Xavier Bourret Sicotte

Tuesday, December 18 2007

Chemistry Experiment
Permanganate Titration

Introduction

Redox describes all chemical reactions in which atoms have their oxidation number changed1.
These reactions often produce a sharp change in the physical properties of the chemicals
involved hence are suitable for titration experiments. Titration experiments are used to
determine the concentration of an unknown reactant and rely on volumetric measurements.
The exact point at which the titration is completed is called the equivalence point and can
easily be found in the presence of a sharp colour change.

Potassium Permanganate KMnO4 is a strong oxidising agent that dissolves in water forming a
deep purple solution. The deeply coloured Manganese +7 solution can undergo a 5-electron
reduction to the pink Manganese (II) in presence of acid.2 The abrupt change in colour when
manganese is reduced makes it a useful chemical for titration experiments.

In this experiment, the titrant Potassium Permanganate KMnO4 of known concentration is

added to an oxalate solution of unknown concentration. The equivalence point of the titration
is seen when the deep purple colour of the Permanganate suddenly changes to a faint pink.
The Redox reaction taking place is balanced as follows:

16 H+(aq) + 2 MnO4-(aq) + 5 C2O42- (aq) => 10 CO2(g) + 2 Mn2+ (aq) + 8 H2O (l)

In acidic environment, the Manganese 7+ is reduced to Manganese 2+ and the oxalic ion
C2O42- is oxidised to Carbon dioxide.

The aim of the experiment is to find the unknown concentration of Potassium Oxalate
solution.

1
Wikipedia, the free encyclopaedia: http://en.wikipedia.org/wiki/Redox
2
http://web.centre.edu/shiba/che132L/redox.pdf
Method

The experiment consists of a volumetric titration. The titrant is the deep purple Permanganate
solution and is reacted with the Potassium Oxalate analyte of unknown concentration.
The apparatus is shown in Fig.13

Fig.1

- Around 0.9 grams of Potassium Permanganate is accurately weighted and dissolved in

a 250 ml conical flask.
- Once the Permanganate is fully dissolved and that no residue can be seen, a glass
burette is filled and zeroed with the titrant.
- A second, smaller conical flask is filled with 25ml of the oxalate of unknown
concentration: the analyte.
- 7 to 8 ml of Sulphuric Acid is added to the analyte.
- The titration is carried out and the equivalence point occurs when the deeply coloured
solution turns pink for more than 10 seconds.
- The volume of titrant required for titration is recorded.
- The experiment is repeated several times.

3
http://www.bioquest.org
Raw Data

The raw data of the experiment consists of the results, the instrumental errors and the
comments made during the titration.

Mass of KMnO4 measured: 0.890 ± 0.001 g

Volume of oxalate of unknown concentration: 25 ml ± 3% `= 25 ± 0.75 ml

Volume of KMnO4 required for titration:

o 1st rough titration: 19.1 ± 0.1 ml
o 2nd titration: 18.5 ± 0.1 ml
o 3rd titration: 18.5 ± 0.1 ml
o 4th titration: 18.3 ± 0.1 ml

Comments:
- The mass was measured using an accurate electronic balance reading to the nearest
0.001g.
- The volume of the analyte was measured using a pipette designed with a 3% error.
- The burette used during the titration could read to the nearest 0.1 ml
- Some crystals were not fully dissolved in the permanganate solution during the
titration.

Processed Data

In order to find the concentration of the oxalic solution, it is necessary to calculate the
concentration of the permanganate titrant.

Molar mass of KMnO4 is: 3 9.0 9 8 3+ 5 4.9 3 8+ 4 ´ 1 6=1 5 8.0 3 6 3g/mol

0.890
Number of moles of KMnO4 used: = 0.00563162 moles
158 .04
Concentration of titrant: 4 ´ 0.0 0 5 6 3 1 6=20.0 2 2 5 2 6 4 7 0M2

0.001
Error on Molarity: δM = ´ 0.02252647 = 0.0003
0.890

Hence concentration of Potassium permanganate is 0.0225± 0.0003M

The balanced equation for the redox reaction is:

16 H+(aq) + 2 MnO4-(aq) + 5 C2O42- (aq) => 10 CO2(g) + 2 Mn2+ (aq) + 8 H2O (l)

The ratio of permanganate to oxalate is 2 : 5 or 1 : 2.5 so the concentration of the oxalate

solution can be found using the equation: (where “m” stands for the permanganate and “o”
for the oxalate).

Cm · Vm
Cm · Vm = 2.5[Co · Vo ] hence Co =
2.5Vo

Taking results from the 2nd titration as an example:

æ18.5 ö
0.0225 ´ ç ÷
æ18.5 ö é æ 25 öù è1000 ø
0.0225 ´ ç ÷= 2.5êCo · ç ÷ú hence Co =
è1000 ø ë è1000 øû æ 25 ö
2.5 · ç ÷
è1000 ø
Co = 0.00666 M

Error calculations for Co are shown bellow:

δCo dCm dVm dVo 0.0003 0.1 0.75

= + + = + +
Co Cm Vm Vo 0.0225 18.5 25
dCo
= 5%
Co

Hence the calculated concentration of the oxalate in the 2nd titration is: 0.0067±0.0003M
Carrying out similar calculations for all 4 titrations, we illustrate the results in Table 1

Table 1

Cm ± 0.0003M Vm ± 0.1ml Vo ± 0.75ml Co /M Error Co

0.0225 18.5 25 0.0067 ± 0.0003

0.0225 18.5 25 0.0067 ± 0.0003
0.0225 18.3 25 0.0066 ± 0.0003

It appears from Table 1 that the mean concentration of the oxalate solution is 0.0067 ±
0.0003 moles/litre

Evaluation

After calculating the concentration of the oxalate solution using the values of three distinct
titrations, it was found that all the results lie within the 5% calculated error range. This
accuracy comes from the neat, simple and effective design of the experiment. Indeed,
titrations are usually reliable experiments since the equipment used produces small errors.
Moreover, the permanganate redox titration is exceptionally reliable because of the sharp
colour change that greatly decreases the inaccuracy of the judgment of the equivalence point.
It should also be mentioned that no additional indicators interfered with the reaction.

Nevertheless, there are several limitations and sources of error that must be taken in account
before reflecting on the success of the experiment.

- The first and most important limitation is the slight scatter in the volume of
permanganate required for titration. The third titration is 0.2ml bellow the first two, a
difference twice the size of the error bar. This limitation may be caused by the slow
dissolution of the remaining permanganate crystals in the solution. Indeed, it was
noted during the raw data collection that some crystals were not fully dissolved when
the titration was carried out. As the phenomenon takes place, the concentration of the
permanganate solution increases hence less volume is required for titration.

- A possible solution is to wait longer, or use a magnetic stirrer so as to fully dissolve all
the crystals in the solution before carrying out the titration. This will allow the
 solution to remain at a constant concentration and will improve the reliability of the
experiment.

- Another limitation is the difficulty in judging on the position of the meniscus in the
burette. The bright colour of the solution decreased the visibility and the accuracy of
the titration readings.
- By taking more readings and repeating the titration a number of times, it is possible to
decrease the effect of this systematic error.

- It is important to mention the possible effects of uncontrolled factors in the

environment, the context, or even the chemistry taking place. Indeed, temperature,
humidity, pressure or luminosity may change the outcome of the experiment. In this
case, we are especially concerned with any factor that may have caused the decay of
the permanganate solution into more complex compounds that would react differently.
- By carrying out the whole experiment in a controlled environment, it is possible to
minimize the effects of such factors. Luminosity and temperature, for example, can
easily be kept constant by running the titration in an isolated environment.

Despite the inevitable effects of these limitations, the results of the experiment lie within the
calculated error bars. The concentration of the oxalate solution was found to be 0.0067 ±
0.0003 moles/litre hence a 4% error bar. The experiment is a success since it was well
controlled and performed. We can have good confidence in the result.