Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

EXPERIMENT 2
Synthesis of Potassium Tris(oxalato)ferrate(III) Trihydrate (K3[Fe(C2O4)3].3H2O)
Objectives
To synthesis a coordination compound, potassium tris(oxalato)ferrate(III) trihydrate

under carefully controlled conditions.
Introduction
Synthesis is a useful technique in all areas of chemistry. This technique is important

because it is the basis for developing new compounds, which may be useful for
animals and vegetation. Most developments in the pharmaceutical industry as well as
the introduction of new and less harmful pesticides are made possible because the
chemicals involved are synthesised and tested in the laboratory. In addition, many
chemical compounds used in everyday life are synthesised from simpler materials.
This experiment involves preparing a substance by reacting known quantities

of chemicals. The expected product is potassium tris(oxalato)ferrate(III) trihydrate,
K3[Fe(C2O4)3]·3H2O. The preparation of this compound involves several steps. Firstly,
ferrous ammonium sulphate, Fe(NH3)2(SO4)2.6H2O, is dissolved in distilled water to
which excess oxalic acid, H2C2O4, is added to make it slightly acidic and the following
reaction occurs.
The preparation of this compound involves several steps. Firstly, ferrous

ammonium sulphate, Fe(NH3)2(SO4)2.6H2O, is dissolved in distilled water to which
excess oxalic acid, H2C2O4, is added to make it slightly acidic and the following
reaction occurs.
Fe(NH4)2(SO4)2.6H2O (aq) + H2C2O4 (aq) → FeC2O4 (s) + H2SO4 (aq) + (NH4)2SO4 (aq)
+ 6H2O (l) ..............(Eq 1)
Ferrous oxalate, FeC2O4, is a finely divided precipitate and tends to be colloidal.

However, heating the solution causes it to coagulate and facilitates separating the
precipitate from the solution.
Next, potassium oxalate solution, K2C2O4(aq), is added to the FeC2O4

precipitate which produces a slightly basic solution to facilitate the oxidation of ferrous
ion to ferric ion by hydrogen peroxide, H2O2. The following reaction takes place:
[Oxidation / 2 electrons lost] 2Fe2+ → 2Fe3+ + 2e−

[Reduction / 2 electrons gained] H2O + HO2− + 2e− → 3OH−
[Overall net reaction] 2Fe2+ + H2O + HO2− → 2Fe3+ + 3OH− ..........(Eq 2)
Note that FeC2O4 is the source of Fe2+ ions in Eq. 2.
The OH− ion concentration of the solution is high enough so that some of the
Fe3+ ions react with OH− ions to form ferric hydroxide (brown precipitate) as follows:
Fe3+ + 3OH− → Fe(OH)3 (s)..........(Eq 3)
With the addition of more H2C2O4, Fe(OH)3 dissolves and the soluble complex
K3[Fe(C2O4)3].3H2O is formed according to:
3K2C2O4 (aq) + 2Fe(OH)3 (s) + 3H2C2O4 (aq) →2K3[Fe(C2O4)3].3H2O (aq) + 3H2O (l)
……….(Eq.4)
Alcohol is added to the solution to cause the complex iron salt to precipitate
since it is less soluble in alcohol than in water.
The complexity of the series of reactions described in equations 1 – 4 may be

greatly simplified by following the Fe2+/ Fe3+ ion throughout. It can be seen that for
every mole of Fe(NH3)2(SO4)2.6H2O used as the starting material, one mole of
K3[Fe(C2O4)3].3H2O will be obtained as the final product.
Fe(NH4)2(SO4)2.6H2O (aq) + H2C2O4 (aq) → FeC2O4 (s) + ...etc (see Eq.1)
FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3(s) + ...etc (see Eq.2 & 3)

(Fe2+ = Fe3+)
Fe(OH)3 + H2O2 + K2C2O4 → K3[Fe(C2O4)3].3H2O (aq) + ...etc (Eq.4)
Safety precautions
All chemicals are toxic. The organic solvents are highly flammable and can be irritating
to body tissues and respiratory tract. Acids are corrosive. Work with care and wear
safety goggles. Wash hands thoroughly with soap and water before leaving the
laboratory.
Apparatus
Balance
125 mL Erlenmeyer flask
Measuring cylinder, 50 mL (2 pieces)
Beakers (100 mL, 3 pieces)
Beaker, 400 mL
Glass rod
Ice bath
Bunsen burner
Tripod stand
Thermometer
Buchner funnel
Vacuum filtration apparatus
Filter paper
Chemicals
Ferrous ammonium sulphate, Fe(NH4)2(SO4)2.6H2O
0.5 M oxalic acid, H2C2O4 (aq)
1 M potassium oxalate monohydrate, K2C2O4·H2O (aq)
3 M sulphuric acid, H2SO4
6% hydrogen peroxide, H2O2
Ethanol
1:1 ethanol/water solution
Deionised water
Procedure
1. Weigh out about 5 g ferrous ammonium sulphate salt. Record the actual weight
used. Put this into a 125 mL Erlenmeyer flask. Dissolve this compound with 15 mL
of distilled water and add 5 drops of 3M sulphuric acid.
2. Add 50 mL of 0.5 M oxalic acid to this solution and heat it to boiling, stirring
constantly to prevent bumping.
3. Remove the Erlenmeyer flask from the heat and allow the yellow precipitate of
FeC2O4 to settle. Decant the supernatant liquid and wash the precipitate using 20
mL of hot distilled water. Swirl the mixture and allow the precipitate to settle;
decant and repeat the washing once more.
4. Add 20 mL of 1M K2C2O4 to the precipitate, stir and heat to 40oC. While the
temperature is at 40oC, immediately add 10 mL of 6% H2O2 dropwise and stir
continuously. Make sure the temperature does not go below 40 oC and not above
50oC during the addition of hydrogen peroxide. Some brown precipitate of Fe(OH)3
may form at this time.
5. Heat the resulting solution to boiling. Add in 20 mL of 0.5 M H2C2O4 all at once
while maintaining the temperature near boiling. The solution should turn clear
green. If some brown residue remains, add more 0.5 M H2C2O4 dropwise while
the solution is boiling, until it turns clear green. However, if the remaining residue
is yellow, it is probably unreacted FeC2O4 and more H2O2 should be added
carefully.
6. If the solution is cloudy, gravity filter it into a clean 125 mL Erlenmeyer flask. If it
is clear, no flitration is necessary. Then while swirling constantly, slowly add 15
mL of ethanol to the solution. Allow to cool in an ice bath prepared in a 400 mL
beaker. Immerse the bottom portion of the flask in the ice bath and slowly stir the
solution until crystals begin to form. Stop stirring and allow the solution to
stand in the ice bath for 20 minutes. A good crop of crystals should have formed
before the solution is filtered.
7. Prepare the vacuum filtration apparatus.
8. Decant the supernatant liquid away from the green crystals. With the aid of a clean
glass rod, transfer the crystals to the Buchner funnel and apply suction for about
2 minutes.
9. Stop the suction and add 10 mL of the 1:1 ethanol/water solution. Wait for 30
seconds and then apply suction for 2 minutes. Repeat this washing process. After
the final wash, allow the suction to continue for a further 2 minutes.
10. Transfer the crystals to a preweighed labelled dry 50 mL beaker. Discard the
wash solutions.
Note: The complex is photosensitive and should not be exposed to light.

Store in a sample bottle/vial wrapped in foil. Keep the crystals for the next
experiment
Useful Molar Masses

K2C2O4 = 166.22 g/mol
Fe(NH4)2(SO4)2.6H2O = 392.13 g/mol
K3[Fe(C2O4)3].3H2O = 491.24 g/mol

Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

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Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

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EXPERIMENT 2

Synthesis of Potassium Tris(oxalato)ferrate(III) Trihydrate (K3[Fe(C2O4)3].3H2O)

To synthesis a coordination compound, potassium tris(oxalato)ferrate(III) trihydrate

Synthesis is a useful technique in all areas of chemistry. This technique is important

This experiment involves preparing a substance by reacting known quantities

The preparation of this compound involves several steps. Firstly, ferrous

Ferrous oxalate, FeC2O4, is a finely divided precipitate and tends to be colloidal.

Next, potassium oxalate solution, K2C2O4(aq), is added to the FeC2O4

[Oxidation / 2 electrons lost] 2Fe2+ → 2Fe3+ + 2e−

Note that FeC2O4 is the source of Fe2+ ions in Eq. 2.

Fe3+ + 3OH− → Fe(OH)3 (s)..........(Eq 3)

The complexity of the series of reactions described in equations 1 – 4 may be

Fe(NH4)2(SO4)2.6H2O (aq) + H2C2O4 (aq) → FeC2O4 (s) + ...etc (see Eq.1)

FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3(s) + ...etc (see Eq.2 & 3)

Fe(OH)3 + H2O2 + K2C2O4 → K3[Fe(C2O4)3].3H2O (aq) + ...etc (Eq.4)

Note: The complex is photosensitive and should not be exposed to light.

Useful Molar Masses

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