SEM OCTOBER 2020 - FEBRUARY 2021

LABORATORY REPORT CHM361

ANALYSIS OF COORDINATION COMPOUND
K3[Fe(C2O4)3].3H2O

NAME : AINUN NUR ANNISA BINTI AZMI

STUDENT ID : 2019228728

GROUP : AS1205_4

CRITERIA FULL OBTAINED

Procedure 2%

Results / Data / Observation (Datasheet) 2%

Data Analysis / Justification / Validation 4%

Question 2%

Discussion 2%

Conclusion 1%

Format 2%

Data Sheet EXP 1 5%

Total 20%
 DATA SHEET

EXPERIMENT 1

Predicting Molecular Shape and Polarity Using VSEPR Theory

Name : Ainun Nur Annisa Binti Azmi

Student ID : 2019228728

RESULTS

Table 1: Molecular shape and polarity prediction using VSEPR theory

 EXPERIMENT 2&3

Analysis Of Coordination Compound K3[Fe(C2O4)3].3H2O

OBJECTIVES

i. To synthesis a coordination compound, potassium tris(oxalato)ferrate(III)

trihydrate under carefully controlled conditions.
ii. To standardize the potassium permanganate solution.
iii. To determine the percentage of ligands in K3[Fe(C2O4)3].3H2O.

INTRODUCTION

The preparation of new compound is one of the most important aspects of any
chemical research. This process is called synthesis. A chemical synthesis is the
application of one or more chemical reactions to bring about the construction of a
desired chemical product. In this experiment, a coordination compound will be
synthesized. The reason for carrying out a chemical synthesis varies depending on
the situation. The production might be of a useful substance found in nature that is
difficult to isolate or creation of a substance with new useful benefit. Regardless of the
purpose, the main focus is to maximize the conversion of reactants to products.

The process of determining the exact concentration of a solution is named as

standardization. The example of analytical procedure often used in standardization is
the titration where an exact volume of one substance is reacted with a known amount
of another substance. In this experiment, the potassium permanganate solution will be
standardized which will then use to determine the percentage of ligands in the
coordination compound.
APPARATUS

EXPERIMENT 2

Balance

125 mL Erlenmeyer flask

Measuring cylinder, 50 mL (2 pieces)

Beakers (100 mL, 3 pieces)

Beaker, 400 mL

Glass rod

Ice bath

Bunsen burner

Tripod stand

Thermometer

Buchner funnel

Vacuum filtration apparatus

Filter paper

EXPERIMENT 3

Part A

Balance

Beakers (two 100 mL, one 250 mL)

Volumetric flask (250 mL)

Storage bottle (250 mL)

Pipette (20 mL)

Pipette filler
Burette and stand

Filter funnel

Conical flask (250 mL)

Thermometer

Part B

Balance

Volumetric flask (250 mL)

Storage bottle (approximately 250 mL)

Pipette (20 mL)

Pipette filler

Burette and stand

Filter funnel

Conical flask (250 mL)

Thermometer

CHEMICALS

EXPERIMENT 2

Ferrous ammonium sulphate, Fe(NH4)2(SO4)2.6H2O

0.5 M oxalic acid, H2C2O4 (aq)

1 M potassium oxalate monohydrate, K2C2O4·H2O (aq)

3 M sulphuric acid, H2SO4

6% hydrogen peroxide, H2O2

Ethanol

1:1 ethanol/water solution

Deionised water

EXPERIMENT 3

Part A

Potassium permanganate solution, KMnO4 0.02 M (300 mL)

Oxalic acid, H2C2O4.2H2O, 0.05 M (250 mL)

Sulphuric acid, H2SO4, 2 M (250 mL)

Part B

Potassium permanganate solution, KMnO4 that has been standardised in Part A (300
mL)

Sulphuric acid, H2SO4 1 M (250 mL)

Complex compound, K3[Fe(C2O4)3].3H2O

PROCEDURES

EXPERIMENT 2

1. About 5 g of ferrous ammonium sulphate salt 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 precipitate 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 go below 40°C and not above 50°C during the addition of hydrogen
peroxide. Some brown precipitate of Fe(OH)3may 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. Stirring
stopped 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 preweighed, labelled dry 50 mL beaker. The
wash solutions were discarded.

EXPERIMENT 3

A. Standardisation of Potassium Permanganate Solution

1. A burette was filled with the 0.02M Potassium permanganate solution, KMnO4 to
be standardised.

2. 20 mL of the standard oxalic acid solution, H2C2O4.2H2O was pipette into a 250
mL conical flask and about 20 mL of 2M sulphuric acid, H2SO4 was added.

3. The solution in the conical flask was warmed to about 80°C

4. The 0.02M Potassium permanganate solution, KMnO4 was titrate against the oxalic
acid solution. The KMnO4 solution was added slowly or manganese (IV) oxide (a
brown solid) may form instead of manganese (II) ion. The end point was reached when
the addition of one drop permanganate solution produced a permanent pink color. The
results were recorded as rough estimation in a table shown below.

4. The steps and titration were repeated until consistent results were obtained. All data
were recorded.
B. Determination of the Percentage of Ligands in K3[Fe(C2O4)3].3H2O

1. About 0.20 g of the coordination compound that was previously prepared was
weighed out. The actual weight used were recorded.

2. The sample was boiled with 50 mL of 1 M sulphuric acid, H2SO4 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 as rough estimation in a
table shown below.

5. The steps and titration were repeated until consistent results were obtained. All data
were recorded.
DATA SHEET

EXPERIMENT 2

Synthesis of Potassium tris(oxalato)ferrate(III) trihydrate

Name : Ainun Nur Annisa Binti Azmi

Student ID :2019228728

RESULTS

1. Mass of Fe(NH4)2(SO4)2.6H2O used = 4 g

2. Moles of Fe(NH4)2(SO4)2.6H2O used = 0.0102 mol

3. Mass of K3[Fe(C2O4)3].3H2O obtained = 4.0715 g

4. Theoretical yield of K3[Fe(C2O4)3].3H2O (moles) = 0.0102 g

5. Theoretical yield of K3[Fe(C2O4)3].3H2O (mass) = 5.0106 g

6. Percent yield of K3[Fe(C2O4)3].3H2O = 81.26 %

Calculations

Question 2:

Moles of Fe(NH4)2(SO4)2.6H2O = 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐹𝑒(𝑁𝐻4)2(𝑆𝑂4)2. 6𝐻2𝑂

𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑓𝑜𝑟 𝐹𝑒(𝑁𝐻4)2(𝑆𝑂4)2. 6𝐻2𝑂

= 4.0044 𝑔
392.13 𝑔/𝑚𝑜𝑙

= 0.0102 mol of Fe(NH4)2(SO4)2. 6H2O

Question 3:

(Mass of filter paper + crystal) - Mass of filter paper = 4.5403 – 0.4688

= 4.0715 g

Question 4:

Fe(NH4)2(SO4)2. 6H2O + H2C2O4 → Fe2C2O4 + H2SO4 + (NH4)2(SO4) + 6H2O

(eq 1)

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

Moles of Fe2C2O4 = 0.0102 mol

FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3 + … etc (eq2)

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

Moles of Fe(OH)3 = 0.0102 mol

3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 → 2K3[Fe(C2O4)3].3H2O + 3H2O (eq3)

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

0.0102 mol Fe(OH)3 = 2 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐾3 [𝐹𝑒(𝐶2𝑂4)3].3𝐻2𝑂

2 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐹𝑒(𝑂𝐻)3

= 0.0102 mole of K3[Fe(C2O4)3].3H2O

Question 5:

Moles = 𝑚𝑎𝑠𝑠
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠

0.0102 moles = 𝑚𝑎𝑠𝑠

491.24 𝑔/𝑚𝑜𝑙

Mass = 0.0102 𝑚𝑜𝑙𝑒𝑠 × 491.24 𝑔/𝑚𝑜𝑙

Mass = 5.0106 g

Question 6:

Percent yield = 𝐴𝑐𝑡𝑢𝑎𝑙 𝑚𝑎𝑠𝑠 x 100%

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑐𝑎𝑙 𝑚𝑎𝑠𝑠

= 4.0715 𝑔 x 100%
5.0106 𝑔

= 81.26 %
EXPERIMENT 3

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

RESULTS

A. 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

B. 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 28.40 30.40

Initial burette reading (mL) 1.50 3.00 5.00

Vol. of KMnO4 used (mL) 24.30 25.40 25.40

Mean vol. of KMnO4 used (mL) 25.40

Questions
Part A

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

concentration of the KMnO4.

Vol of oxalic acid = 0.02L

Molarity of oxalic acid = 0.05M
Vol of KMnO4 = 0.0211L

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

𝑉𝑜𝑙 𝑜𝑓 KMnO4 x Molarity of KMnO4 = 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 KMnO4

𝑉𝑜𝑙 𝑜𝑓 Oxalic Acid x Molarity of Oxalic Acid 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑

0.0211𝐿 x Molarity of KMnO4 = 2

0.02𝐿 x 0.05M 5

Molarity of KMnO4 (concentration) = 0.0190M

2. Why is it necessary to heat the oxalic acid solution?

It is necessary to heat oxalic acid solution because without heating it is a slow process.
An energy is required to be greater than the activation energy for a reaction. So, in
order to increase the energy, temperature must be increased. And the best way to
increase the temperature is 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. Oxalic acid can be used as a primary standard because it is highly pure, stable
and does not change its concentration with environmental factors. In chemistry, a
primary standard is a reagent that is very pure, stable, and not hygroscopic. Oxalic
acid therefore does not absorb any moisture from the air which makes it suitable to be
a primary standard.
Part B

Given that MnO4− ion is being reduced to Mn2+ ion, and C2O4 2− ion is being
oxidized to CO2, by this redox equation.

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.

Titration 1:
Moles of MnO4- = (Molarity KMnO4 (mol/L)) (Volume of KMnO4(L))
= 4.826 x 10-4 mol MnO4-

6 moles of MnO4- = 5 moles of Fe(C2O4)3-

Thus, mol Fe(C2O4)3- = 4.826 x 10-4 mol MnO4- x 5 mol Fe(C2O4)3-
6 mol of MnO4-
= 4.02167 x 10-4 mol Fe(C2O4)3-

1 mol of Fe(C2O4)3- contain 3 mol C2O42-

Mol C2O42- = 4.0217 x 10-4 mol Fe(C2O4)3- x 3 mol C2O42-
1 mol Fe(C2O4)3-
= 1.20651 x 10-3 mol C2O42-

Mass of (C2O4)3- = 1.20651 x 10-3 mol (C2O4)3- x 88 g/mol

= 0.106172g

%w/w = 0.106172g x 100

0.2006g
= 52.93%
Since the result of titration 1 and 2 is the same, the calculation above stays constant.
However, titration 1 and 2 uses different mass of sample.

Titration 2:
%w/w = 0.106172g x 100
0.2008g
= 52.87%

Average %w/w = 52.93+52.87

2
= 52.9%

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

Theoretical value C2O42- = 88.02 g/mol x 3 x 100%

491.25
= 53.75%

% error = | actual value – theoretical value | x 100

theoretical value
= | 52.90 – 53.75 | x 100
53.75
= 1.58%
3. Calculate the percentage purity of the complex.

5 mol Fe(C2O4)33- = 6 mol MnO4-

Therefore, mol Fe(C2O4)33- = 4.862 x 10-4 mol MnO4- x 5 mol Fe(C2O4)33-
6 mol MnO4-
= 4.0217 x 10-4 mol Fe(C2O4)33-

Mass = 4.0217 x 10-4 mol x 491.25 g/mol

= 0.1976 g

% Purify titration 1= 0.1976g x 100 = 98.50%

0.2006g

% Purify titration 2= 0.1976g x 100 = 98.41%

0.2008g

Average % purify = 98.50+98.41 = 98.46%

2
DISCUSSION
In experiment 2, the objective of the experiment is to synthesis the coordination
compound, potassium tris(oxalato)ferrate(III) trihydrate. This experiment was
conducted under a carefully regulated condition following the synthesize procedure.
The predicted final product obtained was K3[Fe(C2O4)3].3H2O. For experiment 3, a
redox titration technique was conducted. Redox titration was based on the oxidation-
reduction reaction between the titrant and the analyte. During the observation in
experiment 2, when oxalic acid was added into the ferrous ammonium sulphate
solution, the formation of yellow precipitate of FeC2O4 was captured.

Fe(NH4)2.6H2O + H2C2O4 → FeC2O4 [yellow precipitate] + … etc (Eq1)

Then, precipitate shifts colour from yellow to brown due to the addition of
K2C2O4 and H2O2. The precipitate-containing solution was decanted, washed
several times and added with potassium oxalate monohydrate. Then, it was heated
again. The brown colour comes from the formation of iron(III)hydroxide due to the
redox reaction that oxidises ferrous iron to ferric ion (Fe 2+→Fe3+), the final reaction is
in equation 2. Oxalic acid was poured into the solution as it was on the hot plate and
the colour changes to green.

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 green crystal was then transferred to a petri dish. After this
process, the potassium tris(oxalato)ferrate(III)trihydrate synthesis is completed. As a
result, the mass of K3[Fe(C2O4)3].3H2O obtained was 4.0715 g while the theoretical
production was 5.0106 g. The percent yield of experiment 2 was determined and the
value of 81.26% was obtained.

In experiment 3, the percentage of ligands of potassium

tris(oxalato)ferrate(III)trihydrate was calculated using the standardisation process. In
part A, the standardisation method started with the standardisation of potassium
permanganate with a standard solution of oxalic acid. The KMnO4 solution was filled
in the burette and the oxalic acid was pipetted and applied to the conical flask along
with 20 mL of H2SO4. After heating, titration between KMnO4 and oxalic acid was
conducted. When one drop of permanganate solution is added to a permanent pink
colour, the end point is reached and recorded. Standardized KMnO4 was obtained by
the end of Part A.

In part B, 0.2006g of K3[Fe(C2O4)3].3H2O from the previous experiment was

weighted. The sample was boiled in a conical flask with sulphuric acid. After cooling,
the KMnO4 was titrated, which was standardized in Part A. The end point was
calculated when one drop of the permanganate solution transforms into a pink colour
of the solution. This happens when there is no oxalic acid left to eliminate the MnO4-
ion in the solution. As a result, the percentage by weight of oxalate ions in the complex
obtained was 52.9% while the theoretical value was 53.75%. Finally, the percentage
of purity obtained was 98.46 %.

While conducting both experiment 2 and experiment 3, there were several precautions
that must be taken care of in order to reduce error and unwanted injuries. Firstly, both
chemical compounds are poisonous. Chemical solvents are easily flammable and can
cause irritation to body tissues and the respiratory tract. Thus, it is important to wear
personal protective equipment (PPE) and to handle the chemical in the optimum
environment. Next, the acids are very corrosive. So, work should be done with extra
caution and wear protective goggles. For further protection, ensure to clean both
hands well with soap and water before leaving the laboratory. Other precautions that
must been taken care is while heating the solution of ferrous ammonium sulphate and
solution of oxalic acid dihydrate since it will bump. Lastly, beware of temperature (at
least 40°C) of solution when add H2O2 into the solution.
CONCLUSION
In conclusion, potassium tris(oxalato)ferrate(III) compound was synthesized
and potassium permanganate solution was standardized. The objective of both of
these experiments were achieved. For experiment 2, the real mass obtained was
4.0715 g and the percentage yield of K3[Fe(C2O4)3].3H2O was 81.26%. On the other
hand, in experiment 3, the percentage by weight of oxalate ions in the complex was
equivalent to 52.9% with 1.58% of error. The percentage of purity was 98.46%. In short,
the experiment was successful.

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https://phdessay.com/lab-report-2/

Chapter 8.09: Quantitative analysis using titration. (2020, August 11). Chemistry
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https://chem.libretexts.org/Courses/Howard_University/General_Chemistry%3A_An_
Atoms_First_Approach/Unit_3%3A_Stoichiometry/Chapter_8%3A_Aqueous_Solutio
ns/Chapter_8.09%3A__Quantitative_Analysis_Using_Titration

Hoang, V. D. (2017). Advances in titration techniques. BoD – Books on Demand.

Gopalan, R. (2009). Inorganic chemistry for undergraduates. Universities Press.