ITEM CONTENT MARKS

Objective The purpose of this experiment is to synthesize potassium

tri(oxalato)ferrate(III) trihydrate K3[Fe(C2O4)3].3H2O.

Introduction Ferrous ammonium sulphate was dissolved in a slightly

acid solution, excess oxalic acid , H2C2O4 is added , and the
balance chemical reaction below show the reaction take
place in the experiment:
Fe(NH4)2(SO4)2.6H2O + H2C2O4 FeC2O4(s) + H2SO4 +
(NH4)2 + 6H2O(l)
FeC2O4(s) is a finely divided precipitateand tends to
collodial. When the solution was heated it may causes the
solution to coagulate and the facilities separating the
precipitate from the solution.
FeC2O4(s) precipitate was added with potassium oxalate
which produces a slightly basic solution for the oxidation of
the ferrous ion to the ferric ion to the by hydrogen
peroxide,H2O2.The following reaction takes place:
H2O + HO2- + 2Fe2+ 2Fe3+ + 3OH-
The OH- ion concentration of the solution is high enough
so that some Fe3+ reacts with the OH- to form ferric
hydroxide that is brown precipitate as follows:
Fe3+ + 3OH- Fe(OH)3
H2C2O4 was added in excess the Fe(OH)3 dossolves and
the soluble complex K3[Fe(C2O4)3].3H2O + 3H2O
Ethanol is added to the solution to cause the complex iron
salt to precipitate.
Results Chemical equation involved :
Fe(NH4)2(SO4)2· 6H2O + H2C2O4  FeC2O4(s) + H2SO4 +
(NH4)2SO4 + 6H2O(l)
Fe3+ + 3OH-  Fe(OH)3(s)
Overall chemical equation :
3K2C2O4 + 2Fe(OH)3(s) +3H2C2O4  2K3[Fe(C2O4)3]·
3H2O + 3H2O
Mass of Fe(NH4)2(SO4)2· 6H2O = 5.0055 g
Mass of K2C2O4 = 3.5085 g
Mass of H2C2O4 = 2.8515 g
The number of mole Fe(NH4)2(SO4)2· 6H2O = 5.0055 g /
392.01 g/mol
=0.0128 mol
Mole Fe(NH4)2(SO4)2· 6H2O = mole of Fe(OH)3
mole of Fe(OH)3 = 0.0128 mol
mole of K2C2O4 = 3.5085 g / 166.22 g/mol
=0.0211 mol
Mole of H2C2O4 = 2.8515 g / 90.02 g/mol
=0.0317 mol
From the overall equation :
3 mol of K2C2O4 ≡ 2 mole of K3[Fe(C2O4)3]· 3H2O
0.0211 mol of K2C2O4 = 0.0141 mol K3[Fe(C2O4)3] · 3H2O

3 mole of H2C2O4 ≡ 2 mole of K3[Fe(C2O4)3]· 3H2O

0.0317 mol of K2C2O4.H2O = 0.0211 mol of K3[Fe(C2O4)3]·
3H2O

2 mol of Fe(OH)3 ≡ 2 mol of K3[Fe(C2O4)3]· 3H2O

0.0128 mol of Fe(OH)3 ≡ 0.0128 mol of K3[Fe(C2O4)3]· 3H2O

The limiting reactant is Fe(OH)3

1)The theoretical yield of K3[Fe(C2O4)3]· 3H2O = 0.0128 mol
x 491.21 g/mol
=6.2875 g
2)Actual yield K3[Fe(C2O4)3]· 3H2O = 0.9777g
3)Percentage yield of K3[Fe(C2O4)3]· 3H2O
=actual yield x 100
Theoretical yield
= (0.9777g / 6.2875 g) x 100%
= 15.55 %
Discussion

Potassium tri(oxalato)ferrate(III) Trihydrate is a

complex of iron with three oxalato ligands (C2O42-) bonded to
every central metal atom . These ligands are bidantate
which is each of them binds to the metal atom at 2 difeerent
places. The chemical formula is K3[Fe(C2O4)3]· 3H2O.

Potassium tri(oxalato)ferrate(III) Trihydrate is hygroscopic

and sensitive in nature.
Fe is acting as a lewis acid reacts with neutral molecule
and acting as a lewis bases.These lewis bases is C2O4 and
H2O are called as ligands.Lewis acid are electron pair
acceptor while lewis base are electron pair donor.
Ferrous ammonium solution was added with the oxalic
acid dihydrate and will formed yellow precipitate , this
reaction can be showned by the chemical equation below:
Fe(NH4)2(SO4)2.6H2O + H2C2O4 → FeC2O4 (s) + H2SO4 +
(NH4)2SO4 + 6H2O
After that the solution was heated to boiling and the
supernatant is decanted.After the substance was added with
potassium oxalate , it is allowed to heat at 40˚C and H 2O2
was added dropwisely.The solution was turn to dark brown
with precipitate for the oxidation of the ferrous ion to ferric
ion, the reaction can be showned from the balance chemical
below:

H2O + HO2- + 2Fe2+ → 2Fe3+ + 3OH-

Fe3+ + 3OH- → Fe(OH)3

Oxalic acid was added until excess, the solution was turned
to colourless solution.
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 → 2K3[Fe(C2O4)3].3H2O +
3H2O
The colourless solution was turn to pale green solution.
The product was obtained by suction filtration process which
is the solution was washed with 30 ml 95% ethanol slowly
and leave the solution to recrystallize.After that the green
crystal is filtered and washed with 1:1 ethano,/ water and
cooled acetone.The mass of green crystal obtained is
0.9777g , the theoretical yield is 6.2875 g and the
percentage yield is 15.55 % .
There is some precaution that we should practices while
doing an experiment is we need to clean all the apparatus
that we used for example conical flask.This is important
because there may have other substances left in the flask
and this can cause our product is contaminated so we dont
get the result.Next , while we are heat the solution of ferrous
ammonium sulphate and solution of oxalic acid dihydrate we
need to slow the hot plate to avoid the bumping of the
solution.While we are doing an experiment there occur
bumping of the solution , some of the solution was bumped
to outside of the conical flask.The mass loss due to the
bumping, so there is large different between 15.55% to
100%.
Conclusion Potassium tris(oxalato)Ferrate(III)Trihydrate , was

K3[Fe(C2O4)3].3H2O synthesize.The actual mass obtained

0.9777g was while the theoretical yield obtained was . So

6.2875 g the theoretical yield is 15.55 % .

References 1) http://htmlimg2.scribdassets.com/6fsjkmdsjkx1jn8/images/2-

2eef2214a7.jpg

2) http://nurulyunaliyana.blogspot.com/2012/11/example-lab-

report-of-synthesis-of.html

3) http://id.scribd.com/doc/52686651/Synthesis-of-Potassium-

Tris-Oxalato-Ferrate-III