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Experiment 3

This experiment details the synthesis of pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2. Ammonium chloride and cobalt chloride hexahydrate are dissolved in concentrated ammonia to form the pentaammineaquacobalt complex. Hydrogen peroxide is added to oxidize cobalt from 2+ to 3+ oxidation state. Concentrated hydrochloric acid is added to displace the aqua ligands, forming the desired product which is a deep purple solid in solution. The product is isolated through filtration, washing, drying and its identity is confirmed through calculation of theoretical and percent yields.

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283 views5 pages

Experiment 3

This experiment details the synthesis of pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2. Ammonium chloride and cobalt chloride hexahydrate are dissolved in concentrated ammonia to form the pentaammineaquacobalt complex. Hydrogen peroxide is added to oxidize cobalt from 2+ to 3+ oxidation state. Concentrated hydrochloric acid is added to displace the aqua ligands, forming the desired product which is a deep purple solid in solution. The product is isolated through filtration, washing, drying and its identity is confirmed through calculation of theoretical and percent yields.

Uploaded by

thina
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© © All Rights Reserved
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EXPERIMENT 3

SYNTHESIS OF PENTAAMMINECHLOROCOBALT(III) CHLORIDE

3.1 OBJECTIVE
Upon completion of this experiment, students should have learned how to:
1. Synthesize pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2

3.2 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 (H2O2, 30 % v/v)
Concentrated hydrochloric acid (HCI)
Methanol
Ice

Apparatus:
Beaker
Dropper
Filter funnel
Watch glass
Hot plate
Magnetic stirrer
Filter paper
Buchner funnel
3.3 PROCEDURES
Synthesis of Pentaamminechlorocobalt(III) Chloride
1. Dissolve 5g of ammonium chloride (NH4CI) in 30 ml of concentrated ammonia (NH3)
solution in a 250 ml beaker. Combination of NH4CI and NH3 guarantees a large excess
of the NH3 ligand. Stir well and continuously. PRECAUTION This step must be
conducted in fume hood.
2. Add 10 g of cobalt(II) chloride hexahydrate (CoCl2.6H2O) slowly. Stir well and
continuously until all CoCl2.6H2O dissolve.
3. Drop wisely 30% (v/v) hydrogen peroxide (10ml) to the slurry by using a dropper.
PRECAUTION Do not add the peroxide too quickly because ammonia may be oxidized.
4. Stir thoroughly after each addition of the peroxide. PRECAUTION Hydrogen peroxide is
a strong oxidizing agent that will cause severe burns and bleaching of skin and clothing.
If spilled on the skin, wash the affected area immediately with water.
5. Continuously stir the solution until all the Co(II) ammine dissolves to form a deep red
solution. This corresponds to the formation of the pentaammineaquacobalt(III) salt. If the
solution is not a deep red, add more H2O2 until the colour change is completed.
6. Wait until the effervescence or bubbles has virtually ceased.
7. Then, dropwise concentrated HCI (30 ml) and stir continuously. PRECAUTION This
step must be conducted in fume hood since fumes of ammonium chloride will be
produced during the neutralization.
8. Heat the mixture on water bath (75° - 85°C) for 20 min. Stir periodically, avoiding the
fumes above the reaction beaker.This incubation period is necessary to allow complete
displacement of all aqua ligands.
9. Your reaction should contain a deep purple solid in a beautiful indigo solution, with
both colours changing somewhat as you stir and heat.
10. Cool the mixture to room temperature in 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, transfer it to an ice bath. Keep it there until its temperature drops below 10°C,
put the Erlenmeyer flask in an ice bath.
11. Use vacuum filtration to collect the product. Wash the product with cool water (30 ml,
0-10C), then with HCl solution (30 ml, 6M), with 10 ml of ice cold methanol. Dry the
sample.
12. Weigh the product. Mass of product must be more than 3.0 g.
13. Keep the sample in desiccator. The product will be used in Experiment 5.
WORKSHEET EXPERIMENT 3

Observations
Reaction Picture Observation
cobalt(II) chloride hexahydrate
is added

30% (v/v) hydrogen peroxide is


added

Hydrochloric acid is added

After 20 minutes in water bath


(75° - 85°C)
After cooled in ice bath

Filtered using vacuum suction

After dried
Mass of ammonium chloride (g)
Mole of ammonium chloride
Mass of cobalt(II) chloride hexahydrate (g)
Mole of cobalt(II) chloride hexahydrate
Mass of filter paper (g)
Mass of filter paper + product
Mass of product (g)
Mass of [Co(NH3)5Cl]Cl2
Write a balanced equation involved for the formation of [Co(NH3)5Cl]Cl2

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

Calculate the theoretical yield (g) for the formation of [Co(NH3)5Cl]Cl2

% yield of FeC2O4 𝐴𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 (𝑔)


%𝑦𝑖𝑒𝑙𝑑 = 𝑥 100%
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 (𝑔)

What is the purpose to use hydrogen peroxide in this experiment?

___________________ ____________________________
DATE LECTURER’S SIGNATURE/STAMP

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