mol of AgNO3 used is equal number of Cl- as counter ion.

2-
Digestion by using sulfuric acid
3-
2[Co(OH2)6] (NO3)2+2(NH4)CO3+8NH3+H2O2 [Co(NH3)4(CO3)]NO3
+2NH4OH+2NH4NO3+12H2O

4-
The C-O bond fission occurs in the intermediate has been established from O18 isotopic exchange
studies in several similar reaction of carbonato complexes.

5-Increase on standing over night due to water enters the complex as ionization ion and Cl ligand
will leave as counter ion then the complex become have 6 ions instead of 4 ions.

6-
To make the complex is dry by removed of water.

7-
As the concentration will be increase the conductance will be decrease due to increase ionic
interaction then must used lower concentration.

8-
I can distinguish between [Co(NH3)4(CO3)]NO3& [Co(NH3)5(CO3)]NO3 by
[Co(NH3)4(CO3)]NO3 CO3 is bidentate while
[Co(NH3)5(CO3)]NO3 CO3 is mono dentate
And I can distinguish between mono & bidentate ligand by using IR-Spectra.

THE END