CHM 361

INORGANIC CHEMISTRY

LAB REPORT

EXPERIMENT 2:
SYNTHESIS OF POTASSIUM
TRIS(OXALATO)FERRATE(III)
TRIHYDRATE (K3[Fe(C2O4)3].3H2O)

EXPERIMENT 3:
Determination of the Percentage of Ligands in
K3[Fe(C2O4)3].3H2O

NAME NUR HIDAYATUNNISA’ BINTI YUSRI

STUDENTD ID 2019250286
GROUP AS120510
LECTURER MADAM NUR NADIRAH BINTI RODZALI

SUBMISSION 7th JANUARY 2022

DATE
 EXPERIMENT 2

SYNTHESIS OF POTASSIUM TRIS(OXALATO)FERRATE(III) TRIHYDRATE (K3[Fe(C2O4)3].3H2O)

OBJECTIVES

 To synthesize 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 the development of new compounds, which may be useful for animals and vegetation.
Because the compounds employed are synthesised and analysed in the laboratory, many
breakthroughs in the pharmaceutical sector, as well as the introduction of new and less hazardous
pesticides, are conceivable. Most organic substances present in daily life, on the other hand, are
made from less complex materials.

The goal of this experiment is to make a compound by reacting known amounts of

substances. K3[Fe(C2O4)3]3H2O is the predicted result, potassium tris(oxalato)ferrate(III) trihydrate.
PROCEDURE

1. 4g of ferrous ammonium sulphate salt was weighed out. The actual weight used was
recorded. 4 g of ferrous ammonium sulphate salt was put into a 125 mL Erlenmeyer flask.
This compound was dissolved with 15 mL of distilled water and 5 drops of 3M sulphuric acid
were added.
2. 50 mL of 0.5M oxalic acid was added to this solution and was heated to boiling, stirring
constantly to prevent bumping.
3. The Erlenmeyer flask was removed from the heat and yellow precipitate of FeC 2O4 was
allowed to settle. The supernatant liquid was decanted and the precipitate was washed
using 20 mL of hot distilled water. The mixture was swirled and the precipitate was allowed
to settle. This step was repeated once again.
4. 20 mL of 1M K2C2O4 was added to the precipitate, stirred and heated to 40⁰C. While the
temperature is at 40⁰C, 10 mL of 6% of H2O2 dropwise was added immediately and stirred
continuously. Make sure the temperature does not go below 40oC and not above 50 ⁰C
during the addition of hydrogen peroxide. Some brown precipitate of Fe(OH) 3 may form at
this time.
5. The resulting solution was heated to boiling. While maintaining the temperature near
boiling, 20 mL of 0.5M H2C2O4 was added all at once. The solution should turn clear green.
More 0.5M H2C2O4 dropwise was added if some brown residue remains, 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
filtration is necessary. Then while swirling constantly, 15 mL of ethanol was added slowly to
the solution and allowed it to cool in an ice bath prepared in a 400 mL beaker. The bottom
portion of the flask was immersed in the ice bath and the solution was stirred slowly 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. The vacuum filtration apparatus was prepared.
8. The supernatant liquid was decanted away from the green crystals. With the aid of a clean
glass rod, the crystals were transferred to the Buchner funnel and suction was applied for
about 2 minutes.
9. The suction was stopped and 10 mL of the 1:1 ethanol/water solution was added. Wait for
30 seconds and then the suction was applied for 2 minutes. This washing process was
repeated. After the final wash, the suction was allowed to continue for a further 2 minutes.
10. The crystals were transferred to a preweighed labelled dry 50 mL beaker. The solutions were
discarded.
RESULTS/DATA ANALYSIS

NO. ITEMS RESULTS

1. Mass of Fe(NH 4 ) 2 (SO 4 ) 2 .6H 2 O used 5.0246 g
2. Moles of Fe(NH 4 ) 2 (SO 4 ) 2 .6H 2 O used 0.0128 mol

3. Mass of K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O obtained 4.9822 g

4. Theoretical yield of K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O (moles) 0.0128 mol

5. Theoretical yield of K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O (mass) 6.2879 g

6. Percent yield of K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O 79.23%

CALCULATIONS

Show all your calculations.

QUESTION 2:

mass of Fe ( NH 4 )2(SO 4)2.6 H 2O

Moles of Fe(NH4)2(SO4)2.6H2O =
molar mass for Fe( NH 4) 2( SO 4)2. 6 H 2O

5.0246 g
¿
392.13 g /mol

¿ 0.01281 mol of Fe( NH 4) 2(SO 4)2. 6 H 2 O

QUESTION 4:

𝐅(NH4)2(SO4)2. 𝟔𝐇2𝐎 + H2C2O4 → Fe2C2O4 + H2SO4 + (NH4)2(SO4) + 𝟔𝐇2𝐎 -1

1 mole of Fe(NH4)2(SO4)2.6H20 = 1 mole of Fe2C2O4

Moles of Fe2C2O4 = 0.01281 mol

FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3 + … etc –2

1 mole of FeC2O4 = 1 mole of Fe(OH)3

Moles of Fe(OH)3 = 0.01281 mol

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

2 moles of Fe(OH)3 = 2 moles of K 3 [ Fe ( C 2 O 4 ) 3 ] .3 H 2 O

2moles of K 3 [Fe (C 2O 4 )3].3 H 2O

0.01281 mol Fe(OH)3 =
2 moles of Fe(OH )3

¿ 0.01281 mole of K 3[Fe (C 2 O 4)3 ].3 H 2O

QUESTION 5:

mass
Moles =
molar mass

mass
0.0128 moles =
491.24 g/mol

g
Mass = 0.0128 moles × 491.24
mol

Mass = 6.2879 g

QUESTION 6:

Actual mass
Percent yield = ×100 %
Theoretcal mas
 4.9822 g
= ×100 %
6.2879 g

= 79.23 %

DISCUSSION
For experiment 2, the essential aim of the experiment is to synthesise the coordination
compound potassium tris(oxalato)ferrate(III) trihydrate under carefully regulated conditions.
The Synthesize procedure was used in experiment 2 to accomplish this goal, while the predicted
final product obtained was K3[Fe(C2O4)3].3H2O. When oxalic acid was added to the ferrous
ammonium sulphate solution, the production of a yellow FeC2O4 precipitate was seen in experiment
2.
Fe(NH4)2.6H2O + H2C2O4 → FeC2O4 [yellow precipitate] + … etc (Eq1)
When precipitate shifts colour from yellow to brown due to the addition of K2C2O4 and H2O2. The
precipitate-containing solution was then decanted, washed several times, and then boiled again with
potassium oxalate monohydrate. The brown colour derives from the creation of iron(III)hydroxide as
a result of the redox process that converts ferrous iron to ferric ion (Fe2+Fe3+), as shown in
equation 2. While the solution was boiling, oxalic acid was put into it until it was completely orange.
If the leftover residue is yellow, hydrogen peroxide can be administered gradually.
FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3 [brown precipitate] + … etc (Eq 2 & 3)
Fe(OH)3 + H2O2 + K2C2O4 → K3[Fe(C2O4)3].3H2 [clear green solution] +… etc (Eq 4)
To facilitate the precipitation of complex iron salt, alcohol was added and after the washing process,
the precipitate was then transferred to a pre-weighed labelled dry 50 ml beaker, stored in a sample
bottle to prevent exposure to any light source. The potassium tris(oxalato)ferrate(III)trihydrate
production is finished after this step. As a result, the mass of K3[Fe(C2O4)3] has increased
significantly. The actual production of 3H2O was 4,9822g, while the theoretical production was
6.2879g. The percent yield of experiment 2 was calculated, and the result was 79.23%.

CONCLUSION
In conclusion, the chemical potassium tris(oxalato)ferrate(III) can be produced and
standardised. Both of these experiments have shown positive results. The true mass achieved in
experiment 2 was 4.9822g, and the percentage yield of K3[Fe(C2O4)3 was 10%. The percentage of
3H2O was 79.23%.