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CHEM101E (Spring 2015)

Experiment #A: Determination of Iron by Reaction with


Permanganate

Experiment #A: Determination of Iron by Reaction with Permanganate


Health & safety
You must follow all health and safety procedures for this experiment.
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.
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 0.3 g of your unknown into
clean 250 mL Erlenmeyer flasks.
Clean your burette thoroughly. Draw about 100 mL of the standard KMnO4 solution (take a note
of the concentration of solution written on the bottle) 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 more samples.
Determine the percentage by weight of iron in the solid sample and deviation.
When the experiments are finished, you must ensure you have cleaned all your apparatus and
tidied your workspace. Noncompliance will result in penalties.

CHEM101E (Spring 2015)

Experiment #A: 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 reaction; 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.