CHM 477

EXPERIMENT 3, 4 & 5
Synthesis of Potassium Tris(oxalato) Chromium(III) Trihydrate,
Copper(II) Oxalate Complexes & Potassium Tris(oxalato) Ferrate(III)
Trihydrate
DR AMALINA MOHD TAJUDDIN
NUR SHAZWANI BINTI AZIZ (2018250776)
INTAN NAZIRA BINTI MUSTAFA KAMAL (2018250966)
INTRODUCTION
Synthesis is a process in which substances combine to form completely new substances. In
this experiment we are synthesizing coordination compound. Coordination compound is the
product of a Lewis acid-base reaction in which neutral molecules or anions bond to central
metal by coordinate covalent bonds. A coordinate covalent bond is a covalent bong in which
one atom supplies both electrons. This type of bonding is different from a normal covalent
bong in a bond in which each atom supplies one electron.

Chromium(III), the most stable oxidation state of chromium, forms a number of complexes,
in which six monodentate ligands surround the cation octahedrally. Two oxalate anions and
two water molecules coordinate the chromium cation to provide oxygen atoms at the corners
of the octahedron.
Copper is transitionalmetal. When potassium oxalate solution was added to Cu 2+ aqueous
solution copper (II) oxalate was formed.
Ferrous ammonium sulphate was dissolved in a slightly acid solution, excess oxalic acid is
added. FeC2O4 is finely divided precipitate tends to colloidal. When the solution was heated it
may causes the solution to coagulate and the facilities separating the precipitate from the
solution. FeC2O4 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. The OH- ion concentration of the solution is high enough so that some Fe 3+ reacts
with the OH- to form ferric hydroxide that is brown precipitate. H2C2O4 was added in excess
the Fe(OH)3 dissolves. Ethanol is added to the solution to cause the complex iron salt to
precipitate.

The amount of coordination compound expected from a given mass of reactants can be
calculated and is called the theoretical yield. The actual mass of coordination compound
synthesized, called the actual yield. The actual mass of coordination compound synthesized,
called the actual yield is usually less than the theoretical yield
𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
%yield = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
OBJECTIVE
The purpose of this experiment is to synthesize potassium tris(oxalate) chromium(III)
trihydrate, K3[Cr(C2O4)3].3H2O , copper(II) oxalate complex and potassium
tris(oxalate)ferrate(III) trihydrate, K3[Fe(C2O4)3].3H2O

APPARATUS AND EQUIPMENT

Conical flask, weighing boat, funnel, glass rod, hot plate, beaker, dropper, suction filtration,
watch glass

CHEMICALS
Experiment 3
5.00g oxalic acid, 10mL water, 1.8g potassium dichromate, 2.10g potassium oxalate
monohydrate, 10mL of 95% ethanol, 1:1 ethanol/water, 13mL of 95% ethanol.

Experiment 4
2.00g copper(II) sulphate pentahydrate, 30mL distilled water, 6.20g potassium oxalate
monohydrate, 30-40mL distilled water(room temperature), cold water

Experiment 5
5.00g ferrous ammonium sulfate, 20mL water, 1mL dilute sulfuric acid, 2.50g oxalic acid
dihydrate, 25mL water, hot water, 3.50g solid potassium oxalate monohydrate, 10mL of 6%
H2O2, 2.00g oxalic acid dihydrate, 30mL water, 30mL 95% ethanol.

METHOD
Experiment 3

1.8g of potassium dichromate was added slowly in a solution of mixture 5.00g of oxalic acid
in 10mL of water. The orange colored mixture was warmed up almost to boiling. 2.10g of
potassium oxalate monohydrate was dissolved in the mixture when the reaction has subsided
and heated to boiling for 5 minutes. The viscous was cooled to room temperature. 10mL of
95% ethanol was added while stirring. Precipitation appear to completed after cooled in ice
after 15-30 minutes. The complex was collected by suction filtration. The crystal was washed
with two portion of 5mL 1:1 ethanol/water followed by 13mL of 95% ethanol. The solid was
placed on glass plate and allowed to dry in oven (about 80ͦ C). the mass of product was
determined hence the percentage yield. The product was transferred into vial to be use in the
next experiment.
Experiment 4
2.00g of copper (II) sulphate pentahydrate was added into 30mL H2O in a small conical flask.
The solution was heated on a hot plate until the solids dissolved. 6.20g of potassium oxalate
monohydrate was dissolved with 30-40mL distilled water in conical flask at room
temperature. The heated copper (I) sulphate was added slowly to the potassium oxalate
solution while swirled slowly to mix. The mixture was chilled in ice bath for 30-60 minutes.
Blue precipitates was obtained after cooling process.
The complex was collected by suction filtration and washed twice with 3mL portions of cold
water. The crystals was dried in oven. The percentage yield was determined. the crystals was
transferred into labelled vial to be used in the next experiment.

Experiment 5
Procedure A
A solution of 2.50g of oxalic acid was added into well stirred solution of 5.00g of ferrous
ammonium sulfate in 20mL of water containing 1mL of dilute sulfuric acid in the beaker. The
mixture was heated to boil and the yellow precipitate was allowed to settle. Supernatant was
decant. 15mL of hot water was added to the yellow precipitate, stirred and decant the
supernatant. Add another 15mL of hot water to the precipitate. 3.50g of solid potassium
oxalate monohydrate was added and heated to approximately 40ͦ C. while the temperature is
at 40ͦ C, 10mL of 6% H2O2 was immediately added dropwise while continuously stirred. The
temperature of the solution was checked periodically to make sure that it is at 40ͦ C (but not
>50ͦ C) during the addition of H2O2. The solution was heated to boil, then 2.00g of oxalic acid
dihydrate in 30mL of water portion was added. Initially 20mL was added, more solution was
added little by little until all the brown precipitated dissolved. The clear solution was heated
to boil, then filtred through a Buchner funnel with well-fitting paper and 30mL 95% ethanol
was added slowly to the solution. The crystals was redissolved by reheating and leaved to
crystalize (keep until next week)

Procedure B
The crystals was obtained by suction filtration. The crystals was washed twice with cooled
1:1 ethanol/water mixture and finally with cooled acetone. The crystals was air dried and
weighed. The complex was stored in a vial and kept for the next experiment.
RESULTS AND CALCULATION
EXPERIMENT 3
Results
1. Theoretical yield of K3[Cr(C2O4)3].3H2O = 5.9690g
2. Mass of K3[Cr(C2O4)3].3H2O = 4.4607g
3. Percent yield of K3[Cr(C2O4)3].3H2O = 74.73%

Calculation
K2Cr2O7 + 7C2H2O4 + 2K2C2O4.H2O → 2K3[Cr(C2O4)3].3H2O + 6CO2 + 3H2O

5.0062𝑔
Number of mole of C2H2O4 =
90.03488𝑔/𝑚𝑜𝑙

=0.0556 mol
1.8015𝑔
Number of mole of K2Cr2O7 =
294.1846𝑔/𝑚𝑜𝑙

=0.006124 mol (limiting reactant)

2.1099𝑔
Number of mole of K2C2O4.H2O =
184.23088𝑔/𝑚𝑜𝑙

=0.01145 mol

1 mole of K2Cr2O7 = 2 mole of K3[Cr(C2O4)3].3H2O

0.006124 ×2
=
1
= 0.012248 mol of K3[Cr(C2O4)3].3H2O

Mass of K3[Cr(C2O4)3].3H2O = mass × molar mass

= 0.012248 × 487.348
= 5.9690g (theoretical)

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
Yield percentage of K3[Cr(C2O4)3].3H2O = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
4.4607𝑔
= × 100%
5.9690𝑔

= 74.73%
EXPERIMENT 4
Results
1. Theoretical yield of K2[Cu(C2O4)2(H2O)2] = 2.8458g
2. Mass of K2[Cu(C2O4)2(H2O)2] = 2.7053g
3. Percent yield of K2[Cu(C2O4)2(H2O)2] = 67.62%

Calculation
CuSO4.5H2O + 2K2C2O4.H2O → K2[Cu(C2O4)2(H2O)2] + K2SO4 + 5H2O

2.0086𝑔
Number of mole of CuSO4.5H2O =
249.68𝑔/𝑚𝑜𝑙

=8.0447 × 10-3 mol (limiting reactant)

6.2001𝑔
Number of mole of K2C2O4.H2O =
184.2𝑔/𝑚𝑜𝑙

=0.03366 mol

1 mole of CuSO4.5H2O = 1 mole of K2[Cu(C2O4)2(H2O)2]

8.0447 × 10-3 mole of CuSO4.5H2O = 8.0447 × 10-3 mole of K2[Cu(C2O4)2(H2O)2]

Mass of K2[Cu(C2O4)2(H2O)2] = mass × molar mass

= 8.0447 × 10-3 mol × 353.75 g/mol
= 2.8458g (theoretical)

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
Yield percentage of K2[Cu(C2O4)2(H2O)2] =
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
× 100%
2.7053𝑔
= × 100%
2.8458𝑔

= 95.06%
EXPERIMENT 5
Results
1. Theoretical yield of K3[Fe(C2O4)3].3H2O = 6.2777g
2. Mass of K3[Fe(C2O4)3].3H2O obtained = 1.2778g
3. Percent yield of K3[Fe(C2O4)3].3H2O = 20.35%

Calculation
Fe(NH4)2(SO4)2.6H2O + H2C2O4 → FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O

5.0078𝑔
Number of mole of Fe(NH4)2(SO4)2.6H2O =
391.89𝑔/𝑚𝑜𝑙

=0.01278 mol (limiting reactant)

2.5053𝑔
Number of mole of H2C2O4 =
130.01𝑔/𝑚𝑜𝑙

=0.01927 mol

‫ ؞‬limiting reactant is Fe(NH4)2(SO4)2.6H2O

2 mole of Fe2+ = 2 mole of Fe3+

3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 → 2K3[Fe(C2O4)2].3H2O + 3H2O

2 mole of Fe(OH)3 = 2 mole of K3[Fe(C2O4)2].3H2O

0.01278 mole of Fe(OH)3 = 0.01278 mole of K3[Fe(C2O4)2].3H2O

Mass of K3[Fe(C2O4)2].3H2O = mass × molar mass

= 0.01278g × 491.21g/mol
= 6.2777g (theoretical)

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
Yield percentage of K3[Fe(C2O4)2].3H2O = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
1.2778𝑔
= × 100%
6.2777𝑔

= 20.35%
DISCUSSION
In this experiment, we have studied how to synthesis coordination compound. Transitional
metals have a distinct tendency to form complex ions. Complex ions can be defined as a
containing a central metal cation bonded to one or more molecules or ions. Coordination
compound typically consist of a complex and a counter ion.
For experiment 3, the coordination compound formed when Lewis acid that is Cu 2+ are
reacted with Lewis base that is C2O4 and H2O. Potassium dichromate dissolved slightly acid
solution, excess oxalic acid is added and the following reaction takes place
8H+ + K2Cr2O7 + 3C2H2O4 + 6K2C2O4.H2O → 2K3[Cr(C2O4)3].3H2O + 6CO2 + 9H2O + 8K+
Orange solution was formed and filtered then leaves for crystallization. Potassium oxalate
was added. Dark green solution was formed and was heated for five minutes. After that we
allowed the solution to cool at room temperature. The dark green crystal was filtered and
washed with 1:1 ethanol/water and followed by 13mL of acetone. The mass of crystal
obtained is 4.4607g. The theoretical yield obtained is 5.9690g. So the percentage yield is
74.73%.
For experiment 4, copper(II) oxalate complexes was formed when copper(I) sulphate
pentahydrate was reacted with potassium oxalate monohydrate. Heated copper(II) sulphate
was added into potassium oxalate solution and the flask was swirled. Cooled the solution in
the ice bath and obtain the crystal blue precipitate by suction filtration. The crystal was dried
in the a oven and mass of copper(II) oxalates complexes was obtained. The mass of
copper(II) oxalates complexes is 2.7053g, theoretical yield of copper(II) oxalate complexes is
2.8458g and the percentage yield is 95.06%
For experiment 5, ferrous ammonium solution was added with the oxalic acid dihydrate and
will formed yellow precipitate, this reaction can be shown by the chemical equation
Fe(NH4)2(SO4)2.6H2O + H2C2O4 → FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O
After that, the solution was heated to boil and the supernatant is decanted. After the substance
was added with potassium oxalate, it is allowed to heat at 40ͦ C and H2O2 was added
dropwise. The solution was turned to dark brown with precipitate for the oxidation of the
ferrous ion to ferric ion. Oxalic acid was added until excess, the solution was turned to
colorless solution. The colorless solution was turned to pale greenish yellow solution. The
product was obtained by suction filtration process which is the solution was washed with
30mL 95% ethanol slowly and leave the solution to recrystallize. After that the crystal is
filtered and washed with 1:1 ethanol/water and cooled acetone. The mass of crystal obtained
is 1.2778g, the theoretical yield is 6.2777g and the percentage yield is 20.35%. The color of
actual crystal obtained should be green but we obtained white crystal. There might be some
error while doing the experiment.
There is large different to achieve 100% of theoretical yield for experiment 5. There may be
error occur when we are doing the experiment. There is some precaution that we should
practice while doing an experiment is we need to clean all the apparatus that we used. This is
important because there may have residue left in the flask and this can cause our product got
contaminated so we did not get the result. Next, we need to be careful when heating the
substance as it will bump when we heat too long. The mass loss due to the bumping, so there
is large different between the percentage yield obtained to 100%.
CONCLUSION
For experiment 3, Potassium tri(oxalato) chromium(III) trihydrate, K3[Cr(C2O4)3].3H2O was
synthesized. The mass of crystal obtained is 4.4607g. The theoretical yield obtained is
5.9690g. So the percentage yield is 74.73%.
Experiment 4, Copper(II) oxalate complexes, K2[Cu(C2O4)2(H2O)2] was prepared. The actual
mass obtained was 2.7053g while theoretical yield of copper(II) oxalate complexes is
2.8458g. So the percentage yield is 95.06%
Experiment 5, Potassium tris(oxalato) ferrate(III) trihydrate, K3[Fe(C2O4)2].3H2O was
synthesized. The actual mass obtained was 1.2778g while the theoretical yield was 6.2777g.
So the percentage yield is 20.35%

QUESTIONS
1. What is the oxidation state of chromium in K2Cr2O7 in the product?

K2Cr2O7
(1)(2) + (Cr)(2) + (-2)(7) = 0
2 + 2Cr – 14 = 0
2Cr = 14 -2
12
Cr =
2
Cr = +6

Oxidation state of Cr in K2Cr2O7 is +6

K3[Cr(C2O4)3].3H2O
(1)(3) + n + (-2)(3) = 0
3+n–6=0
n = +3

oxidation state of Cr in K3[Cr(C2O4)3].3H2O is +3

2. Write two half-equations for each reaction involved in the preparation of the complex
using oxalic acid dihydrate, K2C2O4.H2O and potassium dichromate, K2Cr2O7, and a
balanced equation for overall reaction.

5C2O42- → 10CO2 +10e-

Cr2O72- + 14H+ + 10e- → 2Cr2+ + 7H2O
5C2O42- + 14H+ + Cr2O72- → 10CO2 + 2Cr2+ + 7H2O
REFERENCES
1. https://www.academia.edu/7725871/To_synthesize_potassium_tris_oxalato_chromiu
m_III_trihydrate_K3_Cr_C2O4_3_.3H2O_
2. https://www.academia.edu/7725865/preparation_of_copper_II_oxalate_complexes
3. https://www.academia.edu/7725878/To_synthesize_potassium_tri_oxalato_ferrate_III
_trihydrate_K3_Fe_C2O4_3_.3H2O