XII- CHEMISTRY

EXPERIMENT NO. 2

Volumetric Analysis:
Estimation of unknown KMnO4 using 0.1M Oxalic acid solution
Aim:
To Estimate the strength of the unknown KMnO4 using 0.1M of Oxalic acid
solution.
1. To find the mass of Oxalic acid to prepare 100 ml of 0.1M of Oxalic
acid solution.
2. To find the molarity of unknown KMnO4 solution using 0.1M of Oxalic
acid solution.
3. To estimate the strength of KMnO4 as grams in 1 liter of KMnO4
solution.

Theory:
Oxalic acid a primary standard is chemically (COOH)2·2H2O
(molar mass = 126g/mol)
Oxidising agent: unknown potassium permanganate solution
Reducing agent: standard Oxalic acid solution (COOH)2·2H2O
To prepare 0.1M solution of Oxalic acid, the weight of Oxalic acid required
can be calculated by using the formula:
1 M = 1000 ml = 126 g mol-1
0.1 M = 100 ml = x g
x g = (126 x 100 x 0.1)/ 1000
x = 1.26 g of Oxalic acid to be dissolved in 100cm3 of Distilled Water (D.W)
KMnO4 (molar mass = 158g/mol) is an oxidising agent and it oxidises
carbon (C) present in oxalic acid from +3 to +4 oxidation state.
The manganese (Mn) of KMnO4 is reduced from +7 to +2 oxidation state.
Since both oxidation and reduction happens simultaneously it is called a
redox reaction and the titration is called redox titration.
KMnO4 acts as a self-indicator and the colour at the end point changes from
colourless to pink.

Chemical Reaction:
The chemical reaction and the molecular chemical equation is given below.

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Reduction half reaction –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
Oxidation half reaction –
5(COOH)2 + 5[O] → 5H2O + 10CO2↑
Overall reaction –
2KMnO4 + 3H2SO4 + 5(COOH)2 → K2SO4 + 2MnSO4 + 8H2O + 10CO2↑
The ionic equation involved in the process is given below.
Reduction Half reaction:- [MnO4– + 8H+ + 5e– → Mn2+ + 4H2O] x 2
Oxidation Half reaction:- [C2O42- → 2CO2 + 2e–] x 5
Overall Ionic reaction:- 2MnO4– + 16H+ + 5C2O,2- → 2Mn2+ + 10CO2 +
8H2O

Materials Required:
Chemicals:
Oxalic acid, Potassium permanganate solution, Sulphuric acid
Apparatus:
Chemical balance, Beaker, Glass rod, Butter paper/ Watch glass, Dropper,
Burette, Burette stand, Pipette, Conical/Titration flask, Funnel, Measuring
flask, Weighing bottle, White tile,tripod stand,gauze and burner.

Procedure:
(a) Preparation of 0.1M standard solution of Oxalic acid:
1 M = 1000 ml = 156 g mol-1
0.1 M = 100 ml = x g
x g = (156 x 100 x 0.1)/ 1000
x = 1.26 g of Oxalic acid to be dissolved in 100cm3 of Distilled Water (D.W)
The molar mass of Oxalic acid = 126 g/mol

1. For preparing 100ml of 0.1 Oxalic acid solution, Oxalic acid

required= 1.26 g.Weigh accurately 1.26g of Oxalic acid in a
chemical balance.
2. Transfer the Oxalic acid into the dry beaker. Add about 10cm3 of
distilled water and stir the solution. Transfer it into Standard
measuring flask. Make the solution up to the marked point with

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 distilled water and make sure the Oxalic acid is fully dissolved.
3. Now wash the funnel with distilled water without removing the
funnel from the flask.
4. Make the solution up to the marked point with distilled water and
make sure the Oxalic acid is fully dissolved.
5. This solution is 0.1M standard solution of Oxalic acid.
(b) Titration of potassium permanganate solution against standard Oxalic
acid solution:
1. Wash and rinse the burette and pipette with distilled water and then rinse
with the corresponding solution to be filled in them.
2. Rinse the burette with the potassium permanganate solution and fill the
burette with potassium permanganate solution.
3. Fix the burette in the burette stand and place the white tile below the
burette in order to find the endpoint correctly.
4. Rinse the pipette and conical flask with standard Oxalic acid solution.
5. Pipette out 10 ml of 0.1M standard Oxalic acid solution into the conical
flask.
6. Add a test tube full of sulphuric acid in order to prevent oxidation of
manganese to form manganese dioxide.
7. Heat the mixture upto 60oC before titrating with potassium permanganate
in order to increase the rate of reaction.
8. Note down the initial reading in the burette before starting the titration.
9. Now start the titration, titrate against potassium permanganate solution and
simultaneously swirl the solution in the flask gently.
10. Initially, the purple colour of KMnO4is discharged with Oxalic acid.
11. The appearance of a permanent pink colour reveals the endpoint.
12. Repeat the titration until concordant values are obtained.
13. Note down the upper meniscus on the burette readings.
14. Record the reading in the observation table given below in order to
calculate the molarity of KMnO4 given.

Observations:
1. In burette – KMnO4 solution
2. In Conical flask – 10ml of Oxalic acid + Sulphuric acid +Heat the mixture
upto 60oC
3. Indicator – Self indicator (KMnO4)
4. End Point – Colourless to permanent pale pink colour.
5. Observation Table:

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Sr. SrNo. Volume of Burette Readings in cm3 Final CBR
Oxalic acid (cm3) reading: concordant reading
Initial (V1) Final(V2) V2-V
In1 cm3

1 10

2 10

3 10

6. Pilot Reading: ____________ cm3 to _____________ cm3

Calculation:
M1= Molarity of KMnO4
M2= Molarity of Oxalic acid = 0.1 M
V1= CBR/Concordant reading (from burette)
V2== 10 ml (from pipette)

Using Molarity Equation:

a M1 V1 = b M2 V2 (a, b are n-factor for KMnO4 and Oxalic acid)
KMnO4 = Oxalic acid
5 x M1 x CBR = 2 x 0.1 x 10
M1= (2 x 0.1 x 10)/ (5 x CBR)
M1= _________ M
Strength of KMnO4 = Molecular weight of KMnO4 x Molarity of KMnO4
= 158 x M1
= ___ g L -1

Result and Conclusion:

1. Molarity of given KMnO4 solution is _________ moles/litre
2. The strength of given potassium permanganate solution is _______ g/L

Precautions:
1. Potassium permanganate is dark, so always read the upper meniscus.
2. Rinse the pipette and burette before use.
3. Use dilute sulphuric acid for acidifying the potassium permanganate.

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 4. Clean all the apparatus with distilled water before starting the experiment
and then rinse with the solution to be taken in them.
5. Take accurate readings once it reaches the endpoint and doesn’t go with
average readings.
6. The strength of the unknown solution should be taken up to two decimal
places

Index to be written as follows:

2. Volumetric Analysis: Estimation of concentration and strength of
unknown KMnO4 using 0.1M Oxalic acid solution
Date of Experiment: Monday batch- 10-06-24
Thursday batch- 13-06-24
Date of Submission: Monday batch- 24-06-24
Thursday batch- 27-06-24