Shahjalal University of Science & Technology, Sylhet.

Department of Chemical Engineering and Polymer Science.

LAB REPORT

Group No: 01
Course Name: Equilibrium in Solution: Engg. Aspects Sessional
Experiment No: 03
Experiment Name: Standardization of KMnO4 with standard H2C2O4 solution.
Submitted to:

Dr. Md. Tamez Uddin

Professor,
Dept. of CEP, SUST

Submitted by:

Name Registration No.

Md Afif Abrar 2017332043

Date of Experiment: 18 – 09 – 2018

Date of Submission: 20 – 09 – 2018
❖ Experiment No : 03

❖ Experiment Name : Standardization of KMnO4 with standard C2H2O4 solution.

❖ Experiment Objective : To determine the concentration of potassium permanganate (KMnO4) using

oxalic acid (C2H2O4) primary standard by volumetric analysis (acid-base titration).

❖ Principle of method : Potassium Permanganate, KMnO4, is a strong oxidizing agent. Permanganate, MnO4- , is
an intense dark purple color. Reduction of purple permanganate ion to the colorless Mn2+ ion, the solution will turn
from dark purple to a faint pink color at the equivalence point. No additional indicator is needed for this titration. The
reduction of permanganate requires strong acidic conditions. In this experiment, permanganate will be reduced by
oxalate, C2O42- in acidic conditions. Oxalate reacts very slowly at room temperature so the solutions are titrated hot
to make the procedure practical. The redox reaction is shown below.

MnO4- + 8H+ + 5e- → Mn2+ + 4H2O] x 2

C2O42- → 2CO2 + 2e-] x 5

Overall reaction: 2MnO4- + 16H+ + 5C2O42- → 2Mn2+ + 8H2O + 10CO2

Redox Titration: The titration based on oxidation and reduction reaction between the titrant and analyte is called Redox
titration. Oxidation is the process of the addition of oxygen or removal of hydrogen/electron and reduction involves the
process of addition of hydrogen/electrion or removal of oxygen. Oxidizing agents are substances that gain one or more
electrons and are reduced. Reducing agents are substances that lose one or more electrons and are oxidized. That is,
oxidizing agents are electron acceptors, and reducing agents are electron donors. In redox systems, the titration method
can be adopted to determine the strength of a reductant/oxidant using a redox sensitive indicator. Redox titrations
involving potassium permanganate are called permanganometric titrations. In these reactions, MnO42- ions act as the
self-indicator. Some of the significant terms in titration are defined below.

Standard Solution : In analytical chemistry, a standard solution is a solution containing an accurately

known concentration of an element or a substance. Standard solutions are used
to determine the concentrations of other solutions in titration.

pH Indicator : A pH indicator is a halochromic chemical compound added in small amounts to a

solution so the pH (acidity or basicity) of the solution can be determined visually.

Equivalence Point : The equivalence point, or stoichiometric point, of a chemical reaction is the point at
which chemically equivalent quantities of bases and acids have been mixed. In
titration, the equivalent point is the point at which the pH indicator changes color.

Titrant : The titrant is the solution involved or used in a titration to determine the
concentration of an unknown solution. The titrant is usually the solution of known
concentration.
 Titrate : The titrate is the solution whose concentration is determined using the titrant. The
titrate is usually the solution of unknown concentration.

Burette : A burette is a laboratory equipment used in analytical chemistry for the dispensing of
variable amount of a chemical solution and measuring that amount at the same time. It
is a long, graduated glass tube, with a stopcock at its lower end and a tapered capillary
tube at the stopcock’s outlet.

❖ Uses of pH Indicators : There will be no use of any external pH indicators in this titration because the
Potassium Permanganate used is a pH indicator itself.

❖ Materials :

• Apparatus : 1. Burette : Where the titrate (unknown solution) is kept.

2. Pipette : A tool used to transport a measured volume of liquid.
3. Conical flask : Where the titrant (known solution) is kept.
4. Clamp with stand : It is used to stabilize the burette.
5. Funnel : It helps in pouring the titrate onto the burette.
6. Volumetric flask : It is used to contain a precise volume of solution.

• Chemical Compounds : 1. KMnO4 solution

2. Standard H2C2O4 solution
3. Distilled water

❖ Procedure :

1. First, we prepare 0.1 M standard solution of Oxalic acid by dissolving 3.15 g Oxalic acid in 250 mL
volumetric flask.

2. We then rinse and fill a clean burette with Potassium Permanganate solution and remove the air
bubble, if any, from the nozzle of the burette by releasing some solution through it. The burette
used in the Permanganate titration must have a glass stopcock as rubber is tacked by permanganate
ions.

3. We take 10 mL of 0.1 M Oxalic acid solution in a conical flask and add half of a test-tube full (5 mL)
of 1.0 M H2SO4 to it to prevent the formation of any precipitate of manganese dioxide during the
course of the titration.

4. We heat the oxalic acid solution up to 50° - 60°C before titrating it with potassium permanganate
solution taken in the burette. To increase the visibility of the color change, we place the conical flask
containing the solution to be titrated over a white glazed tile kept below the nozzle of the vertically
fitted burette.
 5. We note the initial reading of the volume of permanganate solution in the burette and add it in
small volumes to the hot oxalic acid solution while swirling the contents of the flask gently. The
violet color of permanganate solution is discharged on reaction with oxalic acid. The endpoint is
indicated by the appearance of permanent light pink color due to a slight excess of permanganate
solution.

6. We repeat the titration till three concordant readings are obtained. Since the solution of KMnO4 is of
dark color, the upper meniscus should be considered for nothing the burette readings.

7. We calculate the strength of Potassium Permanganate solution in mols/litre.

❖ Experiment Data Table :

Volume of titrate
Attempt No. Volume of Volume used Average
analyte/titrant (vf – vi) volume
Initial (vi) Final (vf)

1 10 mL 50.0 mL 46.0 mL 4.0 mL

2 10 mL 45.0 mL 41.1 mL 3.9 mL 3.87 mL

3 10 mL 40.0 mL 36.3 mL 3.7 mL

Chemical Reaction :

5 H2C2O4 + 2 KMnO4 + 3 H2SO4 = 2 MnSO4 + K2SO4 + 10 CO2 + 8 H2O

Calculation :

𝑀𝑃𝑜𝑡𝑎𝑠𝑠𝑖𝑢𝑚 𝑃𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒 × 𝑉 𝑃𝑜𝑡𝑎𝑠𝑠𝑖𝑢𝑚 𝑃𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒 2

𝑀𝑂𝑥𝑎𝑙𝑖𝑐 𝐴𝑐𝑖𝑑 × 𝑉 𝑂𝑥𝑎𝑙𝑖𝑐 𝐴𝑐𝑖𝑑
= 5

2 × 𝑀𝑂𝑥𝑎𝑙𝑖𝑐 𝐴𝑐𝑖𝑑 × 𝑉𝑂𝑥𝑎𝑙𝑖𝑐 𝐴𝑐𝑖𝑑

𝑀𝑃𝑜𝑡𝑎𝑠𝑠𝑖𝑢𝑚 𝑃𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒 =
5 × 𝑉𝑃𝑜𝑡𝑎𝑠𝑠𝑖𝑢𝑚 𝑃𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒

2 × 0.1 × 3.87
𝑀𝑃𝑜𝑡𝑎𝑠𝑠𝑖𝑢𝑚 𝑃𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒 = = 0.015 𝑀
5 × 10
 Therefore, the strength (concentration) of Potassium Permanganate is 0.015 M.

❖ Cautions :

1. We make sure that we wear all proper lab equipment when handling chemicals
2. We should be careful that the clamp in the stand is not too tight to damage the burette.
3. We should not completely open the valve of the clamp in the stand while titrating.
4. We should dispose the acids and bases in a safely in the sink.