Experiment 3 [Oxidation-Reduction

Titration]
Mila Lee
Group 7
24 July 2014

Synopsis
The experiment conducted is about finding the unknown
concentration of potassium permanganate, an oxidizing agent
through titration and be familiar with the process of it. A known
amount of sodium oxalate was measured and reacted with diluted
sulfuric acid and water and then heated to boiling point to speed
up reaction. It was then titrated against potassium permanganate
until the end point of the reaction where the solution turns light
pink. An extra drop of potassium permanganate affects greatly on
the color of the solution. With calculations, the average calculated
concentration of KMnO4 is 0.04906M.
Introduction
This laboratory experiment focuses on oxidation-reduction
titration. Redox reaction is defined as both oxidation and
reduction occurring simultaneously during a reaction. Where
oxidation refers to the gain of oxygen, loss of hydrogen and
electrons and an increase in the state of oxidation, reduction
refers to the loss of oxygen, gain in hydrogen and electrons and a
decrease in the state of oxidation. Oxidation and reduction always
occur together hence, overall electron charge in an equation of
reaction will be zero.
In this laboratory experiment, we are supposed to familiarize
ourselves with the use of titrimetric method to determine
concentration of an oxidizing agent. The objective of this lab
lesson enabled me to learn about oxidation-reduction reaction
through the example we are supposed to work on. Potassium
permanganate, KMnO4 is titrated into heated solution of sodium
oxalate, Na2C2O4 and dilute sulfuric acid, H2SO4 where the molarity
for KMnO4 is unknown. With formulae and the experiment data, we
successfully derived an average molarity for KMnO 4.
Theory
Pure sodium oxalate, Na2C2O4 is a solid salt and a very good
primary standard. It can be used to standardize an oxidizing agent

like KMnO4 which can then be used to determine the percentage

purity of other unknown reducing agent. The reaction is carried
out in the presence of dilute sulfuric acid, which prevents the
formation of the brown, insoluble MnO2 and ensures that the
reduction of the permanganate proceeds according to the
following equation:
5C2O42- +2Mn042- + 16H+ 10CO2 + 2Mn2+ + 8H2O
The end point of the titration occurs when there is first excess of
permanganate ions in the solution being titrated. The solution will
change from colorless to pink and one drop of excess
permanganate is sufficient to cause this color change.
At room temperature, the rate of reaction is too slow to give a
sharp, accurate end point. Thus, the oxalate solution is heated to
60oc to70oc to speed up the reaction.

Procedure
1. 0.25 grams of sodium oxalate were weighed accurately on a weighing
boat using a gravimetric balance and transferred into a 250ml conical
flask.
2. Sodium oxalate was dissolved in 50 milliliters of deionized water
measured with a measuring beaker and 10 milliliters of dilute sulfuric
acid measured with a cylinder.
3. Solution prepared was heated to near boiling point.
4. The solution of aqueous Na2C2O4 was then titrated using potassium
permanganate from a burette.
5. Conical flask was swirled until a permanent light pink color was
observed.
6. Procedure (1)-(5) was repeated until three consistent result was
procured.

Results
Weight of
sodium
oxalate used
(g)
Number of
moles of
sodium
oxalate used
Initial Reading
of burette
(mL)
Final Reading
of burette
(mL)
Volume of
potassium
permanganate
used (mL)
Molarity of
potassium
permanganate

Titration 1
0.2505

Titration 2
0.2503

Titration 3
0.2500

0.00187
moles(3s.f)

0.00187
moles(3s.f)

0.00187
moles(3s.f)

15.6

15.1

15.0

15.6

15.1

15.0

0.04793M
(4s.f)

0.04948M
(4s.f)

0.04975M
(4s.f)

6.2: Using the equation, number of moles = Weight used/

molecular weight, calculate the number of moles used in
each titration and filled in the table below.
For titration 3,
Number of moles of Na2C204 = Mass used Molecular weight
= 0.2500 [2(23)+2(12)+4(16)]
= 0.2500 134
= 1/536

= 0.00186567
= 0.00187 moles (3sf)
6.3 Using the equation, number of moles = molarity x
volume in the solution used, calculate the molarity of
potassium permanganate for each titration and fill in
table.
15.0 ml = 0.015 liters
By stoichiometry,
5 moles of sodium oxalate produces 2 moles of potassium
permanganate.
Hence,
Molarity of KMnO4 = No of mol Volume of solution used
= (0.00186567 2/5) 0.015
= 10/201
= 0.049751
= 0.04975M (4s.f)
6.4 Calculate the average molarity of potassium
permanganate used.
Average molarity = (0.047933 + 0.049481 + 0.049751) / 3
= 0.049055
= 0.04906M (3s.f)
Discussion
In an experiment, results are not always accurate because of a
few factors.
1. When a few drops of potassium permanganate titrant
missed the conical flask,

In that case, the molarity of potassium permanganate will

decrease. When a few drops of potassium permanganate
misses, more will have to be added to ensure the reaction
comes to an end. Hence, volume used will increase. With this
formula,
Molarity = Number of moles of potassium permanganate/
Volume
Molarity and volume are inversely proportional hence when
volume increases, molarity will decrease. Resulting in
molarity being too small.
2. When weighing out the sodium oxalate, the actual
mass is 2.5000g instead of 0.2500g and the weight is
still recorded as 0.2500g.
In this case, when the mass of sodium oxalate increases,
number of moles will increase accordingly by the formula,
No of moles = Sample mass/ Molar mass of compound
Number of moles and sample mass are proportional hence
when the sample mass increases, the number of moles of
sodium oxalate increase as well.
When the number of moles of sodium oxalate increases,
molarity will increase as well.
Molarity = Number of moles of sodium oxalate x 0.4 /
Volume
When number of moles of sodium oxalate increases, molarity
of potassium permanganate will increase as well. Hence,
molarity will be too large.
3. Some of the weighed sodium oxalate is spilled on the
bench top and the weight of the sodium oxalate is
still recorded as the unspilled weight.

In this case, when the mass of sodium oxalate decreases,

number of moles will decrease accordingly by the formula,
No of moles = Sample mass/ Molar mass of compound
Number of moles and sample mass are proportional hence
when the sample mass decreases, the number of moles of
sodium oxalate decreases as well.
When the number of moles of sodium oxalate decreases,
molarity will decrease as well.
Molarity = Number of moles of sodium oxalate x 0.4 /
Volume
When number of moles of sodium oxalate decreases,
molarity of potassium permanganate will decrease as well.
Hence, molarity will be too small.
Conclusion
In summary, the objective of the experiment was completed
which was to familiarize ourselves with the use of titration
methods to find out the unknown molarity of oxidizing agent. The
molarity of potassium permanganate, rounded off to 4 significant
figures, of the oxidizing agent for the 3 titration completed was
0.04793M, 0.04948M and 0.04975M respectively. The average
molarity was hence calculated to be 0.4906M (to 4 significant
figures).
References
1) Singapore Polytechnic Foundation Program Application Science
( CP901Y/Z ) Laboratory Manual Page 15 and 16.