CHM361

INORGANIC CHEMISTRY
LABORATORY REPORT

Experiment No. : 2&3

Title : TRIS(OXALATO)FERRATE(III) TRIHYDRATE

(K3[FE(C2O4)3].3H2O) AND DETERMINATION
OF THE PERCENTAGE OF LIGANDS IN
K3[FE(C2O4)3].3H2O)

Name : NOR IFTIHA BINTI ABDUL AZIZ

No. Matric : 2019217292

Program / Group : RAS1205E

Date of Experiment : 01/11/2021 & 08/11/2021

Lecturer : MISS NUR SYAZANA BINTI NAZERI

Submission Date : 12/01/2022

 EXPERIMENT 2

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

1.0 OBJECTIVE
To synthesis a coordination compound, potassium tris(oxalate)ferrate(III) trihydrate under
carefully controlled conditions.

2.0 INTRODUCTION

Synthesis is the useful technique in all areas of chemistry. As we know, this technique is very
important because it is the basic of developing new compounds which is coordination
compounds. This is also useful for animal and vegetation. In the pharmaceutical industry,
introduction of new and less pesticides are made as well as possible because all the chemicals
involved being synthesised and tested in the laboratory. Moreover, there a lot of chemical
compounds used in our daily life are synthesised from simple materials.

Coordination compound is a compound that have a central metal ion chemically bound by a
coordinate covalent bond to one or more atoms which known as ligands. Therefore, potassium
tris(oxalato)ferrate(III) trihydrate is a metal complex of iron that consists a three oxalate ions
C2O42- acting as ligands were bonded to every central atom. These ligands that bond to central
atom at two different places. Thus, it has a chemical compound with the formula
K3[Fe(C2O4)3].3H2O. The two structure of K3[Fe(C2O4)3].3H2O can be see through the figure 1
above.

For experiment 2, to synthesis the compound K3[Fe(C2O4)3].3H2O whereas by adding a ferrous

ammonium sulphate with oxalic acid. This reaction will form an iron (II) oxalate FeC2O4 which
is the yellow precipitate. Then, potassium oxalate K2C2O4 and hydrogen peroxide was added.
At the end of the technique, the final product was formed.
3.0 PROCEDURE

1. 5 g of ferrous ammonium sulphate was weighed out. The actual weight used was
recorded. Then, it was put into a 125 ml Erlenmeyer flask. The compound was
dissolved with 15 ml of distilled water and was added with 5 drops of 3 M sulphuric
acid.
2. 50 ml of 0.5 M oxalic acid was added to the solution and was heated to boil where it
was stirred constantly to prevent bumping.
3. The Erlenmeyer flask was removed from the heat and the yellow precipitate of FeC2O4
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 participate
was allowed to settle; it was decanted and washing was repeated once more.
4. 20 ml of 1M K2C2O4 was added to the precipitate, it was stirred and heated to 40˚C.
While temperature was at 40˚C, 10 ml of 6% H2O2 drop wise was immediately added
and was stirred continuously. Make sure the temperature did not went below 40˚C and
not above 50˚C during the addition of hydrogen peroxide. Some brown precipitate of
Fe(OH)3 may have formed at that time.
5. The resulting solution was heated to boil. 20 ml of 0.5 M H2C2O4 was added all at once
while maintaining the temperature near boiling. The solution should have been turned
to clear green. If some brown residue remained, 0.5 M H2C2O4 was added drop wise
while the solution was boiling, until it turns clear green. However, if the remained
residue was yellow, it was probably unreacted FeC2O4 and more H2O2 should be
added carefully.
6. If the solution was cloudy, gravity filter it into a clean 125 ml Erlenmeyer flask. If it was
clear, no filtration was necessary. Then while swirling constantly, 15 ml of ethanol was
slowly added to the solution. It was allowed to cool in an ice bath and the solution was
slowly stirred until crystals began to form. Stop stirring and the solution was allowed to
stand in the ice bath for 20 minutes. A good crop of crystals should have been formed
before the solution was 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 1:1 ethanol/water solution was added. Wait for
30 seconds and 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 reweighed labelled dry 50 ml beaker. The wash
solution was discarded.

4.0 RESULTS AND CALCULATION

DATA SHEET

EXPERIMENT 2

Name : Nor Iftiha binti Abdul Aziz

Student ID : 2019217292
Date of Experiment : 01 November 2021
Synthesis of Potassium tris(oxalato)ferrate(III) trihydrate

RESULTS

1. Mass of Fe(NH4)2(SO4)2.6H2O used = 4.0044 g

2. Moles of Fe(NH4)2(SO4)2.6H2O used = 0.01021 mol
3. Mass of K3[Fe(C2O4)3].3H2O obtained = 4.0715 g
4. Theoretical yield of K3[Fe(C2O4)3].3H2O (moles) = 0.01021 mol
5. Theoretical yield of K3[Fe(C2O4)3].3H2O (mass) = 5.0156 g
6. Percent yield of K3[Fe(C2O4)3].3H2O = 81.18%

Calculations
Show all your calculations.

Question 2:
𝑚𝑎𝑠𝑠 𝑜𝑓 Fe(NH4)2(SO4)2.6H2O
Moles of Fe(NH4)2(SO4)2.6H2O = 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑓𝑜𝑟 Fe(NH4)2(SO4)2.6H2O
4.0044 𝑔
= 392.13 𝑔/𝑚𝑜𝑙

= 0.01021 moles of Fe(NH4)2(SO4)2.6H2O

Question 4:
Fe(NH4)2(SO4)2.6H2O + H2C2O4 → FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O – 1

1 mole of Fe(NH4)2(SO4)2.6H2O = 1 mole FeC2O4

So, mole of FeC2O4 is 0.01021 mole

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

1 mole of FeC2O4 = Fe(OH)3

So, mole of Fe(OH)3 is 0.01021 mole

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

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

So,

2 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 K3[Fe(C2O4)3].3H2O
0.01021 mole Fe(OH)3 = 2 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 Fe(OH)3

= 0.01021 mole of K3[Fe(C2O4)3].3H2O

Question 5:
Formula for moles,
Moles = mass/molar mass
So,
𝑚𝑎𝑠𝑠
0.01021 moles = 491.24 𝑔/𝑚𝑜𝑙

Mass = 0.01021 moles × 491.24 g/mol

= 5.0156 g

Question 6:
𝐴𝑐𝑡𝑢𝑎𝑙 𝑚𝑎𝑠𝑠
Percent yield of K3[Fe(C2O4)3].3H2O = 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 × 100%
4.0715 𝑔
= 5.0156 𝑔 × 100%

= 81.18%
6.0 DISCUSSION

In experiment 2, we can see the point of this experiment is to synthesis of the formation of
new compound called coordination compound involves potassium tris(oxalato)ferrate(III)
trihydrate under a carefully balanced conditions. So, the Synthesize method had been used
in this experiment to complete our main objective, whereas the final product that we obtained
was K3[Fe(C2O4)3].3H2O. This synthesis processing mostly used in many chemical
researches. At the same time, this process also involves the number of chemical reactions.
Therefore, the potassium tris(oxalato)ferrate(III) trihydrate was being synthesized by two
processes. The first reaction involves which the ferrous ammonium sulphate salt dissolving in
excess oxalic acid. So, for the process result in the isolation of iron (II) oxalate, Fe2C2O4 was
formed the yellow participate.

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

After that, the compound is being heated for ensuring dehydration and isolation all the iron
became a ferrous oxalate. When all the yellow precipitate confirmed settle, the decantation of
the supernatant is performed. For this step mostly to make sure in removing more oxalic acid
and improved the purity of precipitate.

For the second process potassium tris(oxalato)ferrate(III) trihydrate was formed after addition
of chemicals potassium oxalate, hydrogen peroxide and oxalic acid. In the first step, iron
complex was heating with potassium oxalate then being continuous stirring to prepare a well
mixture suspension for complete the next step which is oxidation. Second, during the addition
of H2O2, we must keep the solution at temperature 40˚C for make sure the iron oxidise in the
suspended particles from ferrous to ferric. Another than that, since they are solid tiny crystals
so they only react between their surface area. Starring for a minutes also being need here.
This step completely dissolves the yellow precipitate. At this moment, a brown precipitate of
Fe(OH)3 forms and is hard to dissolve. This situation will affect the yield as not all the ferric
iron is accessible to make the ferric oxalate molecular anion for produce the clear green
crystals. For addition of potassium oxalate and hydrogen peroxide has appeared, the equation
involved in

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

[Reduction / 2 electrons gained] H2O + HO2− + 2e− → 3OH−
[Overall net reaction] 2Fe2+ + H2O + HO2− → 2Fe3+ + 3OH−
Because of the high concentration of OH− ion brown precipitate was formed. That why the
more oxalic acid had been added to dissolve the brown precipitate so soluble complex was
formed. The full equation is above
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 → 2K3[Fe(C2O4)3].3H2O + 3H2O
At the end, after crystallization, a clear green crystal was formed. Moreover, from this the
actual yield we could get by a weighting. The theoretical yield is calculated by using the
number moles of product from the limiting reactant which is 5.0156 g. Last but not least, the
percentage yield obtained from the formula of
𝐴𝑐𝑡𝑢𝑎𝑙 𝑚𝑎𝑠𝑠
Percent yield of K3[Fe(C2O4)3].3H2O = × 100%he
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠

The percentage yield that we got in this experiment is 81.18%.

8.0 CONCLUSION

In conclusion, the potassium tris(oxalato)ferrate(III) trihydrate compound can be synthesized

by a standardization method. The results from this experiment are obtained. For experiment
2, the real mass obtained was 4.0715g and the percentage yield of K3[Fe(C2O4)3].3H2O was
81.18%. From this experiment, I learned how to understand about the technique of synthesis
the coordination compound with the carefully controlled conditions. I also know how to
prepared the vacuum filtration apparatus in the right way. Even though, this process I think is
very completed but from this I have study a lot of especially for control the complex chemicals
and apparatus to make sure our results that obtained is correct.

8.0 REFERENCES

1. lab manual chm361

2. Chemistry Lab Skills: Synthesis of Potassium Ferrioxalate video. Retrieved from
https://www.youtube.com/watch?v=bOvnCpgFRzg
3. https://www.sciencedirect.com/science/article/pii/B9780444635914000082
4. https://www.chem.wilkes.edu/~mencer/pdf_docs/Coord_Cmpd_Pres.pdf
 EXPERIMENT 3
Determine of The Percentage of Ligands in K3[Fe(C2O4)3].3H2O

1.0 OBJECTIVE

1. To standardize the potassium permanganate solution.

2. To decide the percentage of ligands in K3[Fe(C2O4)3].3H2O

2.0 INTRODUCTION

Standardisation of the potassium permanganate KMnO4 solution is carried out by a titration

process. It is not a primary standard so it can be standardized by using the sodium oxalic
oxalate or oxalic acid. Hence, the oxalic acid had been known as a good primary standard
which is because this compound state in a solid form, as H2C2O4.2H2O. Other than that, this
compound also can be prepared at the very high temperature of purity and is not hygroscopic
or efflorescent. Then, this reaction also occurs in this experiment are oxidation and reduction
reaction. An oxidation-reduction reaction is a reaction in which the electrons transferred
between species or in which atoms change oxidation numbers. Oxidation is the half reaction
in which there is loss of electrons by a species or increase the oxidation number of atom.
Therefore, reduction is the half reaction in which there is a gain of electrons by a species or
decrease of oxidation number an atom. So, reactions involved in this reaction is:

Reduction: 2(MnO4− + 5e− + 8H+ → Mn2+ + 4H2O)

Oxidation: 5(H2C2O4 → 2CO2 + 2e− + 2H+)

Overall reaction:
2MnO4− (aq) + 6H+ (aq) + 5H2C2O4 (aq) → 2Mn2+ (aq) + 8H2O (l) + 10CO2 (g)

3.0 PROCEDURE

A. standardisation of potassium permanganate solution

1. A burette was filled with KMnO4 solution to be standardised.

2. 20 ml of the standard oxalic acid solution was pipette into a 250 ml conical flask and
about 20 ml of 2M H2SO4 was added.
3. The conical flask was warmed to about 80˚C and the permanganate solution was
titrated against the oxalic acid solution. The 0.02 M KMnO4 solution was added slowly
and the solution was shaked as well. The end point was reached when the addition of
one drop permanganate solution produced a permanent pink color. The results were
recorded in the table shown below.
4. The titration was repeated until consistent results were derived.
B. determination of the percentage of ligands in K3[Fe(C2O4)3].3H2O

1. 0.20 g of the coordination compound that was previously prepared was weighed out.
2. The sample was boiled with 50 ml of 1 M sulphuric acid in a conical flask.
3. The solution was allowed to cool to 60˚C and was titrated slowly with the KMnO4
solution provided (KMnO4 that was standardised in part A).
4. The end point was reached when the addition of one drop of permanganate solution
produced a permanent pink color. The results were recorded in a table shown below.
5. The titration and steps was repeated again until consistent results were obtained.

4.0 RESULTS AND CALCULATIONS

EXPERIMENT 3

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

RESULTS

1. Standardisation of Potassium Permanganate Solution

Rough Accurate titrations

estimation 1 2
Final burette reading (mL) 22.20 43.30 21.20
Initial burette reading (mL) 0.30 22.20 0.10
Vol. of KMnO4 used (mL) 21.90 21.10 21.10
Mean vol. of KMnO4 used (mL) 21.10

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

Rough Accurate titrations

estimation 1 2
Mass of K3[Fe(C2O4)3].3H2O (g) 0.2013 0.2006 0.2008
Final burette reading (mL) 25.80 28.4 30.40
Initial burette reading (mL) 1.50 3.00 5.00
Vol. of KMnO4 used (mL) 24.3 25.4 25.4
Mean vol. of KMnO4 used (mL) 25.4
Calculations

Part A

𝑠𝑢𝑚 𝑜𝑓KMnO4 used

Mean vol. of KMnO4 used (ml) = 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡𝑖𝑡𝑟𝑎𝑡𝑖𝑜𝑛

𝟐𝟏.𝟏𝟎 𝒎𝒍+𝟐𝟏.𝟏𝟎 𝒎𝒍
=
𝟐

= 21.10 ml

Part B

25.4 𝑚𝑙+25.4 𝑚𝑙
Mean vol. of KMnO4 used (ml) = 2

= 25.4 ml

5.0 QUESTION

Part A

1. From the average volume of KMnO4 solution used, calculate the concentration of the
KMnO4.

Vol. of oxalic acid = 20 ml

Molarity of oxalic acid = 0.05 M
Vol. of KMnO4 = 21.10 ml

𝑀1𝑉1 𝑎
In titration, 𝑀2𝑉2
=𝑏

2KMnO4 + 3H2SO4 + 5H2C2O4.2H2O→ K2SO4 + 2MnSO4 + 18 H2O + 10CO2

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 KMnO4 ×𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 KMnO4 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 KMnO4

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 Oxalic acid× Volume 𝑜𝑓 𝑂𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑐
= 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑂𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑

(𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 KMnO4 ×21.10 𝑚𝑙) 2

(0.05 𝑀 × 20 𝑚𝑙)
=5

Molarity of KMnO4 = 0.01896 M

(concentration)
2. Why is it necessary to heat the oxalic acid solution?
Yes. Since the reaction between permanganate and oxalate without heating is very
slow process as energy greater than activation, energy is more require for the reaction.
Thus, in order to increase energy, temperature must be increased where by heating
the oxalic acid solution.

3. In this experiment oxalic acid is used as a reducing agent. Could oxalic acid be used
as a primary standard to standardise a solution of a base, such as sodium hydroxide?
Explain your answer.
Yes. It is because the compound is available in solid form and it also can be prepared
at very high degree of purity. Then, the process of titration reaction is quantitatively
consistent, so the end of point reached is very sharp. Moreover, this oxalic acid dose
not absorb any moisture from the air at all, then does it lose the water through
evaporation.

Part B

Given that MnO4− ion is being reduced to Mn2+ ion, and C2O42− ion is being oxidized to CO2,
by this redox reaction.

Oxidation 5[Fe(C2O4)33- → Fe3+ + 6CO2 + 6e− ]

Reduction 6[MnO4− + 5e− + 8H+ → Mn2+ + 4H2O]
Overall reaction: 5Fe(C2O4)33- + 6MnO4 − + 48H+→ 5Fe3+ + 6Mn2+ + 30CO2 + 24H2O

1. Calculate the percentage by weight of oxalate ions in the complex.

Moles of MnO4− = Concentration (M) × Volume (L)
1𝐿
= 0.01896 M × 25.4 ml ÷ 1000 𝑚𝐿

= 4.81584 × 10-4 mole MnO4−

6 moles of MnO4− = 5 moles of Fe(C2O4)33-

5 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 Fe(C2O4)33−
= 4.81584 × 10-4 mole of MnO4− × 6 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 MnO4−

= 4.0132 ×10-4 mole of Fe(C2O4)33-

 In 1 mole Fe(C2O4)33- have 3 mole oxalate ion,
3 𝑚𝑜𝑙𝑒 C2O42−
So, mole of C2O42− = 4.0132 ×10-4 mole Fe ×
1 𝑚𝑜𝑙𝑒 Fe(C2O4)33−

= 1.20396 ×10-3 mole C2O42−

Mass of C2O42− = 1.20396 ×10-3 mole C2O42− × 88.02 g/mol
= 0.10597 g C2O42−
0.10597 𝑔
% w/w = 0.2006 𝑔
× 100%

= 52.83%
So, percentage by weight of oxalate ions is 52.83%

2. Calculate the theoretical value of oxalate ions in the complex.

88.02 𝑔 𝑚𝑜𝑙 × 3
Theoretical value of C2O42− = 491.25 𝑔 𝑚𝑜𝑙 K3[Fe(C2O4)3].3H2O × 100%

= 53.75%

3. Calculate the percentage purity of the complex.

0..10597 𝑔
= (0.2006 𝑔+0.2008 𝑔)/ 2 × 100%

= 52.80 %

6.0 DISCUSSION

In the experiment 3, the percentage of Ligands in K3[Fe(C2O4)3].3H2O were calculated by using

standardisation process. First, this process of standardisation started by adding potassium
permanganate with the standard oxalic acid solution. We can see through Part A, the KMnO4
solution was filled in the burette then the oxalic acid was pipetted and put into a conical flask.
After that, 20 ml of sulphuric acid was added to the flask. After the heating, titration between
potassium permanganate and oxalic acid were obtained. As soon as one drop of KMnO4
solution added, the permanent pink color appeared, the end of point is reached and being
recorded in table shown. Standardisation process was succeed after repeated.
For Part B, 0.20 g of K3[Fe(C2O4)3].3H2O was weighed, it was take from the final product in
the experiment 2. This sample was boiled in the conical flask that have sulphuric acid, H2SO4.
Then, after the cooling, potassium permanganate was titrated same as the process in Part A.
therefore, the end of point being calculated when one drops of KMnO4 solution turn to a
permanent pink color. This situation said there is no oxalic acid left to react with MnO4− ion in
the solution. As for overall reaction in titration shown in below.
Reduction: 2(MnO4− + 5e− + 8H+ → Mn2+ + 4H2O)
Oxidation: 5(H2C2O4 → 2CO2 + 2e− + 2H+)

Overall reaction: 2MnO4− + 6H+ + 5H2C2O4 → 2Mn2+ + 8H2O + 10CO2

The results, concentration of KMnO4 solution was obtained whereas 0.01896 M. The
percentage by weight of oxalate ions is 52.83% and last for the percentage of purity we got
52.80%.

I think there a few of precautions that we must take note when prepared of this experiment,
First, all the chemicals compound was toxic. These chemicals will be easy to cause the
irritation to your body. So, we must extra prepared especially work with wear the safety
googles. Please make sure after this, you must wash hand thoroughly with soup after leaving
the laboratory.

7.0 CONCLUSION

In conclusion, the objective of the experiment in determination of the percentage of Ligands

in K3[Fe(C2O4)3].3H2O was obtained. In the experiment 3, the concentration that was measure
KMnO4 was 0.01896 M. The ratio of oxalate ions is 0.0035 g and last for the percentage of
purity we got 1.74%. Through this experiment, I understand about the concept of
standardisation process. then, I also know how to prepared the titration in the correct way and
if we cannot drop the potassium permanganate solution in well, our results will be not accreted
Moreover, in this experiment, we finally get a permanent pink solution after a process titration.

8.0 REFERENCES

1. Lab manual CHM361

2. Determination of concentration of KMnO4 solution using the oxalic acid - MeitY
OLabs video. Retrieved from https://www.youtube.com/watch?v=HDUd4KqBKa8
3. https://corporatefinanceinstitute.com/resources/knowledge/economics/standardiz
ation/
JOTTER EXPERIMENT 2
JOTTER EXPERIMENT 3