EXPERIMENT 1

SYNTHESIS OF OXALATE COMPLEXES OF IRON

OBJECTIVES
1. Synthesis iron(II) oxalate, FeC2O4
2. Synthesis potassium trioxalatoferrate(III) trihydrate, K3[Fe(C2O4)3].3H2O

INTRODUCTION

Apart from moving as a Lewis base, the oxalate ion can also be referred to as a bidentate ligand
since it can give two braces of negatrons (one from each O) to the Fe (III) or Iron (II) cation
moving as a Lewis acid from two O atoms. Iron can arrange a wide range of composites, the
majority of which have an octahedral geometry. The iron (II) oxalate generated in this
experiment is characterised by a Fe2+ as the cardinal metal cation. This is oxidised to Fe3+ in
order to create the Potassium Trioxalatoferrate (III) Trihydrate composite, which has a Fe3+ as
the cardinal metal cation. Certain composites, such as the Potassium Trioxalatoferrate (III)
Trihydrate composite, are photosensitive because they are unstable to light. For this reason,
such composites must be stored under dark conditions to prevent the Fe3+ ion from turning to
the Fe2+ ion.

CHEMICALS

Ferrous ammonium sulphate (NH4)2 [Fe(H2O)2(SO4)2].4H2O

Oxalic acid dehydrates, H2C2O4.2H2O
Potassium oxalate monohydrate, K2C2O4.H2O
Hydrogen peroxide, H2O2 (30% v/v)
Sulphuric acid, H2SO4 (2M)
Ethanol
Acetone

APPARATUS

Erlenmeyer flask
Beaker
Dropper
Filter funnel Watch glass
Hot plate
Magnetic stirrer
Filter paper
Buchner funnel
JOTTER BATRISYIA
JOTTER LYDIA
PROCEDURE

To start the experiment, we did the Part A which is preparation of Iron (II) Oxalate, FeC2O4.
Firstly, 1.0 mL 2M H 2SO4 is added into 50.0 mL warm water in a beaker then followed by 15 g
(NH4)2 [Fe(H2O)2(SO4)2].4H2O. Then, 100 mL of 10% (w/v) H2C2O4 solution is prepared. Next,
75.0 mL H2C2O4.2H2O solution has been added slowly with rapid stirring. The mixture is heated
gently until boiling. Next, the heat is turned off and the mixture has been brought to room
temperature then wait for the yellow precipitate of FeC2O4 to settle down. After this, the
precipitate is removed by vacuum filtration then washed it thoroughly with hot water (3x 10.0
mL) followed by acetone (3x 10.0 mL). Lastly, the product has been dried in a desiccator after a
few minutes of weighing it. This product is kept and it will be used to synthesise
K3[Fe(C2O4)3].3H2O.

For Part B, firstly a K2C2O4 solution is prepared by adding 5g of K2C2O4.H2O in 15 mL

warm water. Then, 3.25g of FeC2O4 (product from Part A) is added into the warm K2C2O4
solution. The temperature is kept at 40°C by placing the beaker containing K2C2O4 solution on
the hot plate. Next, 15 mL of H2O2 (30% v/v) has been added dropwise while the solution is
stirred continuously. The solution should contain precipitate of Fe(OH)3. Then, the solution is
heated until it boils. After a few minutes, 10 mL 10% H2C2O4 is added dropwise until the
precipitate dissolves. The temperature is kept near the boiling point during the addition of
H2C2O4. After that, the hot solution is filtered by vacuum filtration and 15 mL of ethanol is added
to the filtrate. Re-dissolved those crystals by gentle heating if there are some crystals that have
formed. Then make sure the solution is kept in a dark cupboard to crystallise the compound
because the product is photosensitive. Next, the crystals have been collected under vacuum
filtration then washed with 10 mL of an equal volume mixture of ethanol and water. Lastly, the
product is dried and weighed then kept in the dark environment.
WORKSHEET

Part A Preparation of Iron (II) Oxalate, FeC 2O4

10% (w/v) Volume of H2O (mL) 100 mL

H2C2O4 solution
Mass of H2C2O4 (g) 10.0006 g

Draw the structure of C2O4 -2 and

determine the denticity

Density: 2

Mass of filter paper (g) 0.3629 g

Mass of filter paper + FeC2O4 (g) 7.3670 g

Mass of FeC2O4 (g) 7.0041 g

Physical
properties

Compound Colour
Melting point (° C)

H2C2O4 White 101.5

FeC2O4 Yellow 190.0

K3[Fe(C2O4)3].3H2O Green 100.0

 % yield of FeC2O4
Actual yield: Amount of product obtained from
the experiment
Theoretical yield: Amount of product obtained from
the stoichiometric equation, using the limiting
reactant to determine product

Write a balanced equation for the

formation of FeC2O4 Fe2+ + H2C2O4 + 2H2O → FeC2O4 + 3H2O

Part B Preparation of Potassium Trioxalatoferrate(III) Trihydrate, K3[Fe(C2O4)3].3H2O

30% (v/v) H2O2 Volume of H2O 100.0 mL

solution (mL)

Volume of H2O2 15 mL
(mL)

Mass of filter paper + weighing dish (g) 4.2258 g

Mass of filter paper + weighing dish + 5.8958 g

K3[Fe(C2O4)3].3H2O (g)

Mass of K3[Fe(C2O4)3].3H2O (g) 1.6700 g

% yield of K3[Fe(C2O4)3].3H2O
Actual yield: Amount of product obtained
from the experiment
Theoretical yield: Amount of product obtained
from the stoichiometric equation, using the
limiting reactant to determine product

Write a balanced equation for the

formation of K3[Fe(C2O4)3].3H2O. 3K3[Fe(C2O4)3].3H2O + 2Fe(OH)3 + 3H2C2O4 →
2K3[Fe(C2O4)3].3H2O + 3H2O

What happened to the sample if Due to the sample is photosensitive. Then, if the
exposed to sunlight? sample is exposed to sunlight, the sample will not
be able to crystallize.

Explain the chemical reason for This is because the visible light will reduce Fe3+ to
this observation Fe2+ resulting in no crystals formation.
DISCUSSION

For Part A, combining ferrous ammonium sulphate, (NH4)2[Fe(H2O)2(SO4)2], yields iron (II)
oxalate, FeC2O4. Oxalic acid dehydrates to H2C2O4.2H2O and 4H2O. In order to maintain a low
pH in the ferrous ammonium sulphate solution and avoid the formation of rust-colored iron
oxides and hydroxides, 2M sulfuric acid was first diluted with 50mL of distilled water. Due to
oxalate's high toxicity, adding oxalic acid dehydrates to the solution must be done under a fume
hood. The iron (II) oxalate, FeC2O4, a yellow precipitate is formed.

In Part B, potassium oxalate and iron (II) oxalate were mixed to form a slightly basic
solution, and then hydrogen peroxide was added to the mixture to oxidise the ferrous (Fe2+) ion
to the ferric (Fe3+) ion. When Fe3+ interacts with OH- at a high enough concentration, ferric
hydroxide is formed. The extra Fe(OH)3 was dissolved with the addition of hydrogen peroxide. To
avoid the heat-sensitive hydrogen peroxide dissolving before reacting with all the iron (II) in
solution, the peroxide was slowly added. Since this salt is less soluble in alcohol than it is in
water, ethanol was added to the mixture, and within two to three days, a green crystalline solid
started to precipitate from the mixture. Because any visible light will convert Fe3+ to Fe2+ during
crystallisation, the solution must be kept in the dark environment.

The amount of obtained green crystal is 1.6700 g, with a theoretical yield of 18.8141 g
and an actual yield of 8.88%. There were a few mistakes made both during and after the
experiment, which is why the yield percentage was not 100%. Due to various errors made
throughout the experiment, which were brought on by the filtration and washing processes as
well as some external factors, the yield was lower than expected. The error has had an impact
on the experiment's yield.

CONCLUSION

In this experiment we are able to synthesis iron(II) oxalate, FeC2O4 and potassium
trioxalatoferrate(III) trihydrate, K3 [Fe(C2O4)3].3H2O. A percentage of 43.81% of FeC2O4 and
8.88% of K3 [Fe(C2O4)3].3H2O has been yielded in this experiment respectively in two different
parts.
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