ECHE 222 (Spring 2016)

Experiment #3: Determination of Iron by Reaction with

Permanganate

Experiment #3: Determination of Iron by Reaction with Permanganate

Background
Potassium permanganate, KMnO4, is widely used as an oxidizing agent in volumetric analysis. In acid
solution, MnO4 ion undergoes reduction to Mn2+ as described by the following equation:
MnO4(aq) + 8H+(aq) + 5e Mn2+(aq) + 4H2O
Since the MnO4 ion is violet and the Mn2+ ion is nearly colorless, the end point in titrations using KMnO4
as the titrant can be taken as the first permanent pink color that appears in the solution.
In this experiment, KMnO4 will be employed in order to determine the percentage of iron in an
unknown sample containing iron(II) ammonium sulfate, Fe(NH4)2(SO4)2 6H2O. The titration, which
involves oxidation of Fe2+ Fe3+ by MnO4 is carried out in sulfuric acid solution to prevent the air
oxidation of Fe2+. The end point of the titration is sharpened markedly if phosphoric acid is present,
because the Fe3+ ion produced in the titration forms an essentially colorless complex with this acid.
By determining the number of moles of potassium permanganate used in the titration, the amount
of iron, and the stoichiometry of the reaction, you can work out the percentage by weight of iron in the
solid sample. You should calculate the mean percentage of iron for your values, along with the standard
deviation.
Procedure
Obtain a burette and an unknown iron(II) sample.
Weigh out accurately on the analytical balance three samples of about 1.0 g of your unknown into
clean 250 mL Erlenmeyer flasks.
Clean your burette thoroughly. Draw about 100 mL of the standard KMnO4 solution from the
dispenser which will be located in a fume hood. Rinse the burette with a few milliliters of the
KMnO4 solution three times. Drain and then fill the burette with the KMnO4 solution.
Prepare 150 mL of 1 M H2SO4 by pouring 25 mL of 6 M H2SO4 into 125 mL of H2O, while
stirring.
Add 50 mL of this 1 M H2SO4 solution to one of the iron samples. The sample should dissolve
completely.
Make sure that you record the volume of KMnO4 in the burette. Then, without delay, titrate the
iron solution with KMnO4. When a light-yellow color develops in the iron solution during the
titration, add 3 mL of 85% H3PO4 (be careful with this reagent).
Continue the titration until you obtain the first pink color that persists for 15 to 30 seconds.
Record the final volume of KMnO4 solution left in the burette. This will allow you to work out
what volume was required to react all of the iron in the sample.
Repeat the same as above with the two other samples.

ECHE 222 (Spring 2016)

Experiment #3: Determination of Iron by Reaction with

Permanganate

Post lab questions

1. Write a balanced equation for the reaction of iron (II) ammonium sulfate and potassium
permanganate; you do not need to include non reacting species. (2 marks)
2. Explain why there is a color change in the reaction and why does a color change indicate the end
point of the reaction? (2 marks)
3. Why is sulfuric acid used in this reaction? (1 mark)
4. Why is phosphoric acid used in this reaction? (1 mark)
5. What other methods can be used to monitor the progress of reaction (e.g. for automation
purposes)? (2 marks)
6. If you wanted to assess the chemical kinetics of this reaction, describe how to modify the
experiment and explain using titration in the analysis how to collect the necessary data. You must
indicate any advantages or disadvantages. (4 marks)
Report
You must submit an electronic copy of your report through Moodle. Do not submit a scanned copy of
a hand written report.
Deadline will be 2 weeks from the day of your experiment. Late submissions will be penalized.