UNIVERSITI TUNKU ABDUL RAHMAN

FACULTY OF SCIENCE

BACHELOR OF SCIENCE (HONS) CHEMISTRY

YEAR 1 TRIMESTER 1

UDEC1224 CHEMISTRY LABORATORY II

Name Chan Yong Li

Student ID No. 19ADB04214

Name of Lab Partners 1. Foo Yu Cheng (18ADB02613)

2. Loo Xin Tong (19ADB02955)

Practical Group P3

Practical Sub-group G3

No. of Experiment Experiment 1

Title of Experiment Standardization of Potassium Permanganate Solution by an

Iron (II) Salt

Date of Experiment 10th June 2019

Date of Submission 17th June 2019

Name of Lecturer Dr Ooi Zhong Xian

1.0 Title
Standardization of Potassium Permanganate Solution by an Iron (II) Salt

2.0 Objectives
1. To standardize potassium permanganate solution by an iron (II) salt.
2. To calculate the molarity of the ammonium iron (II) sulphate solution prepared.
3. To determine the molarity of the potassium permanganate solution, KMnO4.
4. To understand the definition of primary standard.
5. To define redox titration.

3.0 Results
Part A: Preparation of a Standard Ammonium Iron (II) Sulphate Solution (0.1M)

Mass of ammonium iron (II) sulphate used = 3.9010 g

Part B: Standardization of Potassium Permanganate Solution

Titration number 1 2 3
Initial volume of burette (cm3) 0.00 21.80 20.00
Final volume of burette (cm3) 21.80 43.60 41.60
Total volume of KMnO4 used (cm3) 21.80 21.80 21.60

( 21.80+21.80+21.60 ) cm 3
Average volume of KMnO4 required for titration =
3
= 21.73 cm3

4.0 Calculations
Part A: Preparation of a Standard Ammonium Iron (II) Sulphate Solution (0.1M)

Mass of ammonium iron (II) sulphate used = 3.9010 g

Molar mass of ammonium iron (II) sulphate = 392.14 g/mol

Mass
Number of moles of ammonium iron (II) sulphate =
Molar mass
3.9010 g
=
392.14 g /mol
= 0.009948 mol

Number of moles
Molarity of ammonium iron (II) sulphate =
Volume
0.009948 mol
=
0.100 L
= 0.09948 M
≈ 0.1 M

Part B: Standardization of Potassium Permanganate Solution

Considering the equation of the reaction:

MnO4- + 8 H+ + 5 Fe2+ → Mn2+ + 5 Fe3+ + 4 H2O

From this equation, 1 mole of MnO4- reacts with 5 moles of Fe2+.

Number of moles of Fe2+ present in the conical flask = Molarity × Volume

= 0.09948 M × 0.025 L
= 0.002487 mol

Ratio of MnO4- to Fe2+ (according to the equation) 1 mol :5 mol

Ratio of MnO4- to Fe2+ (according to the experiment) x mol :0.002487 mol
Let: x = Number of moles of MnO4-

(0.002487 mol)(1 mol)

Number of moles of MnO4-, x =
5 mol
= 0.0004974 mol

Number of moles
∴ Molarity of potassium permanganate =
Volume
0.0004974 mol
=
0.02173 L
= 0.02289 M
≈ 0.02 M

5.0 Discussion
This experiment was an example of redox titration. Ammonium iron (II) sulphate
solution was used as an analyte while potassium permanganate solution was acted as a titrant.
The experiment undergoes a process called standardization as the potassium permanganate
solution was standardized by the ammonium iron (II) sulphate solution. Standardization was
done to determine the exact concentration of the potassium permanganate solution. Potassium
permanganate is a versatile and powerful oxidant that can be used to determine many
substances by direct or indirect titration (Ricca Chemical Company, 2018). However, in this
experiment, the concentration of the potassium permanganate solution was the one to be
determined.

The analyte (ammonium iron (II) sulphate solution) was titrated with potassium
permanganate solution. When the solution turned pale pink, it indicates that the potassium
permanganate solution is in excess. At this point, all the iron (II) ions have fully reacted with
the potassium permanganate solution which was added before the endpoint. The equation of
the reaction is as follows:

2 KMnO4 + 8 H2SO4 + 10 FeSO4 → K2SO4 + 2 MnSO4 + 5 Fe2(SO4)3 + 8 H2O

Besides, titrations with permanganate solution must be carried out in a strong acid
solution. Sulphuric acid is generally used during titrations with permanganate solution to
increase the concentration of hydrogen ions in the solution (Edwardsville High School,
2015). Unlike sulphuric acid, nitric acid and hydrochloric acid may involve in competing for
the oxidation-reduction reactions, which in turn results in reducing the accuracy of the
titration. If the titration was done in a neutral- or alkaline-conditioned solution, instead of
reducing the purple-coloured MnO4- ions to colourless Mn2+ ions, brown precipitate would
form (Chemistry Stack Exchange, 2018). The brown precipitate formed will be MnO 2 due to
the presence of brown-coloured Mn4+ ions. The equation is as follows:

MnO4- + 4 H+ + 3 e- → MnO2 + 2 H2O

In this experiment, the primary standard solution, ammonium iron (II) sulphate
solution was prepared and titrated with potassium permanganate solution to determine the
concentration of the potassium permanganate solution. The molarity of the ammonium iron
(II) sulphate solution prepared from this experiment was 0.09948 M and was approximate to
0.1 M while the molarity of the potassium permanganate solution determined from this
experiment was 0.02289 M and was approximate to 0.02 M.

Iron (II) sulphate crystals, FeSO4.7H2O cannot be used for standardization because the
salt is rendered impure by efflorescence and by atmospheric oxidation to form a brown basic
sulphate result of a reaction of the following type:

12 FeSO4 + 3 O2 + 6 H2O → 4 [Fe(OH)3.Fe2(SO4)3]

The salt, ammonium iron (II) sulphate, Fe(NH4)2(SO4)2.6H2O, is free from these
disadvantages and can be obtained in a high state of purity. In solution, it reacts freely as iron
(II) ion, sulphate ion and ammonium ion while only the iron (II) ion reacts with the
permanganate ion, MnO4-.

In addition, ammonium iron (II) sulphate solution was used as a primary standard due
to its stability and its availability in a highly pure form. Unlike ammonium iron (II) sulphate,
potassium permanganate solution cannot be obtained in a very pure form as it reacts readily
with any reducing substances or even with any organic compounds. Moreover, it is a
photosensitive compound (Ullah, 2017). Hence, potassium permanganate is not suitable to be
used as a primary standard.

Questions
1. Calculate the molarity of the potassium permanganate, KMnO4.

Considering the equation of the reaction:

MnO4- + 8 H+ + 5 Fe2+ → Mn2+ + 5 Fe3+ + 4 H2O

From this equation, 1 mole of MnO4- reacts with 5 moles of Fe2+.

Number of moles of Fe2+ present in the conical flask = Molarity × Volume

= 0.09948 M × 0.025 L
= 0.002487 mol

Ratio of MnO4- to Fe2+ (according to the equation) 1 mol :5 mol

Ratio of MnO4- to Fe2+ (according to the experiment) x mol :0.002487 mol

Let: x = Number of moles of MnO4-

(0.002487 mol)(1 mol)

Number of moles of MnO4-, x =
5 mol
= 0.0004974 mol

Number of moles
∴ Molarity of potassium permanganate =
Volume
0.0004974 mol
=
0.02173 L
= 0.02289 M
 ≈ 0.02 M

2. What is a primary standard?

A primary standard is made from a solid which can be obtained 100% (almost) pure. For
instance, a solution of approximately known concentration is made and used as a primary
standard against a solution which will be standardized. The solution made from a primary
standard is called a standard solution (Ramsden, 2000).

3. Define ‘redox’ titration.

Redox titration is a type of titration that determines the concentration of an unknown
solution (analyte) that contains either an oxidizing or reducing agent. It is based on a
redox reaction between the analyte and titrant, where the analyte is the substance to be
analysed and the titrant is the standardized solution (Lumen, n.d.).

6.0 Precaution steps

1. Sulphuric acid (strong acid) must be added into the conical flask instead of hydrochloric
acid or nitric acid so that the results obtained will be more accurate.
2. Fill in the burette with distilled water and test for absence of leaks from the tip and
stopcock.
3. Rinse the burette with small portions of the titrant solution before the experiment to
prevent dilution of the titrant solution.
4. When setting up the burette, place the burette to a vertical position to reduce parallax
error and make the reading more accurate.
5. Wash the sides (walls) of the conical flask (during the titration) with distilled water to
ensure all of the potassium permanganate solution (added from the burette) has reacted
with the ammonium iron (II) sulphate solution.

7.0 Conclusion
The molarity of the ammonium iron (II) sulphate solution prepared from this
experiment was 0.09948 M and was approximate to 0.1 M while the molarity of the
potassium permanganate solution determined from this experiment was 0.02289 M and was
approximate to 0.02 M.

8.0 References
Chemistry Stack Exchange, 2018. What role does sulfuric acid play in the titration of oxalic
acid and potassium permanganate? [online] Available at: <https://chemistry.stackexchange.
com/questions/38915/what-role-does-sulfuric-acid-play-in-the-titration-of-oxalic-acid-and-
potassium> [Accessed 12 June 2019].

Edwardsville High School, 2015. Redox Titration. [online] Available at: <http://www.ecusd7.

org/ehs/ehsstaff/gbannon/apchem/labs/redoxstandardization.htm> [Accessed 12 June 2019].

Lumen, n.d.. Redox Titrations. [online] Available at: <https://courses.lumenlearning.com/

introchem/chapter/redox-titrations/> [Accessed 12 June 2019].

Ramsden, E., 2000. A-level Chemistry. 4th ed. Cheltenham: Stanley Thornes.

Ricca Chemical Company, 2018. Potassium Permanganate. [online] Available at: <http://

www.riccachemical.com/technical-support/Tech-Tips/potassium_permanganate> [Accessed
12 June 2019].

Ullah, S., 2017. Which one is the primary standard substance and why? [online] Available at:
<https://www.quora.com/Which-one-is-the-primary-standard-substance-and-why- KMnO4-
or-K2Cr2O7> [Accessed 12 June 2019].